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Development and Characterization of nano
International Scientific Spring 2010 NCP, QAU Development and Characterization of Nanocomposite Materials Dr. Fazal Ahmad Khalid Pro-Rector GIK Institute of Engineering Science and Technology Topi, NWFP [email protected] CNT Reinforced Molecular Level Mixing Nanotechnology Growth Info Bio Nano S. Milunovich, J. Roy. United States Technology Strategy. Merrill Lynch. 4 Sept. 2001 History ~ 2000 Years Ago – Sulfide nanocrystals used by Greeks and Romans to dye hair ~ 1000 Years Ago (Middle Ages) – Gold nanoparticles of different sizes used to produce different colors in stained glass windows Milestone 1959 R. Feynman Delivers “ Plenty of Room at the Bottom” 1974 First Molecular Electronic Device Patented 1974 Taniguchi used the term Nanotechnology 1981 Scanning Tunneling Microscopic (STM) 1985 Buckball C60 discovered 1986 Atomic Force Microscopy (AFM) Invented 1987 First single-electron transistor created 1991 Carbon Nanotubes Discovered 2000 US Launches National Nanotechnology Initiative Exciting new science and technology for the 21st century What is Nanoscale Fullerenes C60 12,756 Km 1.27 × 107 m 22 cm 0.7 nm 0.22 m 10 millions times smaller 0.7 × 10-9 m 1 billion times smaller Human hair ~ 80 μm Macro – Micro - Nano Macro or Conventional Machines Build and assemble Micromachines Build in place (m - mm) Nanosystems Brought together by forces at the atomic level (0.1 mm - 0.1 µm) © Deb Newberry 2002,2003,2004,2005,2006,2007 (100- 1 nm) Nanotechnology: Key component of converging technologies Miniaturization of Semiconductor Devices Molecular Engineering Atom Molecular Manipulation DNA-Protein Manipulation Expectation of new technology domain and new market Mechanics Materials & Chemistry Fuel Cell Mo Eng lecular inee ring Mechanically Strong Material mAto ecular on i l Mo ipulat n Ma Se mi mico nia nd tur uct iza or tio n Molecular Carbon Nanotube Electronics NEMS Quantum Nanobio Devices Devices n io A DN tein t o Pr pula i an M Life science Electronics New applications New materials New systems & devices Nanomaterials Synthesis and Physical Fabrication Zero-Dimensional Nanoparticles (oxides, metals, semiconductors and fullerenes One-Dimensional Si Two-Dimensional Si/Ge Nanowires, Nanorods and Nanotubes Thin films (multilayers, monolayer, self-assembled and mesoporous Three-Dimensional Nanocomposites, nanograined, micro- and mesoporous and organic-inorganic hybrids Nanomaterials Size-Dependent Properties Chemical Properties – reactivity, catalysis Surface area to volume ratio - Surface energy ⇑ – high reactivity - Al nanoparticles – energetic materials Thermal Properties - melting temperature Nanoscale melting temperature - Nanocrystal – surface energy ⇑ – melting temp ↓ - CdSe (3 nm) nanocrystal melts @ 700 K (1678 K) Wang,et al, FIU Nanomaterials Size-Dependent Properties Mechanical Properties – strength, adhesion and capillary force Optical Properties – absorption and scattering of light Electrical Properties – tunneling current Magnetic Properties – superparamagnetic effect Nanofluidic properties New Properties promise new applications Properties of Bulk Nanostructured Materials Benefits Strength Toughness Formability Limitations Manufacturing small things big? Structural stability ODS Alloys and Nanocomposites Goa, University of California Increasing Copper Strength • Plastic deformation of copper introduces work-hardening (copper gets stronger) and reduces the grain size • Hall-Petch relation predicts materials get stronger as grain size decreases: σy = σ0 + KHPd-1/2 (Yield strength is inversely proportional to grain size) Material Yield Strength Cold Worked Copper 393 MPa 400 nm Copper 443 MPa 100 nm Nanograin Copper 900 MPa 10 nm Nanograin Copper 2.9 GPa Arzt, MPI Stuttgart Problems in Nanotechnology Create Manipulate Analyze Small objects 1 – 100 nm in at least one dimension Nanomanufacturing - Requirements Nanomanufacturing/ nanofabrication technology should: be capable of producing with nanometer precision components be able to create components be able to produce many simultaneously be able to structure in three be cost-effective systems from these systems dimensions Mimicking the nature Plants are made from cells Cells use molecules (clusters of atoms) from the air, soil and water AFM FEG-SEM FEG-TEM FIB 50 µm 18 Empa Report 2004 Carbon Nanotubes Grown From FIB Prepared Seeds Holes Drilled by FIB and Filled with Iron as Catalyst Carbon Nanotube 200 nm D. Zhou and L.A. Giannuzzi, UCF Gold particles on carbon Applications New Developments in Processing and Characterization Intel processors with features measuring 65 nanometers Important for: Power efficient computing Communication products Gate oxide less than 3 atomic layers thick 20 nanometer transistor Atomic structure 20 Applications in biomaterials Hip Joints - replacements Heart valves Knee Joints - replacements Stents Biomaterials: A material intended to interface with biological systems to evaluate, treat, augment, or replace any tissue, organ or function of the body Williams D. F. The Williams Dictionary of biomaterials 1999,Liverpool (UK): Liverpool University Press 42 Applications in crystalline Diamond MEMS Diamond coating surface morphology: (111)-diamond film (left) and (100)-diamond coating (right). Diamond gears. Diamond accelerometer. Courtesy: J. Lou, W. Milne et al (Cambridge University) Applications Cleaning Up the Environment Field demonstration that iron nanoparticles can remove up to 96% of a major contaminant – trichloroethylene – from groundwater at an industrial site From W. Zhang, Lehigh University Applications Large Increase in Lighting Efficiency • Dept. of Energy estimates that ~20% of energy used in U.S. is for illumination The Cook Nuclear Plant • Nanotechnology quantum dot phosphors hold promise of more economical white light LED lighting • LED-based lighting could cut the electricity used for illumination by as much as 50 percent by 2025; 2X more efficient than fluorescent Lauren Rohwer displays the two solid-state lightemitting devices using quantum dots her team at Sandia National Labs has developed. Capacity ~2 gigawatts Cutting electricity for lighting in half would result in energy savings roughly equivalent to the annual energy production of 50 nuclear reactors Engineering Transport Auto- and Locomotives Naval & Aircrafts Space Defense Nanocomposite Materials Bridges Structures Buildings Sports MMCs PMCs CMCs Energy NanoComposites – engineering, multifunctional coatings, biomedical and devices The Space Elevator Pictures from 26 http://www.space.com/businesstechnology/technology/space_elevator_020327-1.html CNTs Reinforcement ASM handbook 21, (1987) 579 P. J. F. Harris, Int; mat; Reviews 49, (2004) 31 Materials Diameter (µm) Strength (G Pa) Young’s Modulus (G Pa) Thermal conductivity (W/m K) Density (g/cc) Boron 140 3.3~4.0 370~400 100~200 2.3~2.5 SiC 15~145 2.9~4.0 210~400 70~110 2.5~3.5 Al2O3 20 1.5 380 30 3.9 Carbon fiber 7~13 2.1~5.0 240~500 250~600 1.7~2.1 Aramid fiber 12 3.0~3.6 70~180 0.3 1.4 Carbon Nanotubes 0.01~0.04 20~50 600~1200 1800~6600 1.6 CNTs – excellent properties, new applications 3D wafers Significant Market Opportunity National Science Foundation forecasts $1 trillion worth of nanotechnology-enabled products on the market by 2015 $1.4 billion Federal Research and Development Investment in 2008 2005 2010 2015 $273 Million $740 Million $3.8 Billion Source: The Fredonia Group, “Nanomaterials Demand in Composites, 2010”, © 2006 Nanocomposites Advantage: Stronger, Lighter, Less Expensive Game Changing Innovative Traditional CONVENTIONAL COMPOSITE High strength Brittle Lower weight METAL ALLOYS High strength High weight NANOCOMPOSITE High strength Not Brittle Lowest weight CNTs composites in sports industry Nitro LiteTM Ice Hockey Sticks [Montreal Sports] BMC SLC01 Pro MachineTM [Modified from “PezCycling News - What's Cool In Pro Cycling”] Baseball bats [Anaconda Sports] Babolat’s Tennis Rackets [Babolat Inc.] “Thermal management is one of the Interface key concerns in diverse fields such as Load Transfer Heat Transfer Microelectronics and Space Technology” ExtreMat Project Approach to transfer the attractive physical properties of CNTs and diamond to bulk engineering components Traditional Alloys Cu-W New Materials Al-SiC Al-Diamond Cu-Diamond Cu-CNTs New Materials with enhanced thermal conductivity Part of the work on Carbon based NanoComposites C60 “Buckminsterfullerene” Diamond Graphite Single-wall Carbon Nanotube Availability & decline in cost of synthetic diamond & CNTs Rule of Mixture λu = λrVr + λm(1 – Vr) CNT-Cu based Nanocomposites Production of Nanocomposites Powder Metallurgy Contamination & interfacial reactions Mechanical alloying Contamination & damage Compaction – HIP/Sintering Liquid Metal Infiltration (Squeeze Casting) Gas Pressure Infiltration Molecular Level Mixing Production benefits but stability of nanophases Advanced Thermal Management Materials Semiconductors, microelectronic and optoelectronic devices HEAT DISSIPATION THERMAL STRESSES WARPING Thermal Conductivity First Generation: <200 W/m-K C. Zweben, Power Elect. Tech. Feb., 2006 Excellent thermophysical props Reducing cost -Servers, notebook computers -Plasma display, PCBs -Optoelectronic packaging Second Generation: <400 W/m-K Third Generation: >400 W/m-K Nanostructure made from multiple atoms Carbon Nanotubes Electrical properties Metallic or Semiconducting conduction depending on chiralities Appearance of Quantum Effect due to 1-d structure Highly-Effective Electron Emission Metal Semiconductor Transistor, Wiring,FED Strength and Thermal Conductivity Chemical: Adsorption, Storage, Catalysts Chemical modification, Composites Mechanical: Super strong structure Due to C-C bonds Fuel cells Sensors Composite materials Challenges in Processing of CNT Based Nanocomposites Agglomeration - van der Waals forces Stability Conventional Powder Metallurgy No interfacial strength Non uniform dispersion In CNT-polymer matrix Interface is strong CNTs located on surface after mixing of metal/ceramic (no diffusion along/across powders) No improvement in properties New approach Molecular Level Mixing Mixing of CNT and powder in a solution involving molecular level mixing Interaction between the components at the molecular level due to surface functionalization of CNTs CNTs – Cu Matrix (Better Load Transfer) Homogenous distribution of CNTs in the matrix - solution based mixing Avoid damage to CNTs CNT-Cu Based Nanocomposites Functionalized CNTs + ethanol Dispersion CNT dispersion Addition of Cu(CH3COO)2.H2O Mixing Fabrication of nanocomposite powders Suspension of CNT/Salt Precursor Drying process of mixture consists of CNT/Salt Precursor Calcination & Reduction CNT/Cu composite powders Consolidation of nanocomposite powders Attachment of functional groups to remove electrostatic repulsive forces on CNTs Sintering Composite Samples Attachment of Cu ions to functional groups on CNTs Cu ions on CNTs oxidized to form powder Crystalline powder CNT-Cu based Nanostructures SEM Morphology of MWCNTs, TEM images CNT-Cu based Nanostructures Synthesis CNTs dispersion in ethanol CNTs and Copper acetate monohydrate mix Drying (100 °C) and calcination (320 °C) of mix Reduction of copper oxide Uniaxial Cold compaction Sintering @ 900 °C Characterization Interaction Between CNTs & Copper Acetate Monohydrate The absorption at 630 cm-1 and 698 cm-1 was attributed to the presence Cu-O and Cu-N bonding CO2 C- H between copper precursor and the functional group on the surface of carbon nanotubes C- O Cu- O Cu- N Which indicates the interaction O- H Chemical bonding between CNTs and copper matrix enhances the load transfer efficiency from copper matrix to CNTs CNT/Cu based Nanostructures SEM image showing morphology of synthesized Cu particles SEM image showing CNTs and Cu nanoparticles mix CNT Schematic diagram showing CNT implanted on Cu particles SEM image showing diffusion of CNTs in Cu nanoparticles SEM image of sintered composite showing stability of CNT in 5% sample New Developments in Nanotechnology Progress on Processing and Characterization of CNT Based Nanocomposites Application of New Approach - Molecular Level Mixing to achieve better interfacial properties and uniform dispersion of CNTs in copper matrix
