Monday Morning, April 27

Transcription

Keynote Presentation
9:00 a.m. K-1 Oxide Based Electronics - A Coming Technology
Invited Talk
E. Fortunato, P. Barquinha, L. Pereira, R. Martins
Departamento de Ciência dos Materiais, Universidade Nova de Lisboa and CEMOP/Uninova, Caparica, Portugal
Transparent electronics are now a reality and are adding new electronic functionalities onto surfaces. High-performance n- and
p-type Thin Film Transistors (TFTs), prepared by physical vapor deposition (PVD) techniques have already been developed. PVD
processes like rf magnetron sputtering can be performed near room temperature, which makes them compatible with the use of
temperature sensitive, low-cost flexible substrates (polymers, cellulose paper, among others). Besides that, tremendous advances
are coming through liquid solution-based technologies, which is very exciting for ink-jet printing, where the theoretical limitations
are becoming practical limitations. In this presentation, some of the most promising new technologies for n- and p-type thin film
transistors based on oxide semiconductors and their current and future applications will be reviewed. Some of the most promising new technologies for n- and p-type thin film transistors are in the form of nano-films or nanoparticles. Special emphasis will be
given to solution-processes. A summary of the major milestones already achieved with this emerging and very promising technology will be presented.
Symposium on Coating Technologies for the Interconnected Age
9:50 a.m. IA-1 Dropped Your Phone Down the Toilet? No Worries! - Improving the Reliability of Electronic Devices
Invited Talk
S. Coulson
P2I Ltd., Abingdon, United Kingdom
Historically, electronic devices have been protected from accidental splashes and spills using conformal coatings, gasket o-rings or
zip-lock bags. Despite some advantages, there are clear draw-backs from using these approaches. This has led to the development
of plasma enhanced vacuum based processing methods which have demonstrated themselves as viable technologies for mass
manufactured electronics. With 1 in 5 consumers dropping their mobile phone down the toilet and with our more 24/7 lifestyles,
it’s essential that our valuable data, photos, contacts and e-wallets are protected from rain, high humidity, sweat, spilled drinks
and salt water damage. To this end, there is also a desirable level of protection which goes beyond just splashes and spills, where
an electrical barrier to corrosion damage is formed. This means if a treated phone is submerged in water for long periods of time, it
too will be protected. In order to achieve this step change in performance, certain modifications to conventional plasma processing have been adopted. This presentation will cover state of the art liquid damage protection to electronic devices and discuss the
key requirements for achieving a fully dunkable solution for mass manufacturing.
10:30 a.m. IA-2 Doped Molybdenum Oxides for Low-Reflectance Thin Films in Touch Sensor Applications
H. Köstenbauer, D. Lorenz, J. Winkler
PLANSEE, Reutte, Austria
Touch functionality has become an ubiquitous feature of today’s portable electronic devices such as mobile phones, tablet PCs
or smart watches. In most projected-capacitive touch sensor devices, the so-called “metal bridge design” is used, especially when
the sensor diagonal size gets larger. In this architecture the x- and y-ITO sensor lines have to be bridged at the respective crossings
using an opaque metal, typically consisting of a Molybdenum or Mo-alloy single layer or a multilayer film stack (e.g. Mo/Al/Mo).
This design exhibits a major drawback; Under high ambient light conditions with a black LCD screen underneath, the metal bridge
pattern becomes visible to the user as a pattern of dots, due to the high reflectance of the metallic film. In order to optimize the
visual performance of the touch sensor, a low-reflectance bridge metallization comprising MoTa-oxide or Mo-oxynitride layers
is proposed. Low-reflectance doped Mo-oxide films were deposited by reactive sputtering from Mo and MoTa-6 at.% targets.
The optical and electrical properties of the resulting thin films were characterized. In addition, the ability to pattern the films by
photolithography was evaluated by analyzing the wet etch rates in common etching solutions.
505/856-7188 Fax 505/856-6716 • E-mail [email protected] • Web Site www.svc.org
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11:10 a.m. IA-3 Improved Mechanical and Optical Functionality on Transparent Substrates by High Deposition Rate
PECVD Coatings
F. Schwarz, S. Kastl, A. Uhl, D. Hrunski, C. Schmidt, R. Bock, A. Rack
Manz AG, Karlstein, Germany
The interconnected age made smart phones, tablets and other wearable devices our daily companions. The touch screens of
these devices must be pleasing to the eye, comfortable to the touch and be capable of holding up to the real world environment. This can be achieved by highly transparent dielectric coatings on glass or other substrate materials. To achieve the desired
functionality, tuning material properties like refractive index, hardness and intrinsic stress is mandatory. Although this is technically accomplished by sputtering, deposition of several micron thick films for mechanical functions causes very high cost. In this
work we investigated the possibilities of using plasma enhanced chemical vapour deposition (PECVD) with high deposition rates
and on industrial relevant scales as an alternative. The PECVD technology we used is based on inductively coupled plasma (ICP) at
high power densities and additional RF biasing. Several coating materials in the Al-Si-C-O-N compositional system (e.g. SiNx, Al2O3,
SiCON) have been investigated. By varying gas composition, plasma power and bias we could achieve very uniform coatings with
high optical quality and hardness. We will show the possibilities of tuning refractive index and intrinsic stress and of depositing
functional stacks of different materials and/or material properties.
11:30 a.m. IA-4 Roll-to-Roll Vacuum Coating and Device Fabrication Using Flexible Glass Web
Invited Talk
S. Garner
Corning Incorporated, Corning, NY
As displays and electronics evolve to become lighter, thinner, and more flexible, the substrate choice continues to be critical
to their overall optimization. The substrate directly affects improvements in the designs, materials, fabrication processes, and
performance of advanced electronics. With their inherent benefits such as surface quality, optical transmission, hermeticity, and
thermal and dimensional stability, glass substrates enable high-quality and long-life devices. As substrate thicknesses are reduced
below 200um, ultra-slim flexible glass continues to provide these inherent benefits to high-performance flexible electronics. In
addition, the reduction in glass thickness also allows for new device designs and high-throughput, continuous manufacturing
enabled by roll-to-roll (R2R) processes. This invited paper provides an overview of ultra-slim flexible glass and how it enables
high-performance devices using roll-to-roll (R2R) processes. Included are comparisons of flexible glass attributes with those of
alternative flexible substrates as well as a discussion on glass mechanical reliability. Demonstrations of R2R flexible glass processes
such as conveyance, vacuum deposition, slot die coating, photolithography, laser patterning, printing, and lamination will be
described. This discussion will include specific characterization of R2R vacuum deposited films on flexible glass web. These basic
R2R capabilities enable continuous manufacturing methods for high-quality devices on flexible glass substrates. Examples will be
provided of how several R2R process steps have been integrated to demonstrate fabrication of functional electronic devices on
flexible glass completely in a R2R process.
Emerging Technologies
9:50 a.m. E-1 Parylene Coatings for Organic Field Effect Transistors
J. Ulański1, I. Tszydel1, T. Marszałek1, A. Nosal2, M. Gazicki-Lipman2
1
Molecular Physics, Technical University of Lodz, Lodz, Poland
2
Institute for Materials Science and Engineering, Technical University of Lodz, Lodz, Poland
Along with the technology of microscopic electromechanical systems and that of brain-machine interface, organic electronics
constitutes the principal field of high-tech applications of parylene coatings. Within this category, a fabrication of organic field
effect transistors (OFET) makes the most abundant use of these materials, with parylene C being their principal type. The main
advantage of parylene coatings in the OFET technology is their high purity. Depending on a transistor architecture, films of
parylene C play either the role of a gate dielectric, a protective insulator coating, or a device support material. The work presents
a number of applications of parylene C in different OFET devices, developed by the authors. A combination of parylene coatings
of different configurations with zone casted films of organic semiconductors, both n-type and p-type, makes a principal design
of these devices. In this group, the best performance parameters and namely µFE = 0.18 cm2/Vs , Ion/off = 104 and turn-on voltage
< 5V were obtained for a n-type OFET based on a naphthalene bisimide derivative. Another design concerns transistors based
on semiconductor single crystals. In this case, dithiophene-tetrathiafulvalene was used as a semiconductor, with the effect of its
crystalline form on the transistor performance being investigated.
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Society of Vacuum Coaters • 2015 Final Program Abstracts
10:10 a.m. IA-8 ALD Coatings for Enhanced Durability of Electronic Devices
Invited Talk
S. Graham
Georgia Institute of Technology, Atlanta, GA
Thin film coatings can play an important role in the operation of electronic devices including roles such as gate dielectrics, electrodes for organic electronics, and moisture barriers for packaging. Due to the low defect density in this films when deposited by
atomic layer deposition, the opportunity exists to integrate such films into these applications using layers which are less than 50
nm while maintaining excellent or improving device performance. In this presentation, we will discuss the use of robust ALD coatings in flexible solar cells and organic LEDs to create stable low work function transparent electrical contacts. Data has shown the
ability to use coatings as thin as 1 nm to create true rectifying contacts for selective electron injection or collection into electronics. Moreover, these coatings are stable when exposed to harsh humid conditions, allowing for greater environmental durability.
As barrier films, similar coatings allow for the moisture hardening of OPV, OLEDs, and inorganic semiconductors which will also be
presented. Finally, challenges and methods of integration into each platform including sensitivity of the films to particles during
manufacturing will be presented. Models of moisture transport which corroborate the barrier layer performance will be presented.
11:10 a.m. E-2 Perspectives of Development of TCO and TOS Thin Films Based on TiO2 Composites
J. Domaradzki
Wroclaw University of Technology, Wroclaw, Poland
The present work consists of a short review of TiO2-based transparent oxide semiconducting thin films and their possible application in transparent electronics (TE). Research works conducted in the past few years have shown that TiO2 is attracting more
and more attention in TE. At room temperature TiO2 is an insulator with a moderately wide band gap (over 3 eV), high refractive
index (over 2.3) and low intrinsic light absorption. High transparency level of TiO2 makes it as a suitable material for the use as
a coating for many optical purposes, however, its application in TE requires modification of its electrical properties. The present
paper contains a short discussion on the advantages and difficulties of the application of TiO2 in transparent electronics. In the
paper, selected fundamental research of multicomponent thin films based of TiO2 with increased electrical conductivity has been
presented. The thin films were deposited using multitarget magnetron sputtering setup that was created by the authors according
to their own concept.
11:30 a.m. E-3 Structural Electronics and Structural Super Capacitors in Early Warning Systems in Mechanical Heart
Valves: New Concept with Emerging Technologies
A. Subrahmanyam
Department of Physics, IIT Madras, Chennai, India
The concept of early warning (eWAR) systems in bio-medical implants and transplants is new and emerging. Present work
addresses eWAR in Mechanical Heart valves. The global replacement of prosthetic heart valves stands around 280,000 annually; approximately half are mechanical valves. The complications of the mechanical heart valves include primary valve failure,
prosthetic valve endocarditis (PVE), prosthetic valve thrombosis (PVT), thromboembolism, and mechanical hemolytic anemia.
Many of these patients require long-term anticoagulation, and anticoagulant-related hemorrhage may occur. Efforts have been
initiated to address PVT through coatings. A constantly-monitoring early warning system, if embedded into the mechanical valve,
can improve the chances of remedial therapy. Such concepts have been proposed with sensors embedded into the heart valves
with a wireless link; however, the main impediments are (i) positioning of the sensor electronics and (ii) the long lasting and
energy efficient power source to the sensor electronics. The possible solutions seem to be with structural electronics and super
capacitors - the emerging technologies. The constant motion of the mechanical heart valve (driven by the biological energy) can
be converted into electrical energy; this electrical energy can charge a structural super capacitor. Structural super capacitors have
enhanced energy density per gram weight.
11:50 a.m. E-4 Laser Induced Transfer of PVD Coatings from a PET Carrier onto Product Surfaces for Decorative and
Functional Purposes
R. Domnick
ARA-Coatings GmbH & Co. KG, Erlangen, Germany
PVD-processes have been well established for decades – for many applications and in difficult business areas. Although PVD coatings have often big advantages with regard to their optical and functional features in comparison to other coatings, the production costs are relatively high. One method to reduce the production costs without losing the quality of PVD coatings is presented
in this talk. By using roll-to-roll coaters, a standard polymer (e.g. PET) is applied with a metal film, alloy or a layer stack by sputter505/856-7188 Fax 505/856-6716 • E-mail [email protected] • Web Site www.svc.org
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ing or evaporation. Then this coated polymer carrier is placed directly onto the product surface and with a laser beam the coating
is transferred from the carrier onto the product surface. With this method a large bandwidth of different colors and functionalities
can be applied on materials like glass, metal, ceramics, plastics or even textiles. Standard laser hardware and software can be
used to transfer decorative and robust logos, pictures, brand names or other motives on products for marking, identification or
authentication purposes. This new technology for laser induced application of PVD coatings on product surfaces is explained and
examples are shown in this paper. Also the results of the first tests in large area coating transfers are presented.
Plasma Processing
9:50 a.m. P-1 A New Frontier of Plasma Patterning: Atomic Layer Etch
Invited Talk
Y. Zhang
Applied Materials, Sunnyvale, CA
The rapid expansions of plasma etching in nanopatterning are due to the following two reasons. One is to pattern features with
CD’s and pitches much smaller than the limits of 193i lithography technology by using a variety of multiple patterning schemes,
such as Multiple Litho + Etch (LELE), or Self-Aligned Multiple Patterning, such as, Self-Aligned Double Patterning (SADP), etc.
Another is to fabricate nano-structures with CDU controllability in sub-0.2 nm regime to enable the continuous performance
enhancement of devices by introducing a variety of new materials, and changing from 2D planar devices to 3D structures, e.g., FinFETs. Continuous improvements of current plasma etch technologies seem to be able to carry out the tasks of multiple patterning
for the industry to extend to 10nm and 7nm. But can process fine tuning based on current plasma etch tool technologies accomplish the precision requirement of fabricating deep nanometer device structures, e.g., true 3D nanowires All-Around Gate (AAG)
with III-V materials? Conceptually, Atomic Layer Etching (ALE) should be able to help. But the key question is how to realize true
ALE. Do we need any new type of plasma sources, such as “low electron temperature” type of plasma sources, to meet challenges
of ALE? In this talk, some of the new developments, key challenges, and perspective solutions on processes, process integrations,
and plasma etching systems for ALE will be reviewed and discussed.
10:30 a.m. P-2 Application-Oriented Numerical Modeling of Plasma Processes for Material and Biological Applications
A. Obrusnik1,2, P. Synek1, Z. Bonaventura2, J.Vorac2, L. Zajickova2
1
Department of Physical Electronics at the Faculty of Science, Masaryk University, Brno, Czech Republic
2
Plasma Technologies at CEITEC, Masaryk University, Brno, Czech Republic
This contribution presents three numerical models of laboratory complex plasma discharges used for material processing
and bioapplications. All the models presented are strongly application-oriented in that they do not try to be all-encompassing but rather tailored and optimized for a particular application. The first of the models is a gas dynamics/electromagnetic field model of an atmospheric microwave plasma torch operating in an inhomogeneous argon/hydrogen mixture.
The aim of this model is to tackle the complex gas dynamics and heat transfer that strongly influence the shape of the plasma. The second model is a gas dynamics model of a high-frequency plasma jet operating in a rare gas and discharged into
ambient atmosphere. This model has been utilized for quantifying the amount of admixed air at various distances from
the plasma nozzle. The last model is a full plasma model of low-pressure microwave plasma ignited in hydrogen which can
be used for large-scale synthesis of solar cells, nanocrystalline diamond or even graphene. The hydrogen plasma model is
unique in terms of geometry because it combines full 3D geometry for the electromagnetic field with 2D geometry for the
plasma transport equations.
11:10 a.m. P-3 Transparent High Barrier Coating for Electronic Encapsulation
N. Kaabeche1, P. Kelly1, L. Harland2
1
Manchester Metropolitan University, Manchester, United Kingdom
2
BOBST Manchester Ltd., Heywood, United Kingdom
Barrier coatings are widely used to enhance the already existing barrier of plastic substrates against water vapour and
oxygen permeation. SiO 2-based barrier coatings have been applied to polyethylene terephthalate substrates by using
the plasma enhanced chemical vapour deposition (PECVD) technique. Hexamethyldisiloxane was used as the monomer
precursor and oxygen as the reactive gas. This work was carried out in a roll-to-roll coater. Fourier-transform infrared
spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were used to characterize the chemical composition of the coatings. Scanning electron microscopy and atomic force microscopy were used to image the surface
morphology. The main aim was to determine the relationship between the barrier level and the chemical and physical
properties of the coatings. This could be achieved by investigating the relationship between the operating parameters
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(e.g. power, oxygen or monomer flow rates, etc.) and the coating properties, including the permeation barrier. As high
mechanical properties are required for electronic encapsulation, adhesion and barrier retention as function of the
strain were also investigated.
11:30 a.m. P-4 Thin Film Vacuum Polymerization Applications
I. Fernandez1, A. Wennberg1, V. Bellido-Gonzalez2, B. Daniel2, J. Brindley2, H. Li2, D. Monaghan2, F. Papa3
1
Nano4Energy SL, Madrid, Spain
2
Gencoa Ltd, Liverpool, United Kingdom
3
Gencoa Ltd., Davis, CA
Thin film vacuum polymerisation methods have gained interest over the past 20 years. The fields of application extend from small
area biomedical applications to large area barrier applications such those on the food packaging. There are different ways of activating the in-vacuum polymerisation, one of them is in the presence of a plasma. The choice of monomer or monomer mix and
the properties of the plasma discharge will influence the kinetics of the polymerisation process. An additional way to influence
this process is by the gas mix, for monomers and innert (Ar, Ne, etc.) or reactive (O2, N2, etc.) species. The way these species are
injected is also important. The present paper will present data on a pulsed injection modes. A recently developed pulsed injection
valve will be used in order to inject the monomer. For the injection of non-reactive and reactive gases pulsed and non-pulsed MFC
modes will be used. Suitable feedback control methods will be implemented aiming at the control of the process within acceptable variability for its industrial implementation.
11:50 a.m. P-5 Thin Film Coatings for Particle Accelerators
S. Calatroni, P. Chiggiato, P. Costa Pinto, H. Neupert, A. Sublet, M. Taborelli, W. Vollenberg
CERN-European Organization for Nuclear Research, Meyrin, Switzerland
Particle accelerators are complex machines integrating several technological disciplines. Radio-Frequency (RF) is the core technology to accelerate charged particles, magnets are used to bend and focus, vacuum prevents collisions with the residual gas
molecules and, in some machines, cryogenics is necessary to profit of superconducting magnets and accelerating RF cavities as
well as pumping. In all these domains, surface processing plays a crucial role on the engineering of accelerators components. In
this work we present thin film coatings developed and produced at CERN for different applications: Nb for superconductive RF
structures, carbon for mitigation of electron multipacting and Non Evaporable Getters for vacuum and also mitigation of electron
multipacting. The route from small laboratory samples up to large scale production, (more than 1000 m2), will be addressed as well
as present and future developments.
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Monday Afternoon, April 27
The Donald M. Mattox Tutorial Presentation
12:50 p.m. TS-1 About the Possibility for a Holistic Toolbox for the Next Generation of Surface and Coating Optimization Taking the Example of TCOs in Touch Screens
Invited Talk
N. Schwarzer
Saxonian Institute of Surface Mechanics SIO, Ummanz/Rügen, Germany
The next level technological revolution, or “Internet of Things” as it is sometimes called, will not only require new management
and marketing strategies but also demand innovative and sophisticated concepts for products allowing the seamless interaction
of a human being with the internet. The author is convinced that without thin film technology, no satisfying interface solutions
are possible. In order to succeed however, much more knowledge base and holistic development strategies are necessary. In
many applications of thin films, a multitude of physical effects are influencing the lifetime and reliability of the coated parts. So,
often a mechanical contact of the coated body with a counterpart is formed, and there are thermal and intrinsic stresses, radiation, defects communicating with external loads, and electric, thermal and optical fields affecting the coated structure. A typical
example are hard coatings deposited on tools or parts in order to protect them against abrasion and wear. However, there are
many other examples where a multi-physical strength is unavoidably connected with the original purpose of the thin film application. Examples for the latter are thin films intended to provide good electrical contact in switchers and plugs, or optical thin
films on surfaces which are additionally exposed to mechanical contact, like touch screens. Proper characterization and optimization of such structures requires invertable mathematical tools of sufficient holistic character. Unfortunately, as such tools are still
not available, one often finds trial and error or half empirical sensitivity analysis methods in combination with FEM or BEM. By no
means does the author intend to criticize this. On the contrary, especially the incorporation of multi-physical FE- or BE-concepts
has lead to some severe reduction in costs due to substitution of pure trial and error by knowledge based design. Now however, it
is shown within tribological applications that there are ways for some completely analytical tools not only allowing a much better
invertibility compared to discrete models but also an extreme (up to 1000 and more) acceleration of forward evaluations even
for complex layered systems. Interestingly, the methods developed and the solutions found in order to construct these analytical tools are in many cases also applicable to completely different physical effects and applications. This is due to the principle
similarities of the governing equations describing all these effects. This talk will feature the use of these similarities and how they
can be applied for the development of optimized coating structures. Thereby, we will concentrate on the practical side of the new
tools application.
1:40 p.m. IA-5 The Emergence of Flexible Electronics: Opportunities for Vacuum Deposition Technologies
Invited Talk
H. Zervos
IDTechEx Inc., Cambridge, MA
IDTechEx has been following a variety of emerging technologies for over 15 years. In this time, different technologies, components
and devices have seen varying levels of success in commercialization. Examples include OLED displays and lighting, laminar batteries, photovoltaic cells, sensors, printed logic and memory. These technologies could be commercialized in flexible form factor,
which would allow for the proliferation of unbreakable, bendable, wearable devices, a major trend in current consumer electronics
development road maps. Examples of challenges in bringing these to market will be described in the paper including the successful development of manufacturing for displays and backplanes with increased accuracy and resolution as well as the development of high performance flexible barriers for encapsulation of devices sensitive to oxygen and moisture. The most important
developments worldwide will be discussed and the forecasting models developed within IDTechEx will be presented, describing
the market segments IDTechEx studies with a focus on the opportunities enabled through vacuum deposition techniques.
2:20 p.m. IA-7 µm Coatings for nm Precision
Invited Talk
M.L.H. ter Heerdt
ASML Netherlands B.V., Veldhoven, The Netherlands
In order to make the “Internet of Things” possible, the industry strives to keep up with Moore’s law. The newest generation of
lithography, Extreme Ultraviolet (EUV) lithography, requires a vacuum. This requirement opens up opportunities for DLC-type
coatings, because of the incompatibility of non-solid lubrication with vacuum. A recent study shows, however, that vacuum tribol8
ogy is not self-evident. Vacuum coating industry tends to invent new coatings regularly. This obviously has advantages, since new
coatings tend to show better performance. Unfortunately, there is a downside to this as well. In a recent development project on
fasteners, a DLC-type coating was selected and proven to perform well. Upon entering the actual production phase, this coating
no longer met its earlier specifications and no equal alternative could be found, forcing us to redo our investigation. From this
customer’s perspective, there is a tremendous need for standardization throughout the industry.
Coating for Energy Conversion and Related Processes
4:00 p.m. EC-1 Constitution, Microstructure and Electrochemical Behaviour of Magnetron Sputtered Li-Ni-Mn-Co-O Thin
Film Cathodes for Lithium-Ion Batteries
S. Ulrich, M. Strafela, J. Fischer, H. Leiste, M. Rinke, T. Bergfeldt, H.J. Seifert
Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Eggenstein-Leopoldshafen, Germany
Compared to the commercial LiCoO2 cathode material for lithium-ion batteries, Li(Ni1/3Mn1/3Co1/3)O2 has a good thermal stability,
high reversible capacity (290 mAhg-1), good rate capability and is environmentally friendlier. In this work Li-Ni-Mn-Co-O thin film
cathodes have been deposited onto Si and stainless steel substrates by non-reactive r.f. magnetron sputtering from a ceramic
Li1.25(Ni0.42Mn0.21Co0.37)O2 target at various argon working gas pressures from 0.2 to 20 Pa. Coating thickness is about 1 µm. Composition and microstructure were investigated comprehensively. It was found that the elemental composition varies with argon
working gas pressure which was determined by inductively coupled plasma optical emission spectroscopy (ICP-OES) in combination with carrier gas hot extraction (CGHE). The as-deposited films are nanocrystalline and show their highest grade of crystallinity
in the range between 0.2 Pa to 0.5 Pa and at 7 Pa argon working gas pressure. To increase the grade of crystallinity the films deposited at 0.5 and 7 Pa argon working gas pressure were annealed in a furnace. The samples were annealed at different pressures from
10 mPa to 80 kPa for one hour at 600°C in a argon/oxygen atmosphere (Ar:O2 = 80:20). The microstructure of the films varies with
annealing gas pressure and was characterized by X-ray diffraction (XRD) and by unpolarized micro-Raman spectroscopy at room
temperature. Electrochemical characterizations of as deposited and annealed films were carried out by cyclic voltammetry and
galvanostatic cycling in Li-Ni-Mn-Co-O half cells against metallic lithium. Correlations between process parameters, constitution,
microstructure and electrochemical behaviour are discussed in detail. These films are promising candidates for manufacturing of
all solid state thin film batteries.
4:20 p.m. EC-2 Thin Film Battery Manufacturing
D. Mount
Ulvac Technologies, Inc., Methuen, MA
Thin film batteries, are energy storage devices that are ideally suited for powering an ever growing array of portable consumer
devices. These batteries, which are rechargeable lithium-ion batteries, can be manufactured in various form factors, through a
variety of different manufacturing technologies, with varying process flows. The size of these batteries can range from extremely
small, such as those used in implanted medical devices, to about notebook-size, as those used as segments/elements in storage
batteries for PV and wind energy storage. The batteries can also be rigid, or highly flexible. Manufacturing techniques to deposit
the anodes and electrolyte layers of the battery can include both vacuum and non-vacuum-based process flows. Non-vacuum
techniques can include: spin-coating processes, or even printing. The vacuum techniques are usually deposition sequences that
are accomplished by PVD and thermal evaporation. There are two other process steps required to complete a finished thin film
battery, these are: rapid thermal annealing and a packaging/encapsulation step. These latter two process steps are best done
in vacuum systems. Thusly, virtually the entire fabrication sequence for thin film batteries can be accomplished using vacuum
technologies. This paper/talk will address principally the various types of vacuum-based technologies used to fabricate thin film
batteries.
4:40 p.m. EC-3 Designed Nanoparticle Synthesis by Hollow Cathode Sputtering for Surface Treatments
Invited Talk
U. Helmersson
Department of Physics, Linköping University, Sweden
Nanoparticles (NPs) of different designs find applications in numerous present and future applications. We are working with
synthesis of sputtering from hollow cathodes using high power pulses. These hollow cathodes can be designed as long slots for
large area deposition of NPs and the high power pulsing result in efficient ionization of the sputtered material give high materials
utilization and control. In the present project we are working on NPs designed for applications in light emitting polymer surfaces,
catalytic materials for synthesis of methanol from CO2 and selective hypersensitive gas-sensors made from NP decorated
graphene.
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5:20 p.m. EC-4 Fabrication of Rechargeable All-Solid-State Thin-Film Lithium Batteries on Flexible Polymer Substrates
M. Chen, Y. Yan, W.-M. Liu, C. Zhou, Z.-Q. Guo, X.-F. Zhang, Y.-L. Wang, L. Li, G.-L. Zhang
Beijing Institute of Aeronautical Materials, Aviation Industry Corporation of China, Beijing, China
As a new generation of ultrasafe Li-ion batteries, all-solid-state thin-film lithium batteries (TFLBs) replace the traditional liquid
organic electrolyte with solid ceramic electrolyte and the whole materials adopt thin-film form. In particular, flexible TFLBs are
promising key components to drive flexible electronic devices. Here we report low-temperature (LT) fabrication of flexible TFLBs
with Li/LiPON/LiFe(WO4)2 layers (4 µm) by successive r.f. magnetron sputtering and thermal evaporation. Without the conventional
700 post-annealing and crystallization process after deposition of amorphous LiFe(WO4)2 cathode films, the batteries can be
coated even on polymer substrates, such as PET films and Kapton PI films. The lithium ion conductivity of electrolyte LiPON
reaches (1.0±0.1) 10-6 S/cm. The electrochemical characterizations show that the batteries own high specific capacity of 65 µAh/
cm2 with a maximum discharge current of 50 µA, maintain a sustainable discharge capacity of 40 µAh/cm2 over 300 cycles. In the
bending evaluation test, charge/discharge behavior, AC impedance and open circuit voltage of flexible TFLBs also show consistent
and robust high-performance. This fabrication process offers a new method of building TFLBs at LT and paves the way to employ
light and flexible polymer substrates. In the end, possible TFLB mass-production equipment and methods are reviewed and
discussed.
Large Area
1:40 p.m. L-1 Direct Fabrication of Graphene on SiO2 via Thin Film Stress Engineering
Invited Talk
V. Veerasamy
Guardian Industries, Carelton, MI
Direct fabrication of graphene on SiO2 is achieved by selective delamination through microstructural and stress engineering of
a deposited Ni film during CVD growth. Graphene grown at the Ni/SiO2 interface is directly deposited on the SiO2 when the Ni is
removed by in situ or simple mechanical ex situ film delamination. In the reported system, delamination of the Ni film is promoted
by stresses introduced while annealing in a He environment. Highly stressed films annealed at atmospheric pressure undergo in
situ delamination and transfer in situ upon graphene formation at elevated temperature. Low pressure CVD conditions provide
less stressed films for which ex situ delamination of the Ni film is achieved by simple pulling with Scotch tape. Deposited graphene
films are of high quality (Raman ID/IG < 0.2) and coverage. The general principle that thin film stress and interlayer adhesion can
be engineered to achieve dry transfer of an atomic layer material at a metal/dielectric interface is potentially useful for a number
of processes and applications.
2:20 p.m. L-2 Effects of Ion Bombardment Pretreatment on Glass Coating Processes and Post Tempering
J.M. Marco1, R. Alonso2, A. Cueva2, V. Bellido-Gonzalez3, H. Li3, A. Azzopardi3
1
Ariño-Duglass, Zaragoza, Spain
2
Universidad de Zaragoza, Zaragoza, Spain
3
Gencoa Ltd, Liverpool, United Kingdom
Linear Ion Sources have been successfully introduced into glass coating applications, although there are still a large number of
glass coaters where there are other plasma treatments or even non-plasma cleaning solutions implemented. As the glass market
has been struggling economically as the demand for glass is below the current global capacity there is a need for bringing added
value features that attract a very much needed added market value to the final product. The added value sometimes demands a
much more complex coating structure with a very varied coating portfolio which is able to undergo the strenuous transformation
processes or life test which are common for applications where a differential added value on glass can be found. The present
paper will present results on the use of a linear ion source on the treatment for glass and subsequent tempering processes for
different demanding applications. Performance of the ion treated coated glass will be evaluated. This paper is a collaboration
between academia and two industrial partners aiming at a rapid R&D transfer and implementation of the technology.
2:40 p.m. L-3 Substrate Cooling and Tempering during High-Rate Vacuum Coating
J.-P. Heinss, P. Lang, P. Ruppelt, D. Weiske
Fraunhofer Institute for Electron Beam and Plasma Technology FEP, Dresden, Germany
Electron beam evaporation with deposition rates of hundreds of nanometers per second is predestined to fit mass throughput. In
a few cases, high-rate vacuum depositions demand effective cooling of the substrate for exploiting their potential, otherwise, substrate or layer temperature exhibits a limiting factor. The technical challenge is the realization of an effective heat transfer process
10
from the substrate to a cooling device under high vacuum conditions. To achieve this, new cooling equipment for metal sheet and
strip vacuum coating were developed. Mathematical simulations were adapted for the mechanical and the cooling fluid system
design of the apparatus. As a result, the practical realized heat transfer coefficient was extended outgoing from common cooling
drums with 50 up to 1000 W/m2K. The remarkably increased cooling efficiency opens up new technical possibilities: utilization of
very high deposition rates, deposition of thin metal strips and foils, an increase of layer thickness, definition of strip temperature
during high-rate deposition. We demonstrate the first results of using the cooling equipment during electron beam deposition of
metal strips with aluminum. We expect the application of the new substrate cooling equipment next for high-rate vacuum coating
of thin metal foils for energy storage devices, such as batteries.
3:00 p.m. L-4 Process Perfection for Large Area Multi-Layer Coatings
L. Schwab1, J. Ellrich2
1
dr. schwab Inspection Technology, Aichach, Germany
2
Grenzebach Maschinenbau GmbH, Asbach-Baeumenheim, Germany
Functional coatings become increasingly important in architectural, automotive and display glass applications. For complex
functions, typically large areas have to be coated in multi-layer stacks. Due to the shear number of steps and the interdependence
of all steps, even small local variations in a single step may have a significant impact on quality and function. Therefore, to ensure
a reasonable production yield, the process requires uniform, constant and stable conditions regarding all process parameters
and target conditions in large chambers and all stations. In order to recognize and localize variations early on in the process, it is
important to continuously monitor the process at all the important coating stations and on the full surface. It is shown that in situ
spectrometer measurement based on multiplexing technology allows full thickness profile measurement of individual layers in all
important steps. For evaluation of an individual layer at the appropriate station, the results of all preceding measurement stations
are included. By analyzing the trend and profile variation and correlation with process parameters the dominating systematic reasons for variation can be identified and corrected in a straightforward and cost-effective way. This helps to significantly improve
process capability, fully exploit target life cycles, minimize downtime and optimize maintenance intervals.
3:20 p.m. L-5 Large Area Coating - Achieving Superior Layer Uniformity
R. Rank, T. Niederhausen, G. Haasemann, J. Loehnert
VON ARDENNE GmbH, Dresden, Germany
Increasing demands for energy efficiency and ever more stringent customer requirements for architectural glass quality have
led to a steadily growing share of sophisticated thin film layer stacks for large-area glass coating. This in turn requires complete
control over the quality of the individual layers and, in particular, extremely good uniformity of layer thickness. This paper provides
insights on current R&D activities that are undertaken to meet these challenging technological requirements. A high level of
modeling and simulation has been utilized using commercial and proprietary tools in order to gain a deep understanding of the
underlying processes. The resulting knowledge is a great benefit for the design of coating equipment. The paper will highlight
some of the prerequisites for superior layer uniformity and their assessment by various simulation tools such as: Monte Carlo
Simulation of gas flows for uniform pressure distribution in the process chamber, CFD simulation of cooling water in rotatable
targets and its impact on surface temperature and target quality requirements, and magnetic field and plasma simulation for
planar magnetrons with high target yield.
4:00 p.m. L-6 40 Years of Industrial Magnetron Sputtering in Europe
Invited Talk
U. Seyfert1, J. Struempfel2, U. Heisig3, J. Hartung1
1
2
Senior Consultant PVD, Dresden, Germany
3
Research Institute Manfred von Ardenne (retired), Dresden, Germany
In October 1974, the first magnetron discharge supported by a pot magnet was carried out successfully in the former Manfred von
Ardenne Research Institute. The emerging development and progress in microelectronics required efficient coating technologies,
especially for the production of suitable resistors, transistors and rectifiers. Significant sputtering effects could be demonstrated
for the first time with this test, and brought up a new deposition technique. For essential thin-film technologies, most of the
evaporation techniques that had been used until then were limited with regards to the required film properties. As it was already
known at that time, sputtering technologies offered a broad range of coating materials, but suffered from low coating rates.
This bottleneck issue could be solved for the first time by combining sputtering technology with a closed loop magnetic field.
Similar developments were made in several countries in Europe and in the U.S. at that time. Inspired by this 40th anniversary, this
paper provides an overview of the history of magnetron sputtering and of the applications that made the development of this
11
technology necessary. Even if this development was also influenced by a major success in the US, the paper focuses chiefly on
developments in Europe. It also illustrates the progress of magnetron sputtering technology from small circular sputtering sources
to industrially proven tools for large-area coating solutions.
4:40 p.m. L-20 Optical and Mechanical Properties of Ti-, Si-, and Zr-Based Top Layers
J. Oberste-Berghaus, R. Van Nuffel, K. De Jaeger, A. Das, W. De Bosscher
Soleras Advanced Coatings, Deinze, Belgium
Over the last few decades, magnetron sputtering has proven to be a major coating technology for depositing high quality thin
films. The ease of scalability, while maintaining excellent control of all crucial layer parameters, made it appropriate for large area
substrates and high mass productivity. The introduction of the rotating cylindrical magnetron concept has further contributed
to the success of sputtering in large area architectural glass coating. Over the same period, low emissivity coating stacks have
evolved significantly from single silver to the higher performing and more complex triple silver low-E solutions. Functionalities
of individual layers have been extended as well, from pure optical requirements to improved stability against corrosion or after
heat treatment. In this paper, we will have a closer look at potentially improved performance of the top layer of a low-E stack.
Besides optical properties, we will investigate the potential of the top layer to act as a barrier against wear and determinate its
scratch resistance. Properties will be compared between typical alloy layers based on oxides and nitrides of titanium, silicon and
zirconium; deposited from metallic and suboxidic cylindrical target materials.
5:00 p.m. L-8 Tuning Of ITO Coating Properties in the Display Industry: Selected Topics
P. Lippens, C. Frei
Umicore Thin Film Products AG, Balzers, Liechtenstein
Although ITO thin films have been used for a couple of decades now in the display industry, many topics related to their manufacturing have remained untouched. One example of this is the influence of the magnetic stray field on thin film properties. This will
be illustrated in this paper for rotary cathode pairs in comparison with spatially isolated single rotary cathodes. Also, new requirements resulting from the usage of flexible substrates, present new challenges for very thin ITO coatings. Not only are ITO-92.5/7.5
(with only 7.5 wt% SnO2 in the ceramic) coatings better suitable than ITO-90/10 in case of touch sensors on PET, but the market
is looking to further improve the minimum achievable resistivity with this ITO-composition. The paper will show whether various
seed layers can bring an answer to this challenge.
5:20 p.m. L-9 Applying the “Upgraded Berg Model” to Predict Hysteresis Free Reactive Sputtering
E. Sarhammar, T. Nyberg, S. Berg
Solid State Electronics, Uppsala University, Uppsala, Sweden
Reactive sputtering is a popular process to deposit oxides, nitrides and several other compounds. Unfortunately this process
mostly exhibits a hysteresis effect. The hysteresis causes a delicate choice of either a high deposition rate but not a fully oxidised/
nitrided film or a fully formed compound film but at a significantly lower deposition rate. For high reactivity target material/
reactive gas systems, the hysteresis forces the process to flip quite abruptly between these two conditions. Process control may
therefore be quite critical. In this presentation we will use the newly published “upgraded Berg model” to illustrate how hysteresis
is generated. We have selected one simple graph that gives clear indications of how the process may be affected in such a way
as to decrease or even eliminate the hysteresis. Specific values of target size and composition, gas mixture as well as total pressure and pumping speed are processing parameters that may be selected in a way to eliminate hysteresis. We will show that this
behaviour is predicted by the “upgraded Berg model” and also show experimental evidence for such behaviour.
High Power Impulse Magnetron Sputtering (HIPIMS)
1:40 p.m. HP-2 Excellent Adhesion on Plastics using HIPIMS
R. Bandorf1, S. Waschke2, G. Grundmeier2, G. Bräuer1
1
Fraunhofer Institute for Surface Engineering and Thin Films IST, Braunschweig, Germany
2
Technische und Makromolekulare Chemie, Universität Paderborn, Paderborn, Germany
Metallization of plastic parts today is mainly realized using electroplating. Within the European Union the use of chromium VI
will be restricted by 2017 following the REACH directive. This, besides other aspects like environmental friendliness, is driving the
development of alternatives. Using PVD mainly evaporation is used. The drawback is sometimes weak adhesion. Furthermore
lacquers or interface coatings have to be applied before metallization. Using ionized sputtering like high power impulse magnetron sputtering (HIPIMS) opens new horizons for cost effective, environmental friendly plastic metallization with excellent adhesion. First, investigation using titanium as metal on different untreated plastics (PPSU, PEI, PEEK, PESU, PSU) showed significant
12
adhesion improvement using a simple tape test for evaluation when comparing mid-frequency sputtering and HIPIMS. Further
investigation on aluminum deposition on Plexiglas PMMA showed exciting results. Since PMMA is very sensitive to the UV radiation of technical plasmas, direct metallization of the surface by sputtering is not possible. Using ionized sputtering, it was possible
to enhance the adhesion to excellent level passing a combined cross cut and tape test without failure. The study of the interface
reveals some insight in the responsible mechanisms. Results, conclusions and perspectives of HIPIMS for plastic metallization will
be discussed.
2:00 p.m. HP-3 Mechanical Bending of the Indium Tin Oxide Films on Polyethylene Terephthalate Deposited by High Power
Impulse Magnetron Sputtering
Y.-H. Chen, Y.-C. Chen, J.-L. He
Department of Materials Science and Engineering, Feng Chia University, Taichung City, Taiwan
Indium tin oxides (ITO) have been studied extensively because their high electrical conductivity and optical transmittance making
them suitable for a variety of applications. ITO films have been deposited on the glass by high power impulse magnetron sputtering (HIPIMS) in the past demonstrating high electrical conductivity and optical transmittance. By considering the advantages of
low temperature deposition capability, strong film adhesion and dense film brought about by using HIPIMS, this study evaluates
the mechanical bending capability of the HIPIMS prepared ITO on polyethylene terephthalate (PET) so as to realize the feasibility
of using HIPIMS for developing next-generation DC sputtering is also compare. Microstructure, optical transmittance and electrical properties of the obtained ITO films were investigated. The mechanical bending test was performed in compliance with the
ASTM D1593 standard. Static and dynamic tests were performed separately.
2:20 p.m. HP-4 HIPIMS ITO Films from a Rotating Cylindrical Cathode
F.C. Carreri, A. Sabelfeld, H. Gerdes, R. Bandorf, G. Bräuer
High Power Impulse Magnetron Sputtering (HIPIMS) allows the deposition of thin films from plasmas with high metallic ion
content. HIPIMS has been successfully used to deposit indium tin oxide (ITO) films from planar ceramic targets, for several applications including ice-free windows and shaped glass tubes. These films present good conductivity as well as good wear resistance,
derived from a nanocrystalline structure. Nevertheless, industry demands more cost efficient processes. In view of that, the use
of rotatable cylindrical cathodes is a promising alternative due to their many advantages: better material utilization, longer
durability, reduced arcing and more. In this work, ITO films were produced from a rotating cylindrical cathode and the influence
of process parameters (average power, voltage, peak current and pressure) on resulting film properties was investigated. The
depositions were performed at room temperature and then followed by annealing. Electrical and optical properties were analyzed
and process stability and reproducibility were investigated.
2:40 p.m. HP-5 Adjustment of Plasma Properties in Magnetron Sputtering by Pulsed Powering in Mixed Unipolar and
Bipolar Mode
S. Barth, H. Bartzsch, D. Glöss, P. Frach, M. Gittner, R. Labitzke
A new method of pulsed powering the magnetron discharge using a pulsed switching of the anode has been developed. Practically, it is a combination of the conventional unipolar and bipolar pulsed powering, where the time slices of both pulse modes can
be freely adjusted at a time scale smaller than 1 millisecond, i.e., much shorter than necessary for the deposition of one monolayer.
This allows varying the average plasma parameters freely between the typical values of unipolar and bipolar pulse mode. During
deposition of piezoelectric AlN the film stress could be shifted between tensile and compressive by changing the pulse mode ratio
while maintaining piezoelectric properties. Deposition of SiO2 films with low scattering losses while maintaining low substrate
temperature could be accomplished by optimization of the pulse mode ratio. Hence this new parameter gives an additional
degree of freedom for optimization of film properties independent from sputtering power and deposition rate and in addition to
classical deposition parameters such as pressure or temperature.
3:00 p.m. HP-1 Thin Films Deposited by Reactive HIPIMS: From Plasma Diagnostics to Improvement of the Solar Cell’s
Efficiency
Invited Talk
P.-Y. Jouan
Institut des Matériaux Jean Rouxel, Nantes, France
Despite the large amount of research on thin films, there are only a few studies in HIPIMS (High Power Impulse Magnetron Sputtering) plasma diagnostics. In this presentation, we attempt to establish the link between the plasma, the properties of the depos505/856-7188 Fax 505/856-6716 • E-mail [email protected] • Web Site www.svc.org
13
ited thin films by reactive HIPIMS, and a solar cell’s efficiency. The first part deals with the plasma characterization results obtained
by time-resolved mass spectrometry and optical emission spectroscopy (OES) at different distances target substrate. Metallic and
gaseous species in atomic and ionic form were followed during the pulse for different discharge conditions (total pressure, pulse
width, power, and percentage of reactive gas). The second part is dedicated to the characterization of NiO and CIGS thin films.
We will present the influence of the total pressure, pulse width, power, and percentage of reactive gas on the morphology and
structure of thin films. The influence of a post-deposition thermal treatment will be also presented. The techniques used are X-ray
diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), photoelectron spectroscopy (XPS) and
ellipsometry. Finally, we present the characterization of solar cells synthesized with our films, and we try to conclude to the most
effectiveness of plasma parameters.
4:00 p.m. HP-6 Controlled Reactive High-Power Impulse Magnetron Sputtering of Dielectric Oxide Films
J. Rezek, J. Vlcek, A. Belosludtsev
Department of Physics and NTIS - European Centre of Excellence, University of West Bohemia, Plzen, Czech Republic
High-power impulse magnetron sputtering (HiPIMS) with a pulsed reactive gas (oxygen) flow control was used for high-rate reactive depositions of densified stoichiometric ZrO2, HfO2 and Ta2O5 films on a floating substrate. The depositions were performed using a strongly unbalanced magnetron with a planar Zr, Hf and Ta target of 100 mm diameter in argon-oxygen gas mixtures at the
total pressure close to 2 Pa. The repetition frequency was 500 Hz at the average target power density from 29 Wcm-2 to 54 Wcm-2
during a deposition with the duty cycles from 2.5% to 10%. The target-to-substrate distance was 100 mm. For the same duty cycle
of 10%, the deposition rates were up to 120 nm/min for the ZrO2 films, up to 125 nm/min for the Ta2O5 films and even up to 345
nm/min for the HfO2 films. In this presentation, we report on discharge characteristics during the controlled reactive HiPIMS of
these films and on important quantities characterizing the reactive sputter deposition processes, namely, the deposition rate of
films, the deposition-averaged oxygen flow rate and the deposition rate per deposition-averaged oxygen flow rate. A particular
attention will be paid to the choice of a suitable process control parameter, either the average discharge current in a period of a
pulsed power supply or the oxygen partial pressure in a vacuum chamber, for a given deposition. It is based on a time-dependent
response of these two process parameters to constant flow rate pulses of oxygen into the chamber.
4:20 p.m. HP-7 Different Approaches for Controlling a Reactive Sputter Process with MF Superimposed HIPIMS
H. Gerdes1, R. Bandorf1, M. Mark2, T. Schütte3, G. Bräuer1
1
2
MELEC GmbH, Baden, Germany
3
PLASUS, Kissing, Germany
Processes using reactive sputter deposition are gaining more interest since a higher sputter rate can be achieved. Especially for
sputter deposited alumina, the rate drops more than an order of magnitude from metallic to oxide mode. For this investigation
a setup of two cylindrical cathodes of 550 mm and a combination of a HIPIMS and MF-power generators using a commercially
available process control was used. This talk will give an overview of different approaches for a reactive process control in combination with MF superimposed HIPIMS. The discussed feedback systems are based on plasma emission monitors with either optical
filters for single emission lines or with a spectrometer. The controllers are regulating the oxygen flow by piezo-valves or mass flow
controllers or by changing the off-time and therefore the average power. The different approaches will be presented for alumina
on different sputtering plants equipped with planar magnetrons or even rotatables. The results include the voltage and current
characteristics as well as the deposition rates and selected film properties.
4:40 p.m. HP-8 Plasma Pretreatment of Tungsten Carbide and Steels by High Power Impulse Magnetron Sputtering
A.P. Ehiasarian1, A. Oniszczuk1, T.J. Morton1, C.-F. Carlstrom2, M. Ahlgren2
1
HIPIMS Technology Centre, Sheffield Hallam University, Sheffield, United Kingdom
2
Sandvik Coromant, Stockholm, Sweden
Coated cutting tools are used for the majority of today’s manufacturing operations. In a given cutting operation, the adhesion
of the coating to the substrate is directly related to the lifetime of tools. Adhesion is commonly enhanced by the use of gaseous
plasma to preclean the substrate and present a surface free of oxides for the growth of the coating. Metal plasmas are often
more efficient due to the shallow implantation of metal into the substrate which enhances the wettability of the surface during
nucleation of coatings of the same material. The effects of metal ion implantation on the depth and chemistry of the interface
and the microstructure of the surface are not sufficiently understood due to the relatively constrained parameter space available
from conventional metal ion sources. In this experiment tungsten carbide (WC), high speed steel and stainless steel were treated
in the environment of a High Power Impulse Magnetron Sputtering plasma. The plasma chemistry was evaluated quantitatively
by a combination of optical emission spectroscopy and plasma-sampling energy-resolved mass spectroscopy. Ion fluxes and
14
deposition rates were measured simultaneously to obtain ion-to-neutral ratios. The measurements confirmed a strong rarefaction
of the gas and indicated that rarefaction of the metal species may take place as well. Both single- and double-charged metal ions
were detected. No significant delay between the gas and metal plasma was observed within a pulse. The plasma diagnostics
results were used as input to modelling calculations of penetration depth and chemistry near the substrate surface. Metal ions
were found to penetrate approximately 4 nm into the WC substrate. The maximum implanted content of metal was found to
increase as plasma became metal ion dominated and the metal ionisation degree increased. Surface roughness of polished
substrates increased due to the pretreatment as observed by atomic force microscopy, whereas as-received surfaces showed
negligible differences. The etching removed preferentially smaller grains leaving behind a stronger substrate. Grain boundaries
were also preferentially etched and the waviness factor was used to quantify the difference between samples. The etching rates
corresponded to the ion flux to the substrate. The mechanisms linking the plasma chemistry, surface chemistry and the adhesion
of the coatings are discussed. Optimal parameters for improved adhesion are determined.
5:00 p.m. HP-9 Higher Ionization and Deposition Rate of High Power Impulse Magnetron Sputtering Assisted by External
Magnetic and Electric Field
X. Tian1, J. Hu1, R. Kou1, C. Gong1, P.K. Chu2
1
State Key Lab of Advanced Welding and Joining, Harbin Institute of Technology, Harbin, China
2
Department of Physics and Materials Science, City University of Hong Kong, Hong Kong, China
High power impulse magnetron sputtering (HIPIMS) has attracted much attention since it was proposed late in the 1990s. A high
ionization rate of HIPIMS leads to a higher plasma reactivity for preferred microstructure and higher critical load for PVD applications. However, lower deposition rate of HIPIMS technology has limited its wide industrial applications due to a higher pulse
voltage applied to an MS target. A higher deposition rate accompanied by a higher ionization rate may be achieved using external
energy fields. In our HIPIMS system, a coil is equipped around the magnetron target to induce strong EXB effect. The substrate
current may be increased by a factor of 2 or more if a proper current flows through the coil, accompanied by an intensified glow
discharge. If an external electric field is utilized, the glow discharge may be further intensified and much larger substrate current
is observed. The novel HIPIMS technology leads to a thicker film with smooth surface. The higher critical load of deposited films is
easily achieved using this set up, even at a low processing temperature.
15
Monday Evening, April 27
Heuréka! Post-Deadline Recent Developments
7:00 p.m. H-1 A Newly Developed Spectroscopic Plasma Monitoring Tool
T. Schütte
PLASUS GmbH, Kissing, Germany
With rising complexity of and demands on layer composition and structure, process control of coating plasmas becomes
inevitable for process development, process optimization and production. Using standard emission spectroscopy techniques
information on process relevant species is available but the data is not processed and evaluated simultaneously in real-time. This
may be sufficient for laboratory use where specific knowledge and man power is present. However, for industrial applications and
production lines, automated stand-alone systems are required for real-time process control. A newly developed spectroscopic
plasma monitoring tool allows stand-alone spectroscopic plasma monitoring of all process relevant species in real-time in industrial environments. Large area or multi-chamber application can be covered with a multi-spectrometer setup and integration to
the system control is done by industrial interfaces. Examples for different objectives are presented such as quality control and
quality assurance, system diagnostics and fault detection and active process control. Applications ranges from batch type PECVD
processes over microwave driven large area coatings, confocal multi-target multi-gas sputtering and process control of HIPIMS.
7:20 p.m. H-2 Magnetized Hollow Cathode Activated Magnetron
L. Bardos1,2, H. Barankova1,2, A. Bardos1, M. Bernick3, R. Newcomb3
1
BB Plasma Design AB, Uppsala, Sweden
2
Uppsala University, Uppsala, Sweden
3
Angstrom Sciences, Inc., Duquesne, PA
A parallel-plate hollow cathode over the target of the planar magnetron can share the magnetron magnetic field and lead to a
new type of high-density plasma device. Detailed principles of such arrangements are explained. The hollow cathode activated
magnetron produces intense and stable plasmas in a wider interval of gas pressures as compared to the conventional magnetrons
at the same power. Results of the first experimental tests of this arrangement on a commercial planar magnetron with Ti target are
presented and its capabilities are discussed. The device can be arranged in several modifications, which enables new synergetic
combinations of sputtering and arc evaporation regimes.
7:40 p.m. H-3 High Energy Plasma Beam Source for Flexible Application in Thin Film Technology
W. Decker1, K. Schafsteck2, R. Hilberg2
1
Iacten Consulting, Beaver Falls, PA
2
HS-PlasmaTec, Hainburg, Germany
Presented here is a plasma beam source that finds a multitude of applications in thin film coating technology. The unique design
of the plasma source, which combines the generation of high density neutral plasmas through RF excitation and a specifically
designed magnetic field arrangement allows to use the same source for surface cleaning (plasma treatment), ion beam sputtering,
Plasma CVD or Ion Assisted E-Beam deposition. Furthermore, the technology allows the design of specific shapes – round, triangular or linear with lengths of more than 1 meter. Results obtained from different applications of the source will be shown, including,
but not limited to surface cleaning, surface etching and thin film deposition of various oxide films.
8:00 p.m. H-4 Performance of a Linear Open Drift Path Magnetron Cathode
D. Glocker, J.S. Busch
Isoflux Incorporated, Rochester, NY
A linear open drift path magnetron cathode has been built and operated with a combination of RF and DC power. The Al target is
66 cm long by 8 cm wide and a relatively uniform magnetic field extends across the face of the target. The magnetic field, in combination with wings at the sides of the target, confines the secondary electrons produced at the target surface, but the electron
drift is not constrained to a closed path. The deposition rates of Al2O3 and Al have been measured as functions of position along
the length of the cathode under a variety of conditions. At low pressures the Al2O3 deposition rate reaches a constant value within
a distance of 40 to 50 cm. The maximum rate scales with total power, but the distance needed to reach the maximum rate does
not change significantly. At higher pressures the Al2O3 deposition rate continues to increase along the full length of the cathode.
The Al metal deposition rate increases approximately linearly along the length of the cathode, independent of conditions. The
potential for simple high utilization planar magnetrons will be discussed.
16
Monday Evening, April 27
8:20 p.m. H-5 Advanced Mid-Frequency Power Supply with Unique Output Feature for Arc- and Defect Free Reactive
Processes
M. Glück1, F. de Campos Carreri2,3, G. Moser1, H. Müller1
1
J. Schneider Elektrotechnik GmbH, Offenburg, Germany
2
CAPES Foundation, Ministry of Education of Brazil, Brasília, Brazil
3
Magnetron sputtering is a widely used deposition method for applying thin film coatings. Deposition of materials in reactive
coating processes can cause high arcing rates during normal operation. To avoid high arcing rates, it’s necessary to implement
a power supply technology, which can deliver power with low stored output energy into the process. By using a current source
output characteristic it’s possible to fulfill these requirements with another advantage. An inherent current source avoids increasing current in case of arcing condition. A bipolar power supply will be presented, which addresses these features. Experimental
evidence will be presented on the example of a deposition layer of strain gauges. For strain gauges, an insulating alumina oxide
layer with a high breakdown voltage is mandatory. Homogenous defect free layers can only be reached with an arc-less process.
With the presented power supply approach serious coating processes can be managed properly with promising results.
8:40 p.m. H-6 Rotary Cathode Sputter Zone Hardware and Process Optimization Using Advanced Finite Element Analysis
P. Morse
Sputtering Components, Owatonna, MN
The use of finite element analysis is explored to determine the optimum hardware configuration and process settings for sputtering processes. This analysis can help to eliminate costly and time-consuming trial and error testing. The heat transfer inside the
cathode between the water cooling system and the target material is analyzed to determine the effects of the internal structures
and the maximum power densities that can be reached with target materials. Outside the cathode, the sputter flux distribution
profile is simulated to determine the collection efficiencies and deposition rates onto nearby shields or other internal surfaces. Gas
manifolds are also simulated to optimize the output and keep a constant flow per unit length along the manifold. The configurations and results for each of the simulation processes are examined along with the validation metrics.
17
Tuesday Morning, April 28
8:30 a.m. K-2 Sensor Technology: From Automotive to Mobile (Phone) Applications
Invited Talk
C. Herweg
Robert Bosch GmbH, Stuttgart, Germany
Sensors are a key element of a modern car. Since 1998 yaw rate sensors produced by silicon micro machining are used in
the Electronic Stabilization Program - ESP®. This anti-skidding system saves thousands of lives each year and avoids up
to 80% of all skidding accidents. The technological basis for this was created by the development of the deep reactive
ion etching process for silicon wafers in the research labs of Bosch. The consequent progress in the field of MEMS based
sensors led to flexible and cost-effective Inertial Sensor Cluster, nowadays not only part of automotive sensors, but to be
found in mobile phones, tablets, control units of video game consoles, etc. Reducing the emission of a combustion engine
car to the minimum is a challenging task. First steps towards this vision have been taken nearly 40 years ago, when an
oxygen sensor in the exhaust gas, called lambda sensor, was introduced to control the fuel-air-mixture in the engine. Today
several connected sensors measure and control the emission of CO, CO2, NOx and particles. Whereas silicon based sensors
typically utilize vacuum based processes (sputtering, PECVD, PVD and ALD) the modern exhaust sensors need a productive
combination of adjacent techniques like thermal spraying without plasma, printing and casting technologies. The further
connection of these sensors, the interconnection of things and services will drive the technology development and the
market in the next years.
Coatings and Processes for Biomedical and Environmental Applications
9:20 a.m. MED-1 3D Electrospun Scaffolds for Vascular Graft Applications: Fine Tuning of Properties by Plasma-Assisted
Etching and Coating
H. Savoji1,2,4, M. Maire4, A. Hadjizadeh3, A. Ajji1,3, S. Lerouge4,5, M.R. Wertheimer1,2
1
École Polytechnique de Montréal, Institute of Biomedical Engineering, Montreal, Canada
2
École Polytechnique de Montréal, Department of Engineering Physics, Montreal, Canada
3
École Polytechnique de Montréal, Department of Chemical Engineering, Montreal, Canada
4
Centre Hospitalier de l’Université de Montréal, Laboratory of Endovascular Biomaterials, Research Centre, Montreal, Canada
5
École de Technologie Supérieure, Montreal, Canada
Primary requirements for synthetic vascular prostheses are biocompatibility, bioactivity, and favorable morphological and
mechanical properties. In this research electrospinning, plasma etching and plasma polymerization (PP) were combined to
fulfill those criteria. More particularly, we aimed to create scaffolds for subsequent cell-seeding that possess optimal mechanical, morphological and surface-chemical properties in the luminal and media layers. The first set of scaffolds were random
electrospun poly(ethylene terephthalate) (ePET) nano-fiber mats, which mimic the morphological and mechanical properties
of the extracellular matrix of native blood vessels’ lumen. Amine-rich thin PP coatings, deposited via capacitively coupled radiofrequency (r.f.) plasma, enabled confluent monolayer pre-endothelialization of the lumen. Regarding the media layer, ePET
nano-fibers were radially highly oriented; in order to bring their mechanical properties in line with those of natural blood vessels, a substantial reduction in Young’s modulus had to be attained. For this purpose three different plasma etching techniques
were investigated: (i) atmospheric pressure (“HP”) corona discharge in air; low-pressure (ii) r.f. discharge; and (iii) discharge in a
microwave plasma asher, the latter two in pure oxygen (O2), or O2 mixture with Ar or CF4. By far the best results were achieved
using (iii): without visible damage to the fibers, changes in surface composition and drastically improved wettability/wicking
resulted in improved adhesion and growth of smooth muscle cells.
9:40 a.m. MED-2 Characterization of Titanium Nitride Thin Films Deposited on Nylon 6 Nanofibers Substrates by High
Vacuum Magnetron Sputtering and Titanium Nitride Nanotubes Manufacture
D.M. Mihut1, K. Lozano2, C. Hilario2
1
Mechanical Engineering Department, Mercer University, Macon, GA
2
Department of Mechanical Engineering, University of Texas Pan American, Edinburg, TX
The present research is investigating the optimal conditions for titanium nitride thin films depositions onto pristine Nylon 6
nanofibers manufactured using the forcespinning® method. High vacuum magnetron sputtering system was used for depositing titanium nitride coatings while the morphology and chemical composition of the structures were characterized using the
scanning electron microscopy/ scanning transmission electron microscopy (SEM/ STEM), scanning electron microscopy/ energy
18
dispersive X-ray spectroscopy (SEM/ EDS) and X-ray diffraction analysis. The structures were later exposed to different heat
treatment processes in-vacuum in order to create the nanotubular titanium nitride structures.
10:00 a.m. MED-3 Development of Nanostructured CrN/NbN Coatings for Medical Prosthesis Using HIPIMS
P.Eh. Hovsepian1, A.P. Ehiasarian1, Y. Purandare1, A. Sugumaran1, I. Khan2
1
Materials and Engineering Research Institute, Sheffield Hallam University, Sheffield, United Kingdom
2
Biomet Europe, Swindon, United Kingdom
CoCrMo alloy has a long history of successful use for the manufacture of medical devices due to its unique combination of
mechanical, tribological and corrosion properties. Despite this, the alloy does contain ions which are suspected to trigger an allergic reaction in a small number of patients. To address this application a novel nanoscale multilayer structured CrN/NbN coating
was developed. In order to improve coating adhesions and density a novel HIPIMS technique was employed both for substrate
pretreatment and coating deposition. Thus, the synergy between smart materials (Nb is recognised for its biocompatibility and
electrochemical stability and Cr for its tribological behaviour), unique coating structure (controlled on nanoscale range) and
advanced deposition method (providing ionised plasma conditions for the coating growth) has been successfully exploited to
produce this application tailored coating. LAXRD and TEM analyses revealed coating nanoscale multilayer structure. The coatings
were deposited with high thickness uniformity on real implants. Characterisation results revealed high adhesion of HF1, high
hardness of 33 GPa and Young’s modulus of 381 GPa. Low friction coefficient (0.49) and dry sliding wear coefficient, Kc (4.94 x
10-16 m3N-1m-1) were recorded. In potentiodynamic polarisation experiments, the coatings showed excellent corrosion resistance
outperforming many other PVD coatings.
10:40 a.m. MED-4 PVD for Medical Device Applications
Invited Talk
R. Radhakrishnan
Medtronic, Inc., Santa Clara, CA
Medical devices are intended for use in the diagnosis of disease or other conditions, or in the cure, mitigation, treatment, or prevention of disease, in man or other animals. They should demonstrate safety and efficacy in their intended use. Safety and efficacy
of these devices depends on many characteristics such as biocompatibility, surface chemistry, surface morphology, and electrical
and mechanical properties. Often the base materials that are used to produce these devices do not provide all functionalities.
In such cases these devices are coated to obtain specific functional properties. Coatings provide additional properties without
compromising the properties of underlying substrate materials. Physical vapor deposition (PVD) is a suitable process of choice
for metal and ceramic coatings. This presentation will provide an overview of the PVD coating and its applications for medical
implants, its advantages and limitations as well as methods for characterization of such coatings.
11:20 a.m. MED-5 Development of Effective QCM Biosensors by Cyclopropylamine Plasma Polymerization and Antibody
Immobilization using Cross-Linking Reactions
E. Makhneva1,2, A. Manakhov1, L. Zajícková1,2, P. Skládal3
1
European Institute of Technology (CEITEC), Masaryk University, Brno, Czech Republic
2
Faculty of Science, Masaryk University, Brno, Czech Republic
3
RG Nanobiotechnology, Masaryk University, Brno, Czech Republic
Biosensors have been extensively developed and applied for biomedical and environmental study. Although there are many
different types of biosensing techniques, all these methods require immobilization of biomolecules (DNA, antibody, enzyme) onto
the sensor surface. Because of the high reactivity of primary amine groups, amine-rich films are extensively employed for numerous biomedical and environmental applications. In this work, cyclopropylamine pulsed plasma polymerization is employed to
deposit stable amine-rich thin films on the surfaces of QCM biosensors. The antibody specific to human serum albumin (anti-HSA)
was attached to the QCM surface via crosslinkage obtained by the intermediate reaction with glutaraldehyde. We have tested a
number of QCM-biosensors with two types of nanofilms prepared using two different plasma set-ups. In first group of samples
(type-1), the substrate was placed at a floating potential, while in the second group (type-2), the subtrates were self-biased. All
steps of the bio-immobilization were controlled by XPS and FT-IR to characterize surface and layer (bulk) chemistry. After each
step of bioimmobilization, the change of the QCM resonant frequency was measured. The increase of the mass after each chemical reaction was observed for the QCM-biosensors coated by the type-1 film. These samples also exhibited highest response
towards the anti-HSA antigen. The QCM-biosensors coated by a type-2 films exhibited lower and irregular change of the mass and
therefore they were less reliable for the measurement. The biosensors of the first type have the highest efficiency and are very
promising for future use in the biosensing field.
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11:40 a.m. MED-6 Evaluating True Coating Properties from an Indentation Measurement Series – A New Combination of
Calotte Grinding and Indentation Tests
N. Bierwisch, N. Schwarzer
Depending on the material structure (e.g. layer thicknesses, Young’s moduli ratios, etc.) and the indentation device capabilities
(e.g. force range), it’s often not possible to measure the true coating parameters without any substrate (or underlaying material)
effect. A few years ago, a model and dedicated software packagae was developed which allows the determination of true generic
material parameters (like Young’s modulus and yield strength) for a coating by knowing the parameters of the substrate and all
underlaying layers. To apply this approach to a complex multi-layer stack of different materials, one needs to stop the production
process after every added layer. Then the indentation measurements are performed to determine the material parameters for the
top coating. This analysis is repeated for every layer in a possibly very complex coating structure. This approach has severe drawbacks: Firstly, it’s not always possible to coat the complete structure layer by layer and perform the measurements after a layer
was added. Secondly, it is possible that during the coating process the parameters of the underlaying layer are changed, because
of some interface effects. One of these effects could be the creation of a mixed zone of both materials with different mechanical
parameters. Because the calotte grinding tests are widely used to determine the layer thicknesses, we thought about using the
possibility to directly access the deeper parts of a complex layer stack by applying a combination of calotte-grinding and subsequent indentation testing. We created a new module which analyses a series of indentation measurements which were performed
from the inside (focal point) to the outside of the calotte test crater. So it’s possible to perform tests on the substrate and all layers.
This module was built into the software package FilmDoctor®, which subsequently analyses such a measurement series starting
with the substrate measurements. All evaluated values are used for the next iteration step of the new analysis method. At the end
the material parameters for all layers are determined without the need of stopping or changing the production process.
Large Area Coatings
9:20 a.m. L-10 From Lab to Production, Examples for Technology Transfer of PVD-, CVD- and Atmospheric Pressure Plasma
Processes
Invited Talk
V. Sittinger, L. Schäfer, M. Armgardt, M. Höfer, M. Thomas, M. Eichler, A. Laukart, M. Vergöhl, S. Bruns, T. Zickenrott, A. Pflug, C.-P.
Klages, G. Bräuer
Different examples of technology transfer from Lab to Production will be shown in this presentation. We show the development
of sputtered TCOs from ceramic ZnO:Al2O3 targets for thin film photovoltaics upscaling on to 5.5 m2. For this application a homogenous etching process to achieve efficient light trapping was especially necessary by simultaneously ensuring low absorption
and high conductivity. The development of diamond coated ceramics is an example for the transfer of a chemical vapor deposition technology. At the beginning the large area hot filament assisted chemical vapor deposition process has been adapted to
the substrate materials silicon nitride and silicon carbide. Subsequently, structure and uniformity of the diamond films and the
reliability of the diamond deposition process was adapted to the requirements of seal applications. Extended field tests with
diamond coated silicon carbide face seals demonstrated the high performance in “bad actor” applications. For several years, these
diamond face seals have been available on the market for sealing applications offering extreme wear resistance, low friction and
outstanding durability. Another example is the development of EOSS® coater, a tool for the production of precision optical filters,
which is based on a number of successive activities and research projects. This includes a research project to improve the process
stability of reactively sputtered optical coatings, and also projects in the field of monitoring the optical properties during deposition. Particles which play an important role in optical technologies were also in the focus. The new platform EOSS involves now the
results of the different development and is available on the market today. The prototyping of new coater concepts is accompanied
by simulation of the gas flow and plasma discharge dynamics. In recent years atmospheric pressure plasma processes become
more and more interesting for different applications. With partners from industry the pretreatment of technical textiles using
dielectric barrier discharge (DBD) have been optimized to improve wetting behavior of water- and oil-repellent finishings. In the
meanwhile two DBD stations are implemented in the production with a treatment width of 1500 mm and 3200 mm, respectively.
Another project was the installation of a R2R-plasma-printing system with a treatment width of 450 mm for area-selective pretreatment of polymers at a Japanese company. The minimal resolution of the plasma-printing process is 25 µm and it can be used
prior to subsequent wet-chemical coating processes.
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10:00 a.m. L-11 Silver - One of the Last Frontiers for Rotatable Targets: Cold Spray Technology and Economic
Considerations
A. Seapan1, T. Bruha2
1
SAFINA Materials Inc, Conroe, TX
2
SAFINA a.s., Vestec, Czech Republic
Silver is one of the few materials in a low-E film stack which remains predominantly on a planar cathode platform. Meanwhile,
newer regulations and evolving coated glass products are driving growth in triple silver layer stacks. Traditional challenges for
silver rotatable targets have been economic feasibility, grain size non-uniformity, and subsequent uniformity challenges of the
as-deposited films. In this context, triple silver layer stack products demand even stricter requirements on deposited silver layer
uniformity. Cold spray is a highly kinetic process that is a relatively new technology now being applied to Ag rotatable targets to
produce very fine grain, homogeneous rotatable targets. Technical characteristics and advantages of cold sprayed Ag targets will
be covered and compared with alternate technologies for producing Ag rotary targets. The talk will describe the Ag cold spray
manufacturing steps and discuss the cost implications of the various process steps. Additionally, the presentation will broadly
explore the financial considerations of evaluating rotatable silver targets.
10:40 a.m. L-12 On-line Adjustable Magnetics in Rotatables for Improved Layer Uniformity
N. De Wilde, I. Van de Putte, W. De Bosscher
Soleras Advanced Coatings, Deinze, Belgium
Tendencies towards higher demanding and multifunctional thin film coating stacks can be translated into more stringent requirements of individual layers with respect to composition and performance. In addition, accurate control of the uniformity of these
layer properties across ever increasing substrate sizes is becoming essential. In the past, unbalancing the (reactive) gas flows
across the substrate was often the only way for realizing the required thickness control, however frequently leading to undesired
compositional variations in the deposited layer. Sputtering from rotating cylindrical targets incorporating a new magnetic solution may provide an adequate solution. The system allows for remote control and online adjustment of layer thickness uniformity
without the need for having gas compensation and without the need of stopping the sputtering process. Besides this essential
feature of controlling uniformity, the magnetic system may contribute significantly in realizing high quality layers and better
performing stacks. In this paper, we will present the capabilities of the system and explain how certain sputter parameters (power
level and magnetic field strength) influence the local and global deposition rate. Some added value opportunities for double and
triple silver architectural coatings will be discussed. Implementation in the display industry opens interesting new possibilities.
11:00 a.m. L-13 Large Area Coating: Solutions and Opportunities from High Power Pulsing
D. Christie, J. Pankratz, B. Kowal, H. Walde
Advanced Energy Industries, Inc., Fort Collins, CO
Magnetron sputtering is used to deposit large area multi-layer structures for photovoltaic (PV) panels, flat panel displays (FPD), architectural and automotive glass, and flexible webs. Pulsed power is used for reactive deposition of dielectrics. It enables reactive
sputtering of dielectrics that are essentially impossible with straight DC, owing to periodic discharge of the voltage on dielectric
films deposited on the target itself, preventing target arcs and helping to mitigate anode coverage. The concept was introduced
in the 1970s. Pulsed reversal was developed industrially in the 1990s. Further innovation broadened the solution space to include
control of material characteristics like morphology and crystallinity, and process measurement and control. Pulsed techniques
for dual magnetron sputtering (DMS) enable reduced energy consumption by operation at the minimum frequency consistent
with stable process operation. Now stable processes are possible at lower frequencies due to faster arc handling and reduced arc
energy. Greater rate can be achieved by running incrementally higher on the transition curve, by controlling the working point
of each magnetron in the DMS pair. Process measurement and control are enhanced by quasi-DC conditions accessed by quasicurrent source pulsed power solutions. New developments, key solutions, and opportunities driven by pulsed power capabilities
are presented.
11:20 a.m. L-14 Ensure High Deposition Rate and Excellent Film Quality with Mid-Frequency Power Supplies
U. Richter
TRUMPF HUETTINGER GmbH + Co. KG, Freiburg, Germany
Over the past two decades, mid-frequency power supplies in the multi-kilowatt range have evolved into a common tool for dual
magnetron sputtering. To achieve excellent film quality and deposition rate an effective arc management becomes more and
more important. New delay-free and high-precision sensing of voltage and output current enables effective arc detection by
envelope observing. This followed by ultrafast and short arc treatment keeps residual energy delivered to the arc lowest as possible while it maintains the medium output power to the process at the set level even in arc burst situations. Another factor that
21
defines the film quality as well as deposition rate is the operating frequency; here it is possible to adjust the working frequency
independently of the output power. Lastly, new power supplies enhance plasma without any mains frequency related ripples to
reduce the tendency of arcing during power peaks. The paper presents test results of the new design features, leading to better
process regulation and stability under difficult conditions.
11:40 a.m. L-15 Raising the Bar for Oxide Deposition Rates
D. Pelleymounter
Advanced Energy Industries, Northfield, MN
Sputtering non-conductive oxides at a high deposition rate for a long period of time has always been a goal for process engineers.
When sputtering these types of oxides DC with one magnetron, the anode goes away and the process dies. The proven solution
for this is the use of AC power delivery with two magnetrons. The AC solution results in a loss of deposition rate at the same power
of about 20% from the initial DC one magnetron design. However, end blocks for rotatable magnetrons have limited current
capability that limits maximum power. Now a new way to sputter non-conductive oxides exists. Using two bi-polar pulsed DC
power delivery systems and a floating anode added to the AC style dual magnetron sputtering zone we can achieve high deposition rates by delivering more power than is possible with the AC solution. This can be as high as 2x the deposition rate of AC.
The floating anode stays thermally hot to desorb oxide deposited on it. If a gas manifold is embedded the anode, the secondary
plasma emissions at the gas orifices will keep the anode clean for long periods of time. Methodology and results are presented.
12:00 p.m. L-16 Achievements with Bipolar Power Supplies in Dual Magnetron Processes
K. Ruda1, P. Ozimek1, P. Lesiuk1, A. Klimczak1, M. Baran2
1
TRUMPF Huettinger Sp. z o.o., Zielonka, Poland
2
Institute of Control and Industrial Electronics, Warsaw University of Technology, Warsaw, Poland
In the last couple of years, fast development of DC technology has provided bipolar power supplies capable of working in the
medium frequency range in dual magnetron processes. This new approach opens various possibilities of optimizing the processes
in order to combine high deposition rate with excellent film quality and user friendly operation. The possibility of the flexible
formation of output signals and their influence on plasma parameters and coating results gain a lot of interest from the scientific
and industrial communities. This paper presents power supply behavior in different plasma processes like reactive sputtering,
PECVD (Plasma Enhanced Chemical Vapor Deposition) with field results. The influence of different plasma conditions on signal
shape is one of the major topics. As a result of experience in operation in hard process environments, innovative arc management
algorithms are being developed and presented. Finally new features of bipolar power supplies like power equalization for avoiding unsymmetrical wear of cathodes, adjustable frequency for finding balance between arc and deposition rate are discussed
as well.
Emerging Technologies
9:20 a.m. E-5 Thin Film Process Control and Optimization through Predictive Modeling
G. Atanasoff, C. Metting
AccuStrata, Inc., College Park , MD
There is a lack of process control capability for optically thin (below 5-10 nm) or thick (over 15-20 µm) films and coatings or compound films where the right chemical composition is critical for the film properties. This problem is aggravated as new-generation
structures become more complex. The non-adequate process control leads to increased product cost due to excessive waste of
energy, materials and labor. In this work we employ broadband in situ optical monitoring, statistical modeling and pattern recognition algorithms to trace the deposition process as it occurs and compare it to a theoretical model or historical statistical information about previous processes with high yield and quality. The learning and reasoning algorithm provides for prediction of process
outcome before its completion, detection of process drifts and impairments and generation of corrective actions to improve the
subsequent process steps leading to seamless adaptive process control. We present experimental results for real-time monitoring
and predictive modeling of epitaxial growth of LED structures, having both thick GaN films and extremely thin quantum well
InGaN layers, during manufacturing of high brightness LEDs. Improvement of wafer uniformity, wafer-to-wafer, run-to-run and
reactor-to-reactor repeatability and increased LED packaging yield results in reduced LED cost $/lumen.
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9:40 a.m. E-6 Thin Film Coating Process Calibration by Index Dispersion Enhanced Monitoring
W.E. Rodgers, L.S. Ring
Eddy Company, Apple Valley, CA
Methods are presented to calibrate thin film design programs to individual coating chambers by measuring properties unique to
each coating system and process therein. After calibration, parts coated on the system precisely match their design without need
for iteration. The methods are based on the use of Index Dispersion Enhanced (IDEM). IDEM monitoring allows for measurement of
the actual Index Dispersion of each non-absorbing thin film deposition process of a specific optical coating machine. Differences
between theoretical and actual index dispersion of vapor deposited materials were found to be a primary cause for thin film
coating deviations from the intended design. Examples of otherwise difficult to produce coatings are provided.
10:00 a.m. E-7 Improvement of Optical Coating Properties Deposited by Reactive Electron Beam Evaporation Processes
with Closed Loop Reactive Gas Control
F. Papa1, V. Bellido-Gonzalez2, D. Mongahan2
1
2
Gencoa Ltd. Liverpool, United Kingdom
Reactive and ion assisted electron beam evaporation processes have been used to deposit optical coatings, such as titanium
dioxide, for several decades. These processes are rather robust and inexpensive. However, some applications require a stricter
control over the oxygen partial pressure in the system during evaporation in order to control coating properties. For this reason,
the relative measurement of the oxygen partial pressure is achieved by optical emission monitoring of a remote plasma sensor
attached to the vacuum chamber. The emission intensity is then fed back into a closed loop controller that regulates the oxygen
gas flow. The investigation of what happens with regards to oxygen partial pressure during a standard process with constant
oxygen flow as well as with active partial pressure control has been done. It was found that control over the partial pressure has
a profound influence on the thermal stability of titanium dioxide coatings after annealing. The effect of active partial pressure
control on indium tin oxide and silicon dioxide coating properties will also be discussed.
10:40 a.m. E-8 Operation of a Combined Sputter Deposition and Ion Source
D. Glocker1 and R. Belan2
1
Isoflux Incorporated, Rochester, NY
2
Kurt J. Lesker Company, Jefferson Hills, PA
A multi purpose source has been constructed that can operate either as a magnetron sputtering cathode, an end-Hall ion source,
or both simultaneously depending on the applied voltage. A conical electrode with a major diameter of 6.5 cm and included
angle of 90 degrees is combined with a magnetic field that forms a plasma trap above the electrode and also extends beyond the
electrode opening. A hot filament generates electrons when operating as an ion source. Using an Al electrode, all three modes of
operation have been demonstrated. Sputtering with an applied voltage of -390 V produced an Al film at a specific deposition rate
of 4.0 (nm/min)/(W/cm2). By applying +340 V to the electrode at an Ar pressure of 1 mT and filament current of 25 A, a thermally
grown SiO2 layer was etched at a rate of 5.2 nm/min. Finally, using a 40 kHz bipolar power supply to apply an alternating positive and negative voltage to the electrode at a total power of 200 W, a reactively sputtered Al2O3 film was deposited arc-free at a
specific rate of 1.1 (nm/min)/(W/cm2). The values for n and k (632 nm) for the Al2O3 were 1.67 and 0.001 respectively.
11:00 a.m. E-9 Circular Ion Sources for Plasma Enhanced Atomic Layer Deposition Applications
V. Bellido-Gonzalez1, D. Monaghan1, H. Li1, F. Papa2, H.D. Ngo3,4, P. Mackowiak5
1
Gencoa Ltd., Liverpool, United Kingdom
2
3
University of Applied Sciences Berlin, Berlin, Germany
4
Fraunhofer Institut IZM, Berlin, Germany
5
TU Berlin, Berlin, Germany
Atomic Layer Deposition (ALD) has been slowly gaining acceptance in the field of thin film deposition. There are many benefits of
ALD, however, in terms of deposition rates and management of reactive gas species in complex 3D structures there is still a long
road ahead. A particular area of growth has been Plasma Enhanced ALD (PEALD). PEALD has been introduced in order to lower the
temperature requirements for the ALD process and also in order to control the properties of the ALD deposited film. The industrialization of such process presents a number of challenges. In PEALD, it is of interest to control the nature and degree of interaction
of such plasmas with the surface chemistry. Plasma sources which can control the energy of the ion beam are of special interest.
From the point of view of industrialization, Linear Ion Sources (LIS) could help move ALD processes into mass production. LIS’s
have been slowly pushing their way through into vacuum coating technology market for over 15 years. Only last year a small
23
circular ion source, which can replicate the functional properties of large LIS’s was introduced. This development enables a rapid
transition from prototyping to manufacturing. The use of such a source is interesting for PEALD as the processes developed in the
lab could be easily implemented at an industrial level. The present paper will present the development PEALD processes using
such a circular ion source.
11:20 a.m. E-10 Characterization of a High-Throughput Batch Fixture for Atomic Layer Deposition
C.A. Outten, J.R. Abiva, D.W. Konopka
Denton Vacuum, Inc., Moorestown, NJ
The focus of the present work is the evaluation of 3D/batch fixtures for Atomic Layer Deposition (ALD) applications. ALD is
an attractive process technology for the deposition of ultrathin, conformal thin film coatings. There is significant interest in
leveraging the unique benefits of ALD for optics, medical devices, and sensors. However, ALD processes exhibit inherently lower
deposition rates than traditional physical vapor and chemical vapor deposition due to the self-limiting nature of ALD surface
reactions. To increase throughput, high-capacity batch-style fixtures were designed and tested in a cross flow ALD reactor. Fixtures
were evaluated that support individual substrates and 3-dimensional assemblies. An initial fixture was designed to minimize
non-uniformities in deposited films due to non-laminar flow in the reactor and thermal gradients in the fixture. The goal was to
demonstrate film thickness uniformities of < ± 0.5% on each individual wafer and substrates. Thermal aluminum oxide ALD films
were deposited under a variety of process conditions, substrate temperatures, and fixture loading factors. Film thickness and
index of refraction were measured using a profilometer, reflectance spectrometer, and spectroscopic ellipsometer. Thickness and
temperature uniformity data will be presented along with assessments of the impact to throughput and tool productivity.
11:40 a.m. E-11 A New Auto Frequency Tuning Algorithm
C.H. Bock, H. Windisch, F. Freiburger
TRUMPF Huettinger GmbH + Co. KG, Freiburg, Germany
One countermeasure to fast plasma impedance variations is auto frequency tuning where on a sub-millisecond timeframe the
RF-power generator sets its fundamental to a frequency value with better matching. Conventional solutions for auto frequency
tuning work with a trial and error algorithm that jumps to a new frequency, tests the reflected power and decides to either
proceed or turn back, or use complex impedance measurement to deduce the tuning information. However, these solutions suffer
from inadequate performance and occasionally get stuck. In our new approach the RF fundamental is constantly FM-modulated
with a selectable modulation frequency. If this modulated RF hits the “matching slope” of the chamber the reflected power will
not only be frequency modulated but also amplitude modulated. Special double demodulation yields a signal representing the
steepness and sign of the matching slope, i.e. its derivative, which may readily be used as the tuning information. The algorithm
is tweaked to not get latched at local reflection minima while displaying a smooth and tempered behaviour close to the tuning
optimum. The competitive regulation tendencies of the frequency tuning algorithm and a mechanical matchbox are illustrated
and two solutions are disclosed. Experimental results illustrate the capabilities.
Protective, Tribological and Decorative Coatings
9:20 a.m. T-1 From 3D to 2D in MAX Phases as the Natural Ternary Nanolaminates
Invited Talk
V. Vishnyakov
University of Huddersfield, Huddersfield, United Kingdom
MAX phase materials are ternary carbides and nitrides of transitional elements with naturally nanolaminated structure and unique
combination of properties. Reduction of the materials dimensionality down to few or even single monolayer, so named MXene
materials, leads to new properties which can be utilised in renewable energy harvesting, energy storage and microelectronic
devices and sensors. For instance, stacked 2D layers demonstrate high charge capacity for lithium rechargeable batteries. It is also
possible by physical vapour deposition methods to combine MXenes with such materials as graphene and boron nitride nanotubes. This allows tuning electronic properties of individual layers and resulting structures.
10:00 a.m. T-2 Effects of Surface Treatments and Coatings on Tribological Performance of Ti-6Al-4V in the Mixed Fretting
and Gross Slip Regimes
D. Cressman, B. Tury, G.L. Doll
Timken Engineered Surfaces Laboratories, The University of Akron, Akron, OH
Although titanium alloys are chemically resistant and have desirable mechanical properties, these materials are known
to experience high wear rates and friction when they are in contact and in relative motion with themselves or most other
24
materials. In this study, titanium-containing MoS2 and Ti containing amorphous carbon coatings have been applied to
Ti-6Al-4V discs and were examined in mixed fretting and gross slip regimes against uncoated, NiPO4, and MnPO4 coated
counter faces. Experiments were carried out at two different temperatures and wear coefficients were obtained for the
various materials pairs. Whereas the smallest friction and wear coefficients were obtained for MnPO4/Ti-MoS2 pairs at both
high and low temperature, the NiPO4/Ti-MoS2 coupling is incompatible. On the other hand, NiPO4/Ti-aC appears to be a
very compatible materials pair.
10:40 a.m. T-3 Protective Hard ZrN-TiN Multilayer and Nanolaminate Coatings
A. Raveh1,2, Z. Rożek1,3, T. Poirié1, E. Herrera1, E. Bousser1, L. Martinu1, J.E. Klemberg-Sapieha1
1
Department of Engineering Physics, École Polytechnique Montréal, Montreal, Canada
2
Advanced Coatings Center, Rotem Industries Ltd., Arava, Israel
3
Institute for Nanomaterials, Advanced Technologies and Innovation, Technical University of Liberec, Liberec, Czech Republic
The influence of deposition parameters on the low residual compressive stress and grain size, while retaining the high hardness,
may affect the thermal stability and the tribological properties of the coatings. In this study, we deposited different combinations of single-layer ZrN and TiN, as well as double-layer and multilayer ZrN-TiN coatings, and we investigated their structure and
mechanical properties. The coatings were prepared with various pulse modulation periods by pulsed-DC magnetron sputtering.
The Zr and Ti targets were pulsed in asynchronized mode, both at 300 kHz and 1.1 µs reverse time. A total thickness of approximately 1 µm for each coating was obtained by adjusting deposition time. In the case of the nanolaminate coatings, the number of
sublayers was selected to be in the range of 100 to 1000 for an individual layer thickness of 1 to 10 nm (bilayer period λ of 2 to 20
nm). It was found that the nanolaminates with smaller λ improve hardness, fracture toughness, adhesion and wear. For example,
the hardness of the multilayers was 32 GPa which was significantly higher than the 21 GPa of TiN or 18 GPa of ZrN single-layer
coatings. In addition, a smaller λ led to lower friction coefficient µ. Specifically, µ ~0.5 of the single-layer coatings decreased to
0.15 for the multilayer. With respect to tailoring the substrate-coating interface, the Ti-6Al-4V substrate was nitrided to form a solid
solution of nitrogen in titanium α-(Ti,N). The nitrided layer leads to improved the adhesion, that was confirmed by an increase of
the scratch test critical load by one order of magnitude compared to samples with no nitriding.
11:00 a.m. T-4 Modified Diamond-Like Carbon Coatings (a-C:H:X) for Anti-Fouling Applications
M. Keunecke1, I. Bialuch1, M. Weber1, C. Stein1, K. Bewilogua1, G. Bräuer 2
1
2
Institut für Oberflächentechnik, Technische Universität Braunschweig, Braunschweig, Germany
Amorphous hydrogenated diamond-like carbon films (a-C:H) are well known for their high hardness, high wear resistance and
low friction coefficients. The incorporation of additional elements leads to considerable modifications of the coating properties,
e.g. silicon containing a-C:H:Si coatings provide low friction coefficients and lower surface energies. Incorporation of Si and O
(a-C:H:Si:O) leads to highly hydrophobic coatings with still lower surface energies (< 25 mN/m). Both types of coatings had antiadhesive properties. Modified DLC coatings were prepared by Plasma Enhanced Chemical Vapor Deposition (PECVD) processes,
powered with radio frequency, bipolar pulsed DC voltage or by a linear micro wave plasma source in industrial scale coating
machines. The different DLC modifications can be combined in a multilayer coating for optimization of properties. The developed
modified DLC films with low surface energies and high wear resistance are promising for several technical applications, e.g. for
forming or pressing tools or for reduction of fouling effects in heat exchangers. These coatings were used to realize an alternative
approach for inside coating of pipes. After coating deposition on flat metal sheets followed a cold forming process to fabricate a
pipe and a welding along the joint line to close the pipe.
11:20 a.m. T-5 Influence of Precursor Ratio on the Tribological and Tribochemical Performance of Microwave PECVD
Hydrogenated Diamond-like Carbon Films
H. Zhao1, C. Wang1, D. Scurrb2, T. Liskiewicz1, I. Kolev3, A. Neville1
1
University of Leeds, Institute of Functional Surfaces (iFS), School of Mechanical Engineering, Leeds, United Kingdom
2
University of Nottingham, School of Pharmacy, Nottingham, United Kingdom
3
Hauzer Techno Coatings, Venlo, Netherlands
Diamond-like carbon (DLC) films continue to be used widely in the automotive industry due to their good mechanical properties
and tribological performance. Both industry and academia are interested in further improvements in the tribological performance
of this category of carbon films. A high deposition rate process for hydrogenated diamond-like-carbon (a-C:H), microwave excited
plasma enhanced chemical vapour deposition (μW-PECVD) method was investigated in this study. Microwave PECVD DLC films
were deposited on TE77 pin-on-plate samples for tribological tests. A normal PECVD DLC film was tested as reference. The MW
DLCs that were produced using high precursor gas ratios (80 and 90%) provided slightly lower friction and wear than low gas ratio
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(60 and 70%) ones. Raman spectra results showed different carbon sp3 content was obtained as a result of different gas ratios. The
adsorption of some key P-based additive functional groups on DLC films was assessed. The link between functional group adsorption and tribological performance is discussed in this paper.
11:40 a.m. T-6 Industrial Microwave Carbon-Based Coatings on Plastic and Metal Substrates
I. Kolev1, D. Doerwald1, H. Zhao2, A. Nevile2, R. Tietema1, J. Landsbergen1
1
IHI Hauzer Techno Coating, Venlo, The Netherlands
2
School of Mechanical Engineering, University of Leeds, Leeds, United Kingdom
In the past decade, automotive, aviation, as well as aerospace and wind industries have shown interest in improving the efficiency,
viability and lifetime of their products applying PVD coatings. Carbon-based, such as DLC, are the most frequently used and are
applied on hundreds of millions, mostly steel, components. They enable a reduction of wear and friction in modern engine platforms. To further increase the number of applications for DLC coating a further cost reduction of the coating process is required.
There is a clear trend to a more widespread use of plastic parts. The demand for reliable and fast techniques allowing functional
coatings on plastics is rapidly growing. These plastic parts often need to satisfy tight functional requirements. Carbon coatings
are one possible way to match them. Many components and parts nowadays require not only functionality, but also an appealing
decorative finish. DLC coatings offer both. In this paper, the properties of the microwave carbon-based carbon coatings on plastics
and metal substrates in an industrial coater are discussed. Results show the advantage of the technology in terms of deposition
rate and possibility to coat nonconductive parts. The influence of the process parameters on the main coating properties, among
which polymer surface activation, hardness, adhesion and deposition rate is presented. Tribological properties, such as wear
resistance and coefficient of friction are measured and reported as well.
26
Tuesday Afternoon, April 28
12:30 p.m. T-8 Multilayer PVD Coatings with High Corrosion Resistance at High Temperatures
J.A. García1, S. Mato2, I. Ciarsolo1, F.J. Pérer Trujillo2, J. Barriga1
1
IK4-TEKNIKER, Eibar, Spain
2
Complutense University of Madrid, Madrid, Spain
Electric generation power plants search to increase thermal efficiency of conversion processes in steam turbines, to reduce fuel
consumption and emissions of greenhouse gases such as CO2, SO2, and NOx. This requires developing materials able to resist
steam conditions at 650-700°C since ferritic-martensitic steels, which have been commonly used due to their excellent mechanical
properties at high temperature, show limited oxidation resistance. Although high temperature alloys, as nickel-based alloys, can
be used at the mentioned temperature regime, coatings have been of interest in recent decades. Following this approach, the
surface characteristics of the substrate are changed in order to prolong its service life at extreme conditions. In this work several
coatings deposited using cathodic arc evaporation have been developed: CrN, ZrN, TiN and two different multilayers based in
Ti and Cr nitrides. Some of the coatings were thick in order to prevent corrosion, but trying to optimize adhesion: film thickness
varies from 3 to 10 microns. The long term oxidation resistance of the coatings was evaluated at 650ºC in 100% steam atmosphere.
Good results were obtained with the following coating structure: TiN(1.5 µm)/TiCrN(5.7 µm)/CrN(1.1 µm).
12:50 p.m. T-9 Nano-Grained Hard Protective Titanium Carbide Coatings Prepared by PECVD
J. Lengaigne1, E. Herrera1, A. Raveh1,2, E. Bousser1, L. Martinu1, J.E. Klemberg-Sapieha1
1
École Polytechnique de Montréal, Department of Engineering Physics, Montréal, Canada
2
Rotem Industries Ltd., Advanced Coatings Center, Arava, Israel
The unique properties of titanium carbide (TiC), such as high hardness and elastic recovery, high corrosion resistance at elevated
temperatures and high electrical conductivity make TiC very attractive as a protective coating for nuclear, aerospace and tool
applications. In this study, coatings were prepared by Radio-Frequency Plasma Enhanced Chemical Vapor Deposition (RF-PECVD)
onto silicon and Ti-6Al-4V alloy substrates using titanium tetrachloride (TiCl4) and acetylene (C2H2) in argon-hydrogen mixtures.
The deposition was performed at a substrate temperature of 400°C and an RF self-bias voltage of -400 V while studying the effect
of the H2 concentration and the C2H2:TiCl4 ratio on the coating structure and the mechanical properties. The controlled parameters
were found to affect the phase formation, grain size and orientation, as well as hardness H, Young’s modulus E, internal stress σ,
wear resistance and adhesion. In order to improve the adhesion to the Ti-6Al-4V substrates, nitriding or carburizing was performed
prior to the deposition. XRD revealed that the grain size varied between 6 and 12 nm for different H2 and C2H2 concentrations. The
high hardness of 32-35 GPa as well as the highest H/E, and H3/E2 ratios were correlated either with the smallest grain size and the
(111/200) peak ratio, or to the highest H2 concentration (67 vol.%) in the gas feed. Alternatively, the coating with the maximum
H (36 GPa), H/E, and H3/E2 was obtained with lower H2 (~20 vol.%) and low C2H2 concentrations (~1 vol.%). The role of hydrogen
and acetylene in the gas feed as dominant parameters affecting the structure and properties of the coatings is presented and
discussed.
1:10 p.m. T-10 The Influence of TiC Buffer Layers on the Structure and Mechanical Performance of Diamond Films on
Cemented Carbide
M. Liu1, T. Zhu1, Y. Chen1, J. DiBattista2, E. Chan2, Y. Yang2
1
Department of Electronic Information Materials, Shanghai University, Shanghai, China
2
Darly Photonics Composite Materials (Shanghai) Corp., Shanghai, China
Titanium carbide (TiC) is one of the most widely applied hard coating materials used today. Recently it has been used as buffer
layer between diamond films and cemented carbides to improve adhesion strength. The influence of TiC buffer layers, prepared
by co-sputtering, on the structure of diamond films along with the resultant effect on adhesion and wear resistance have been
investigated. Results show that improved physical properties of this multi-layer coating results from the TiC buffer layer reacting
with tungsten carbide (WC) during the deposition of the diamond film. It was found that the preferred orientation of diamond
film is (111) with a grain size between 50-100nm with a hardness of 38.9GPa, where the hardness of TiC layer is 17.5GPa. A relationship was discovered between chemical etching pretreatment and TiC layer thickness that can greatly enhance adhesion strength
between the TiC and diamond layer. Lastly, improvements in wear resistance are described related to the coefficient of friction of
the multi-layered films.
27
Poster Session
Poster-2 How to Design Contact Experiments Properly to Test the Adhesion Performance of a Coating Substrate System
N. Bierwisch, N. Schwarzer
Adhesion is a very important factor of the application performance of new material combinations. Nowadays, we deal with
more complex material structures. The increased complexity is caused on one hand by the inner structure of the used coatings
itself (e.g. gradients, composites) and by the increased amount of used coatings’ so-called multi layer stacks. This makes it difficult to find the right experimental setup to produce the maximum stresses at certain regions. In the case of testing adhesion
performance, the goal is to produce the maximum stresses at the interfaces between the used coatings. It will be shown how the
measurements have to be performed to test the adhesion performance at every interface within our material structure. In principle and for completely homogenous materials it is always possible to extract measurement information from certain well selected
areas within a half space by the means of normal indentation testing. Within the talk it will be shown how this can be achieved by
properly selected measurement conditions with respect to contact area and load or tip shape and load. Unfortunately, this nice
possibility of actually “steering” the “Point Of Interest” (POI) of any indentation test is not given in the case of layered materials. So,
as a mere byproduct of the development of a measurement optimizing software tool for optimum parameters for indentation
and scratch it was discovered that it is not possible to select every point in a simple coating substrate system in order to obtain
measurement information dominated by an area around that very point. This is caused by “Shadow Effects” coming from either
the substrate or the coating and hindering the POI to show the inelastic behavior one is interested in, because inevitable inelastic
behavior at other positions within the compound are shadowing the process and point of interest.
Poster-3 Quantifying Time-Dependent Mechanical Behavior of Visco-Elastic Materials or Materials at Elevated
Temperatures
M. Fuchs, N. Bierwisch, N. Schwarzer
Saxonian Institute of Surface Mechanics, Ummanz, Germany
The mechanical behavior of all materials at elevated temperatures or of polymers and some metals even at room temperature are
significantly time-dependent. Therefore, appropriate measurement techniques and analysis procedures are necessary to quantify
their mechanical behavior in terms of, for instance, time-depedent elastic modulus as well as storage and loss modulus. However,
it has long been a topic of discussion why different mechanical experiments like uniaxial tensile test, rheological shear test or
contact experiments (e.g. nanoindentation, scratch) or even the same test performed in quasi-static or dynamic mode result
in partially dramatic differences with respect to the mechanical parameters being extracted from these tests. The presentation
will elaborate why this is the case and how the various tests can be properly linked respectively used to analyze the mechanical
behavior of visco-elastic materials such that identification of generic material parameters is possible rather than a plain qualitative
testing. The physical and mathematical extensions necessary to describe the effects playing a role in this are quite demanding and
surprisingly holistic. In addition, it will be shown how these new methods in conjunction with the well-established Oliver&Pharr
method extended for coatings can be applied to properly determine time-depedent mechanical properties of thin films by indentation creep testing taking examples of polymers and metals. Finally, an outlook will be given how these procedures could be
developed to new standards for more reliable truly physical parameter identification of viso-elastic materials and their interfaces
(e.g. adhesion).
Poster-4 Nanocoatings for Corrosion Protection of Titanium Alloy in Aggressive Environment Containing Fluoride Ions
M. Grobelny1, M. Kalisz1, M. Sochacki2, J. Szmidt2
1
Motor Transport Institute, Warsaw, Poland
2
Institute of Microelectronics and Optoelectronics, Warsaw University of Technology, Warsaw, Poland
Titanium alloys are the materials characterized by a combination of such properties as low density and an advantageous ratio
of mechanical strength to yield strength. They are also highly resistant to corrosion processes in an aqueous environment and,
compared to other metallic materials, are characterized by the best biocompatibility. These features allowed the use of titanium
alloys as a construction material in many applications, such as chemical and petrochemical industry, automotive industry, as well
as biomedical applications - implants. Titanium belongs to a highly reactive group of materials having a very negative normal
potential amounting to E0 = -1.63 VNHE. A negative normal potential also reflects a high affinity of titanium for oxygen and the
creation of a stable and passive oxide layer on the metal surface, closely adhering to the substrate. However, in the environment
of acidic pH (pH ca. 2) the protective layer is unstable and the processes of corrosion of metallic Ti or its alloys are initiated. This
phenomenon is accelerated in the presence of aggressive ions such as fluoride ions. There are many technologies and methods
of surface modification to increase the corrosion resistance of titanium and its alloys. Among them are the plasma methods (e.g.
28
Plasma Enhanced Chemical Vapor Deposition process - PECVD) and magnetron methods (magnetron sputtering). These methods
allow the thin layers to be generated with high corrosion resistance. The paper focuses on the comparative studies of corrosion
and mechanical behaviour of Ti6Al4V titanium alloy after deposition of protective nanocoatings: TiN, SiN and graphene. The tests
were done by means of voltametric measurements in a fluoride solution and in SBF environment. Surfaces of the coatings were
characterized using nanoindentation measurements and atomic force microscope and Raman microscopy.
Poster-5 Comparison of Structural, Mechanical and Corrosion Properties of Thin Graphene/TiO2 Hybrid Systems Formed
on Ti-Al-V Alloy in Biomedical Applications
M. Kalisz1, M. Grobelny1, M. Mazur2, D. Wojcieszak2, M. Dominik1,4, M. Świniarski3, J. Domaradzki2, D. Kaczmarek2
1
Motor Transport Institute, Centre for Material Testing and Mechatronics, Warsaw, Poland
2
Faculty of Microsystem Electronics and Photonics, Wroclaw University of Technology, Wroclaw, Poland
3
Faculty of Physics, Warsaw University of Technology, Warsaw, Poland
4
Institute of Microelectronics and Optoelectronics, Warsaw University of Technology, Warsaw, Poland
Titanium and titanium alloys are widely used in a variety of engineering applications, where the combination of mechanical and
chemical properties is of crucial importance. Aerospace, chemical and automotive industries as well as medical device manufacturers also benefited from the outstanding properties of titanium alloys. Even though titanium alloys exhibit high strength and
toughness, in some environments they are susceptible to chemical and electrochemical degradation. They may corrode and wear,
leading to the degradation of material properties. In order to improve the mechanical and electrochemical properties of titanium
alloys surface, surface modification is often required. TiO2 has been investigated for several years as a possible candidate for a
wear resistant and corrosion barrier coating. Properties of titanium oxide depend on the deposition process and its parameters.
In this study, we have developed two types of coating systems on titanium alloys surfaces: TiO2/Ti-Al-V and graphene/TiO2/Ti-Al-V.
TiO2 thin films were prepared using two types of reactive magnetron sputtering process: pulsed and constant. The structural and
chemical composition of obtained coating systems, were analyzed using Raman spectroscopy, scanning electron microscopy and
spectroscopic elipsometry. The hardness of the obtained coating systems was analyzed using a nanoindenter. The anticorrosion
properties of the coating were done by means of voltametric measurements.
Poster-6 Characterization and Study of Gas Barrier Property Using PECVD of Silicon Nitride Film by Radio Frequency
(40MHz) Plasmas at Low Temperature
J.S. Lee, K.S. Shin, S.B. Jin, J.G. Han
Center for Advanced Plasma Surface Technology, Sungkyunkwan University, Suwon, Korea
Silicon nitride (SiNx) has important applications in many devices such as optical wave-guides, gate insulator in thin film transistors
and antireflection layer and barrier layer in photovoltaics and microelectronics. Accordingly, extensive investigations have been
carried out on the deposition processes and characteristics control of silicon nitride films by employing a variety of techniques
for over two decades. Additionally, stoichiometric silicon nitride has been prepared by direct nitridation of silicon, nitrogen ion
implantation into silicon or sputtering of silicon in nitrogen ambient or chemical vapor deposition at high temperature. Among
them, considering the damage of silicon surface during process, PECVD has great significance due to its low temperature
processing which can allow film fabrication on polymer substrates for applications like barrier coatings. Furthermore, PECVD at
higher RF excitation frequency can be beneficial in dissociating and exciting the radicals that play a crucial role in the growth
of the film over using 13.56 MHz. This paper aims at PECVD of SiNx films on polyethylene terephthalate (PET) substrates at
low temperatures (~60°C) environment by changing the process parameters, e.g., nitrogen flow rate and rf power at 40 MHz.
Nitrogen gas and Hexamethyldisilazane (HMDSN) are used as the main precursors and argon as the carrier gas. Optical emission
spectroscopy (OES) employed to investigate radical generation and plasma characteristics. OES results show that N2 emission
intensities increase with an increasing power and nitrogen flow rate. On the basis of OES diagnostics, the favorable conditions are
optimized. The films are analyzed with FT-IR and UV-visible spectroscopy. The films have high qualities that WVTR as a single layer
with 200 nm thickness and transmittance is around 90% at 550 nm.
Poster-7 Square Wave or Sine Wave: Choice of Power Supply in MF Sputtering
M. Heintze1, S. Ulrich2,
1
TRUMPF Hüttinger GmbH + Co. KG, Freiburg, Germany
2
For the deposition of dielectric thin films, dual magnetron sputtering with medium frequency excitation (MF-DMS) is widely
established. The most obvious advantages of MF over DC excitation is the long term process stability without adverse effects of
an insulating coating on the anode and the reduced arcing due to self-extinction at polarity change of the MF power. Also, dense
films with fine grains are preferably obtained by MF sputtering due to the ion flux caused by the magnetic shielding at the anode.
29
For MF power supplies in industrial sputter coaters, two substantially different design approaches are available: (1) the resonant
output circuit leading essentially to a sine wave excitation and (2) bipolar pulsed excitation with an essentially rectangular output
waveform. Yet, little information is available on possible advantages of either power supply type for the process. In this paper we
aim to give a comprehensive overview of how the choice of power supply may affect the final process. Results are shown on the
influence of the output waveform and of the operating frequency on the ion flux and energy to the substrate. Available data on
how the coating properties are affected are presented.
Poster-8 Design and Testing of a Coating System to Extend the Use of Commodity Plastics in Engineering Applications
S. Carley, A. Neville, H. Zhao
Institute of Functional Surfaces (iFS), University of Leeds, Leeds, United Kingdom
Physical vapour deposition (PVD) and plasma enhanced chemical vapour deposition (PECVD) techniques have been used to
deposit thin films on commodity, engineering and specialty plastics for different purposes. Applications of which vary from
decorative coatings, optical filters/coatings, and more recently as gas permeation barriers for electronics manufacture. However,
due to the low adhesive characteristics of polymers and the inherent mechanical property mismatch between substrate and
coating, little is known about the characteristics of hard coatings when considered as a system in conjunction with soft, compliant
substrates. In this study, an industrial scale PECVD system was used to deposit DLC coatings on three plastics; ABS, PP and PTFE.
The substrate-coating systems were analysed using 90° peel and scratch tests to determine the effects of substrate plasma treatments prior to film deposition and the importance of including an adhesion interlayer. The mechanical properties of the coatings
were determined using nano-indentation and microhardness testing. Micro-scale hardness measurements show an increase in
surface hardness of up to 50% when a hard thin film has been deposited onto the plastic. However, the mechanical properties of
the relatively soft substrate limit the ability of the coating-substrate system to support a load.
Poster-9 Evaluating the Corrosion Behaviour of PVD Al-Based Coatings by Characterising the Relaxation Time of the Open
Circuit Potential in (AC)DC/AC Cyclic Tests
F. Indeir, A. Matthews, A. Leyland
Department of Materials Science and Engineering, University of Sheffield, Sheffield, United Kingdom
A recently developed (AC)DC/AC cyclic test method is used to evaluate the corrosion behaviour of PVD Al-based coatings. The
technique can induce relatively rapid coating degradation as the cathodic reactions at the coating/metal interface produce OHions and H2 gas. The (AC)DC/AC cyclic test steps involve characterising the coating properties using electrochemical impedance
spectroscopy (EIS), a DC cathodic potential step (this is applied for a given period of time to induce the electrochemical reactions
that cause coating damage) and a potential relaxation stage (when the open circuit potential (Eoc) is monitored over a given time
for the coating to reach a stable Eoc condition). This relaxation time defines when cathodic reactions stop and the processes such
as electrolyte/ion travel from the coating, pore formation, corrosion reactions and double layer stabilisation that were accelerated (by DC polarisation) reach the steady state. The analysis of Eoc during the (AC)DC/AC cyclic test involves the regression of
an expression describing the potential relaxation which includes two summed terms attributed to the end of cathodic reaction
and to expulsion of electrolyte ions from the coating. The new (AC)DC/AC test technique provides a rapid evaluation of corrosion
degradation behaviour of PVD AlCr(Ti) coatings in a shorter time (≤ 24hrs) than traditional EIS and SST tests (days or weeks). The
influence of applied DC was determined by subjecting constant voltages of -0.5V -1V, -1.5V and -2V to the PVD Al-based coating
relative to the stable Eoc value.
Poster-10 Co-Sputtered Bismuth Tungstate Coatings with Visible-Light Photocatalytic Activity
M. Ratova, G.T. West, P.J. Kelly
Surface Engineering Group, School of Engineering, Manchester Metropolitan University, Manchester, United Kingdom
Photocatalysis is a promising method of air and water decontamination and surface cleaning/sterilisation. Titanium dioxide, or
titania, is the most widely used photocatalyst because of its stability, non-toxicity and low cost. However, titania exhibits low
quantum efficiency due to fast recombination of photogenerated charge carriers. Furthermore, due to its relatively high band gap
value, it requires UV irradiation for activation. Consequently, there is a need for new solar-light activated photocatalytic materials
with high quantum efficiency and bismuth tungstate films are potential candidates. These coatings were deposited, for the first
time, by reactive pulsed DC magnetron co-sputtering onto soda-lime glass substrates. Varying the power delivered to the bismuth
and tungsten targets allowed control over the Bi/W ratio in the coatings, and therefore the structural and optical properties of
the coatings. As-deposited coatings were characterised with amorphous microstructures and were annealed at 673K to develop
crystallinity. The visible light photocatalytic activity of the coatings, analysed using the methylene blue degradation test, was
found to be superior to that of a commercial titania-based photocatalytic product.
30
Poster-11 High Speed, High Resolution Coating Inspection
T.A Potts
Dark Field Technologies Inc., Orange, CT
The ability to inspect coatings, at high speed and high resolution has been a long-standing industry need. Coating and post-coating operations can exceed 100m./min. and defects of 10µm – 100µm must be detected. This is not possible for human inspectors.
Process upsets often go undetected, reducing yield. As coating occurs on one side of the film or glass, stable and reliable reflection
inspection is required. The inability of conventional inspection systems to reliably operate in a production environment in reflection has frustrated the industry; missed defects and false hits plague these systems. Solid State Laser Reflection (SSLR) technology
solves these problems. Line scan cameras and solid state lasers are married together inside a single scan unit for the first time. This
scanner is easily installed even in the tightest locations. All active modules are in a single unit, located on one side of the film or
glass. In addition, SSLR is self-aligning, operates in ambient light and requires no maintenance. System theory will be explained
and a number of application examples and results will be presented.
Poster-12 Consequences of Roll-Barrier Contact in Roll-to-Roll Processing of a Permeation Barrier
H. Klumbies1, S. Kreher1, J. Fahlteich2, F. Nehm3, L. Mueller-Meskamp3, P. Schlott1, S. Van Eek1, T. Winkler1
1
FHR Anlagenbau GmbH, Ottendorf-Okrilla, Germany
2
3
Institut fuer Angewandte Photophysik, TU Dresden, Dresden, Germany
Flexible organic devices like organic light emitting diodes or organic solar cells require ultra-high barrier films to protect them
from ambient moisture. The usual configuration of such a barrier film is a polymer web coated with one or more inorganic layers.
While for a new barrier film concept the inorganic layer deposition can be done in a sheet to sheet process, roll to roll coating is
mandatory when it comes to the pilot or the production scale. One of the issues coming up with this upscaling is physical contact
of the barrier layer to other objects like rolls or the polymer web when being rolled up. Reducing or even avoiding these contacts
leads to more expensive coater designs. To avoid unnecessary costs, such design limitations should be introduced only when their
importance for the barrier quality has been proven. In this study, we systematically evaluate the consequences of physical contact
between barrier layers and rolls using calcium corrosion tests to render the mechanically introduced damages visible and quantify
their influence on the water vapor transmission rate of the barrier.
Poster-13 Aluminium Oxide Barrier Layers and their Conversion for Packaging Applications
C. Struller1,2, P. Kelly1, N. Copeland2, V. Tobin3, H. Assender3, C. Holliday4, S. Read4
1
Surface Engineering Group, Manchester Metropolitan University, Manchester, United Kingdom
2
Bobst Manchester Ltd., Heywood, United Kingdom
3
Department of Materials, University of Oxford, Oxford, United Kingdom
4
Innovia Films Ltd., Wigton, United Kingdom
Inorganic transparent barrier layers, such as aluminium oxide coatings deposited onto polymer films, have been drawing attention in recent years and have emerged as an attractive candidate for flexible food packaging materials. For this application,
barrier properties against water vapour and oxygen are critical in order to ensure shelf life and meet consumer expectations.
Aluminium oxide coatings not only provide barrier properties, but also only require a thickness in the nanometre range. These
ceramic barrier coatings are now being produced via industrial high speed vacuum deposition techniques. Nevertheless, the
coated polymer films need to be further converted for their final packaging application, e.g. via slitting, printing and lamination.
These downstream process steps can pose a risk of stress or damage to the thin barrier layer. This study reports on the deposition
of aluminium oxide layers via reactive thermal evaporation of aluminium, as well as their conversion via lamination and slitting.
Additionally, acrylate flash evaporation layers were explored, as a topcoat applied in order to protect the coating for conversion
purposes and also as an undercoat in order to modify and enhance the substrate surface. The barrier performance before and
after these process steps was investigated as well as surface topography.
Poster-14 Optical Damage Performance of Widegap Semiconductor Transparent Electrodes
S. Elhadj1, J. Bude1, J. Adams1, M. Menor2, J.H. Yoo1, T. Olson1, J. Lee1, A. Samanta3, C. Stolz2
1
Materials Science Division, Lawrence Livermore National Laboratory, Livermore, CA
2
Laser Systems Engineering, Lawrence Livermore National Laboratory, Livermore, CA
3
Lawrence Livermore National Laboratory, Physics Division, Livermore, CA
In this study we seek to describe how transparent conductive electrode properties such as microstructures, defects, conductivity,
and carrier mobility contribute to optical damage performance in high power laser applications, and how these parameters relate
to specific materials, fabrication processes, and to enhanced laser annealing. Specifically, our initial focus is on ITO and doped
31
ZnO thin films on fused silica substrates exposed to a nanoseconds pulsed laser at 1064 nm wavelength. Similar results on other
widegap semiconductors are also described. We use large aperture, high power optical damage tests techniques on exit surfaces
to probe optical damage mechanisms up to 20 J/cm2 characterized by microscopy. In turn, microstructural and electrical thin film
measurements are related to the apparent optical damage mechanisms and properties of the films. In general, we find that 1)
the optical damage performance is strongly dependent on the number of test cycles performed, affecting lifetime performance,
and 2) evidence that suggests the presence of single defects in amorphous ITO films, which will be discussed. The optical damage
performance can be affected by pre-exposure laser processing of the films under controlled conditions to minimize precursor
related damage events.
Poster-15 Flash Lamp Annealing of Large Area Substrates via Stitching of Exposure Fields
H. Gross, G. Haasemann, O. Khvostikova
Rapid thermal processing using flash lamps has been well established in the production of silicon wafers and shows great potential for other applications like low-E or TCO films. The technology saves energy and floor space compared to thermal treatment in
a furnace. For processing of large area substrates, the flash lamp module size must be tailored to suit customer demands. For example, treatment of jumbo-size architectural glasses with a single flash would require a lamp array of enormous size at excessive
investment costs. However, annealing of large area substrates can be performed with a flash lamp array of a smaller size compared
to the substrate area when exposure fields are stitched together by a relative movement of substrate or lamp array. This poster
presents experimental results of rapid thermal treatment of large area low-E and TCO films by an industrial R&D tool. Technological
requirements for homogeneous flash lamp annealing using stitching of exposure fields and a comparison of experimental results
with optical simulations are shown.
Poster-16 Influence of Sputtering Atmosphere on Crystal Quality and Electrical Properties of Zirconium Aluminum Nitride
Thin Films
G. Ke1, Y. Tao1, Z. He1, Y. Bian1, Y. Chen1, J. DiBattista2, E. Chan2 and Y. Yang2
1
Department of Electronic Information Materials, School of Materials Science and Engineering, Shanghai University, Shanghai,
China
2
Darly Photonics Composite Materials (Shanghai) Corp., Shanghai, China
Zirconium aluminum nitride thin films (Zr0.11Al0.89N) were prepared on quartz glass substrates using DC reactive magnetron co-sputtering with an unbalanced magnetic field. The influence of sputtering atmosphere was investigated with respect to N2/Ar-flow ratio
and their total pressure, on crystalline structure and the electrical properties of resultant Zr0.11Al0.89N films. It was determined that the
optimal value of N2/Ar-flow ratio and their total pressure are: 1:1 and 0.6 Pa respectively. The results show that Zr0.11Al0.89N films have a
c-axis preferred oriented wurtzite structure with larger grain size compared to that with suboptimal condition. The dielectric constant
and resistivity of Zr0.11Al0.89N film reach a maximum of ~16 in a frequency range of 103~106 Hz and 3.88×1011 Ω·cm, respectively, which
are all superior to that with suboptimal condition. In addition, the dielectric loss of the Zr0.11Al0.89N film tends to 0.01 in the frequency
range, much lower than that with suboptimal condition. In summary the Zr0.11Al0.89N film deposited using optimized conditions
exhibit higher values for resistivity and dielectric constant and much lower dielectric loss when compared to pure AlN films.
Poster-17 PVD Modules for Predeposition RF Plasma Etch and AC Reactive Sputtering of Piezoelectric AlN Thin Films for
Electroacoustic Devices
V. V. Felmetsger
OEM Group Inc., Gilbert, AZ
Maximal piezoelectric response and low acoustic losses can be achieved in polycrystalline AlN thin films when they exhibit a
columnar microstructure with the majority of the grains precisely oriented in the (0002) crystallographic direction perpendicular
to the substrate surface. Since in a variety of modern electroacoustic devices, such as FBAR, SMR, and Piezo MEMS, a piezoelectric
AlN film is prevalently deposited on a metal bottom electrode, success criteria to achieve strong preferred orientation in AlN involve
the formation of a highly textured bottom electrode with an atomically smooth surface as well as the delivery of sufficient kinetic
energy to the adatoms reaching the growing AlN film surface. The most effective PVD technology satisfying these criteria consists of
predeposition etching of a substrate in Ar plasma, deposition of an ultrathin AlN seed layer to enhance the oriented crystallization
of the subsequently deposited metal electrode, and reactive sputtering of the AlN piezoelectric film using the highly ionized plasma
of an ac powered S-gun magnetron. In this presentation, we describe the design features and operation of a planarized capacitively
coupled rf (13.56 MHz) plasma source and a dual-cathode S-gun magnetron for ac (40 kHz) reactive sputtering. We investigate
the effects of non-reactive rf plasma etching and sputter conditions on Si wafer surface morphology and crystal orientation of the
bottom electrode and subsequently deposited AlN films.
32
Poster-18 Comparison of the Large-Area Reactive Sputter Processes of ZnO:Al and ITO Using Industrial Size Rotatable
Targets
V. Linss
The most commonly sputtered transparent conductive oxide (TCO) materials are aluminium doped zinc oxide (ZnO:Al) and
indium tin oxide (ITO). The deposition of these TCO materials is complex as it involves optimizing conductivity, transparency, and
thickness over a large substrate area. Although compound ceramic sputter targets are the standard in industry, exploring reactive
sputtering from metallic targets is interesting in that it may substantially reduce the target cost. This paper compares the reactive
sputter deposition of ZnO:Al and ITO from an industrial scale rotatable single magnetron (RSM) with a tube length of 1.7 m. It will
be shown that both processes are very distinct and thus very different control mechanisms have to be chosen in order to control
the working point of the reactive process. Whereas the global working point of the reactive ZnO:Al process can be controlled
by parameters of the power supply only, this is not possible for the reactive ITO process. Here, the partial pressures or optical
emissions have to be controlled as well. Suitable tools for the basic characterization of the reactive processes are the well-known
hysteresis and voltage-current characteristics at different reactive gas flows.
Poster-19 Linear Scanning Magnetron Array – Providing Deposition Uniformity with Improved Efficiency
A. Riposan, D. Brown, V. Kudriavtsev, C. Smith, T. Bluck
Intevac, Santa Clara, CA
High productivity vacuum PVD system cost of ownership is very sensitive to sputtering target utilization. In this paper we discuss
linear scanning magnetic array (LSMA), and the process design methodology which is required to achieve excellent plasma
confinement. In turn, this can lead to most uniform film deposition and best possible planar target erosion profile. The optimization method we use employs a combination of theoretical simulations and experimental measurements. Target utilizations above
60%, and lead-to-trail deposition uniformity below 2% were achieved.
Poster-20 Fast Digital-Controlled Multi-Step Process of Ultra-Smooth Diamond-Like Carbon Thin Films
J. Xie, J. Cho, P. Leahey, T. Bluck, A. Zanetto
Intevac Inc., Santa Clara, CA
Hard disk drives play a vital role in the Information Age by packing trillions of bytes of digital data in compact recording devices
which consist, in part, of magnetic recording layers. An ultra-thin layer of microscopically smooth diamond-like carbon thin film
is the main defense that protects the magnetic recording film stack from oxidation. To improve the diamond-like carbon film
properties so as to facilitate gains in recording density, digital-controlled plasma processing technologies are implemented for
a wide range of pulsing frequency and duty ratio of delivered power to achieve greater ionization efficiency of the hydrocarbon
gas precursors. Responsive digital control enables pre- or post-processing steps being integrated in the same chamber along with
the diamond-like carbon process. Advanced features such as arc monitoring and suppression ensure process stability and repeatability in high throughput production environment. This presentation will provide an overview of the digital control technologies
as well as the enhanced properties of diamond-like carbon thin films.
Poster-21 TiCxNy Thin Films for Decorative Applications Produced by Cathodic Arc Deposition
L. Milschi1, I. Belahsen1,3, G. C. Lain2, E.R. Petry1, F. Cemin1, J. Catafesta1, C.A. Figueroa1,2
1
Centro de Ciências Exatas e Tecnologia, Universidade de Caxias do Sul, Caxias do Sul-RS, Brazil
2
Plasmar Tecnologia Ltda., Caxias do Sul-RS, Brazil
3
Ecole Européenne d’Ingénieurs en Génie des Matériaux, Nancy, France
Thin film deposition can modify the material properties. The material surface can improve the wear resistance (tribological property) or change the resistivity (electrical property). Moreover, these thin films have different colors that are interesting for decorative applications. The Carbonitride Titanium (TiCxNy) thin films are known to improve the wear resistance, contributing to increase
the useful life of industrial tools. TiCxNy films have been drawing attention of the industry due to the yellow-gold color that the film
presents, been applied mainly in metals and glasses for decorative purposes. The color and other properties depend on deposition parameters and stoichiometry of the produced films. In this sense, the objective of this work is to investigate the color change
of the TiCxNy hard films produced by cathodic arc deposition, modifying the flow rate of N2 and CH4 in the deposition process. The
samples were analyzed by X-ray diffraction, scanning electron microscopy, glow discharge optical emissions spectroscopy and
nanohardness. The X-ray pattern diffractions indicate fcc structure with preferential orientation for (111) plane. The hardness of the
films has not changed significantly with different concentrations of nitrogen and carbon. The increased concentration of carbon in
the films produced samples with colors ranging from a yellow-gold to brownish-yellow.
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Poster-22 Antibacterial Response of Structures Consisting of Silver Nanoparticle Coated and Ampicillin Incorporated
Polymer Nanofibers
H. Cortez1, R. Reyna1, D. Mihut2, K. Lozano1, L. Materon3
1
Mechanical Engineering Department, The University of Texas Pan American, Edinburg, TX
2
Mechanical Engineering Department, Mercer University, Macon, GA
3
Biology Department, The University of Texas Pan American, Edinburg, TX
The research is investigating the antibacterial effect of different types of polymer nanofiber structures obtained as membranes.
The forcespinning method was used to create nonwoven polymer nanofibers by incorporating ampicillin sodium salt in the
polymer solution prior to the forcespinning process. Additionally, the nanofiber polymer structures were coated with silver
nanoparticles via DC magnetron sputtering deposition. The structures were investigated using the scanning electron microscopy,
X-ray diffraction and atomic force microscopy. The antibacterial properties of the membranes consisting of polymer nanofibers
based structures were tested following the protocol against different types of bacteria (e.g. Staphylococcus aureus and Escherichia
coli).
Poster-23 PECVD Fabricated Novel Boron Carbide/Aromatic Composite Materials for Neutron Voltaic and Device
Applications
B. Dong1, R. James1, E. Echeverria2, M.S. Driver1, P.A. Dowben2 and J.A. Kelber1
1
Department of Chemistry, University of North Texas, Denton, TX
2
Department of Physics and Astronomy, The Nebraska Center for Materials and Nanoscience, University of Nebraska, Lincoln, NE
Boron carbide based materials have many applications ranging from neutron detection, spintronics, neutronvoltaics and photocatalysis. However, these materials are poor conductors and exhibit short electron-hole separation (EHS) life times, which limits
their applications in neutron detection and photo-catalysis. To enhance the EHS and conductivity of the boron carbide based
semiconductors, novel films were fabricated by co-deposition of aromatic compounds (pyridine, diaminobenzene, pyridine,
pyrimidine, etc.) with ortho-carborane using plasma enhanced chemical vapor deposition (PECVD). Chemical bonding of the
PECVD films was studied using x-ray photoelectron spectroscopy (XPS) and FTIR. The increase in B (1s) binding energy and the
presence of multiple features in the N (1s) spectrum indicates that the N atom in the aromatic ring is bonded to the icosahedral B
atom. Ultra-violet photoelectron spectroscopy (UPS) indicates that the electronic structure of the composite films can be tuned by
varying the aromatic precursors. The states near the top of valence band is derived from aromatic units, implying that the states
near the bottom of conduction band are associated with ortho-carborane. The alteration in the electronic structure results in the
enhanced EHS and conductivity of boron carbide based polymers. These novel composite materials derived from ortho-carborane
and pyridine exhibited excellent heterostructure diode characteristics and improved neutron detection efficiency even under zero
bias.
Poster-24 The New Evaporation System for Steel Strip Coating
K.H. Nam, T.Y. Kim, Y.H. Jung
POSCO Technical Research Laboratories, Gwangyang-si, South Korea
Many kinds of evaporation systems for wide steel strip coating have been developed to obtain the cost effective coating by means
of high rate deposition. Jet PVD, especially, is emerging as a very efficient method for Zn and Mg coating on steel strip. However,
the coating speed of Jet PVD is lower than that of conventional galvanizing line, and Zn-Mg alloy coating with one evaporator
is impossible. For the achievement of Zn-Mg alloy coating with high deposition rate on 1.5m wide steel strip, we are developing
a new evaporation system which consist of an electromagnetic levitation heating unit, vapor guide unit, vapor injection nozzle,
etc. In this paper, the schematic diagram including a specification of the new evaporator will be presented. We will also report the
performance of this system and control method of coating speed as well as width.
Poster-25 Thermoelectric Properties and Film Morphology of Si/SiC Thin-Film Amorphous Multilayers Grown by Ion Beam
Sputtering
C. Cramer1, C. Farnell1, C. Farnell1, R. Geiss2, and J.D. Williams1
1
Department of Mechanical Engineering, Colorado State University, Fort Collins, CO
2
Department of Chemistry, Colorado State University, Fort Collins, CO
Multilayers (MLs) of 31 bi-layers with 10 nm layer thickness of Si/SiC were deposited on silicon, quartz, and mullite substrates
using a high-speed, ion-beam sputter deposition process. The samples deposited on silicon substrate were used for imaging
purposes and structure verification as they did not prove to allow for accurate measurements of the material. Seebeck coefficient
and electrical resistivity are reported as a function of temperature and used to compare film performance on mullite and quartz
substrates. Thermal conductivity was measured for one sample and used to find the figure of merit for all samples tested. X-ray
34
diffraction (XRD) spectra show the amorphous nature of the films. Scanning electron microscopy (SEM) and transmission electron
microscopy (TEM) are presented that document film morphology. The mobility of the multilayer films was measured using a Hall
measurement system. Samples were measured three times over the temperature range from 300 K to 900 K to document the
changes in the films with temperature cycling. The highest mobility of the MLs was 1.0 cm2/Vs. The highest Seebeck ever recorded
for a Si/SiC multilayer systems is observed at 870 K to be -2600 µV/K. The highest figure of merit, zT, for the multilayers in this
study was 0.08 at 870 K.
Poster-26 Sputter Deposition of High Density Diamond-Like-Carbon for Scratch Protection of Touch Panel Cover Glass
D.W. Brown
Intevac, Inc., Santa Clara, CA
High Density DLC Coatings, >2.6 g/cm2, have been achieved with carbon target sputtering processes using unique source design
and non-standard target/substrate geometries. Initially designed and tested for the deposition of the carbon overcoat on computer hard disks, optimized variations of these coatings deposited with scaled-up sources are now being implemented on touch
panel cover glass for scratch protection. Effects on material properties of target-to-substrate geometry, reactive gas addition, and
magnetic plasma confinement will be presented.
Poster-28 Full Face Erosion Planar Cathodes as a Low Cost “Cylindrical Rotatable” R&D Tool
A. Vetushka1, D. Monaghan1, V. Bellido-Gonzalez1, R. Brown1, A. Azzopardi1, H. Li1, F. Papa2
1
Gencoa Ltd., Liverpool, United Kingdom
2
Gencoa in USA, Davis, CA
The industrial field of magnetron sputtering has been seeing a rapid transition from large area planar to large area rotatable cathodes. Most of the R&D labs however have remained with equipment that would require a large investment in order to implement
relevant rotatable cathode technology. In many cases the downsizing on cathode diameter and cathode length has large implications in the relevance of the research itself. In addition the R&D lab finds it very difficult to justify the large target consumable bill
associated with the rotatable cathode targets. In order to facilitate a suitable and relevant research which could be applied to
rotatable technology this paper will present the use of circular magnetron sources with rotating plasma which can simulate some
of the benefits of the rotatable cylindrical cathode technology, such as a clean target and the ability to maintain clean anode in a
dual cathode sputtering. The present paper will present the development of one of these tools. The sputtering of ITO target has
been chosen as comparative example between the planar and cylindrical target technology. Results will be presented.
Poster-29 Comparison of Aluminum Zinc Oxide and Indium Tin Oxide for Transparent Conductive Oxide Layer in Liquid
Crystal Display Devices
L. Weng1, A. Varanytsia1, T.-C. Lin1, J. Yang2, D. Rooney2, R. McGinnis2, L. Shunk2, L.-C. Chien1
1
Liquid Crystal Institute, Chemical Physics Interdisciplinary Program, Kent State University, Kent, OH
2
SCI Engineered Materials, Columbus, OH
Facing the ever-growing scarcity of indium, aluminum zinc oxide (AZO) has been proposed as a substitute for indium tin oxide
(ITO), which is currently widely used in liquid crystal display products. In this study, the optical and electrical performance of AZO
and ITO as transparent conductive oxide (TCO) is compared, and AZO’s viability in Twist-Nematic liquid crystal displays is demonstrated. The target is to minimize AZO’s electrical resistivity, to maximize the transparency and to adjust the etching process in
a way that fine structures of a few microns could be produced. Aluminum Zinc Oxide layer is found to have comparable performance in transparency and conductivity as indium tin oxide layer judging from the measurement results of transmission spectrum
(78%-82%) and sheet resistance (80-120 Ohms/square). The electro-optical performance including transmittance-voltage curve
and response times of fabricated TN LC cells shows negligible variation. It is with great potential that AZO based substrates can
replace the ITO substrate in liquid crystal display devices while keeping an overall same high performance. Finally, it is notable
that the manufacturing process of AZO layer should be further studied for high resolution displays based on AZO based transparent conductive materials.
Poster-30 Hydrophobic Coating of the Cover-Glass Surface by Using a Rotating Plasma Module
C.-H. Chang, K.-Y. Lin, K.-F. Lee, S.-C. Lin
Advance Machinery Technology Division, Industrial Technology Research Institute, Hsinchu, Taiwan
In this poster, a two-stage process combines plasma surface modification treatment and medicament spray coating was studied
for the hydrophobic surface coating of cover-glass for 3C electronic products. The plasma treatment was used to hydrophilicmodify the cover-glass surface in the first stage. The plasma module contains four plasma jets and a rotating mechanism to
produce a uniform plasma ring. Therefore, plasma treatment can effectively enlarge the process area, and also significantly reduce
35
the process temperature. The effective range of plasma module is 4 inches, and after the plasma treatment process, the contact
angle with water is smaller than 10 degrees, which can improve the hydrophobic medicament adhesion property in the second
process stage. After thermal baking at 120˚C, the contact angle with water is larger than 115 degrees. The surface characteristic
after plasma treatment in different conditions will also be presented.
36
Wednesday Morning, April 29
8:30 a.m. K-3 Graphene Micro-Webs and Other Things: 3D Nanoscale Connectivity for Interconnected World
Invited Talk
K. Ostrikov1, 2
1
Commonwealth Scientific and Industrial Research Organization, Lindfield, Australia
2
Queensland University of Technology, Brisbane, Australia
Essential electronic, optical, and magneto-optical components of functional elements that will enable the “Internet of Things” are
expected to have several highly-unusual properties and features that will meet several requirements including excellent connectivity, ultra-fast responses, unprecedented data storage and processing capacity, controlled energy harvesting, generation,
storage and release, and several others. Here we consider thin films made of graphene micro-webs and other plasma-produced
nanomaterials and explore their unique three-dimensional webs and other arrangements that enable nanoscale connectivity,
energy storage, sensing and other functionalities that might potentially be of interest for the development of the “Internet of
Things”. Unique physical and chemical properties of these nanomaterials are discussed and related to the specifics of vacuum
coating technologies used to fabricate them. One unique and most recently discovered “thing,” coined graphene microwell,
can be inter-networked to form three-dimensional graphene micro-webs that enable excellent communication between the
vertical carbon nanowalls, underlying horizontal few-layer graphene sheets, and external networks. Several three-dimensional
micro-networks made of plasma grown and post-processed carbon nanotubes are also introduced. Non-equilibrium conditions
of low-temperature plasmas play a major role in the formation and shape, as well as structural, morphological features of various
plasma-made interconnected nano-“things” such as graphenes and other related nanocarbon materials. Examples also include
vertical, horizontal, and hybrid embodiments of graphene-like structures such as vertical graphene nanosheets, single- and fewlayer horizontal, substrate-supported graphenes, and other hybrid structures. The various “things” enabled by the plasma-specific
effects represent very interesting networked microscopic systems both for fundamental studies and advanced applications in the
Interconnected Age.
Coatings for Energy Conversion and Related Processes
9:20 a.m. EC-5 An Economic Analysis of Photovoltaics versus Traditional Energy Sources: Where are we Now and Where
Might we be in the Near Future?
Invited Talk
M. Woodhouse
National Renewable Energy Laboratory, Golden, CO
This presentation will show representative technology roadmaps for four photovoltaic technologies: wafer-based monocrystalline
silicon, polycrystalline single-junction cadmium telluride, single-junction gallium arsenide, and organic-based solar cells. The
cost modeling results for these roadmaps, expressed in dollars-per-watt, will then be shown, as will estimates of the resulting
levelized cost of electricity (LCOE), expressed in dollars-per-kilowatt hour. These PV LCOE estimates will then be compared to the
EIA’s current and projected LCOE estimates for electricity generation from the traditional sources—including coal, natural gas,
hydropower, and nuclear. Finally, the LCOE estimates will be translated to a dollars-per-gallon of gasoline equivalent, for the case
of electric vehicle charging with distributed residential and commercial PV systems.
10:00 a.m. EC-6 Atomic Layer Deposition for Interface Engineering in Dye Sensitized and Perovskite Solar Cells
V. Zardetto1, F. Di Giacomo2, T.M. Brown2, A. Di Carlo2, A. D’Epifanio3, S. Licoccia3, E. Kessels1, M. Creatore1
1
Department of Applied Physics, Eindhoven University of Technology, Eindhoven, The Netherlands
2
Centre for Hybrid and Organic Solar Energy (CHOSE), University of Rome - Tor Vergata, Rome, Italy
3
Department of Chemical Science and Technologies, University of Rome - Tor Vergata, Rome, Italy
Next to the synthesis and development of a.o. (thin) highly absorbing active layers and highly transparent and conductive
contacts, literature points out how essential it is to engineer the several interfaces present in a PV structure at nanoscale level,
in order to obtain higher power conversion efficiencies. An accurate control at interface level is also of utmost importance for
the most recent, low-cost PV technologies, dye-sensitized solar cells (DSCs) and organometal halide perovskite solar cells, where
nano- and meso-structured 3D interfaces are present. Atomic layer deposition (ALD) is a technique widely acknowledged for the
fact that it can fulfill the demands on accurate control of film (opto-chemical) properties and thickness often at the sub-nm level,
also in the field of PV technologies. In this contribution, we address the benefits of ALD when applied to meso-structured DSCs
and to the novel class of hybrid organometal halide perovskite solar cells. In both architectures, the deposition of thin ALD metal
37
oxides leads to the amelioration of the device photo-voltage and current by suppressing selected interfacial charge recombination processes. Specifically, ALD Al2O3 passivation layers on mesoporous structures and different compact blocking layers on TCOs
enable to suppress the charge recombination processes at the several complex interfaces within the device. Furthermore, another
example is reported, where ALD of Pt nanoparticles allows for efficient charge transfer processes at the interface between the
liquid electrolyte and a highly transparent counter electrode (CE) in a flexible DSC.
10:20 a.m. EC-7 Enhancement of Electrical and Optical Properties of Reactively Sputtered ITO Films by Flash Lamp
Annealing
C. David1, Y. Zhang1, P. Prunici1, B. Tinkham1, A. Panckow1, A. Kastner2, C. Simons2
1
Solayer GmbH, Kesselsdorf, Germany
2
Heraeus Materials Technology GmbH, Hanau, Germany
Thin ITO layers are commonly used in applications where highly conductive and transparent thin film systems are necessary for
large area applications such as displays, touch panels, electroluminescent devices, electrochromics, energy efficient window
systems and photovoltaics. At present the best ITO quality is attained with films deposited by means of magnetron sputtering
using ceramic targets. In this study the ITO layers deposited by reactive magnetron sputtering from a rotary indium-tin target are
evaluated. Reactive sputtering processes possess high potential for reducing production costs by employing low cost targets and
achieving high deposition rates; however attaining uniform large area coatings with this method is quite a challenge. Nevertheless, it has been demonstrated that the reactive ITO process can be successfully controlled when applied with process control
devices such as lambda probes and plasma emission spectroscopy. A promising approach to improve the properties of reactively
sputtered ITO films is the application of post-growth treatment by flash lamp annealing. This has been applied for ITO samples
that have been deposited at various temperatures. The greatest enhancement in both electrical and optical properties has been
observed for samples with the lowest initial transmission values.
11:00 a.m. EC-8 Commercialization of Large Area Dynamic Glazing
Invited Talk
S. Kailasam
View, Inc., Milpitas, CA
Electrochromic glazing offers the promise of significant energy savings and enhanced occupant comfort all while maintaining a
connection to the outdoors and preserving natural light. Despite these benefits, commercialization of this technology has proven
to be a challenge and few offerings exist on the market today. This presentation will review key areas in commercialization of large
area electrochromic glazing including achieving the required performance, ensuring durability in field operation, and scaling up
to large sizes (5’x10’) in order to serve a majority of the architectural glass market. Performance in electrochromic glazing is often
described in terms of dynamic range, switching speed, and quality of the viewable area. Electrochromic technology is generally believed to have the most potential of the chromogenic technologies due to the ability to have external control of visible
transmittance combined with a large dynamic range. A high quality viewable area is one that has full coloration to the perimeter
of the glazing with no distracting features. Durability is particularly challenging as many of the technologies being researched
today operate on the principle of absorption rather than reflection. The heat generated due to solar exposure combined with
UV radiation can result in unacceptable changes in performance over time. Proper selection of materials and product design
are paramount to ensuring long term durability in the field. Finally, scalability to large areas requires precise uniformity in film
thickness, microstructure and composition of the deposited coating. Equally important, it requires specific device characteristics
to enable complete switching across the viewable area without the use of additional bus bars in the viewable area. View, Inc. has
overcome these challenges and began shipping large area electrochromic glazing from its high volume manufacturing facility in
Olive Branch, MS in November of 2012. A number of case studies will be presented that demonstrate the value of electrochromic
glazing in both commercial and residential applications.
11:40 a.m. EC-9 Electrochromics and Thermochromics: Towards a New Paradigm for Energy Efficient Buildings
C.G Granqvist
The Ångström Laboratory, Uppsala University, Uppsala, Sweden
About forty percent of the World’s primary energy is used for heating, cooling, lighting and ventilating buildings. New nanotechnologies are able to decrease the use of energy significantly at the same time as the comfort and amenities of the building are
improved. This talk surveys a number of options, mostly based on work in the speaker’s laboratory. Foci lie on windows and glass
facades with electrochromic and thermochromic properties. Functional principles, thin film preparation and properties, new
plasmonic nanomaterials, and technological prospects are discussed.
38
12:00 p.m. EC-11 Investigation of the Effects of AR Stacks on the Structure, Optical and Mechanical Properties of
Transparent Conductive Oxide Thin Films
J. Liu, H. Wang
State Key Laboratory of Green Building Materials and National Research Center for Glass Processing, China Building Materials
Academy, Beijing, China
Transparent conductive oxides have a multitude of applications for solar energy utilization and for energy savings. Sn-doped
indium oxide (ITO) film with antireflective (AR) stacks were deposited on glass substrates by magnetron sputtering. Two kinds of
AR multilayer structures (triple-layer AR stacks: Air | SiO2 | ITO | Al2O3 | Glass, double-layer AR stacks: Air | SiO2 | ITO | Glass) and ITO
single layer were designed for comparison. The crystal structure, spectral properties from visible to infrared range, mechanical
properties including hardness, elastic modulus, and pull-off adhesion were systematically investigated for ITO film with and
without AR stacks. The results revealed that Al2O3 bottom AR layer helps to reduce the structural stress and increase the number of
oxygen vacancies in the ITO film deposited on it. And then, the optical transmittance in the range from 380nm to 1100nm, infrared
reflectance from 2.5 m and 48 µm, and hardness, elastic modulus, pull-off adhesion for ITO multilayer were improved. The good
performance of the triple-layer ITO AR stacks indicates that they are promising for low emissivity coated glass on architectural,
automotive glazing and solar thermal collectors.
Plasma Processing
9:20 a.m. P-6 A Novel Magnetron Sputtering ECR Ion Source - An Emerging Tool for the Production of High Current Metal
Ion Beams and Large Area Surface Processing
T. Weichsel1, U. Hartung1, T. Kopte1, M. Kreller2, A. Silze2, G. Zschornack3,4
1
2
DREEBIT GmbH, Grossroehrsdorf, Germany
3
Institute of Solid State Physics, Dresden University of Technology, Dresden, Germany
4
Institute of Ion Beam Physics and Materials Research, Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden, Germany
High current metal ion sources are utilized for large surface irradiation and implantation such as in the photovoltaics and semiconductor, medical or optical industries. For this purpose, a novel ion source prototype was developed, which combines magnetron
sputter technology with electron cyclotron resonance (ECR) ion source technology - a so called magnetron ECR ion source
(MECRIS). An integrated ring-shaped sputter magnetron with an Al target is acting as a metal atom source. It is able to supply a
metal atom load rate of at least 1E18 atoms/s for Al, which is necessary to produce a milliampere Al+- ion beam. For large area
processing, a new 30 keV-irradiation facility was developed to scan the ion beam over a target width of 200 mm. Spatially resolved
double Langmuir probe and optical emission spectroscopy measurements were used to study the modes of operation of the ion
source: sputter magnetron, ECRIS, and MECRIS plasma. Electron density and temperature as well as Al atom density were determined as a function of microwave power, sputter magnetron power, and magnetic field configuration. The presentation covers the
MECRIS and ion beam facility design as well as conclusions of plasma diagnostics and first ion extraction experiments. This work
was supported by the European Fund for Regional Development of the European Union and the Freistaat Sachsen under Grant
Nos. 100106678 and 100096350.
9:40 a.m. P-7 Aspects of RF Power on Rotary Cathodes
P. Morse, R. Lovro, T. Strait
Sputtering Components, Inc., Owatonna, MN
Articles in literature report the effects of a superposition of RF and DC power applied to ITO sputtering. Recently, this application,
in the context of rotary targets, has been reported. In the present article, the previous data is re-examined and new data is reported. In order to better characterize the usefulness of this processing technique, we combine optical and electrical characteristic
metrics into a merit function. Additionally, new data on uniformity concerns, which arise with the use of RF power, is presented.
This data indicates the limits of achievable uniformity using RF power on rotary cathodes.
10:00 a.m. P-8 Drift Waves in Magnetron Sputtering Plasmas
M. Siemers, A. Pflug, T. Melzig
High speed optical measurements revealed plasma drift waves as an inherent feature of magnetron sputtering plasmas. This holds
true not only for high power impulse magnetron sputtering (HiPIMS) but also for magnetron discharges at significantly lower
power densities. The latter allows for model based investigation of these drift waves using an in-house developed Particle-in-Cell
39
Monte Carlo (PIC-MC) simulation tool. The PIC-MC simulation lets us delve deeper into the origination of the drift waves as well
as their practical relevance in magnetron sputtering applications. Accordantly we will show some exemplary 3d3v simulations to
demonstrate the effect for different parameter settings. Experimental data will confirm the simulation results directly and indirectly regarding the drift waves’ effect on ion impact energy and sputter homogeneity.
11:00 a.m. P-9 Carboxyl-Rich Films Prepared by Maleic Anhydride – Acetylene Copolymerization Using Atmospheric
Pressure Dielectric Barrier Discharge
L. Zajickova1, A. Manakhov1, M. Michlicek1, M. Elias1, E. Makhneva1, J. Cechal2, D. Pavlinak1
1
Masaryk University, Brno, Czech Republic
2
Brno University of Technology, Czech Republic
Plasma polymerized carboxyl-rich films have been applied for adhesion promotion, bio-immobilization and cell colonization
thanks to their high reactivity towards nucleophilic groups. However, the majority of available data represents the polymerization of acrylic acid using low pressure plasma. The aim of this work is to present the stable carboxyl-rich coatings prepared by
atmospheric dielectric barrier discharge. DBD is a method of choice for a low cost, upscale ability and environmental friendliness. We have investigated the plasma co-polymerization of maleic anhydride and acetylene in the DBD. Thin films containing
anhydride and carboxyl groups were deposited on silicon wafers and PCL electrospun nanofibers. The DBD was characterized by
optical emission spectroscopy, while the surface chemistry and the morphology of the samples were studied by Fourier transform
infrared spectroscopy, X-ray photoelectron spectroscopy combined with chemical derivatization of COOH environment (CD-XPS)
and scanning electron microscopy (SEM). In adjusted condition the film exhibited more than 5 at.% of carboxyl groups estimated
by CD-XPS. Treatment also led to improved wettability of nanofibers, as the WCA decreased from 115 ± 2° to unmeasurable value
close to 0° (liquid soaked immediately into nanofibrous material).
11:20 a.m. P-10 Crystalline AZO Film Synthesis of High Conductivity at Low Temperature by Particle Energy Control with
Diagnostics in Remote Magnetron Sputtering
J.S. Lee, S.B. Jin, B.B. Sahu, J.B. Kim, M. Kumar, J.G. Han
Department of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon, Korea
Aluminum doped zinc oxide (AZO) thin films were prepared on polymer and glass substrates using a dual planar magnetron
sputtering system with facing magnetic fields in which the plasma is confined between the targets with ICP antenna arrangement. The magnetic field is varied between dual facing magnets. The substrate is placed outside the confined plasma region in an
off-axis position to prevent radiant heating from the heated target surface to the substrate and energetic particle bombardment.
In addition the off-axis position prevents bombardment by energetic sputtered particles which may damage to the polymer
substrate. The film is successfully synthesized without any damage to the polymer at temperatures less than 100 . The electrical
and optical properties of AZO film are investigated using a sheet resistance and UV-visible spectroscopy, respectively. In addition,
XRD analysis reveals that ICP antenna power affects the crystal orientation and microstructure of the AZO thin films. The sputtering gas composition is observed to be an important control factor to determine the structural properties of the AZO films. The film
structure changes with the plasma parameters as measured by optical emission spectroscopy. The grain size increases from 20.64
nm to 22.54 nm with increasing ICP antenna power, because the C-axis length is almost similar at the same film thickness. Oxygen
vacancies are supposed to donate two free electrons for conduction, but suitable oxygen deficient films show increasing optical
transmittance from 85% to 88%, and lower optical band gap from 3.78 to 3.82 eV. The transmittance of the films is controlled with
the optimization of ICP antenna power. The paper discusses the behavior of AZO film with various properties by controlling the
process parameters in confined magnetron sputtering discharge at low substrate temperatures i.e. less than 100 .
11:40 a.m. P-11 Hydrogen Radical Generation and Optimization in a Remote Plasma Source
S. Polak1, D. Carter1, A. Bhoj2, A. Roy2
1
Advanced Energy Industries, Fort Collins, CO
2
ESI US R&D Inc., Huntsville, AL
Recent studies evaluating a new, capacitively-coupled, VHF, remote plasma source have yielded improved understanding of
plasma characteristics and distribution, both within and downstream of the plasma generating device. Empirical data from Langmuir and IEDF probes can now be augmented by an evolving, simulation-based plasma model. Commercially available, multiphysics code allows for simultaneous calculation of electromagnetics, fluid flow, heat transfer, species chemistry and transport in
non-equilibrium discharges. Work to date has focused primarily on inert chemistries, but as the accuracy and validity of the model
has improved, the ability to predict more complex systems and phenomena has become possible. One of the more compelling
systems for study is hydrogen, due to its widespread use across numerous industrial applications. This paper reviews recent work
on the evaluation and characterization of the VHF source using both parametric simulations and empirical assessments. Based on
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the amalgamation of these results, a set of optimization criteria are determined for maximizing production of hydrogen radicals.
Since the device under review is intended for remote installation, additional attention is placed on conditions needed for optimizing delivery of desired species to a downstream work piece.
12:00 p.m. P-12 Controlling the Flux of Reactive Species in Electron Beam Generated Plasmas
S.G. Walton, D.R. Boris, S.C. Hernández, Tz.B. Petrova, and G.M. Petrov
Plasma Physics Division, U.S. Naval Research Laboratory, Washington, DC
Electron beam generated plasmas are characterized by high plasma densities (> 1010cm-3) and very low electron temperatures
(< 1 eV). This makes them well-suited for the treatment of very thin films (e.g. graphene) or atomic layer processing (etch or
deposition) techniques where high fluxes of low energy ions are desirable. In this work, we focus on controlling the flux of reactive
species incident to substrates located adjacent to magnetically collimated electron beam generated plasmas. In particular, we
discuss strategies for regulating both the type and energy of the ions at the substrate surface. We use a suite of diagnostics
including Langmuir and RF impedance probes along with a mass-resolved ion energy analyzer to show how various operating
parameters can be changed to control both the bulk plasma properties and the ion flux at the surface. This work is supported by
the Naval Research Laboratory Base Program.
Optical Coatings
9:20 a.m. O-1 Mixed Oxides for Optical Functional Coatings Prepared by Magnetron Sputtering
S. Bruns, T. Zickenrott, M. Vergöhl
Nowadays, optical coatings are specified by more than only reflectance and transmittance bands. Mechanical properties are the
focus of particular interest for antireflective coatings on consumer electronics like smartphones, tablet computers and watches.
The material characteristics of typically used oxides can be changed by the process parameters in magnetron sputtering processes
but naturally only within a small range. Sometimes the properties are contradicting, for example a material with a high hardness
and low refractive index. The combination can be achieved by the deposition of intermediate materials, mixtures from high
refractive and low refractive index oxide materials. We prepared different material combinations using two dual magnetrons with
cylindrical cathodes in a turntable deposition system including heating and additional plasma source. Besides single thin films,
layer stacks with mixed oxides will also be shown with respect to optical and mechanical properties.
9:40 a.m. O-2 Nanostructured ZnO Films Prepared by Hydro-Thermal Chemical Deposition and Microwave-Activated
Reactive Sputtering
Y. Alajlani1,2, C. Zhao1, S. Moh1, D. Gibson1, Y.Q. Fu1, F. Placido1
1
Thin Film Centre, Scottish Universities Physics Alliance (SUPA), University of the West of Scotland, Paisley, United Kingdom
2
Department of Physics, Jazan University, Jazan, Saudi Arabia
Nanostructured, highly porous, films of zinc oxide have been prepared by hydro-thermal chemical deposition (HCD) and by
microwave-activated and DC reactive sputtering (MARS) for applications in sensors and solar cells. SEM/EDX, XRD, Raman and
optical constant measurements are presented, demonstrating the pronounced effect of microwave power on the nanostructure of
films prepared by MARS and the marked differences between films grown by the two methods. While the structures obtained by
HCD are highly crystalline and grow as nano-rods, the MARS films are initially dense with subsequent increase in porosity, leading
to unusual conical structures with hemi-spherical caps.
10:00 a.m. O-3 Metrology of Optical Coatings: The R&T Direct Absorption Method for the Determination of Low
Absorption Levels in Dielectric Films
R. Vernhes, L. Martinu
Department of Engineering Physics, École Polytechnique de Montréal, Montréal, Canada
Assessing absorption in optical thin films can be challenging, especially when extinction coefficient values are in the range
of 10-4 or below. Although sophisticated techniques have been developed for such purpose over the years (laser calorimetry,
photoacoustic measurements), there is still a need for a simple, quick and low-cost method that would determine both the film
thickness and optical properties [n(λ), k(λ)] from a single measurement with a high level of accuracy. Thanks to recent advances in
UV-VIS-NIR spectrophotometers, in particular the possibility to perform multi-angle Reflection/Transmission measurements with a
single accessory, combined to an optimized measurement methodology, we show that it is possible to evaluate the film thickness
and refractive index from R/T measurements performed at low angle of incidence, while determining the extinction coefficient
down to 10-5 from R/T measurements carried out near the Brewster angle of the coating in p polarized light. We also demonstrate
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how modeling errors can be significantly reduced by fitting absorption spectra (A=1-R-T) rather than R and T separately. This new
methodology is exemplified for several practical cases displaying various degrees of complexity.
11:00 a.m. O-4 Infrared Spectroscopic Analysis of Thin Films
Invited Talk
H. Tompkins1,2,3
1
Consultant, Chandler, AZ
2
Physics Department, New Mexico State University, Las Cruces, NM
3
Physics Department, University of Missouri, Columbia, MO
In this presentation, we will consider using infrared radiation as a probe to analyze thin film materials. We will consider analysis
methods which use the intensity of the radiation (FTIR and IRAS) and methods which use the ellipsometric parameters Psi
and Delta (IR-VASE). Molecular vibrations and absorption bands will be discussed. In the mid-IR spectral region, many thin film
materials have both transparent regions and regions with absorption bands. We present several examples from transmission
and refection intensity methods. Spectroscopic ellipsometry in the IR region is then introduced and we give several examples of
substrates and thin films. We show how the absorption bands and the transparent regions can synergistically provide information
which is otherwise unavailable.
11:40 a.m. O-5 Imaging of Impurities and Imperfections, Micro- and Nanoscaled Pattern on Surfaces and in Films:
Microscopic Techniques vs. Ellipsometry
U. Beck, A. Hertwig, M. Sahre, M. Weise, J.M. Stockmann
BAM, Berlin, Germany
Surface engineering requires reliable quality control. Both the detection of impurities and the measurement of micro-/nanoscaled pattern are essential. Atomic force microscopy (AFM) has the advantage of both high vertical and lateral resolution.
However, a near-field technique is difficult to operate under robust environments. Optical microscopy (OM) makes use of normal
incidence in the physical far-field. Vertical resolution is related to focal length, lateral resolution limited by the diffraction. Imaging
ellipsometry (IE) makes use of oblique incidence in the technical far-field. Because of oblique incidence, IE is polarisation- sensitive and gives access to the electronic structure of materials. By means of a Scheimpflug-configuration the entire field-of-view
is analysed simultaneously, i.e. optical constants and layer thicknesses can be retrieved with a vertical resolution similar to AFM,
lateral comparable to OM at magnification 200. Near Brewster-angle and for p-polarised light at incidence, the clean substrate
does not contribute to the reflected signal. Hence, there is a huge contrast to impurities or pattern. It is shown that IE has a great
potential to identify impurities, to detect pattern and to measure thicknesses also on larger areas. Several application examples
are discussed in detail and compared for the different inspection techniques (AFM, OM, IE).
12:00 p.m. O-6 Finite-Difference Time-Domain Method for Data Analysis of Spectroscopic Ellipsometry
Y. Foo, J.A. Zapien
Center of Super Diamond and Advance Films (COSDAF) and Department of Physics and Material Science, City University of Hong
Kong, Hong Kong SAR, China
Variable Angle Spectroscopic Ellipsometry (VASE) data analysis using the finite-difference time-domain method (FDTD method)
could provide a general method to indirectly resolve the optical properties and structural information of structurally complex
samples, including periodic and non-periodic nanostructured thin films. Specifically, our results demonstrate extraction of
structural information from 1D periodic structures. In this contribution, we show the accuracy limit of this approach by calculating the SE response of both metallic and dielectric ideal thin films. We then demonstrate a practical multi-parameter broadband
optimization of the SE response from 1D periodic structure. This method requires a variable angle variable wavelength approach
in acquiring SE measurements as to overcome wide band frequency response limits in the FDTD method model. We address the
challenge of this approach by comparing different strategies in the selection of angle of incidence (AoI) and wavelength for both
SE measurement and FDTD method modeling. This FDTD–SE approach inherits the distinctive advantages of the FDTD method: (i)
calculation of spectral broadband results from a single simulation; (ii) sources of error are well understood (iii) potential to simulate arbitrary general subwavelength to nano-sized structures (iv) natural capacity as a time-domain technique to study complex
optical phenomena such as plasmonic and non-linear effects; and (v) ability to visualize field dynamics.
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Large Area Coatings
9:20 a.m. L-17 Holistic Approach of Plasma, Transport and Film Growth Simulation
T. Melzig1, A. Pflug1, M. Siemers1, S. Lucas2, P. Moskovkin2, A. Daniel3, M. Jupé4, M. Turowski4
1
2
Université de Namur, Namur, Belgium
3
Centre de Recherches Métallurgiques (CRM), Liège, Belgium
4
Laser Zentrum Hannover e.V. (LZH), Hannover, Germany
The virtual coater concept comprises the combination of plasma, transport and film growth simulation. This allows for process
development on a purely virtual bases and the substitution, at least partly, of costly experiments. The CAPRICe project is an
ambitious attempt to realize the virtual coater concept by combining Particle-in-Cell Monte Carlo (PIC-MC) plasma and transport
simulation with kinetic Monte Carlo (kMC) and Molecular Dynamic (MD) simulation of film growth. Within the scope of CAPRICe
most of the modeling results are validated by means of deposition experiments. As an example we present simulated properties
of metallic titanium films deposited on various substrate and coater geometries under different process conditions in comparison
with experimental results in order to demonstrate the applicability and quality of the holistic simulation approach.
9:40 a.m. L-18 Multi-Scale Mechanical Behaviour of Plasma Electrolytic Oxide (PEO) Coatings on Aluminium Alloys
A. Jarvis1, A. Yerokhin1, N. Schwarzer2
1
2
The mechanical behaviour of coatings in tribological and other contact applications depends on a specific length scale, ranging
from the nano through to the macro regime. Coating wear and/or failure depends on what scale this interaction takes place
at, from asperity interaction involving only the surface of the coating through to situations where the interface and substrate
characteristics dominate the behaviour. Plasma electrolytic oxide coatings (PEO) on an aluminum alloy were used to illustrate
this point. A series of instrumented hardness indentations ranging from nano through to macroscopic were made to provide a
range of mechanical contact length scales, and the results correlated to the coating tribological behaviour. The indentations and
corresponding wear tests were modeled by a contact mechanics approach using an analytical solution. This was used to explain
the various interactions.
10:00 a.m. L-19 Deposition of a Release Coatings via an RF Low Pressure Plasma Process and Comparison to the Plasma
Deposition at Atmospheric Pressure
K. Vissing, M. Ott, P. Bitomsky, U. Lommatzsch
Fraunhofer Institute for Manufacturing Technology and Advanced Materials IFAM, Bremen, Germany
Coatings that exhibit low adhesion on their surface can be used for easy-to-clean surfaces or for demolding applications. For
demolding applications a release coating allows to remove (demold) the fabricated part from the mold without the need for
additional release agents in the liquid state. Therefore the part can immediately further processed and no additional cleaning to
remove residuals from the release agent is necessary. A new and innovative process using a roll-to-roll process in a capacitively
coupled RF low pressure plasma is presented. The coating thickness can be up to several microns and is typically based on silicon
organic chemistry. The process not only allows to deposit a release coating directly inside a mold, but also on a polymeric film. The
film coating process allows for much higher flexibility in the application and reduces the coating cost dramatically. The deposition
process and results for the demolding of polyurethane components will be presented. In addition the coating properties and the
characteristics of the deposition process will be compared to an atmospheric plasma process.
10:20 a.m. L-7 Layer Stack Diversity for Different Substrates and Applications
C. Köckert, M. Berendt
The structure of a layer system can be defined primarily by its single-layer materials and their layer thicknesses. Using the example
of a triple low-E coating, it is shown in the present paper that the choice of the individual layer materials, the kind of manufacturing process and the required individual layer thicknesses crucially depend on the used substrate and the specific application.
Depending on the specific application there are different versions for one layer system fulfilling the same specification. For
example, non-controlled, fully reactive MF-processes from rotatable cathodes are widely used for architectural glass applications.
In the case of web coating the requirements with respect to UV radiation intensity, thermal load into the sensitive substrate, deposition rate and gas separation partly dictate other processes and materials. The optical and thermal properties of the layer stack
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for a coated single glass pane must be corrected for the application in an insulating glass unit by tuning the layer thicknesses of
relevant layers. When using the coating in a laminate instead of an insulating glass unit, the layer thicknesses must be corrected
again. The same applies to plastic webs. The optical properties of a single coated PET-substrate differ from the properties of the
same substrate laminated between two glass panes using PVB. The thickness of the individual layers need to be adjusted again in
order to meet the specification. Finally, depending on the type of substrate there are also different requirements with respect to
further processing of the coated substrate which also need to be solved differently.
Vendor Innovators Showcase
11:20 a.m. V-1 Remotely Adjustable Magnet Bar (RAM -Bar™) for In Situ Uniformity Adjustment
J. Schmeling, R. Lovro, P. Morse, M. Gallentine, T. Strait
Sputtering Components Inc., Owatonna, MN
Sputtering Components formally announces the release of its Remotely Adjustable Magnet Bar (RAM -Bar™) system to the North
America and European thin film coating markets. Since notifying the industry of its initial design work at last year’s SVC conference, SCI has made tremendous progress through internal R&D efforts and customer beta-site installations. Performance data
will be discussed proving the capability of achieving thin film uniformities of better than ± 1%. The RAM-Bar™ is designed to offer
system operators the ability to adjust the magnet array position, relative to the cathode surface, during the sputtering process.
The standard pitch of adjustment points on the magnet array is 300mm with adjustment capability up to 20mm. The RAM-Bar™
can operate in conjunction with any one of SCI’s standard magnetic arrays (TRM-Bar™, mQRM-Bar™, and QRM-Bar™) allowing for a
wide range of applications that require different magnetic strengths, sputter angles, target diameters, and material utilizations. It
is also used with the standard family of SCI End Blocks that offer low-cost and highly reliable operation.
11:30 a.m. V-2 Advancements in Sputtering Technology
D. Bingaman
Kurt J. Lesker Company, Jefferson Hills, PA
In this spotlight the Kurt J. Lesker Company will update the industry on some of its new thin film deposition solutions.
11:40 a.m. V-3 Ultrafast Arc Management for High Deposition Rates in Reactive Magnetron Sputtering
P. Wiedemuth, M. Heintze
HÜTTINGER Elektronik GmbH + Co. KG, Freiburg, Germany
High deposition rates, good process stability and excellent film quality are key factors in determining productivity of reactive magnetron sputtering processes. Although nowadays high-power magnetrons with efficient target cooling as well as power supplies
of up to about 200 kW are available, in practice this often cannot be utilized. The reason is increasing process instability that can
occur at high power densities. In particular high arc-rate and associated interruptions in the deposition process limit the operating
range and thus the average deposition rate which can be achieved. The paper presents the latest development results obtained
with respect to arc detection and arc treatment which are now available for industrial applications. The key factors are real time
monitoring and processing of electrical output parameters. New analysis methods enable reliable and extremely fast detection
and treatment of arcs and thus interrupting the process as little as possible. This is a prerequisite for achieving high deposition
rates in reactive magnetron sputtering.
11:50 a.m. V-4 Superimposed Pulse Power-Technology
G. Mark, M. Mark
MELEC GmbH, Baden, Germany
MELEC’s SIPP-Technology (Superimposed Pulse Power-Technology) using HiPIMS (High Power Impulse Magnetron Sputtering)
combined with DC, mid-frequency or radio frequency 13,56 MHz (bias) opens a new horizon in pulse plasma technology. The
development of MELEC’s pulse power controller continues and is focused on advanced technology to create new additional
features and advantages. This technology is applicable for: co-sputtering, unipolar and bipolar pulse pattern. Pulse patterns are
freely adjustable for both positive and negative pulse parameters through a graphic user-interface of the interactive software. The
highest deposition-rate will be reached by using HiPIMS combined with DC or mid-frequency. The SIPP-Technology prevents the
poisoning and reduces the arcing especially in the reactive mode.
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12:00 p.m. V-5 New Compact External Mount Rotary End Block for Small Systems and Higher Packing Density
S. Williams, D. Crowley, P. Morse, M. Rost, T. Strait
Sputtering Components Inc, Owatonna, MN
Sputtering Components, Inc. will introduce the most recent addition to the external mount end block line – the CM-Series end
block. This cathode combines high-performance and reliability with a compact, light-weight design. Weighing in at an average
weight of just 16kg, the CM-Series end block is designed to fit into smaller systems where planar cathodes have historically been
the preferred choice. The compact design of the CM-Series end block allows for higher packing density and the opportunity for
customers to switch between planars and external mount cathodes in the same position. The CM-Series end block integrates with
SCI’s TRM-Bar™, QRM-Bar™, or the mQRM-Bar™ magnetics, as well as our e-Cathode™ lid systems. SCI will present performance
data, including options for smaller ID targets and highlight features that are common to all SCI end blocks.
12:10 p.m. V-6 HS-Group – Your Source for High End Vacuum Coating Equipment and Service
W. Decker1, R. Hilberg2, K. Schafsteck2
1
Iacten Consulting, Beaver Falls, PA
2
HS-PlasmaTec, Hainburg, Germany
The recent merger of Hilberg Vakuumtechnik and Onlink Technologies provide you with a single source for your vacuum processing needs. Vacuum Coating Systems for: Inline Sputter, Web Coating, Decorative Coatings, Specialty Equipment. Coating
Components: Quatron High Energy Density Plasma Sources. Upgrade Services and Vacuum Parts. This presentation will provide
a rough overview of our portfolio as well as a detailed look at our newest web coating development utilizing inductively heated
evaporation sources for flexible web coating applications.
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Wednesday Afternoon, April 29
Vendor Innovators Showcase
1:50 p.m. V-7 CODE Software Generation 4 – Easy, Enhanced and Elegant Optical Thin Film Analysis and Design
W. Theiss
W.Theiss Hard- and Software, Aachen, Germany
Coatings for technical applications need optical characterization during research, design and production. Optical modeling is the
method of choice to understand and optimize thin film properties. Our CODE software combines excellent modeling capabilities
with very flexible graphical user interfaces. Version 4 is dedicated to simplify the necessary steps for good solutions. Unexperienced or occasional users are guided by a few mouse clicks to a satisfying solution of their problem. Power users get advanced
tools to organize their work and to built up their own network of thin film solutions. Simple and advanced applications of CODE
are shown in a live demonstration of the software.
2:00 p.m. V-8 Banded Wavelength Ellipsometry for Thin Film Characterization
B. Johs
Film Sense, Lincoln, NE
Ellipsometry is a well known optical technique for measuring the thickness and index of refraction of thin films. Ellipsometry is
especially useful for determining the thickness of ultra thin films (<10 nm) and for determining the optical constants of materials.
However, the cost and complexity of traditional ellipsometer systems can be limiting factors for many applications. The Film Sense
FS-1 Banded Wavelength Ellipsometer provides an affordable option for many thin film measurements. The FS 1 incorporates
a novel 4 LED light source (that never needs replacement or alignment), and a no-moving-parts ellipsometric detector (for fast
measurements and long term reliability). The ease of use makes the FS-1 ideal for routine thin film measurements in the lab or
production floor, and its compact size makes the FS-1 ideal for integration with thin film deposition chambers. In this talk, a brief
introduction to ellipsometry will be presented first, followed by a discussion of advantages and applications of the FS-1.
2:10 p.m. V-9 Increasing Vacuum Tool Throughput and Process Yield: The Importance of Thermal Performance when
Selecting a Cryochiller for Optimal High-Speed Water Vapor Pumping
C. Rebecchi
Brooks Automation, Inc., Fremont, CA
Water vapor is the primary reason for slow pumpdown in high vacuum systems. Water vapor and dissociated oxygen are also generally unwanted vacuum process contaminants that can both physically and chemically affect product quality and yield. High-speed
water vapor pumping is critical in large-scale commercial vacuum processes, where the highest possible tool throughput, product
quality and process repeatability are all considered necessary. Installing a large cryosurface directly inside the vacuum process chamber is often the most effective method to increase the overall water vapor pumping speed in a high vacuum system. A cryochiller for
applications inside vacuum process chambers should be able to quickly cool and defrost cryosurfaces, thus eliminating the need for
high vacuum valves or ports that limit vacuum conductance. This presentation will demonstrate why low temperature performance
and cryosurface area are two key parameters to consider when comparing two cryochillers with similar maximum cooling capacities.
2:20 p.m. V-10 LOOKING FOR: Film Thickness, Color, Sheet Resistance, or R/T Characteristics? Use an omtsYs TFA
N. Hecker-Denschlag, M. Eberhardt, B. Keil
m-u-t GmbH, Neu-Ulm, Germany
Are you looking to determine the thickness of a thin film (e.g. ITO or ultra high barriers or DLC) using a contact-less method? Do
you simultaneously want to know the sheet resistance of the ITO? m-u-t’s omtsYs TFA (Thin Film Analysis) device can be used for
these applications and more during factory bring-up, as well as quantity control during fabrication. For thin films on substrate
materials ranging from PET, glass, metal sheets, and semiconductors, quantities like film thickness, color, reflection/transmission
characteristics or sheet resistance often need to be determined to ascertain whether the end-product is within specification. This
is true whether the film is produced using vacuum deposition or roll-to-roll processes. With an omtsYs TFA, these quantities can
be determined even in-vacuum, on rough surfaces, for wet films, or for layer stacks. Our newest omtsYs TFA comes standard with
TEC5 spectrometer systems covering the spectral range from 380 – 2200 nm. We can determine film thicknesses for semitransparent materials between 10 nm – 50µm and for metals down to thicknesses of < 2nm. Our expertise lies in meeting your measurement needs for industrial 24/7 applications! Let us demonstrate our measurement and analysis capability. Send us your samples
for a free preliminary analysis.
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Wednesday Afternoon, April 29
2:30 p.m. V-11 Elastic and Plastic Property Measurement for Thin Films Using Nanoindentation
D. Yang
Ebatco, Eden Prairie, MN
Hardness testing is a valuable and revealing technique for characterizing material mechanical properties. Hardness testing has
been in use in various forms and has driven the improvement of engineering design, quality control and failure analysis in a
variety of manufacturing and industrial applications. Nanoindentation, sometimes referred to as instrumented or depth-sensing
indentation, is a newer, promising, yet challenging hardness testing technique for measuring mechanical properties of materials
and devices at nanoscale. It has been developed and improved upon dramatically over the past decades, benefiting from everincreasing applications and improvement of transducer technology and computer hardware and software. In this presentation,
nanoindentation in characterization of nanomaterials, thin films and coatings for elastic and plastic properties will be introduced
and discussed.
2:40 p.m. V-12 Minimizing the Influence of External Factors that Affect Coating Hardness Measured by Nanoindentation
R. Nair
Fischer Technology, Inc., Windsor, CT
Nanoindentation has become the preferred methodology to measure fundamental mechanical properties of coatings. While these
instruments have become easier to operate, nanoindentation is still a sensitive test that is affected by several extrinsic and intrinsic
factors. The user must be cognizant of environmental factors in the laboratory like vibration and air currents. Coating properties
like porosity and roughness can also cause errors in the calculated data. These factors which are a fairly common occurrence in
real world scenarios cause false contact detections and force-displacement curves that lead to inaccurate estimations of contact
area. As a result there are large errors and variations in the calculated hardness and elastic modulus values. This presentation
discusses various approaches used in the new FISCHERSCOPE® HT2000 S to minimize the effect of environmental factors. For
example, improvements in the physical design of the HT2000 S have significantly increases precision and accuracy of measurements on BK7 glass in some labs.
The Donald M. Mattox Tutorial Presentation
1:00 p.m. TS-2 Magnetron Sputtering: An Unfinished Journey
Invited Talk
A. Anders
Lawrence Berkeley National Laboratory, Berkeley, CA
Cathode disintegration, as sputtering was originally called, has its humble beginnings in the 19th century with ingenious inventions
closely related to generating electrical power and establishing “empty space,” vacuum. We celebrate Geissler and his glass chambers,
Ruhmkorff’s induction coil, and Grove’s observation of coatings next to a cathode tip (1852), followed by Wright’s systematic fabrication of thin films (1877). Paving the way in the 1930s for later breakthroughs, Penning described the trapping of electrons in certain
electric and magnetic field configurations, concepts leading to the development of our modern magnetrons in the 1970s (Chapin,
Clarke, Penfold and Thornton). This, however, was just the beginning of an incredible success story that affects everybody’s life
today as magnetron sputter deposition enabled a wide range of product developments. Different magnetron geometries (planar,
rectangular, cylindrical), scaling, rotating targets, dual magnetrons, and magnetrons in hybrid configurations with other discharges
expanded the availability and variety of coatings. Plasma transport and thin film growth theories laid the basis for optimization.
Pulsing at radio-frequency (rf) made the use of insulating targets possible, and medium frequency (mf) pulsing, fast gas feedback
loops, and fast arc suppression circuits were major advancements to minimize unwanted arcing, especially for reactive deposition
conditions (early 1990s). Magnetic unbalancing brought plasma assistance to the deposition process (1980s), and pulsing at extreme
peak power densities introduced plasma-deposition by HiPIMS and HiPIMS-like processes at the turn of the millennium. Yet, there are
surprising features to be discovered, explained, and exploited, such as the recent (2012) observations of traveling ionization zones
or “spokes”, which have profound influence on magnetron operation and particle fluxes to the substrate. The journey in the world of
magnetron sputter deposition is far from finished, which becomes abundantly clear when looking at its history in a time lapse format.
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Thursday Morning, April 30
8:30 a.m. K-4 Roll-to-Roll Processing for Flexible Devices and Components Utilized in Wearable and Mobile Electronics
Invited Talk
N. Morrison
Applied Materials Web Coating GmbH, Alzenau, Germany
Roll-to-Roll (R2R) production of flexible electronic devices (active matrix TFT backplanes, OLED frontplanes and touch screens)
combine the advantages of the use of inexpensive, lightweight and flexible substrates with high throughput production to enable
new form factor products with exceptional robustness and mechanical stability. Significant cost reduction opportunities can
also be found in terms of processing tool capital cost, utilized substrate area and process gas flow when compared with batch
processing systems. Nevertheless, material handling, device patterning and yield issues have limited widespread utilization of
R2R manufacturing within the electronics industry. Recently, significant advances have been made in device patterning enabling
the mass production of a variety of flexible electronic devices. These techniques are now so advanced that feature sizes of less
than 40 nm can be produced on thin film layer stacks deposited on 50 µm thick polymeric substrates and features down to less
than 20 µm on thick film processed screen printed metal layers for narrow bezel applications. Significant challenges also exist in
terms of the layer deposition technologies used in R2R manufacture of these devices. Unlike traditional semiconductor or display
based cluster tool platforms, R2R systems require processing substrates in a continuous fashion with rolls up to several kilometers
in length. Depending upon the process itself, this imposes a limitation in terms of the mean time before cleaning (MTBC) and in
some cases the particle management strategy. A variety of different web handling and coating technologies/platforms to enable
high volume R2R manufacture of both active and passive components utilized in display have been developed. The work presented in this paper therefore describes the principal challenges inherent in moving from lab/pilot scale manufacturing to high
volume manufacturing. Results will be presented for both amorphous silicon and IGZO TFT backplanes, ITO based touch panel
devices in addition to high barrier performance layers and stacks for both substrate encapsulation and barrier film for final device
encapsulation. The paper also addresses areas where both thick and thin film processing technologies can be combined.
9:20 a.m. T-12 Wear Mechanism of Mo-W Doped Carbon-Based Coating during Boundary Lubricated Sliding
P. Mandal, A.P. Ehiasarian, P.Eh. Hovsepian
Nanotechnology Centre for PVD Research, Sheffield Hallam University, Sheffield, United Kingdom
2µm thick Mo-W doped carbon-based coating (Mo-W-C) was successfully deposited by combined HIPIMS and UBM techniques.
The tribological behaviour of this coating was investigated by pin-on-disc tests using 100Cr6 steel and Al2O3 balls at room
temperature and at 200°C. The tests were carried out under boundary lubricated condition using highly viscous engine oil. Room
temperature experiments using steel counterpart showed friction coefficient of 0.033, which was lower than a number of stateof-the-art DLC coatings. Experiments carried out with the Al2O3 counterpart revealed that the DLC coating retained its friction
coefficient (µ=0.079) in both room and 200°C temperatures. However, a significant reduction in friction coefficient was noticed
for Mo-W-C coating from room temperature to 200°C (µ=0.072 to 0.051). Furthermore, Raman spectroscopy was used for better
understanding of the wear mechanism of Mo-W-C coating during sliding. The graphitic carbon particles (from coating) and metal
sulphides (WS2 and MoS2, where metals from coating and sulphur from engine oil) were found as wear products. The increase in
temperature promoted the formation of these solid lubricants at the asperity contacts during sliding and decreased the friction
coefficient. Thus, it is concluded that the tribochemical wear mechanism governs the tribological behaviour of the Mo-W-C coating in boundary lubrication conditions.
9:40 a.m. T-13 DLC Films on Glass and Plastic by In-Line PECVD
J. Madocks, P. Ngo
General Plasma, Inc., Tucson, AZ
Diamond-like carbon (DLC) films are deposited on glass and plastic by a novel AC ion source. Unlike past ion beam DLC deposition processes, the operation of the AC ion source is not hindered by electrode coating. This problem is overcome as the dual
electrodes of the source are alternately sputter cleaned. This improvement enables constant voltage and stable DLC coating
operation over long production runs. Additionally, the dense ion beam emitted from the AC Ion Source is ideal for depositing DLC
on insulators where substrate biasing is not practical. In this presentation, film performance data including hardness, abrasion
resistance, friction, adhesion and optical measurements are presented. The source physics are reviewed and long term stability
data for discharge voltage, coating performance and uniformity are shown.
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10:00 a.m. T-7 Carbon Based Multifunctional Coatings for Oil-Less Hermetic Compressor Applications
Invited Talk
J.D. Biasoli de Mello1,2
1
Laboratório de Tribologia e Materiais, Universidade Federal de Uberlândia, Uberlândia, Brazil
2
Laboratório de Materiais, Florianópolis, Universidade Federal de Santa Catarina, Brazil
Household refrigeration represents 17.3% of home energy consumption in the USA and 47% in Brazil. This article overviews a multidisciplinary approach to develop a traditional hermetic compressor (oil lubricated, with several rotating parts), into an oil-less,
linear motion, innovative compressor, with improved efficiency, versatility and sustainability. This involves the development of
surface engineering processes combining purpose-oriented phases applied to soft substrates to achieve high wear resistance and
load support and low friction coefficient. Initially, the role of the environment (air, CO2 and R600a) on the tribological behavior of
a commercially available Si-rich multifunctional DLC coating deposited on AISI 1020 steel is illustrated. In sequence, the influence
of the thickness of different layers (DLC and CrN) on sliding wear is analyzed. Results are presented using an original approach (3D
triboscopic maps) for two distinct configurations (increasing load and constant load) and findings are confronted with numerical
simulations using Film Doctor®. Finally, a low cost process to obtain a multifunctional coating (different nitrided layers + DLC) is
described, which uses a unique thermal cycle reactor capable of coating parts in industrial scale with reduced cost.
11:00 a.m. T-14 Studies of Porosity in Ceramic Titanium Nitride Oxide PVD Coatings
Z. Wang, J. Crowshaw, M. Akkaoui
Tanury Industries, Lincoln, RI
Titanium Nitride Oxide (TiNOx) coatings exhibit many positive attributes such as a wide color choice for decorative purposes,
high heat resistance, dielectric with strong durability and improved scratch-resistance compared with pure metal, and antibacterial properties related with biocompability. Cathodic arc deposition was utilized to deposit TiNOx coating on a polished brass
substrate plated with nickel and chrome. The problem is that some areas the size of ~ 0.3µm in diameter had no coating or poor
adhesion, and the substrate area was exposed. Scanning electron microscope (SEM) with Energy Dispersive X-ray analyzer (EDS)
showed that the poor coating area had some abnormal elements such as fluorine, aluminum, silicon, calcium, potassium, sodium
or chlorine from area to area instead of elements from plating or the PVD coating. In order to resolve this problem, different kinds
of plating or cleaning processes were employed and several PVD coating parameters were modified to improve the coating
results. This paper will discuss these experiments and their results.
11:20 a.m. T-15 Plasma Immersion Ion Deposition (PIID) of Diamond-Like Carbon (DLC) Coatings for Automotive and
Petroleum Applications
R. Wei, C. Ellis-Terrell, C. Rincon, and J. Lin
Southwest Research Institute, San Antonio, TX
Diamond-like carbon (DLC) coatings have been studied for many years and commercially applied to a number of automotive
components including cam followers, camshafts, gears, bearings, wrist pins, fuel injectors, etc. The coatings are generally deposited using a physical vapor deposition (PVD) process and the thickness is typically less than 5µm. Plasma immersion ion deposition (PIID) process, a chemical vapor deposition (CVD) process, has been developed for nearly two decades. Compared with PVD
processes, the PIID process has no limit of the deposition chamber size, requires no sample rotation and hence promises an even
lower production cost. In addition, a much thicker coating (>>5µm) can be prepared. Besides automotive, the petroleum industry
now finds a number of practical applications. In oil and gas (O&G) exploration and production, a thick coating is necessary due to
the severity of the environments. In particular, a coating has to withstand the erosion/abrasion from sand carried by the fluid. In
addition, corrosion resistance is required almost all the time because many components expose to Cl-containing water, acids, and
humid air either downhole or in the open field. In certain environments, thick scales of mixed oxides or hydroxides containing Ca,
Ma and other rare earth elements can grow. It is not only just annoying but also detrimental. Therefore, anti-scaling properties of a
coating are required. Furthermore, in some applications, a coating with good hydrophobicity, ice-phobicity or even oleophobicity
is highly desired. Standing above all PVD or CVD coatings, it seems that the DLC coating may be the only one that is capable of
meeting all the challenges. In this presentation, we will present the latest research and development of the PIID process and the
thick DLC coatings (10-30µm). We will present the deposition techniques for outer surfaces of 3-D components with thick coatings
at a high deposition rate and for the inner surface of long pipes (10-24 m). Then we will present the DLC erosion/wear resistance,
corrosion resistance, hydrophobicity/oleophobicity and anti-scaling properties. Finally, selected applications for O&G will be
discussed.
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11:40 a.m. T-16 Minimizing Mechanical Losses of Rolling-Sliding Contacts in Automobile Power Train by Diamond-Like
Carbon Coatings under Elasto-Hydrodynamic Lubrication
K. Bobzin1, T. Brögelmann1, K. Stahl2, K. Michaelis2, J. Mayer2, M. Hinterstoisser2
1
Surface Engineering Institute, RWTH Aachen University, Aachen, Germany
2
Institute for Machine Elements, TU Munich, Garching, Germany
An efficient power train technology contributes to sustainable lowering of greenhouse gas emissions in terms of reducing mechanical losses and saving fossil fuels. Due to the periodic or continuous operation in mixed and boundary friction, minimization
of mechanical losses of highly loaded components in automobile power train, such as crankshaft bearings and gear wheels, offer
massive potential for target achievement. Application-related investigations of diamond-like carbon (DLC) coatings ZrCg (a:C-H/
ZrCg) and nanocomposite (nc)-ZrC (a C:H/ZrC) in lubricated rolling-sliding contacts in twin-disc and a gear efficiency test rig, revealed great potential of ZrCg for efficiency improvement in automobile gear box by reducing mechanical losses up to 34% under
elasto-hydrodynamic lubrication (EHL) compared to uncoated gear wheels. With regard to crankshaft bearings, ZrCg and nc-ZrC
coated modified prototype bearings showed a friction advantage of up to 30% in EHL compared to series bearings in an engine
test bench. This yet largely unknown favorable effect of DLC coatings under rolling and sliding conditions in EHL can be attributed
to the thermophysical properties of DLC coatings, opening doors to new possibilities in tribology and efficiency improvement.
12:00 p.m. T-17 New and Most Recent Ultra-Hardness Findings – Real or Nonsense?
M. Fuchs, N. Schwarzer
Quite recently Huang et al. reported having synthesized nanotwinned diamond structures with “unprecedented hardness and
stability.” It is claimed that these structures are ultra-hard reaching a Vickers hardness of up to 203 GPa at a normal load as high
as 4.9 N. Hence, they would be twice as hard as ordinary diamond. This work will critically review the above mentioned work. The
first part will provide insight into the details of the measurements and elaborate whether or not the techniques utilized in both
experiment and subsequent analysis were sufficient to substantiate these claims. In the second part, first principle approaches
presented in will be applied in order to show whether or not the law of energy conservation does allow such hardness results
from a pure theoretical point of view. Based on the aforementioned methods, this work will be topped off with an investigation of
construction parameters theoretically necessary to construct a diamond structure twice as hard as natural diamond giving explicit
limits for lattice constant, elastic modulus, and Poisson’s ratio.
WebTech Roll-to-Roll Coatings for High-End Applications
9:20 a.m. IA-9 Flexible OLEDs for Display and Lighting Applications
Invited Talk
T. van Mol
Holst Centre, TNO, Eindhoven, The Netherlands
Flexible OLED technology, be it for lighting or display applications, need ultra-high quality thin film flexible barrier performance,
with zero tolerance for black spot appearance during the lifetime of the product. Flexible OLED lighting panels will be presented
that even after more than 2000 hours in 60˚C/90%RH accelerated lifetime conditions show zero defects. Latest results will be
presented in upscaling the production process of OLED lighting panels towards roll-to-roll. Also AMOLED displays using oxide TFTs
and high-quality moisture barrier were fabricated on ultrathin, flexible plastic substrates to give maximum mechanical flexibility.
Total display thickness is below 150 m, and repeated rollability at 1 cm roll radius has been demonstrated.
10:00 a.m. W-1 Ultra-High Multi-Layer Barriers on Weathering Stable Substrates for Outdoor Application
J. Fahlteich1, C. Steiner1, O. Miesbauer2, S. Amberg-Schwab3, K. Noller2, N. Schiller1
1
Fraunhofer Institute for Electron Beam and Plasma Technology and COMEDD - FEP, Dresden, Germany
2
Fraunhofer Institute for Process Engineering and Packaging IVV, Freising, Germany
3
Fraunhofer Institute for Silicate Research ISC, Würzburg, Germany
Flexible and organic electronic devices for photovoltaic, display and lighting applications attract growing interest in applied
research and industry. However, flexible devices need to be encapsulated with a permeation barrier system for their protection
against degradation caused by harmful gases such as water vapor and oxygen. The required properties of the barrier system –
commonly a coated polymer film – strongly depend on the application environment of the device. Both photovoltaic devices
and OLED devices in automotive application require outdoor stability against wheathering, UV light and high temperature
(damp-heat-test at 85°C / 85% r.h.). This paper focuses on the adaption of a roll-to-roll manufactured ultra-high multi-layer
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permeation barrier film for outdoor application by replacing the commonly used PET polymer substrate with wheathering stable
fluoropolymer films (ETFE, PVDF and ECTFE). The barrier technology itself is based on reactively sputtered oxide barrier layers and
a wet-coated interlayer of inorganic-organic hybrid polymers (ORMOCER®s). Challenges for the deposition of the constituents of
the multi-layer on fluoropolymer substrates will be discussed. Finally, barrier films on fluoropolymer substrates are tested under
simulated climate conditions (UV-Test, Damp-Heat-Test) and in a long-term outdoor test in comparison to reference systems on
PET and PEN substrates.
10:20 a.m. W-2 Roll-to-Roll Vacuum Coating System for Development of Flexible Substrates for OLED Lighting
H. Tamagaki1, K. Tanaka1, A. Oishi1, T. Furukawa2
1
Kobe Steel, Ltd., Takasago, Japan
2
Innovation Center for Organic Electronics, Yamagata University, Yonezawa, Japan
A multi-functional roll-to-roll (R2R) coating system was developed for a research project for the “Yamagata University Organic Thin
Film Device Consortium,” which intended to develop flexible substrates with an alternative electrode of ITO for OLED lighting. The
project intends to study three types of flexible substrates (ultra-thin flexible glass, stainless steel foil and plastic film), so that the
system is designed to carry out R2R deposition on 300 mm wide webs of these substrates from dual-magnetron or DC magnetron
sputtering cathodes. The system has a web handling system with wider tension range, larger diameter guide rollers and a main
drum with wider temperature control range than standard R2R equipment for plastic film. Furthermore, for a plastic film, the
system also has a function of PECVD process to deposit transparent high barrier coatings that are required for OLED application.
This paper will give an overview of the research project and then will focus on the R2R deposition system. Some of the experimental results will be discussed.
11:00 a.m. W-3 Ultra-High Moisture Barriers from PVD and ALD at a Wide Range of Climate Conditions
F. Nehm1, H. Klumbies1, J. Fahlteich2, L. Müller-Meskamp1, K. Leo1
1
Institut für Angewandte Photophysik, TU Dresden, Dresden, Germany
2
Ultra-high moisture barriers are highly demanded because of the strong progress in the field of organic electronics. However,
their water permeation mechanics such as sorption and diffusion are rarely examined in detail although they are fundamental to
the success of flexible organic devices. Predicting a water vapor transmission rate (WVTR) for unmeasured climate conditions is
not trivial even for simple barrier systems. We show extensive climatic studies on sputtered and atomic layer deposited diffusion
barriers. WVTRs are measured by an electrical calcium test at temperatures from 20-68°C and relative humidities from 10-90%.
We find the WVTR directly proportional to the absolute humidity at a given temperature, promoting Henry’s law for sorption.
For substrates without a barrier, proportionality is temperature independent, but the WVTR of barrier films show temperature
independence only until 38°C. A temperature-induced change in permeation of the barrier itself is concluded. Additionally, we
ascertain diffusion constants and water concentrations within the barrier using fit routines for the transient regime of calcium test
data. We have produced and characterized barriers with qualities down to at least 2E-5 g/m2d at 38°C and 90%rh.
11:20 a.m. W-4 Low Temperature Plasma-Assisted Atomic Layer Deposition of Silicon Nitride Moisture Permeation
Barriers
A.-M. Andringa, A. Perrotta, K. de Peuter, H. Knoops, E. Kessels, M. Creatore
Department of Applied Physics, Eindhoven University of Technology, Eindhoven, The Netherlands
Encapsulation of OLEDs and thin film PV is required to minimize device degradation induced by moisture ingress. Silicon nitride
moisture permeation barriers have been fabricated using low temperature plasma-assisted atomic layer deposition (ALD), a
technique that is known to yield densely packed, highly uniform and conformal films. The deposited films have been characterized
in terms of refractive index and chemical composition by spectroscopic ellipsometry (SE), XPS and FTIR, respectively. The calcium
test has been performed to determine the intrinsic water vapor transmission rate (WVTR). Intrinsic WVTRs in the order of 10-6 g/
m2/day for 10-40 nm thick silicon nitride layers indicate an excellent barrier quality. The microstructure of the layers was studied
by ellipsometric porosimetry (EP), using water (d = 0.3 nm), ethanol (d = 0.4 nm) and toluene (d = 0.6 nm) as probe, adsorptive
molecules. Adsorption/desorption isotherms have been recorded by monitoring changes in refractive index of the films and
multilayer adsorption on top of the layer when exposed to the vapour of the probe molecule. Irrespective of the tested deposition
conditions (deposition temperature in the range 80-120C), no uptake of the probe in the layer is observed, indicating the absence
of accessible pores larger than 0.3 nm in diameter. The multilayer formation follows a type II isotherm. These results demonstrate
the non-porous nature of the silicon nitride films and confirm the excellent results in terms of intrinsic WVTR values.
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11:40 a.m. W-5 Recent Advances in Vacuum Deposited Hard Coats on PET Film
J. DiBattista, E. Chan, Y. Yang
Darly Custom Technology, Inc. Windsor, CT
Films coated with an anti-abrasive hard coat layer are important starting materials for numerous flexible electronic applications.
Specifically, transparent conductive oxides (TCO’s) like indium tin oxide (ITO) where a smooth hard surface is required prior to
sputter deposition. It is has been shown that film surface quality is directly related to TCO properties like conductivity, optical
transmittance, haze and adhesion. Traditional hard coats used for TCO production are deposited in atmosphere and cast from
solvent or water based acrylate systems. The roll-to-roll vacuum technique to be described can produce hard coatings on optical
grade film substrates using a 100% solids process eliminating the need to remove solvents or water. The process involves vacuum
deposition and curing of organic precursors on a substrate rendering the surface with anti-abrasion characteristics that duplicate
the performance of conventional wet chemistry processes. Results show the efficacy of this vacuum deposition method for coating an optically clear PET film with an anti-abrasive hard coat layer.
12:00 p.m. W-6 Mechanical Properties of Thin Barrier Coatings Deposited by PE-ALD on Polymer Films
P. Fayet1, E.R. Dickey2
1
Tetra Pak (Suisse) SA, Romont, Switzerland
2
Lotus Applied Technology, Hillsboro, OR
Thin oxide barrier layers were deposited on polyethylene terephthalate (PET) polymer films by plasma enhanced atomic layer
deposition (PE-ALD) in a roll-to-roll machine allowing sequential exposure of the polymer film to the chemical precursors due to a
movement of the film through physically separated zones. TiO2 and mix-oxides, TiO2/AlO3, barrier-coatings were analyzed according to Kelly-Tyson theory of stress transfer, assuming a perfectly plastic interface between the coating and the polymer substrate.
In this framework, the interfacial adhesion and the cohesive strength of coating were determined as a function of the metal oxide
nature and the respective coating thickness using the uniaxial fragmentation test method. The outstanding toughness of the ALD
layers and their high work of adhesion to the polymer film will be discussed. An example of a simple packaging material structure
will be given showing the behavior of the ALD in a converting line.
Optical Coatings
9:20 a.m. O-7 The Reversed Admittance Locus
A. Macleod, C. Clark
Thin Film Center Inc., Tucson, AZ
An admittance locus is normally drawn from the surface admittance presented by the interface with the substrate to the
transformed surface admittance presented by the entire coating. A comparison between this terminating admittance
and that of the incident medium immediately yields the reflectance and phase change on reflectance and there are also
many other properties that can be extracted. The reversed admittance locus starts with the point at which it is desired to
terminate the locus and draws the locus backwards as though it terminated at that desired point. The reversed locus is not
the forward locus of the coating in reverse where the incident medium is now acting as the substrate and the substrate the
incident medium. In the reversed locus the thicknesses of the layers are considered to be negative and as their negative
thicknesses increase they are drawn counterclockwise. The reversed locus answers the question “Where must the locus
have come from if it terminates at the chosen point?” A very simple example is the V-coat where we readily see the necessary structure by drawing the reversed locus for the layer nearest the incident medium and the forward locus for the layer
next to the substrate. The V-coat solution is given by the point or points of intersection. However there are much more
involved examples including some structures such as coherent perfect absorbers and other switches where it presents a
solution or demonstrates the infeasibility of a proposed solution.
9:40 a.m. O-8 Do it Yourself – Automated Thin Film Design using Genetic Algorithms
W. Theiss
W.Theiss Hard- and Software, Aachen, Germany
The selection of an appropriate thin film stack as solution for a given optical design problem requires experience. First the
materials have to be selected and put into the right sequence, then the layer thicknesses have to be optimized. Whereas the final
thickness adjustments can easily be done by a computer, material selection is usually ‘man made’. If a thin film expert is not available for some reason, the development of the coating is blocked. One can overcome this problem applying a genetic algorithm
to thin film design; In many cases it is sufficient to state the optimization problem and let the algorithm develop the solution
52
in an evolutionary process. The principle of the method is explained, and its strength and limitations are discussed. Typical
industrial thin film stacks (architectural glass coatings, AR coatings, optical filters) are used to demonstrate the application of the
method.
10:00 a.m. O-9 From Design through Manufacture with Direct Monochromatic Monitoring
A. Zoeller, M. Boos, D. Arhilger, H. Hagedorn
Leybold Optics GmbH, Alzenau, Germany
For the production of high performance multilayer systems with tight specifications and large number of layers, optical monitoring is essential. Substantial progress was achieved by the introduction of direct monitoring on the rotating substrate holder. Prior
to the manufacturing of optical coatings the so-called monitoring strategy has to be established by selecting the appropriate
monitor wavelengths. Computer process simulation is used for confirmation and if necessary for modification of the monitoring
strategy. It is also useful for optimization of the monitoring parameters and pre-production analysis. The paper will present first
experiences with a new tool for automatic selection of monitoring parameters. The sequence from design through monitoring
strategy, pre-production analysis and real coating runs will be presented on the basis of some challenging applications. The
applications will include band-pass filters with λ/4 and non λ/4 designs, notch filter and broadband anti reflection coatings.
10:20 a.m. O-10 A New Generation of Optical Monitoring Techniques for Optical Thin Films
B. Barney
Telemark, Battle Ground, WA
Much has been discussed over the past several years about optical monitoring and control of optical thin films in relation to broad
band monitoring. Many have suggested that the idea of broadband monitoring will allow a more precise end of a layer with the
ability to modify the recipe after the completion of each layer. Some have suggested that modifying the recipe after a given layer
could improve yields and performance of the subsequent film. This paper will discuss the progress to date on broadband monitoring in light of these suggestions and the current state of technology expanding on how current methods of layer endpoints
improve system performance and yields.
11:00 a.m. IA-11 Complex Optical Coatings for Sensor Applications and on Zeonex Substrates for Light Weight Mobile
Applications
Invited Talk
T. Geldhauser
Optics Balzers AG, Balzers, Principality of Liechtenstein
Modern electronic devices open up an interesting market for optical coatings, ranging from antireflection coatings on displays,
filters for optical sensor systems in the NIR/IR to light weight wearable display technology. This gives rise to an increasing demand
for environmentally stable and hard coatings on intrinsic soft plastic substrates with optical quality like cyclic olefin copolymer
(COC). We will present coating solutions on Zeonex® ranging from ARC, dielectric mirrors to beam splitters which have the desired
stability on the substrate and withstand hard environmental and physical tests. The infrared controls in modern electronics, like
time of flight systems (gesture control, etc.) need complex coatings on as thin as possible glass but also plastic substrates, e.g.
0.2 mm. We will show how amorphous silicon is a very good candidate for designing, e.g. band pass filters. Compared to typical
dielectric materials, very thin coatings with a low number of layers can produce superior blocking in the visible, steep edges of the
band pass and low angle dependence of optical properties in combination with a very good control on the bow of thin substrates.
Different processing approaches with low temperature as well as high temperature deposition have been shown to give high
quality layers, processing at low temperatures opens up the path to deposition on temperature sensitive substrates.
11:40 a.m. O-11 Deposition of Complex Optical Interference Filters on Polymer Substrates by Magnetron Sputtering and
PECVD Processes
T. Neubert1, M. Vergöhl1, K. Rohwer2, A. Simon2
1
2
INFITEC GmbH, Ulm, Germany
Polymer substrates for optical coatings have some significant advantages such as cost, weight and mechanical flexibility. However,
the deposition of complex optical interference filters on plastics is much more challenging than the deposition on glass. Important issues are the temperature and plasma stability of the substrates, their surface quality (roughness), the adhesion of the coated
layers, the different thermal expansion of polymers and the oxide layer systems and the strain in the layers caused by mechanical
deformation of the coated substrates. In this work we present the results of experiments to deposit interference filters with thicknesses > 3 µm and layer counts > 30, which can be used, for example, as triple notch filters for channel separation in 3D projection
53
systems. In detail, we compared a filter deposited by magnetron sputtering with a filter in which some of the sputtered layers have
been replaced by PECVD layers. The energetic input of different deposition sources and process parameters (planar and rotatable
sputter sources, PECVD) is investigated. The spectral performance of the filters was compared with the optical designs. In addition,
other application relevant properties such as crack onset strain and environmental stability is presented.
12:00 p.m. O-12 Optical Coatings by High Speed Rotary Spatial ALD
E.R. Dickey1, W.A. Barrow1, B. Aitchison2
1
2
MLD Technologies, Eugene, OR
Traditionally, Atomic Layer Deposition (ALD) has been a process based on the sequential pulsing and purging of precursors into
a single reaction chamber containing the substrates. Thin films made using this technique have been shown to have excellent
physical and optical properties, as well as unique properties such as high conformality, enabling uniform coating of highly irregular surfaces. However, the growth rates of films made using this method are generally very low, particularly when low substrate
temperatures are used. In this work, a new “spatial” Plasma Enabled ALD method, based on a rotating disc substrate holder, is
used to grow optical thin films at relatively low substrate temperatures with growth rates in the range of two to ten angstroms
per second on the entire substrate batch. Processes for SiO2, TiO2 and Ta2O5 are demonstrated, and the individual film properties
including elemental composition, optical constants, surface roughness, and conformality are characterized. The technique is then
used to demonstrate deposition of a 4-layer broadband anti-reflection coating on glass and polymer substrates. Scaling of the
process to larger disc-based geometries, as well as drum-based systems, is also discussed.
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Thursday Afternoon, April 30
Special Lunchtime Presentation
12:40 p.m. SP-1 Enabling a New Generation of Mobile Devices through Wafer-Level Integration of Optical Filters and
Electronics
Invited Talk
F.J. Van Milligen
Optical Security and Performance Products, JDSU, Santa Rosa, CA
The rapid growth in optical sensors in automobiles, cell phones, gaming, and wearable devices has driven the convergence
of optics and electronics, and specifically optical coatings and semiconductor processes. This convergence has created an opportunity for the optical coating supplier to think in the terms of consumer electronics: high volumes, high yields, low cost, and
rapid turnaround. Often, these coatings are directly deposited on customer-defined areas of active semiconductor devices. This
demands that the processes be compatible with semiconductor protocols for temperature, cleanliness, material selection, etc. In
such a case, the processing of the optical coating cannot impact the electrical performance or reliability of the underlying sensors. In this paper we will discuss the challenges that must be met, discuss potential approaches and highlight some of the many
products that are pushing the technical envelope.
1:20 p.m. T-18 Mechanical, Tribological and Corrosion Properties of Aluminium-Toughened PVD Nitrogen-Doped
Chromium Coatings
J. Kavanagh, C. Iamvasant, A. Leyland, A. Matthews
It is known that the properties of PVD metallic thin films can be modified significantly by the incorporation of interstitial elements
such as nitrogen. In particular, PVD processing allows interstitially-located elements to be introduced in high supersaturation (far
beyond the solubility limits predicted by equilibrium thermodynamics); such ‘doped’ coatings (eg. nitrogen-doped chromium) can
exhibit a high H/E ratio and excellent wear- and corrosion-resistant properties. Although CrAlN ceramic PVD films (often with high
Al-content, above 50at.%) have received much attention in recent years, little or no attention has been paid to metallic-alloy coatings of Cr-Al – particularly in the Cr-rich composition region. The Al-Cr binary equilibrium phase diagram indicates that between
5-10at.% Al can be easily dissolved into Cr between 400°C and 600°C without the formation of brittle inter-metallic phases (in
practice, the ‘non-equilibrium’ solubility limit for Al during PVD processing may be much higher still) – with the potential for high
hardness, combined with a lower elastic modulus and increased coating resilience and toughness. In this study, we report the
deposition of PVD CrAl(N) coatings and attempt to optimise the characteristics of the coating with respect to Al and N content, for
both wear and (sacrificial) corrosion properties. The coatings are characterised by measuring the nanoindentation hardness and
the wear resistance (reciprocating-sliding, microabrasion and impact tests). The coating structure is characterised by SEM (crosssection analysis), EDX, XRD and AFM for surface topography. Open circuit potential and potentiodynamic polarisation corrosion
tests are also performed.
1:40 p.m. T-19 Sliding Wear Behaviour of Graphene against Ti-6Al-4V: A Comparison with Polycrystalline Diamond and
Hydrogenated Diamond-Like Carbon Coatings
S. Bhowmick, A. Banerji, M.Z.U. Khan, A.T. Alpas
Mechanical Automotive and Materials Engineering Department, University of Windsor, Windsor, Canada
This study evaluates the role of graphene in mitigating titanium adhesion and reducing friction. Pin-on-disk type tests were performed to study the tribological characteristics of multilayer graphene (IG/I2D ratio > 1) sliding against titanium alloy (Ti-6Al-4V) in
air (20% RH) and compared with other carbon based coatings, namely hydrogenated diamond-like carbon (H-DLC) and polycrystalline diamond (PCD). The highest running-in coefficient of friction µR (0.45) was observed in case of H-DLC while the PCD showed
lower µR of 0.32. A low µR of 0.10, was recorded when the tests were carried out against graphene. Results suggested that the
graphene surface was passivated faster than the H-DLC and PCD. Experimental evidence for passivation of surface carbon atoms
by H and OH molecules was provided by HR-XPS. Micro-Raman analyses of the transfer layer on Ti-6Al-4V and graphene showing
an increasing intensity of D-band, suggesting an increased disorder of C-network, with increasing RH. Multiple layers of graphene
were transferred to the counterface according to cross-sectional HR-TEM of the counterface. The transfer layers consisted of 4-21
graphene nano-layers with d-spacings (0.34 nm-0.38 nm) larger than that of graphite suggesting an increase in the interlayer
lattice spacing of the planar graphene to accommodate the passivating molecules.
55
2:00 p.m. T-20 The Effect of Growth Conditions on the Surface Energy, Optical Properties and Saline Corrosion Resistance
of Amorphous Chromium Oxide Thin Films Prepared by Reactive Magnetron Sputtering
J. Kavanagh1, A.M. Oje2, A.A. Ogwu2
1
Department of Materials Science and Engineering, Sheffield University, Sheffield, United Kingdom
2
Thin Film Centre, School of Engineering, University of the West of Scotland, Paisely, United Kingdom
We have investigated the effect of growth conditions dominated by a mixture of Frank van der Merve and Volmer-Weber growth
mode on the properties of chromium oxide thin films prepared by reactive magnetron sputtering. The films were characterised by
SEM, EDAX, AFM, XRD, XPS, FTIR and Raman spectroscopy. The surface energy of chromium oxide was probed using XDLVO surface energy measurements with a goniometer. The optical properties of the film was measured using a spectrophotometer in the
wavelength range of 300 – 800 nm to obtain the optical band gap and ellipsometry was used to obtain the n and k components
of the complex refractive index. The corrosion properties of the prepared films were measured by open circuit potential, Tafel
plot and potentiodynamic polarisation in saline solution. We report our finding on the inter-relationship between the film growth
mode, dispersive/polar components of the surface energy and the corrosion resistance of the films. This information is necessary
to identify a processing window for application areas for chromium oxide thin films requiring optical transmission and resistance
to environmental degradation.
2:20 p.m. T-21 PVD Chromium Coatings Replacing Decorative Chromium Electroplated Coatings on Plastics
G. Vergason1, M. Fitch1, R. Smith1, T. Jochum2
1
Vergason Technology, Inc., Van Etten, NY
2
jobaTEC GmbH, Sankt Wendel, Germany
Traditional electroplated chromium coatings on plating-grade ABS contain hexavalent chromium and are being phased out due
to long standing issues of health and environmental hazards and waste stream reclamation. In Europe, the implementation of
the REACH initiative will effectively ban hexavalent chromium in 2017 and leading industries such as Automotive, Sanitary or
Appliances are searching for a reliable alternative for PoP (plating on plastic). Since the 1970s, PVD chromium coatings have been
available, but have lacked production viability due primarily to a lack of environmental durability and/or a tendency to stresscrack when subjected to thermal cycling. Alloying and nanolayered depositions have produced coatings that have controlled
stress cracking, but have not been able to produce the true chromium appearance that designers demand. New techniques have
been developed to produce chromium coatings that can withstand thermal cycling without stress-cracking and exhibit excellent
environmental durability. These new sputtered chromium coatings do not require a protective top coat. Visually the chromium
coatings are similar to those of electroplated decorative chromium. They can also be altered in appearance to achieve certain
design effects. This paper will discuss the technical challenges and testing results of this new PVD coating technique.
2:40 p.m. T-22 A New Energetic Approach to Ion Plating Plasma Assisted IPPA and its Innovative use in a Roll-to-Roll
Configuration for Chains Treatment
C. Misiano1, P. Matarazzo1, M. Pezzilli1, E. Bemporad2
1
Romana Film Sottili, Anzio, Italy
2
University of Roma 3, Rome, Italy
The Ion Plating Plasma Assisted IPPA deposition technology is based on the energizing, by biasing, of ionized condensing particles
and supporting the growing film with ions and particles bombardment. The revised version of Thornton Structure Zone Diagram
performed by André Anders including plasma based deposition and ion etching, added to the substrate temperature the energy
contribution due to the growing film bombardment and, besides, replaced the process pressure during the sputtering deposition
with the energy of condensing particles. The aim of the work described in this paper, was to increase the range of experimental
results to correlate the microstructure and the stress of deposited film with the following deposition parameters: 1) the mass
of bombarding particles (by changing the process gas, He, N2, Ar ); 2) the energy of bombarding particles up to 2500 eV; 3) the
deposition rate. The most interesting results obtained are concerning the identification of process parameters to realize amorphous layers of oxides, sulphides and metal films. As practical new industrial use of IPPA, the decorative treatment of chains, is also
described. A new configuration in laboratory scale was realized and tested obtaining treatments with protective and chromatic
effects on chain lengths of about 6 meters.
56
3:00 p.m. T-23 Tribological Properties of Titanium Doped Tungsten Disulphide/Titanium Multilayers Applied as Superficial
Protection during Limit Layer Lubrication
J.M. González1, C. Ortega1, H. Mohseni2, T.W. Scharf2, F. Sequeda1
1
Universidad del Valle, Laboratorio de Recubrimientos Duros y Aplicaciones Industriales RDAI, Cali, Colombia
2
University of North Texas, Laboratory for Moving Mechanical Assemblies LaMMA, Denton, TX
Deposition of the titanium doped tungsten disulphide/titanium multilayers on 304 stainless steel substrates was performed by DC
magnetron co-sputtering, with 1.5 µm total thickness and different modulation periods. Coatings were applied under limit layer
lubrication using Pin-On- Disc in combination with a conventional liquid lubricant (ISO viscosity grade=220, viscosity-100°C =28.3
mm2/s), used in difficult access installations, closed loop gear boxes, bearings and circulating or spraying lubricated systems, to
solve problems during liquid lubricant failure. Coated surfaces showed low friction coefficients sustained near 2500 cycles in room
atmosphere and more than 50000 cycles when combined whit liquid the lubricant, in a 100°C temperature. Multilayer behavior
was related to morphology, crystalline structure, chemical composition, mechanical properties and adhesion. Coatings showed
low hardness and elastic moduli compared to substrate, but increased plastic deformation resistance, resulting in high adhesion
and plastic deformation as dominant mechanism during dynamic scratch tests. Analysis performed shows that coating protects
the surface once the liquid layer fails, providing extra lubrication and solving the problems generated with liquid lubricant mixed
with different particulates, due to high adhesion, low flocculation and sedimentation of the coating.
3:20 p.m. T-24 On the Physicochemical Structure of the Silicon-Containing Adhesion Interlayer in DLC Deposited on
AISI 4140
E.R. Petry1, F. Cemin1, L.T. Bim1, C.M. Menezes1, M.E.H. Maia da Costa2, I.J.R. Baumvol3, C. Aguzzoli1, S.S. Tomiello4, C.A. Figueroa1,4
1
Universidade de Caxias do Sul, Centro de Ciências Exatas e Tecnologia, Caxias do Sul-RS, Brazil
2
PUC-Rio, Departamento de Física, Rio de Janeiro, Brazil
3
Universidade Federal do Rio Grande do Sul, Instituto de Física, Porto Alegre, Brazil
4
Plasmar Tecnologia Ltda., Caxias do Sul, Brazil
Diamond-like carbon thin films (DLC) show strident properties such as high wear resistance and ultra-low friction. However, a
widespread use regarding energy efficiency issues in the automobile industry is neglected due to the poor adhesion of DLC on
steel and/or expensive technologies. DLC adhesion on steel can be achieved by nanometric bonding interlayers containing silicon,
which are particularly beneficial to mitigate the high compressive stress and the thin film mismatching, promoting stronger
chemical bonds between the interfaces. In this work, the physicochemical properties of SiCx:H interlayers deposited from two
different liquid precursors, tetramethylsilane (TMS) and hexamethyldisiloxane (HMDSO), were studied and correlated to the adhesion behavior of DLC on AISI 4140 steel. The Si interlayers were deposited at different temperatures from 50˚C to 500˚C and the
DLC was deposited at 80˚C by a low-cost pulsed DC-PECVD technique assisted by electrostatic confinement. The chemical depth
profiling was performed by GD-OES. Hardness, friction coefficient and critical load were analyzed by nanoindentation and nanoscratch tests. In both liquids precursors, the thickness of the SiCx:H interlayers decreases as the interlayer deposition temperature
increases. Good enough adhesion of DLC was reached at an interlayer temperature deposition of 200˚C for HMDSO and 300˚C
for TMS.
WebTech Roll-to-Roll Coatings for High-End Applications
1:20 p.m. IA-10 Roll to Roll Processing of Thin Flexible Energy Devices
Invited Talk
B. Berland
ITN Energy Systems, Inc., Littleton, CO
ITN Energy Systems is developing roll-to-roll, microwave PECVD deposition of window films to help reduce the over 5 quads of
energy lost through windows annually in the U.S. alone. The use of pulsed microwave PECVD provides a unique combination of
controlled ion energy, plasma density, and plasma chemistry to enable low temperature deposition of optical quality films on PET
substrates. ITN initially has demonstrated the microwave PECVD process with low-e window films. While low-e coatings directly
on glass have become common in new window markets, the U.S. has over 100,000,000 existing homes and numerous commercial
building, many of them having poor quality windows that would benefit from a retrofitable window film. ITN’s low-e window coatings employ low cost oxide based materials that have been deposited at rates >100 angstroms per second to support a window
film than can be manufactured for <$1/ft2 in volume. Further, the low-e coating can be tuned to optimize energy response in both
the solar and thermal infrared regions to minimize energy use across a range of climate zones.
57
2:00 p.m. W-7 Tailoring Roll to Roll ALD Barrier Processes for OLED, Thin Film PV, and Commercial Packaging Applications
W.A. Barrow, B.L. Danforth, E.R. Dickey
Recent advances in Atomic Layer Deposition by substrate translation (“Spatial” ALD) have enabled roll to roll processing of ALD
barrier films at high speed, with permeation properties equal to or better than barrier films produced in classical pulse-based
ALD batch systems. Most research and development in ALD barriers to date has been conducted using Al2O3 processes based
on trimethylaluminum (TMA) as the aluminum precursor and either water, ozone, or oxygen plasma as the oxygen precursor.
However, this material, when deposited at low temperature, has several drawbacks, limiting its practical applications. In this work
we examine alternative ALD chemistries and processes based on homogenous mixtures of binary oxides, which are individually
optimized for the requirements of each application. For OLED displays and lighting, processes are demonstrated that provide
water vapor transmission rates (WVTR) under 1 * 10-5 g/m2/day with long term stability under moderate environmental testing.
For thin film photovoltaic applications, processes are demonstrated which provide WVTR under 5 * 10-4 g/m2/day, and survive
the required harsh environmental test conditions of 85°C, 85% RH for 2000-3000 hours. For commercial packaging applications,
processes are demonstrated at the high web speeds required in this industry, in the range of 5 to 10 meters per second, with
WVTR under 1 * 10-2 g/m2/day, and projected coating costs totaling less than $0.05 per square meter.
2:20 p.m. W-8 Nanostructuring of Ethylene Tetrafluoroethylene Films by a Low Pressure Plasma Treatment Process
C. Steiner1,2, J. Fahlteich1, E. Rädlein2
1
2
Technische Universität Ilmenau, Ilmenau, Germany
A vacuum plasma treatment is used to create stochastic nanostructures on ethylene tetrafluoroethylene (ETFE) films. Such
nanostructures exhibit excellent anti-reflection properties and allow control of surface wetting properties. Therefore, the nanostructures have good application potential in the field of displays, large area organic electronics and solar cells. In this paper, a
three-step reactive dual-magnetron plasma process is used to prepare nanostructured surfaces on ETFE in a vacuum roll-to-roll
coater. The process includes deposition of an oxide seed layer, a plasma etching step and an oxide top coat. The plasma etching
step itself is done using a dual-magnetron system with a pure oxygen atmosphere. The influence of different process parameters
like plasma power, oxygen flow, target materials for seed layer and top coat on structure formation and surface properties is
investigated. It is possible to adjust the static water contact angle from hydrophilic to hydrophobic by using different oxides for
top coat. A maximum antireflective effect on ETFE is achieved by both side treatment, showing a transmittance of 98.7% at 600
nm wavelength. ETFE is used because it is known to be weathering stable in outdoor application. The weathering stability of the
nanostructured surfaces is discussed.
2:40 p.m. W-9 Roll to Roll Sputtered Titanium and TiO2 from a Dual Rotatable Cathode, using Open and Closed Loop
Process Control and Comparing AC and Square Wave Bipolar Power Delivery
D. Wickens, N. Butcher
Bobst Manchester Ltd., Heywood, United Kingdom
Comparison of titanium sputter characteristics from a 1 m wide dual rotatable cathode on a roll to roll sputter coater was investigated. Multiple power modes were explored for the difference in deposition rates between DC, pulsed DC, sinusoidal AC, square
wave bipolar and bipulse. Square wave bipolar power provided a 100% duty waveform with AC-like delivery and bipulse delivered
a square waveform of a sinusoidal nature (90% duty). Hysteresis behaviour of bipolar, bipulse and AC at 10 RPM and 2 RPM were
investigated, monitoring the plasma impedance, plasma emissions and process stability (arc behaviour). Sheet resistance and
the reflection and transmission spectrometry were obtained in situ to provide information on the coating properties and optical thicknesses of the deposited TiO2 at a range of closed loop set points. Increasing the rotation speed altered the hysteresis
behaviour due to the difference in time the cathode spent outside of the erosion path, altering the cathode surface characteristics.
Closed loop TiO2 control demonstrated superior deposition rates compared to open loop, however, care needed to be taken not to
sacrifice the desired optical properties of the film for improved rate.
3:00 p.m. W-10 Applying Co-Sputtering to Increase DDR during Deposition of Titanium Oxides and Silicon Oxides
V. Kozlov, J. Kazuss, E. Machevskis
SIDRABE Inc., Riga, Latvia
Although vacuum deposition technologies are highly developed, the industry is searching for effective solutions to tackle such
topical issues as increasing productivity of coating deposition processes, optimising characteristics of known materials as well
as creating materials with new, unique characteristics. A great interest lies in researching coatings of multi-component oxides,
nitrides or carbides that can be deposited applying reactive magnetron sputtering. One approach is to use magnetron sputtering58
traditional targets with complex composition: metal alloys, oxide or nitride ceramics or their mixtures. Making alloys composed
of two metals whose melting temperature differs by several hundred degrees is an unsolvable task due to the limited solubility
of the components. The source materials for manufacturing powder, metal and ceramic targets are expensive, the manufacturing
technology is complex and this is reflected in the high prices of ceramic targets. Low thermal conductivity of ceramic targets limits
sputtering power and coating deposition rate. Another approach is simultaneous magnetron sputtering with two (or more) elemental targets of metal or ceramics, i.e., co-sputtering. The work examines co-sputtering application possibilities to increase DDR
during deposition of silicon and titanium oxides. Possibilities to achieve coatings with different compositions are also discussed.
The co-sputtering process is scaled-up to large-size coating areas and increase of power in processes.
Optical Coatings
1:20 p.m. O-13 Broadband and Wide-Angle Antireflection Coatings Containing Plasma-Etched Organic Layers
U. Schulz, F. Rickelt, P. Munzert, H. Ludwig, N. Kaiser
Fraunhofer Institute for Applied Optics and Precision Engineering IOF, Jena, Germany
Direct plasma etching is a powerful method for producing antireflective (AR) nanostructures on organic layers and substrates.
Normally, the structure depth achievable by a single etching step is limited to approximately 100 nm. Therefore, the AR performance is excellent in the visible spectral range for normal light incidence on planar substrates. A more sophisticated application
is a curved lens in which the AR function is maintained throughout the visible spectral range and over an extended range of
incident light angles. Based on theoretical knowledge, it is widely accepted that interference stacks have limitations that cannot
be overcome with currently available compact thin-film materials and that a gradient layer of sufficient thickness would provide
the best possible AR performance for wideband or wide-angle AR applications. In this work, multiple inorganic and organic layers
are used to build up AR coatings with a decreasing effective index from the substrate side to the surrounding air. By depositing
and etching of organic layers step-by-step a broadband antireflective performance can be achieved. Experimental results will be
presented together with the simulation of the optical properties. In particular, the behavior at higher light incidence angles was
improved markedly by adding the second structured layer.
1:40 p.m. O-14 Antireflection Coating Production Process Without An EBeam Source and Without Scattering
R.R. Willey1, K. Patel2
1
Willey Optical, Consultants, Charlevoix, MI
2
Luma Optics Pvt Ltd, Mumbai, India
The most common antireflection coatings in the industry today use electron beam sources for their deposition, which require a
large capital investment and have some other undesirable characteristics. These characteristics might include: lack of uniformity
and reproducibility due to melt-in variations, sweep variations, and rate instabilities. The predominant low index material used
throughout the world is silicon dioxide, which also can have uniformity and reproducibility problems. A production process is
described which uses only resistance sources, which are much less complex, are more reproducible, and are easier to control.
Magnesium fluoride is a most desirable material to use because of its low index of refraction and reproducible deposition results,
but it tends to have scattering and stress problems. It is possible to reduce the scattering and stress by interjecting thin high index
layers into the thicker MgF2 layers. These thin layers can be accommodated in the “normal” designs without significant effect on
the spectral performance. Experiments to optimize these “lamination” processes and designs are described.
2:00 p.m. O-15 Advanced Deposition Technology for Astronomical and Space Applications, Part II: Ion-Assisted Filtered
Cathodic Arc Deposition (IFCAD)
M.L. Fulton, R.S. Dummer, M. Zimmerman
Surface Optics Corporation, San Diego, CA
During the SVC 2012 Technical Conference the authors presented their unique 3.3 meter diameter chamber, equipped
with an e-beam, resistance source, and Ion Assisted Deposition (IAD) system mounted on a movable stage that translates
under a large rotating substrate providing computer controlled uniform depositions on a variety of optical surfaces. NASA’s
Kepler primary mirror, for example, was successfully coated with protected silver using the 3.3 meter chamber technology.
In 2014, a Filtered Cathodic Arc (FCA) source was added to the movable deposition platform, providing a powerful new
capability to the large area coating chamber. Many astronomical and space optical applications will benefit from the IonAssisted Filtered Cathodic Arc system, particularly due to the protective Diamond-Like-Carbon (DLC) coating. In addition
to the well-established superior DLC coating that is being designed for Space Craft Windows and IR optical component
protection, there are: Transparent Conductive Oxides (TCO); primary metal coatings (gold, silver, and aluminum); metal ox505/856-7188 Fax 505/856-6716 • E-mail [email protected] • Web Site www.svc.org
59
ides and nitrides (like Al2O3 and TiN); and other strategic materials. The development of IFCAD processes, in the 3.3 meter
chamber, like: large IR mirrors (DLC protected Au); terrestrial telescope mirrors; space craft windows and other applications
will be discussed.
2:20 p.m. O-16 Advanced Optical Coating
A. Luca1, R. Müller1, R. Stober1, J. Landrock1, J. Mai1, P. Gawlitza2, S. Braun2, M. Sarstedt1
1
Roth & Rau AG, Hohenstein-Ernstthal, Germany
2
Fraunhofer for Material and Beam Technology IWS, Dresden, Germany
Ion beam sputtering has been used for smoothing of silicon and quartz glass substrates and for deposition of nanometer multilayers for high-end optical applications in extreme ultraviolet (EUV) and in X-ray. The tool IonSys1600 is equipped with two linear
ion beam sources, a rotatable drum of targets, movable substrate and shaper with pre-calculated velocity maps. Two ion beam
sources, one directed to the target and the second to the substrate, provide reproducible and precise application of ion beam
sputtering technol-ogy to etch, smooth or figure substrates or to deposit high quality nanometer multilayers. We will present
smoothing of silicon substrate to microroughness of 0.11 nm rms (AFM scan length 5 µm). Examples of high precision ion beam
sputter deposition are shown on Mo/Si, DLC/Si and Ni/C multilayers which have been characterized by x-ray reflectometry.
2:40 p.m. O-17 Precision Multilayer Coating for Large High-End Mirrors
A. Luca1, R. Müller1, A. Eibisch1, J. Landrock1, J. Mai1, R. Stober1, P. Gawlitza2, S. Braun2, M. Sarstedt1
1
Roth & Rau AG, Hohenstein-Ernstthal, Germany
2
Fraunhofer for Material and Beam Technology IWS, Dresden, Germany
Modern astronomy and advanced photolithography methods today use nanometer multilayers to handle extreme ultraviolet
(EUV) and soft X-ray radiation. Using magnetron sputtering, it is possible to deposit thin layers in the sub-nm range with small surface roughness. This contribution introduces a series of tools equipped with sputtering magnetrons and sophisticated substrate
movement. It is shown that high precision and stability of key components allow coatings required by EUV lithography. Measured
reflectivity values (λ = 13.5 nm, θ = 5°) of a 50 multilayer stack of Mo/C/ Si are higher than 69%. With a properly designed system
and well calculated velocity profile, the relative spatial homogeneity of λ50 (the wavelength center position between the 50%
reflectivity values) is higher than 99.9% on a diameter of 450 mm. For high throughput the systems operate with six magnetrons
and with different materials (samples up to 680 mm). For telescope mirrors, where sizes are typically a few meters, a different
approach using one magnetron and shaping systems is shown.
60

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