Far infrared scattering on plasma crystals - Ruhr
Transcription
Far infrared scattering on plasma crystals - Ruhr
Far infrared scattering on plasma crystals Dissertation zur Erlangung des Grades eines Doktors der Naturwissenschaften an der Fakultät für Physik und Astronomie der Ruhr-Universität Bochum vorgelegt von Jens Ränsch Bochum 2009 1. Gutachter: Prof. Dr. J. Winter 2. Gutachter: Prof. Dr. H. Soltwisch Tag der mündlichen Prüfung: 21.04.2009 Diese Arbeit widme ich meiner Familie. Meiner Mutter, die mich stets unterstützt und mir Halt gibt. Meiner Frau Liudmila, die mir mit ihrer Liebe Kraft und Ausdauer schenkt. Meiner jüngst geborenen Tochter Anna, die so viel Freude in unser Leben bringt. Meinem Bruder Martin und meinem Vater – ich werde sie immer in meinem Herzen tragen. I devote this work to my family. To my mother, who always stands by me and keeps me grounded. To my wife Liudmila, who gives me energy and patience through here love. To my recently born daughter Anna, who brings so much pleasure to our lives. To my brother Martin and to my father – I will always carry them in my heart. Contents 1 Introduction 1 2 Theoretical background 5 2.1 Lasers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 2.1.1 General principle of lasers . . . . . . . . . . . . . . . . . . . 5 2.1.2 The pump laser . . . . . . . . . . . . . . . . . . . . . . . . . 6 2.1.3 The FIR laser . . . . . . . . . . . . . . . . . . . . . . . . . . 9 2.2 Gaussian optics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 2.3 Capacitively coupled plasma discharges . . . . . . . . . . . . . . . . 16 2.4 Complex plasmas . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 2.4.1 OML theory . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 2.4.2 Non-isotropic plasmas—streaming ions . . . . . . . . . . . . 24 2.4.3 Barrier in the effective potential . . . . . . . . . . . . . . . . 27 2.4.4 Ion-neutral collisions—angular momentum not conserved . . 28 2.4.5 “Closely packed” dust grains . . . . . . . . . . . . . . . . . . 30 2.4.6 Summary of OML theory and neglected effects . . . . . . . . 30 2.4.7 Forces acting on dust particles in a plasma . . . . . . . . . . 31 2.4.8 Producing plasma crystals . . . . . . . . . . . . . . . . . . . 39 Light scattering by small particles . . . . . . . . . . . . . . . . . . . 43 2.5.1 Some basics of scattering theory . . . . . . . . . . . . . . . . 44 2.5.2 Rayleigh scattering by one particle . . . . . . . . . . . . . . 47 2.5.3 Scattered radiant flux at the detector . . . . . . . . . . . . . 50 2.5 3 Setup 55 3.1 The laser system . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56 3.1.1 The CO2 laser . . . . . . . . . . . . . . . . . . . . . . . . . . 56 3.1.2 The FIR resonator . . . . . . . . . . . . . . . . . . . . . . . 60 3.1.3 The mirror system . . . . . . . . . . . . . . . . . . . . . . . 64 vii viii Contents 3.2 The scattering arrangement . . . . . . . . . . . . . . . . . . . . . . 67 3.3 The plasma chamber . . . . . . . . . . . . . . . . . . . . . . . . . . 72 3.4 Setup for calibration scattering experiments . . . . . . . . . . . . . 76 3.5 CCD camera diagnostics and video analysis . . . . . . . . . . . . . 77 4 Results 4.1 81 Properties of the laser system . . . . . . . . . . . . . . . . . . . . . 81 4.1.1 FIR laser operation and beam characteristics . . . . . . . . . 81 4.1.2 The FIR laser power . . . . . . . . . . . . . . . . . . . . . . 84 4.1.3 Characteristics of the beam splitter . . . . . . . . . . . . . . 86 4.2 Results of calibration scattering experiments . . . . . . . . . . . . . 88 4.3 The crystal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91 4.3.1 Design optimisations for producing plasma crystals . . . . . 91 4.3.2 Extended plasma crystals . . . . . . . . . . . . . . . . . . . 94 4.3.3 Flat crystals . . . . . . . . . . . . . . . . . . . . . . . . . . . 96 Scattering by the crystal . . . . . . . . . . . . . . . . . . . . . . . . 99 4.4 5 Conclusion 105 Bibliography 115 Chapter 1 Introduction A variety of technological reactive plasmas is used to manufacture or treat different types of products. Some examples of such products are micro processors, flat screens, solar cells, mechanical tools, and lamps. Those plasmas often suffer from small particles growing and levitating in the plasma volume and falling down onto the work piece thereby often damaging or even destroying it. A huge research effort has therefore been initiated to understand growth and behaviour of such nano or micro particles, often called dust. During the studies of the micro particle behaviour several groups discovered a new state of dusty plasmas called plasma crystal in the year 1994 (e.g. [1, 2]1 ). The dust particles acquire a negative charge due to their accumulation of plasma electrons and ions and the higher mobility of the electrons. The inter particle electrostatic potential energy is much higher than the individual kinetic energy in a plasma crystal. The particles move only around their equilibrium positions and typical crystalline structures can be observed. These structures are similar to those observed in solids which are usually studied e.g. with X-ray diffraction techniques. The aim of this work is therefore to develop and qualify a setup for diffraction experiments on plasma crystals. Methods applied in solid state physics like the powder diffraction or the rotating crystal method are intended to be applied with this setup. These kinds of experiments reveal information about the global structure, defect density, and stability of a crystal. Further, dynamic processes like melting, structural phase transitions, waves, and fluctuations can be investigated using such methods. They always provide insight into global properties of the crystal like defect density, density of structure domains, and temperature changes through the 1 [1] Chu: Direct observation of coulomb crystals and liquids in strongly coupled rf dusty plasmas, 1994 [2] Thomas: Plasma crystal: Coulomb crystallization in a dusty plasma, 1994 1 2 Chapter 1 Introduction recording of the Debye–Waller factor. A different and worldwide extensively applied approach for analysing plasma crystals uses visible laser illumination and CCD (Charge Coupled Device) cameras to observe the light scattered by the individual particles. The movements of individual particles can be tracked and analysed with video analysis techniques. Illuminating the plasma crystal with a thin laser sheet gives a 2D image of a single lattice plane of the plasma crystal. Valuable information about particle movements within this small part of the crystal can be extracted and analysed. Other techniques illuminate the whole plasma crystal with an extended laser beam and observe the scattered light with two or three CCD cameras obtaining a 3D image of the whole crystal. However, all such methods suffer from shadowing effects and therefore can analyse small parts of the crystal or small crystals only. A different approach uses holographic images of the plasma crystal [3]2 . The 3D particle positions of all particles of the crystal are encoded within the holographic image. A drawback of this method is the very time consuming analysis of such pictures by which the 3D particle coordinates must be calculated from the image. The calculation time dramatically increases with the number of particles of the plasma crystal and only small systems can be analysed. However, the diffraction method proposed in this work may solve the problem of being restricted to small parts of a plasma crystal. The video analysis is also used in this work to characterise the plasma crystals while optimising their structure and stability. The diffraction methods can be tested and evaluated with the results of the video analysis of small parts of the crystals and vice versa. For the first time it would be possible to perform the “classical” diffraction experiments on a crystalline system simultaneously to the direct observation of the individual particles. Furthermore the method presented here may open the door for investigations of the dynamics and fluctuations of colloidal plasmas on a new global scale. Wave phenomena, phase transition dynamics, or temperature fluctuations may be analysed on a global perspective parallel to the video analysis of the individual particle movements. This can provide information about hitherto not accessible phenomena. The mean particle distance within a typical plasma crystal roughly lies between 100 µm and 500 µm. Therefore the wavelength range of the far infrared (FIR) has been chosen to do the diffraction experiments. A FIR wave guide resonator pumped by a CO2 laser has been built and characterised. A scattering arrangement has been 2 [3] Block: Structural and dynamical properties of Yukawa balls, 2007 3 developed consisting of a Yolo telescope, several tilted mirrors, and a motorised positioning system. Most window materials are not transparent in the far infrared region of the spectrum. A cylindrical polymer (TPX) plasma chamber has therefore been built because it provides roundabout optical and FIR access to the plasma crystals. The whole setup has been characterised and tested by recording diffraction peaks from a golden mesh deposited on a GaAs wafer. This demonstrates the principle of the method. The first part of this dissertation (Chapter 2) provides background information about lasers and optics, plasma discharges and complex plasmas, and light scattering by small particles. Chapter 3 describes the setup followed by the results in Chapter 4. A conclusion is given at the end. 4 Chapter 1 Introduction Chapter 2 Theoretical background This chapter briefly describes basic principles of the far infrared (FIR) laser system, important aspects of capacitively coupled plasma (CCP) discharges, complex and colloidal plasmas, and the theory of light scattering by an ensemble of particles. 2.1 Lasers The first section deals with lasers in general. The succeeding sections are about the CO2 pump laser and the FIR resonator itself. 2.1.1 General principle of lasers Detailed descriptions can be found e.g. in [4, 5, 6, 7, 8]3 . The acronym “laser” means “light amplification by stimulated emission of radiation”. To build a laser one needs a medium (in the case at hand it is a gas), an energy source, and a resonator. In principle the laser medium can be a solid, a fluid, a gas, or a plasma. Examples of the different laser types are diode lasers, dye lasers, optically pumped FIR lasers, and CO2 lasers. Such a FIR and CO2 laser are used in this work. The energy source excites (pumps) the atoms or molecules4 within the laser medium into a higher energy state. An excited molecule can relax into a lower energy state spontaneously or it can be stimulated to relax. In a laser this stimulation is done by the laser photons that travel back and forth within the resonator. They 3 [4] Siegman: Lasers, 1986 [5] Eichler: Laser – Bauformen, Strahlführung, Anwendungen, 1998 [6] Kneubühl: Laser, 1991 [7] Das: Lasers and Optical Engineering, 1991 [8] M. Young: Optics and Lasers, 1992 4 The term “molecule” is used in the following. 5 6 Chapter 2 Theoretical background disturb the excited molecules and force them to relax into the lower laser level. The photons that are emitted via this process have the same wavelength and phase like the already existing photons. The new photons are emitted into all directions and only the very few that accidentally travel nearly parallel to the resonator axis are stored within the resonator. The maximum inclination angle between the laser axis and the direction of the photons which still leads to the storage of the photons depends on the resonator design. But the laser photons not only induce stimulated emission of radiation, they can be absorbed by the laser medium as well. The Einstein coefficient for absorption of a photon of a given wavelength describes the probability that this photon is absorbed by a molecule. This molecule is thereby excited from a lower energy state into a higher one. The Einstein coefficient for stimulated emission describes the probability of the exact reverse process. These Einstein coefficients have the same value. To achieve laser activity the stimulated emission must dominate otherwise laser photons will just be absorbed. Therefore the molecular energy distribution of the laser medium must be inverted by the energy source. That means the distribution is no longer a Boltzmann distribution but there are more molecules in a higher energy level (the higher laser level) than in a lower (the lower laser level). This is called “population inversion”. Additionally the lifetime of the lower laser level must be shorter than that of the higher level to ensure that the lower level is not filled by relaxed molecules which would destroy population inversion. If the molecular energy distribution of the medium is inverted in this way then a weak beam of laser photons that travels through the medium along the resonator will be amplified. The degree of this amplification is called “small signal gain”. The amplification is due to the additional photons that are produced via stimulated emission and that have the same wavelength and phase like the original incoming laser photons of the weak beam. A small fraction (≈ 1%) of the laser photons is allowed to leave the laser through one mirror of the resonator. This is the laser beam. The photons of this beam all have the same wavelength and phase which means they are coherent. 2.1.2 The pump laser In this work a tunable, electrically excited CO2 laser (model PL5, Edinburgh Instruments Ltd.) is used as energy source to pump the far infrared (FIR) laser 7 Fig. 2.1: The CO2 molecule. A: At rest, B: Symmetrical stretching mode, C: Bending mode, and D: Asymmetrical stretching mode. active vapour within the home made FIR resonator. The CO2 laser can produce 80 lines with wavelengths between 9.2 and 10.8 µm and a power of 50 W at the strongest line. The laser active medium of the CO2 laser is a gas mixture consisting of 7 % CO2 , 18 % N2 , and 75 % He. The CO2 molecule is a three-atomic linear molecule with double bonds between the carbon and the oxygen atoms (O=C=O). The CO2 molecule can perform three normal vibrational modes as sketched in Fig. 2.1 (taken from [9]5 ). The upper laser level is the asymmetrical stretching mode (part D of Fig. 2.1, [6]6 ). In this mode the carbon atom and one oxygen atom first approach each other while the second oxygen atom departs from the carbon atom and then vice versa. Assuming no coupling between these modes they are denoted by a triple of vibrational quantum numbers n1 –n3 as shown in Fig. 2.1. The superscript of the second vibrational quantum number n2 designates the angular momentum quantum number l. This vibrational state—the bending vibrational mode—is twofold degenerated: The carbon atom can oscillate within the plane of this paper (as sketched) or perpendicular. When these two modes coexist an angular momentum appears. This gives rise to the angular momentum quantum number l of this mode. Additionally all vibrational modes are degenerated into several rotational energy states with rotational quantum numbers J. The molecule can rotate around the symmetry axis which is perpendicular to the long axis of the molecule. This leads 5 [9] Schornstein: AUFBAU UND CHARAKTERISIERUNG EINES FERNINFRAROT-RESONATORS, 2006 6 [6] Kneubühl: Laser, 1991 8 Chapter 2 Theoretical background 27 25 23 J 21 19 18 24 10P 10R 6 0 collisional excitation 9P2 collisional excitation (0 00 1) 9 R2 Energy ~0.1meV v=1 collision 26 24 J 22 20 18 26 24 22 J 20 18 0 (1 0 0) (0 20 0) (0 11 0) N2 v=0 CO2 ground state (0 00 0) Fig. 2.2: Energy level and excitation scheme for the CO2 laser with the splitting of vibrational levels into rotational levels and examples of laser lines. to a high number of possible transitions between the different vibrational states. Fig. 2.2 shows a sketch of the CO2 laser energy levels and the excitation and relaxation scheme. The CO2 molecule can be excited into the first vibrational state (0 00 1) in two ways: by collisions with excited nitrogen molecules or by collisions with electrons of the plasma discharge of the CO2 laser. The energy difference between the first vibrational energy level of nitrogen and the first vibrational level of CO2 is only about 0.1 µeV. This is by far smaller than the thermal energy at room temperature (≈ 0.03 eV). Furthermore the nitrogen molecule has no permanent dipole moment. This is the reason why radiative transitions between different vibrational levels within the same electronic state are forbidden for nitrogen. Therefore this first vibrational state of nitrogen has a relatively long lifetime which increases the probability of such a collision that transfers energy from the nitrogen to the CO2 molecule. The excited CO2 molecule in the asymmetrical stretching mode can relax into the symmetrical stretching mode ((0 00 1) → (1 00 0)) emitting a wavelength of about 10.4 µm or into the bending vibrational mode ((0 00 1) → (0 20 0)) emitting a wave- length of about 9.4 µm. The selection rules for vibrational and rotational transitions are: ∆n = 1, ∆l = 0, ±1, ∆J = ±1, ∆J = 0 forbidden [6]. 9 Fig. 2.3: Molecules within the FIR resonator. A: methyl alcohol, B: formic acid. The different lines of the CO2 laser are denoted according to the selection rules, energy levels, and wavelength involved in a transition (Fig. 2.2). An example is the line 9P36. The “9” stands for the wavelength region of this line of 9.4 µm and denotes a transition into the (0 20 0) vibrational state of the CO2 molecule. The “P” describes that the transition goes with ∆J = −1. Transitions with ∆J = +1 are designated with “R”. The different sets of laser lines are therefore referred to as “P branch” or “R branch”. The “36” of this example denotes the rotational quantum number J = 36 of the lower state into which the transition occurs. The de-excitation of the lower laser levels is very important for laser activity because the population inversion has to be maintained. The lifetimes of the lower laser levels is very long regarding radiative transitions (1–10 ms, [6]7 ). Therefore collisions of the CO2 molecules with other molecules or with the walls are necessary. This is one reason for using helium within the gas mixture. The lower laser levels of the CO2 molecules are de-excited through collisions with helium and the upper laser level is almost not affected. Furthermore helium has a high thermal conductivity and cools the laser gas. 2.1.3 The FIR laser The vapours of methyl alcohol (CH3 OH) and formic acid (HCOOH) are used as laser active media in the FIR laser resonator. They are cylindrical, slightly asymmetrical, and have a permanent dipole moment which is necessary for radiative excitation. These molecules are vibrationally excited by the CO2 laser radiation. 7 [6] Kneubühl: Laser, 1991 10 Chapter 2 Theoretical background 1. vibrational excited state radiation io at K’ CO2 laser K e J’+2 J’+1 J’ J’-1 it xc J+2 FIR J+1 J radiation J-1 n re a ax tio n l vibrational ground state Fig. 2.4: Energy levels of the FIR active molecules and excitation and relaxation scheme. For methyl alcohol the vibration and rotation are indicated in Fig. 2.3 (taken from [9]8 ). The energy difference between vibrational states of these molecules is about 0.13 eV. This corresponds to a wavelength of about 10 µm. Therefore the CO2 laser can be used as pumping source. But the pump wavelength of the CO2 laser and the absorption wavelength of the FIR molecule have to coincide very accurately because both have only narrow line width. The molecules emit FIR radiation during their relaxation from a higher rotational level within the first vibrational state to the adjacent lower rotational level in that state (Fig. 2.4). The FIR laser output power is dependent on resonator length and can be calculated within the Manley–Rowe limit using [10]9 : PF IR = 1 λP δPP . 2 λF IR (2.1) Abbreviations: PF IR and PP : FIR laser and pump laser power, λP and λF IR : pump laser and FIR laser wavelengths, δ: fraction of pump energy which is absorbed by the gas within the FIR resonator: δ =1− 1 . exp N α(ν)L (2.2) Abbreviations: α(ν): frequency dependent absorption coefficient of the pump wavelength, N : effective number of round trips of the pump radiation before dissipated 8 9 [9] Schornstein: AUFBAU UND CHARAKTERISIERUNG EINES FERNIFRAROT-RESONATORS, 2006 [10] Hodges: High-Power Operation and Scaling Behavior of CW Optically Pumped FIR Waveguide Lasers, 1977 11 by losses which are different from absorption by gas, L: resonator length. Equation (2.2) shows that a longer FIR resonator can produce higher output powers. The losses within the FIR resonator are significant (≥ 2%, [11]10 ) for: λ2F IR L > 0.05. a3 (2.3) Increasing the resonator radius thus leads to a decrease of the losses. Nevertheless, a resonator with a very large radius is disadvantageous because the molecules are de-excited through collisions with the wall. The de-excitation rate has to be large to maintain population inversion which is necessary for laser activity. Furthermore: In resonators with very large radii the FIR radiation is absorbed by the gas again. Within a resonator of a small radius the rate of de-excitation of molecules at the wall is higher and the working pressure is higher. This leads to a higher output power. But a smaller resonator radius leads to higher propagation losses. Usually FIR resonators therefore have diameters between 20 and 50 mm. The pumping and relaxation rates determine the value of the working pressure for the FIR resonator. The relaxation from a higher rotational level into a lower one is very fast (time constant τR ∝ 10 nsT orr−1 increases with pressure [12]11 ). In contrast the relaxation between the vibrational levels is very slow. Therefore the lower laser level has to be de-excited by collisions either with the resonator wall or with other laser molecules in the gas phase. The rate of diffusion to the wall is inversely proportional to pressure and square of resonator diameter: rν,dif f usion ∝ 1/(pd2 ). The collision rate within the gas is proportional to gas density and thus to pressure: rν,collision ∝ n ∝ p. The pressure can be decreased in order to increase the collision rate with the wall. But this decreases the collision rate for collisions between molecules in the gas phase to the same amount. A smaller resonator radius is therefore more suitable to increase the collision rate with the wall. In this work two resonator diameters have been used: 48 mm and 32 mm and the smaller diameter resulted in higher FIR output powers [9]12 . The optimum working pressure for the FIR laser is also determined by the absorption of pump power which is proportional to pressure. All these effects lead to a working pressure between 10 and 30 Pa in the present case. 10 [11] Degnan: The Waveguide Laser: A Review, 1976 11 [12] Jacobsson: REVIEW: OPTICALLY PUMPED FAR INFRARED LASERS, 1989 12 [9] Schornstein: AUFBAU UND CHARAKTERISIERUNG EINES FERNINFRAROT-RESONATORS, 2006 12 Chapter 2 Theoretical background The low pressure of 10 to 30 Pa inside the FIR resonator leads to Dopplerbroadening of the FIR line [12]: √ ∆νF IR = 7.162 × 10−7 ν0 T M −1 . (2.4) Abbreviations: ν0 : centre frequency of the FIR line, T : temperature (≈ 300 K), M : molecular mass in amu. The Doppler line widths of the lines of methyl alcohol (CH3 OH, M = 32, λ1 = 118.834 µm and λ2 = 170.567 µm) are thus ∆ν1 = 5.5 MHz and ∆ν2 = 3.9 MHz. The longitudinal mode spacing of the resonator ∆νres = c/2L = 100 MHz is much broader than these Doppler line widths (L = 1.5 m, fixed resonator length). The FIR line can be adjusted by tuning the resonator length. The CO2 laser pump line 9P36 is used to produce a FIR line of λF IR = 170.567 µm. This pump line has a wavelength of λCO2 = 9.695 µm, a frequency of νCO2 = 30.9 THz, and a Doppler line width of ∆νCO2 ≈ 60 MHz (eq. (2.4), with T = 300 K and M = 44 amu). Using eq. (2.4) again for methyl alcohol (T = 300 K and M = 32 amu) gives a line width of ∆νF IR ≈ 70 MHz for absorption of the pump line. Because of these small line widths the pump and absorption wavelengths have to coincide very precisely to achieve laser activity as mentioned above. Therefore only a few FIR lines can be stimulated using one type of gas and different FIR laser gases have to be used to increase the number of available FIR lines. 13 2.2 Gaussian optics The diffraction of FIR laser beams is very strong in free space (in contrast to optical laser beams) and Gaussian beam theory has to be applied to describe their propagation [4, 5]13 . The intensity of an ideal Gaussian beam is given by [5]: ! 2r2 I(r,z) = Imax exp − 2 . (2.5) ω(z) Abbreviations: Imax : peak intensity at z, r = 0, r: radial coordinate, z: distance from beam waist in beam direction, ω(z) : beam radius. The beam radius at distance z from the beam waist writes: ω(z) = ω0 s 1+ z2 . zR2 (2.6) Abbreviations: ω0 : radius of beam waist, zR : Rayleigh length. The Rayleigh length Fig. 2.5: Propagation of a Gaussian beam. The change of the beam radius from ω0 at the beam waist to ω(z) at a distant location is shown. The curved dashed lines denote the wave fronts of the beam. The radius of curvature R(z) of these wave fronts increases towards the beam waist up to infinity. θ is the asymptotic angle of divergence. zR is the distance from z = 0 at which the Gaussian beam radius is ω(zR ) = √ 2ω0 . The Rayleigh length thus marks a range where the beam is only slightly divergent (Fig. 2.5, taken from [5]). The value b = 2zR is called focal length or confocal parameter. With zR = πω02 /λ eq. (2.6) writes for the beam diameter: s 16λ2 z 2 d(z) = d0 1 + 2 4 . π d0 13 [4] Siegman: Lasers, 1986 [5] Eichler: Laser – Bauformen, Strahlführung, Anwendungen, 1998 (2.7) 14 Chapter 2 Theoretical background Fig. 2.6: Focussing of a Gaussian beam by a lens. The small beam waist after the focussing leads to a more divergent beam. The case of a spherical mirror is similar with focal length f = R/2, R denoting the radius of curvature of the mirror. a and a′ denote the distances of the beam waists to the lens/mirror. Far away from the beam waist z ≫ zR and z 2 /zR2 ≫ 1 hold and the beam expansion becomes linear: ω(z) = ω(0) z/zR . The angle of divergence θ thus writes: ω(z) ω0 λ 2λ = = = . θ∼ = z zR πω0 πd0 (2.8) The FIR resonator has two plane mirrors and produces a divergent FIR beam. To focus the FIR beam to a diameter of about 2 cm at the centre of the plasma chamber a Yolo telescope has been designed and built. This telescope consists of two spherical mirrors and the desired focal lengths of these mirrors have been calculated using the following formulae (Fig. 2.6, taken from [5]). The distance of a beam waist after a focussing element (here: spherical mirror) is given by: a′ = −f + f 2 (f − a) . (f − a)2 + zR2 (2.9) Abbreviations: a′ : distance beam waist to spherical mirror after focussing, f : focal length of mirror (f = R/2, R: radius of curvature), a: distance beam waist to mirror before focussing, zR : Rayleigh length of beam before focussing (zR = πd20 /4λ). The beam diameter at the waist after focussing writes: d′0 = p d0 f (a − f )2 + zR2 . (2.10) Abbreviations: d′0 : beam diameter at the waist after focussing, d0 : beam diameter at the waist before focussing. A computer program has been developed to calculate beam diameters, beam spot position, and spot size using equations (2.7), (2.9), and (2.10). This program has 15 a graphical interface and has been used to design the mirror arrangement of the setup. To ensure that a Gaussian beam passes almost completely through an aperture the diameter of the aperture should be at least two times the diameter of the beam [5]. Real laser beams are not ideally Gaussian and have larger diameters. Therefore the mirrors designed and manufactured for this work are as large as possible. 16 Chapter 2 Theoretical background 2.3 Capacitively coupled plasma discharges This section briefly describes some aspects of capacitively coupled plasma (CCP) discharges. There are several books, monographs, and papers about CCP discharges— see e.g. [13, 14, 15, 16]14 . Therefore only the most important and relevant details of CCP discharges are discussed here. Plasma production and maintenance The plasma is ignited between two parallel plates within a vacuum chamber. A sinusoidal voltage is applied to one of the plates (electrodes) and the other electrode is grounded. The first free electrons of the discharge are produced through impact ionisation by incoming cosmic radiation for example. Such electrons are then accelerated in the electric field of the powered electrode. They gain kinetic energy and ionise other background gas atoms through impact ionisation. The thus newly created electrons are accelerated and ionise further atoms—an electron avalanche sets in, the plasma is ignited. The plasma is maintained through further impact ionisation of background gas atoms by electrons. The bulk plasma density n0 is obtained from the energy balance of the system. Equating the absorbed to the lost power gives [14]: Pabs = n0 uB Aef f ET . (2.11) Here Pabs is the total power absorbed in the plasma, uB is the Bohm velocity: p uB = kB Te /mi , (2.12) Aef f is the effective wall area of the chamber where plasma particles are absorbed, and ET is the total energy lost from the system when an electron–ion pair is lost. ET depends on the electron temperature. Equation (2.11) shows that the plasma density is proportional to the absorbed power and thus to the input power. The plasma density also depends on the pressure of the background gas. The electron–neutral collision frequency ν increases with pressure and so does the ionisation rate. A higher pressure thus results in a higher electron density and thus in a smaller Debye length. 14 [13] Raizer: Radio-Frequency Capacitive Discharges, 1995 [14] Lieberman: Principles of Plasma Discharges and Materials Processing, Second Edition, 2005 [15] Hargis: The Gaseous Electronics Conference radio-frequency reference cell – A defined parallel-plate radiofrequency system for experimental and theoretical studies of plasma-processsing discharges, 1994 [16] Olthoff: The Gasous Electronics Conference RF Reference Cell – An Introduction, 1995 17 The electron temperature is obtained from the particle balance. Equating particle loss at surfaces to volume ionisation gives [14]: n0 uB Aef f = Ki ng n0 V, (2.13) where Ki is the rate constant for electron–neutral ionisation (in m3 /s), ng is the background gas density, and V is the plasma volume. The bulk plasma density n0 cancels out. Inserting the Bohm velocity and Ki → Ki(Te ) [14] one obtains: mi Te = 2 Ki(Te ) kB ng V Aef f 2 . (2.14) Equation (2.14) shows that the electron temperature depends on the plasma volumeto-surface ratio. Therefore the electron temperature is mainly determined by the plasma chamber geometry. Electrical properties of a capacitively coupled plasma The radio-frequency (rf) power generator of this setup produces a sinusoidal voltage at 13.56 MHz. The power generator is connected to a matching network consisting of a high pass filter and a blocking capacitor (chapter 3, p. 74). This blocking capacitor disconnects the powered electrode from the power generator for direct current (dc). Therefore (and due to the high mobility of the electrons) the powered electrode charges up negatively with respect to ground. The corresponding voltage (relative to ground) is called self-bias [13]15 . But the grounded electrode also acquires a negative charge—at least with respect to the plasma. There is a potential drop from the positive plasma potential to the zero potential of the grounded electrode. The voltage ratio of powered and grounded electrode (electrode voltages measured with respect to the bulk plasma) depends on the area ratio of powered and grounded electrode [13]: q Vpowered Agrounded = Vgrounded Apowered (2.15) with q ≤ 2.5. The reason for this relation lies in the fact that the same current has to flow through both electrodes. The smaller electrode therefore draws a higher current density and has to have a higher potential difference to the bulk plasma than the larger electrode. 15 [13] Raizer: Radio-Frequency Capacitive Discharges, 1995 18 Chapter 2 Theoretical background Fig. 2.7: presheath Sheath near a and wall. ne , ni , n0 : electron, ion, and gas density, λi : ion mean free path. When the powered electrode is connected to ground via a low pass filter the self-bias drops to zero but the plasma potential increases [13]. Therefore there is a voltage drop between bulk plasma and electrode as well. Small dust particles (diameter about 10 µm) which are introduced into the plasma charge up negatively due to the high mobility of electrons compared to that of ions. They are repelled by the electric field resulting from the self-bias or from the grounded electrode. They can be stored, levitating within the plasma some millimetres to centimetres above the lower electrode. At this position there is a force balance mainly between gravity and the electric force (sec. 2.4.7, p. 31). The sheath As described in the previous subsection the plasma chamber walls charge up negatively and the plasma potential is positive. Therefore there exists a transition layer in which the potential drops from the bulk plasma value to the wall potential. This transition layer is called plasma–wall sheath near the wall. Figure 2.7 schematically shows electron and ion density profiles and the potential profile in bulk plasma and sheath (taken from [17]16 ). As can be seen in Fig. 2.7 the ion density is less reduced compared to the electron density in the sheath close to the wall. This is because the electrons are more mobile 16 [17] Lieberman: PRINCIPLES OF PLASMA DISCHARGES AND MATERIALS PROCESSING, 1994 19 and are reflected by the negative wall potential whereas the ions are attracted by it. The sheath edge is defined as the point where the ions reach the Bohm velocity (eq. (2.12), p. 16). At this point the densities of electrons and ions start to diverge and a positive space charge develops that shields the electrons from the wall. The Bohm velocity arises when writing down energy and flux conservation of the ions within a collisionless sheath [13, 14, 18]17 . The thickness of the sheath is a few electron Debye lengths λDe (eq. (2.25), p. 23). The ions must enter the sheath with the Bohm velocity to ensure ion flux conservation. Therefore there must exist a presheath in which the ions are accelerated to that velocity by ambipolar electric fields. In this presheath ion and electron density are equal. The presheath thickness is of the order of the ion mean free path which is several times larger than the electron Debye length. Due to the variation of ion and electron density in presheath and sheath the ion and electron Debye lengths vary as well in these regions. Therefore the Debye sheath around a dust particle is not spherically symmetric but deformed or polarised. This polarisation of the Debye sheath leads to a ‘∇λD ’ force acting on dust particles which is described in section 2.4.7 (p. 33). The lower part of Fig. 2.7 shows the behaviour of the potential in presheath and sheath. The potential decreases weakly in the presheath and strongly in the sheath. Nevertheless, Tomme et al. show that the sheath potential can be well approximated by a parabola [19]18 . This leads to an electric field that increases linearly toward the electrode. This electric field gives rise to the electric force that supports the negatively charged dust particles. The ions enter the sheath with Bohm velocity and are further accelerated by the electric field. They stream with supersonic velocity and exert an ion drag force on the dust particles which levitate in presheath and sheath (sec. 2.4.7, p. 35). 17 [13] Raizer: Radio-Frequency Capacitive Discharges, 1995 [14] Lieberman: Principles of Plasma Discharges and Materials Processing – Second Edition, 2005 [18] Chen: PLASMA PHYSICS AND CONTROLLED FUSION, 1984 18 [19] Tomme: Parabolic plasma sheath potentials and their implications for the charge on levitated dust particles, 2000 20 Chapter 2 Theoretical background 2.4 Complex plasmas Complex or dusty plasmas consist of neutrals, electrons, ions, and nanometre or micrometre sized particles (so called dust). Under certain experimental conditions the dust particles can arrange themselves in ordered and stable (crystalline) structures [1, 2]19 . This state is then called “plasma crystal” which is the subject matter. A plasma crystal can form when the inter particle potential energy Epot is much higher than the individual dust kinetic energy Ekin (Epot /Ekin > 170) [20, 21]20 . Epot depends on the charge of the grains. This steady state charge is predominantly determined by the balance of ion and electron currents onto the grains in lowtemperature plasmas [22]21 . Other charging currents might be e.g. photo electron emission due to UV radiation, thermionic and secondary electron emission, field emission, radioactivity, and impact ionisation, some of which are relevant e.g. in astrophysical environments [23, 24]22 . The dust particles become negatively charged in most technological plasmas due to the high mobility of electrons compared to that of ions. In the following some theoretical considerations are presented about the charging mechanisms relevant to the case at hand. The traditional orbital motion limited (OML) theory is developed in some detail. Afterwards different effects are briefly described that can change currents, grain charge, floating potential of a dust grain, and the potential distribution around the grain. 2.4.1 OML theory The simplest way to describe charging currents, acquired charge, and floating potential of a dust grain in a plasma is the orbital motion limited (OML) approach [25]23 . The OML theory does not include any information or assumption about the potential distribution around the dust particle. It just uses conservation laws of energy and angular momentum for ions and electrons to calculate cross sections, currents, and grain charges. In doing this some simplyfying assumptions are made 19 [1] Chu: Direct Observation of Coulomb Crystals and Liquids in Strongly Coupled rf Dusty Plasmas, 1994 20 [20] Fortov: Complex (dusty) plasmas: Current status, open issues, perspectives, 2005 21 [22] Bouchoule (editor): Dusty Plasmas, 1999 22 [23] Melzer: Introduction to Colloidal (Dusty) Plasmas (Lecture Notes), 2005 [2] Thomas: Plasma Crystal: Coulomb Crystallization in a Dusty Plasma, 1994 [21] Ikezi: Coulomb solid of small particles in plasmas, 1986 [24] Shukla: Introduction to Dusty Plasma Physics, 2002 23 [25] Mott-Smith: THE THEORY OF COLLECTORS IN GASEOUS DISCHARGES, 1926 21 to obtain the different charging currents and cross sections. These are as follows. Assumptions in OML theory: 1. Isotropic plasma. 2. Maxwellian velocity distribution of electrons and ions within the plasma. 3. No effective barrier in the potential. 4. No collisions between ions and neutrals which implies conservation of angular momentum of the ions. 5. Isolated dust grains—no “closely packed” grains. 6. Pure electrostatic interaction between electrons, ions, and the dust particles. 7. Shielding is described by the Debye length λD which includes a linearisation (|eφf | ≪ kB Te ). Currents within OML theory Following [23] in writing down the energy balance for an ion coming from the 2 far distant plasma 12 mi vi,0 = 21 mi vi2 + eφf and using the conservation of angular momentum one obtains the critical impact parameter and thus the cross section for ion collection for mono-energetic ions: 2eφf 2 σc = πa 1 − , 2 mi vi,0 φf < 0. (2.16) Here a is the dust grain radius, φf is the dust grain floating potential, mi and vi,0 are ion mass and velocity far away from the dust particle. This cross section is larger than the particle geometric cross section (σ = πa2 ) due to the attraction of the positively charged ions by the dust (φf < 0). The ion charging current is given by the cross section for ion collection and the ion current density: dIiOM L = σc (vi )dji = σc (vi )ni evi f (vi )dvi , where ji = ni evi is the ion current density, ni and vi are ion density and velocity, and f (vi ) is the ion velocity distribution which is assumed to be Maxwellian: f (vi ) = 4πvi2 mi 2πkB Ti 3/2 mi vi2 exp − 2kB Ti (2.17) 22 with Chapter 2 Theoretical background R∞ 0 f (vi )dvi = 1. Ti and kB are the ion temperature and Boltzmann’s con- stant, respectively. The ion charging current is obtained by integration over the Maxwellian velocity distribution from zero to infinity with the result: eφf OM L 2 , (2.18) Ii = πa ni evth,i 1 − kB Ti p where vth,i = 8kB Ti /πmi is the ion thermal velocity (mean velocity in a Maxwell distribution). The electron current can be obtaining the cross section for derived analogously, 2eφ f electron collection: σce = πa2 1 + me v2 which is smaller than the geometric cross e,0 section because of the repulsion of the electrons by the negatively charged dust grain (φf < 0). Integration of the electron current density over the Maxwell distribution gives: eφf . (2.19) = −πa ne evth,e exp kB Te Here the integration starts at a minimum electron velocity given by the floating p potential (vmin = −2eφf /me ) because the electrons have to overcome the elecIeOM L 2 trostatic barrier due to the negatively charged dust grains. Interpreting this equation it is the thermal electron current to a neutral particle but reduced by the Boltzmann factor because the electrons are repelled by the negatively charged dust grain. Potential distribution within OML theory The steady state floating potential of a grain is obtained by equating electron and ion current which yields: eφf 1− = kB Ti r ne vth,e exp ni vth,i eφf kB Te . (2.20) This equation can be solved numerically for φf . The potential distribution in the vicinity of the dust particle is obtained by solving Poisson’s equation: e (ni − ne ) (2.21) ǫ0 using a Boltzmann distribution for electrons and ions for the simplest case: eφ(r) , (2.22) ne,i (r) = n0 exp ± kB Te,i ∆φ = where the plus sign is for electrons and the minus sign for positive ions. By inserting this into the Poisson equation and linearising (assuming |eφ(r) | ≪ kB Te,i ) one 23 obtains: φ , (2.23) λ2D with the linearised Debye length λD defined by the electron and ion Debye lengths: ∆φ = 1 1 1 = 2 + 2 . 2 λD λDe λDi These write in particular: (2.24) r ǫ0 kB Te,i , (2.25) e2 n0 where n0 is the electron density in the far distant (quasi-neutral) plasma. In the λDe,i = case of spherical symmetry the solution of the linearised Poisson equation (2.23) is the Debye–Hückel potential or screened Coulomb potential [22]: r−a a . φ(r) = φf exp − r λD (2.26) The linearised Debye length is closer to the ion Debye length for plasmas with Te ≫ Ti as it is the case in this work. The Debye–Hückel potential has been derived here with the certainly not fulfilled assumption of ions with a Boltzmann distribution. Nevertheless, a more detailed discussion of the ion density distribution under OML conditions leads to the same result for the potential [22]24 . Grain charge within OML theory The grain charge Qd is now approximated by assuming the grain capacitance to be C = 4πǫ0 a(1 + a/λD ) that reduces to the vacuum value for λD ≫ a and ap- plying Qd = Zd e = Cφf . Here Zd denotes the number of charges on the grain and φf is the grain floating potential calculated from equation (2.20) (p. 22). This approximation is problematic because it uses the Debye length and therefore includes the linearisation |eφf | ≪ kB Te which “is not satisfied for a floating sphere” [26]25 . However, for the case λD ≫ a it yields quite good results at least for conducting spheres compared to the results of a self-consistent numerical particle-in-cell (PIC) simulation by Hutchinson [26]. OML theory is the standard theory for the description of particle charging phenomena in an isotropic plasma. However, some effects and phenomena are neglected but lead to big changes in grain charge, current, and potential distribution. Some of these effects are described in the next sections with a summary and comparison in sec. 2.4.6 (p. 30). 24 [22] Bouchoule (editor): Dusty Plasmas, 1999 25 [26] Hutchinson: Ion collection by a sphere in a flowing plasma: 3. Floating potential and drag force, 2005 24 Chapter 2 Theoretical background 2.4.2 Non-isotropic plasmas—streaming ions The dust grains in the experiments presented here levitate near the lower electrode in the plasma–wall sheath or presheath region. The plasma is certainly not isotropic in these regions and the ions are streaming toward the electrode with very high and even supersonic velocity. Therefore the first two assumptions underlying the OML theory (isotropy and Maxwell distribution) are not valid in the presented situation. In the following only the ion currents to dust particles are treated because the ions have a major effect on structure and dynamics of plasma crystals. Furthermore, electron streaming has no effect since streaming velocities of electrons are far below the electron thermal velocity [27]26 . Currents with streaming ions Drifting ions can be included in the OML theory through a drifting Maxwellian velocity distribution: f (vi ) = 4πvi2 mi 2πkB Ti 3/2 mi (vi − ui )2 exp − 2kB Ti . (2.27) Here ui denotes the ion drift velocity. A different ion current to the dust particle is then obtained if the OML cross section for ion collection is used [20, 28]27 . When the drift velocity ui is very large (ui ≫ vth,i ) one can replace vth,i with ui and kB Ti with 21 mu2i in equation (2.18) (p. 22) for the OML ion current yielding: Ii = πa2 ni eui (1 − 2eφ/mi u2i ) (2.28) for the ion current to a dust particle in the case of very fast streaming ions and conducting spheres [23]. Grain charge with streaming ions The dust grain charge computed by the OML theory is quite accurate for conducting spheres even with ion flow when the Debye length is much larger than the sphere radius [26]. Hutchinson describes a fully self-consistent numerical approach which uses the particle-in-cell (PIC) method [26]. Especially insulating spheres are difficult to describe analytically because they charge up asymmetrically. The results show that for insulating spheres the OML theory predicts a grain charge that is 26 [27] Lampe: Interactions between dust grains in a dusty plasma, 2000 27 [20] Fortov: Complex (dusty) plasmas: Current status, open issues, perspectives , 2005 [28] Whipple: Potentials Of Surfaces In Space, 1981 25 Fig. 2.8: Dimensionless dust particle charge z = |Z|e2 /(4πǫ0 akB Te ) of an isolated spher- ical particle as a function of ion drift velocity ui in Mach numbers or normalised to vth,i . The calculations are for three different electron-to-ion density ratios and correspond to an Ar plasma with Te /Ti = 100. An increasing charge due to a decreasing ion collection cross section (eq. (2.16), p. 21) is followed by a charge decrease due to the positive space charge near the electrode. by far too low, meaning that the real charge is more negative. The reason for this lies in the development of a strong negative potential on the side of the insulating grain that is downstream to the ion flow. The ion flux reaching the dust surface is much smaller on this downstream side. Fortov et al. discuss the behaviour of the particle charge in the sheath region near the electrode as a function of the ion drift velocity ui [20] (Fig. 2.8, taken from [20]). The ion velocity increases towards the electrode due to the linearly increasing (averaged) electric field in the sheath [19]28 . Therefore this discussion is also a discussion of particle charge as a function of height above the electrode. At low ui the charge is constant and equal to the OML charge. The charge firstly increases when ui > vth,i . This is due to the decreasing collection cross section for ions with increasing ion velocity; see equation (2.16) on page 21. The dust particle charge decreases again when the ion drift velocity becomes several 10 times the ion thermal velocity. This is because a positive space charge develops near the electrode where ui is high. This leads to a higher ion flux to the dust particles compared to the electron flux. Therefore the particle charge gets less negative. A dust particle can thus even become positively charged when it comes very close to the electrode. Potential distribution with streaming ions The surface potential varies with position on the surface of insulating spheres because of the asymmetrical charging. The local current density is zero in this case. 28 [19] Tomme: Parabolic plasma sheath potentials and their implications for the charge on levitated dust particles, 2000 26 Chapter 2 Theoretical background Fig. 2.9: Contour plot of the ion density, showing ion focusing, for three different velocities of ion flow. The plot is presented in the grey-scale topography style; regions A correspond to ion densities ni < ni0 , and regions B correspond to ion densities ni > ni0 . The ions are focusing behind the grain, thus forming a region with highly enhanced ion density. The distances are given in units of the electron Debye length. A conducting sphere acquires a constant surface potential which is not positionally dependent. The total current density is zero in this case. An ion cloud is formed downstream the dust particle due to the ion flow toward the electrode. Ions coming from the distant plasma are attracted by a dust particle. Therefore the ion trajectories are bended toward the dust particle and eventually end at the particle surface. But not all ions fall onto the dust grain. So, the dust grain acts as a focusing lens for the streaming ions. A dust particle located below will be attracted by the positively charged ion cloud [29, 30, 31]29 . This has important consequences for the particles of a plasma crystal. They can arrange in vertical strings with one dust grain located directly below another. A perturbed region of plasma density—a wake—can be formed downstream a dust particle at low pressure (low collisional damping), high electron-to-ion temperature ratios (low Landau damping), and Mach numbers of the ion velocity around M = 1 [27]30 . The ion density can show several maxima and minima over several 10 Debye lengths downstream the dust particle [32]31 (Fig. 2.9, taken from [32]). Lampe et al. show the weakening of the wake effect with increasing pressure up to ≈ 10 Pa [27]. A pronounced wake is thus not expected in the presented experiments of this work since the working pressures are much higher (up to 100 Pa). Nevertheless, the first pronounced maximum in ion density certainly develops in 29 [29] Melzer: Structure and stability of the plasma crystal, 1996 [30] Melzer: Transition from Attractive to Repulsive Forces between Dust Molecules in a Plasma Sheath, 1999 [31] Melzer: Laser manipulation of particles in dusty plasmas, 2001 30 [27] Lampe: Interactions between dust grains in a dusty plasma, 2000 31 [32] Maiorov: Plasma kinetics around a dust grain in an ion flow, 2001 27 the present case and leads to the observed particle string formation. In such a particle string several dust grains are aligned vertically—one grain directly below the other. 2.4.3 Barrier in the effective potential The trajectory of an ion approaching a negative dust grain will be bended and the ion will eventually fall onto the grain provided the impact parameter is below the critical one. But if the ion has a high angular momentum (within the central potential φ(r) of the grain) it can miss the grain even if the impact parameter is low enough. The ion velocity is simply not strictly enough directed toward the dust grain in this case. From the view point of the potential this means that there is a barrier in the potential [20, 27]32 and one has to use an effective potential which is derived from the energy balance: 1 2 E = Ekin + Erot + Epot = m vr2 + vΘ + eφ(r) , 2 2 with mvΘ = 2 r2 m2 vΘ mr 2 = L2 mr 2 (2.29) (L is the angular momentum of the ion and r the distance to the grain). The effective potential thus writes: Uef f = eφ(r) + L2 , 2mi r2 (2.30) with vr and vΘ being radial and angular velocity. Thus some low energy ions can be reflected from this potential barrier reducing the ion current to the dust grain and leading to a lower grain charge (more negative). Fortov et al. [20] estimate the applicability of the OML theory regarding the neglect of this potential barrier to be good in cases with λD > 5a. Since the potential barrier is very small in most of the cases [33, 34, 35]33 only ions with low kinetic energy are reflected from this barrier. Therefore the decrease of the ion current to the dust particle due to the potential barrier is only a weak effect. 32 [20] Fortov: Complex (dusty) plasmas: Current status, open issues, perspectives, 2005 33 [33] Lampe: Trapped ion effect on shielding, current flow, and charging of a small object in a plasma, 2003 [34] Sternovsky: Ion collection by cylindrical probes in weakly collisional plasmas: Theory and experiment, 2003 [35] Lampe: Effect of Trapped Ions on Shielding of a Charged Spherical Object in a Plasma, 2001 28 Chapter 2 Theoretical background 2.4.4 Ion-neutral collisions—angular momentum not conserved The OML theory neglects ion–neutral collisions in the calculation of the grain charge even though there must be such collisions to maintain the Maxwell distribution in the ambient plasma. It is simply assumed that an ion is coming from a Maxwellian plasma and eventually hits the grain but certainly without a further collision. But collisions in the vicinity of a dust grain can be quite important even if the ion mean free path li is much larger than the screening length λD [20, 33, 34, 35]. Since the working pressures in the case at hand are fairly high (1 to 100 Pa) a discussion of the influence of ion–neutral collisions on dust grain charge and shielding seems most appropriate. In the presented case the argon density lies roughly between 2 × 1020 m−3 for a pressure of 1 Pa and 2 × 1022 m−3 for 100 Pa. An estimation for the total ion– neutral collision cross section is given in [14]: σitotal ≈ 10−14 cm2 . This cross section includes elastic scattering and charge transfer collisions. The ion mean free path −1 li = ng σitotal then lies between about 4 mm for a pressure of 1 Pa and 0.04 mm for 100 Pa. Grain charge with collisions Especially ion–neutral charge-exchange collisions have a great impact on ion current, grain charge, and shielding. Every such an event creates a new ion with only the thermal velocity of the background gas. This new ion can then easily be absorbed by the grain which leads to a higher ion current onto the grain and thus to a lower charge (less negative). The cross section for charge-exchange collisions between ions and neutrals is higher than that for specular reflection for the relevant ion energies. Furthermore, some newly created ions may perform orbits around the dust particle depending on their initial energy and angular momentum. If the kinetic energy is too large, the ion can escape from the particle—if the energy is too low, it will fall onto the dust grain. Potential distribution with collisions Lampe et al. derive a condition for ions to be trapped in the potential well near the dust grain [33]: r2 φ(r) < a2 φ(a) (r: distance between an ion and the grain, a: grain radius). Thus a positive shielding cloud is created which is “trapped” in the 29 particle potential very near the grain and moves together with the dust grain. This is essentially different to the usual Debye shielding: The trapped ion cloud provides additional shielding against external electric forces thus changing the interaction with other dust grains. Such an ion cloud can even be polarised leading to vander-Waales interactions between dust particles. In the usual Debye case shielding is provided by ions and electrons that move through the entire plasma and are not bounded to a dust grain. These moving ions and electrons cannot screen external electric forces. The creation rate of trapped ions is proportional to the ion–neutral collision frequency ν and so is the loss rate of the trapped ions. They can be scattered out of the potential trap or—more probably—fall onto the grain after a further collision. Therefore the number of trapped ions within the Debye shield of a dust particle is independent of the neutral gas pressure in the “weakly” collisional regime [36]34 . But the creation rate is proportional to the plasma density and so is the density of the trapped ions. Currents with collisions Lampe et al. derive an expression for the ion flux to a dust grain including collisions (but not streaming ions) which gives the following ion current [33]: Iicoll 2 ≈ πa ni evth,i eφf r3 1− + 2T kB Ti a li . (2.31) Here rT is a shielding radius determined by the equality of potential and thermal energy of an ion: Epot = Eth : eφ(rT ) = − 23 kB Ti . It means that an ion created in a charge-exchange collision at this distance is likely to be trapped. In this “weakly” collisional regime the ion current increases with pressure due to the higher plasma density and accordingly more frequent charge-exchange collisions within the sheath surrounding the grain. But if the pressure increases to much higher values eventually the “strongly” collisional regime is reached. In this regime the ions make many collisions and the motion is mobility controlled [20]. Since the mobility decreases with increasing pressure the ion flow onto the dust particle decreases as well. Therefore there exists a maximum in the ion current onto a grain when the neutral gas pressure is increased. 34 [36] Goree: Ion Trapping By A Charged Dust Grain In A Plasma, 1992 30 Chapter 2 Theoretical background 2.4.5 “Closely packed” dust grains The quasi-neutrality condition of the plasma has to include the charge on the dust grains—especially when the dust density is very high: ni = ne + Znd . The electron density is depleted due to the absorption of electrons by the dust grains making the ion density larger than the electron density. Therefore the individual dust grain charge is reduced (less negative) because there are not enough electrons in the vicinity of a single particle to provide the negative charge that would arise in the case of an isolated particle in a plasma without other dust particles. The Havnes parameter describes the strength of this effect: P = |Z|nd /ne . If P ≪ 1 the grain charges tend to the value of an isolated particle while in the case of P ≫ 1 the grain charges are reduced significantly [20, 23]35 . Furthermore, closely packed dust grains can distort trajectories of electrons and ions when the inter grain distance is smaller than the typical interaction length between electrons/ions and the dust particles. This can also lead to a charge reduction [20]. 2.4.6 Summary of OML theory and neglected effects The orbital motion limited (OML) theory describes the charging of a dust grain in a plasma in the most simple way. It assumes an isotropic, Maxwellian plasma without ion–neutral collisions and potential barrier. The interaction between dust particles is assumed to be purely electrostatic. Using the conservation of energy and angular momentum for an incoming ion a cross section for ion collection is derived. Integration of the product of this cross section with the ion current density over a Maxwell distribution leads to the ion charging current. The electron charging current is derived analogously. By equating these currents the floating potential can be calculated numerically. Solving Poisson’s equation by assuming a Boltzmann distribution for electrons and ions one obtains the Debye–Hückel potential with the linearised Debye length. Finally, the grain charge is calculated inserting a certain expression for the grain capacitance which is multiplied by the floating potential. Table 2.1 summarises the effects which are not governed by the OML theory but lead to a different charge on dust grains. 35 [20] Fortov: Complex (dusty) plasmas: Current status, open issues, perspectives, 2005 [23] Melzer: Introduction to Colloidal (Dusty) Plasmas (Lecture Notes), 2005 31 Mechanism Grain charge compared to OML Streaming ions more negative (strong effect) Insulating grains more negative (strong effect with streaming ions) Barrier in effective potential more negative (weak effect) Ion–neutral collisions less negative (strong effect, trapped ions) Closely packed grains less negative (strong effect) Table 2.1: Effects on grain charge for different mechanisms not included in OML theory. Streaming ions lead to a higher negative grain charge because less ions reach the grain on the downstream side and the ion collection cross section decreases with increasing ion velocity. PIC simulations reveal a higher negative dust grain charge for insulating particles compared to conducting particles. This is even enhanced by streaming ions. These effects are important for the presented case since the dust particles levitate near the lower electrode in the sheath or presheath region of the plasma where ions are streaming with even supersonic velocity. A barrier in the potential distribution around a grain arises because of the angular momentum of incoming ions. But this barrier in the effective potential is only small, typically. Thus only low energy ions are reflected from it and this effect is of minor importance. Ion–neutral collisions in the vicinity of a dust grain increase the ion current to the grain and thus reduce the grain charge strongly. Especially charge-exchange collisions are very important. Through such a collision a slow ion is created that is effectively attracted by the dust grain. The pressures used in this experiment lie between 1 and 100 Pa and are thus fairly high. Ion–neutral collisions thus play a significant role. When the dust number density is very high the electron density is depleted compared to a dust free plasma. Therefore the grain charge is less negative compared to a single particle within a plasma without any further dust grains. This effect is of minor importance because dust densities are not that high in the present case. Different ion currents and potential distributions are listed in table 2.2. 2.4.7 Forces acting on dust particles in a plasma Dust particles in a plasma are subject to various forces. The relevant forces are briefly described in this chapter and the appropriate formulae are given. Detailed 32 Chapter 2 Theoretical background Theory OML Streaming ions Collisions Ion current Ii πa2 ni evth,i 1 − eφf kB Ti ≈ πa2 ni eui (1 − 2eφf /mi u2i ), ui ≫ vth,i 3 rT eφf 2 ≈ πa ni evth,i 1 − kB Ti + a2 li Potential φ(r) φf ar exp − r−a λD ion wake, numerics trapped ions, numerics Table 2.2: Ion currents and grain potentials for different effects included. derivations and discussions can be found in several textbooks and articles e.g. [20, 22, 23, 24]36 . The main forces which determine the levitation height of the dust particles above the lower electrode are gravity and the electric force. Gravity pulls the particles out of the plasma volume whereas the electric force confines them. Some of the forces depend on the ratio of grain radius to Debye length (a/λD ). This ratio is not generally small as far as plasma crystals are concerned. Debye spheres can partly overlap making strong coupling between grains possible. Gravity Gravity is the most intuitive force of all: 4 F~G = m~g = πa3 ρ~g , 3 (2.32) where m is the dust particle mass, ~g the gravitational acceleration, and ρ the particle density. Gravity is thus proportional to the cube of the dust particle radius. Electric force The vacuum electrostatic force Qd E is a good approximation of the electric force provided the dust grain is conducting and the radius is small compared to the Debye length [22]. The Debye sheath around the dust particle does not screen the particle from an external electric field E (e.g. originating from the electrode or from other grains). This is so because the Debye sheath is not attached to the dust grain but just a local variation of the plasma density. The ions and electrons that constitute the Debye shielding are moving through the entire plasma. Their respective densities and velocities are changed in the vicinity of a dust grain, but they are not attached to the grain. 36 [20] Fortov: Complex (dusty) plasmas: Current status, open issues, perspectives, 2005 [22] Bouchoule: Dusty Plasmas, 1999 [23] Melzer: Introduction to Colloidal (Dusty) Plasmas (Lecture Notes), 2005 [24] Shukla: Introduction to Dusty Plasma Physics, 2002 33 The situation becomes different when collisions are taken into account. Then a number of ions can be trapped in the potential well near the dust grain (sec. 2.4.4, p. 28). These trapped ions can move together with the particle and effectively screen an external electric field. Applying the capacitor model of section 2.4.1 (p. 20, C = 4πǫ0 a(1 + a/λD )) to the grain one obtains: a ~ ~ ~ FE = Qd E = 4πǫ0 a 1 + φf E. λD Here, a is the particle radius, λD the Debye length, and φf the floating potential of the particle. This formula reduces to ~ F~E = 4πǫ0 aφf E (2.33) in cases with λD ≫ a. The electric force is then proportional to the dust particle radius. Effects that can change this expression of the electric force are e.g. polarisation of the conducting grain and polarisation of the shielding cloud in the sheath of a discharge. But the force induced by the polarisation of a conducting grain is exactly cancelled out by an ion drag force that is induced by that polarisation [37]37 . The same authors derived a force present in sheath and presheath regions where the Debye length changes spatially. The sheath electric field polarises the Debye sheath around the particle. This ‘∇λD ’ force writes: Q2 ∇λD F~∇λD = − d 8πǫ0 (λD + a)2 (2.34) and points in the direction of decreasing Debye length and thus toward higher plasma densities (eq. (2.25), p. 23). It supports the electrostatic force in levitating the dust particles above the lower electrode. Bouchoule et al. calculated the ratio of the ‘∇λD ’ force to the electrostatic force and found that it is of the order of a/λD [22]. The ‘∇λD ’ force can therefore only be neglected in cases with λD ≫ a which is not necessarily true in the case of plasma crystals. Ion focus A different electric and attractive force between dust grains can arise in the case of streaming ions when two or more dust particles are located below each other. As 37 [37] Hamaguchi: Polarization force on a charged particulate in a nonuniform plasma, 1994 34 Chapter 2 Theoretical background Fig. 2.10: Interparticle forces in a dust molecule. described in section 2.4.2 (p. 24) an ion cloud can develop beneath a dust particle when ions are streaming by [27, 29, 30, 31, 32]38 . This means a positive space charge is generated which attracts the grain directly below. Melzer gives the equation of motion for the lower particle of a two particle system [30]: Qupper Qlower d x. md ẍ = −md β ẋ − (ǫ − 1) d 4πǫ0 d3 (2.35) Here x is a small deviation from the vertically aligned situation, md is the dust particle mass, β is the friction coefficient for the dust particles within the neutral background, and Qupper and Qlower are the charges of the upper and lower dust d d grain. ǫ denotes the ratio of attractive (due to ion focus) to repulsive force (due to negative dust charge). d gives the vertical distance between the upper and lower particle (Fig. 2.10, taken from [30]). This electric force caused by the ion focus is of particular importance for the observed vertical dust particle rows of up to several 10 particles in the presented experiment. But in a plasma crystal the situation is more complex. The ion cloud of a neighbour dust molecule within a plasma crystal also attracts the lower particle. Therefore the situation sketched in Fig. 2.10 should be unstable: If the lower particle moves towards a neighbour dust molecule it is more and more attracted to it and finally would reach an equilibrium position in the middle between the two dust 38 [27] Lampe: Interactions between dust grains in a dusty plasma, 2000 [29] Melzer: Structure and stability of the plasma crystal, 1996 [30] Melzer: Transition from Attractive to Repulsive Forces between Dust Molecules in a Plasma Sheath, 1999 [31] Melzer: Laser manipulation of particles in dusty plasmas, 2001 [32] Maiorov: Plasma kinetics around a dust grain in an ion flow, 2001 35 molecules. The fact that this does not happen (at low pressures) is due to the ion stream and the resulting space charge which is not shown in Fig. 2.10 but indicated in Fig. 2.9 (p. 26). The downstream dust particle of a dust molecule stays relatively straight downstream the upper particle due to the higher ion density there (region B in Fig. 2.9, dark regions) compared to regions well aside (region A in Fig. 2.9). Ion drag A dust grain in a plasma is continuously bombarded by ions and electrons. The plasma particles (electrons and ions) thus exert a force (a drag) to the grain. The force caused by electrons can be neglected because of their low mass. The ion drag force consists of two parts: (i) the collection force and (ii) the orbit force. (i) The collection force arises due to collisions of ions with the dust particle. The ions immediately stick to a dust grain in a collision and transfer their momentum to the dust particle. Using the cross section for ion collection (equation (2.16), p. 21) the collection force is obtained: F~coll 2 where vs = u2i + vth,i 1/2 2eφf = mi vs ni πa 1 − ~ui , mi vs2 2 (2.36) is the mean ion velocity [23]39 . The collection force is thus proportional to the square of the dust particle radius. (ii) The orbit force is exerted by ions which are not collected by the grain but deflected in its electric field. The cross section for Coulomb collisions between an ion and a dust particle reads after Barnes et al. [22, 38]40 : ! 2 2 λ + b D π/2 σcCoul = 2πb2π/2 ln , b2c + b2π/2 (2.37) where bπ/2 = eφf a/mi vs2 is the impact parameter (using Qd = 4πǫ0 aφf ) with the asymptotic scattering angle of π/2 and bc is the critical impact parameter at which an ion is collected. The logarithm is the so called Coulomb logarithm. This expression only includes ions approaching the dust particle with a critical impact parameter bc < λD . The orbit force is then given by F~Orbit = ni mi vs σcCoul u~i which 39 [23] Melzer: Introduction to Colloidal (Dusty) Plasmas (Lecture Notes), 2005 40 [22] Bouchoule: Dusty Plasmas, 1999 [38] Barnes: Transport Of Dust Particles In Glow-Discharge Plasmas, 1992 36 Chapter 2 Theoretical background reads in total: Barnes F~Orbit (eφf a)2 ln = 2πni mi vs3 λ2D + b2π/2 b2c + b2π/2 ! u~i . (2.38) The orbit force is thus proportional to the square of the dust particle radius as well. Khrapak et al. have included ions that approach the dust particle closer than λD regardless of their initial impact parameter [39]41 . Every ion is included whose minimal distance to the dust grain is λD . This leads to a considerably higher cross section for Coulomb collisions in the case of sub-thermal ion flow (ui < vth,i ) and thus to a higher orbit force. This Khrapak expression for the orbit force is thus applicable in the presheath region of the discharge. Using again Qd = 4πǫ0 aφf the orbit force writes [39]: Khrapak F~Orbit √ 8 2π eφf = + ni a2 mi vth,i 1 + 2 3 2mi vth,i eφf 2 2mi vth,i !2 Λ u~i , (2.39) where Λ is the Coulomb logarithm integrated over the shifted Maxwellian distribution: Λ=2 Z 0 ∞ 2λD x + ρ0 exp (−x) ln dx. 2ax + ρ0 (2.40) 2 ρ0 = Qd e/(4πǫ0 mi vth,i ) is the Coulomb radius. The scattering angle is large for ions with an impact parameter less than ρ0 and small otherwise. The thermal ion velocity vth,i is used here because ui < vth,i in the presheath region where this formula holds. In comparison of these both ion drag forces (equations (2.36)—collection force, (2.38)—orbit force for super-thermal, and (2.39)—orbit force for sub-thermal ion flow) the following can be concluded: Both ion drag forces are proportional to the square of the dust particle radius (∝ a2 ) and to the ion drift velocity (∝ ui ). However, the orbit force is proportional to the inverse cube of the mean velocity 1/2 2 vs = u2i + vth,i (or to the inverse cube of the thermal ion velocity in the sub- thermal regime) whereas the collection force has contributions proportional to vs−1 and to vs itself. Thus the orbit force is large at small vs (and small drift velocities ui ). It is the dominant contribution to the ion drag in the range ui ≤ 4vth,i (see Fig. 2.11 taken from [23]). The collection force dominates the ion drag at higher drift velocities. 41 [39] Khrapak: Ion drag force in complex plasmas, 2002 37 Fig. 2.11: Comparison of ion drag forces. Total force, collection force, and orbit orbit force are shown. The orbit force is dominant for small ion drift velocities. This diagram is of general validity (normalisation to πa2 mi ni ). The graph is thus independent of dust size, ion mass, and ion density. Neutral drag Ions bombard a dust grain in a plasma and so do neutrals. The neutral drag force can be calculated using the Epstein formulae for pressures below i.e. 100 Pa: 4 F~N = − πa2 mN nN vth,N (~uD − ~uN ) , 3 (2.41) where mN , nN , and vth,N are mass, density, and thermal velocity of the neutrals, respectively. (~uD − ~uN ) is the relative velocity between dust particles and neutrals [22]42 . Thus the neutral drag is proportional to the square of the dust particle radius and to the relative velocity of dust grain and neutrals. The effects of the neutral drag force are clearly seen in the experiments and strongly influence plasma crystal formation. Therefore only low and constant flow rates of Argon gas have been used in this work to minimise neutral drag. Thermophoresis A further force can act on the dust particles when the neutral gas temperature is not uniform. Then the thermal velocity of neutrals coming from the hot side is higher than the thermal velocity of neutrals coming from the cold side. Thus a net force is exerted on the dust particle. This force is proportional to the temperature gradient and reads [22]: 32a2 F~th = − 15vth,N 5π 1+ (1 − α) κT ∇TN , 32 (2.42) where κT and TN are the thermal conductivity of the gas and gas temperature, 42 [22] Bouchoule: Dusty Plasmas, 1999 38 Chapter 2 Theoretical background respectively. Thus the thermophoretic force is proportional to the square of the dust grain radius and to the temperature gradient. α is the so called accommodation coefficient which describes the type of neutral particle reflection considered: α = 0 for specular reflection and α = 1 for perfect diffuse reflection. Perfect diffuse reflection means that the neutral particle is first adsorbed at the dust particle surface, reaches the dust particle temperature, and is then desorbed. The value of α can be adjusted to account for intermediate cases. Influences of the thermophoretic force on the dust particles have been observed in this experiment with values of ∇TN as small as 1 Kcm−1 . Experiments are therefore performed under stable temperature conditions in the laboratory without draught. The forces discussed so far are present in plasma crystals as well as in the case of only a few particles in a plasma. The next two forces are found only in plasmas with a high dust particle density. Shadowing force Ions hit a dust particle and exert a force—the ion drag. In a uniform plasma with no directed ion flow and no density variations the total ion drag to a dust particle is zero. This is so because equal numbers of ions hit the dust grain from each side with equal mean velocities. If there are two nearby dust particles—particle A and B—particle A can collect some ions which would hit particle B if particle A was not there. The ion drag coming from the inter particle region is smaller than the ion drag originating from outside. Therefore there exists a net force which pushes the particles closer to each other. This force is proportional to a4 /r2 where r is the inter particle distance [40]43 . Long range repulsion Far distant dust grains can influence each other via a long range force. This force is repulsive and originates from the influence of dust particles on ion trajectories. The trajectory of an ion may be bended due to the presence of other dust particles in a way that the ion may therefore hit a specific dust particle which it would miss without the other dust grains. This force is therefore a kind of “dust-particlemediated-ion-drag”. It is proportional to Z 2 a/r3 [40]. 43 [40] Tsytovich: Dust plasma crystals, drops, and clouds, 1997 39 Force Dependencies; equation Important in. . . Gravity a3 , ρparticle ; (2.32) whole plasma Electric force a, φf ; (2.33) sheath Ion focus x, d−3 , Qd ; (2.35) sheath, presheath Ion drag—collection a2 , ni , φf , vs + vs−1 ; (2.36) sheath Ion drag—orbit, ui > vth,i Ion drag—orbit, ui < vth,i Neutral drag Thermophoresis Shadowing force Long range repulsion 2 a , ni , φ2f , vs−1 (Barnes); (2.38) −3 a2 , ni , φ2f , vth,i (Khrapak); (2.39) a2 , nN , vth,N , ~uD − ~uN ; (2.41) sheath a4 , r−2 , r= b particle separation dense dust cloud −1 a2 , vth,N , −∇TN ; (2.42) a, r −3 presheath whole plasma whole plasma dense dust cloud Table 2.3: Different forces acting on dust particles in complex plasmas, their dependencies on particle radius and plasma properties, and the region where they are important. Table 2.3 lists the forces discussed and their dependencies. 2.4.8 Producing plasma crystals The particles in a complex plasma levitate in regions of the discharge where the different forces are balanced. The force balance is reached near the lower electrode in the sheath or presheath region of the plasma. A relatively strong electric field exists in these regions. It is therefore advantageous to have a plasma with an extended sheath to produce extended plasma crystals. Sinceqthe sheath thickness lies in the range of several electron Debye lengths with λDe = ǫ0ek2Bn0Te , a high electron temperature Te and a low electron density n0 are favourable. The latter is proportional to the input power of a capacitively coupled discharge (eq. (2.11), p. 16 and [14, 41]44 ). Therefore the experiments were carried out with the lowest input power possible (5 W or below). The electron density increases with the discharge pressure (sec. 2.3, p. 16). A low discharge pressure seems therefore suitable to produce big plasma crystals. But a high friction force (neutral drag) is needed to damp the dust particle motion as much as possible. This makes higher pressures more appropriate. Therefore an 44 [14] Lieberman: Principles of Plasma Discharges and Materials Processing – Second Edition, 2008 [41] Boeke: Lithium-Atomstrahl-Spektroskopie als Diagnostik zur Bestimmung von Dichte und Temperatur der Elektronen in Niedertemperaturplasmen, 2003 40 Chapter 2 Theoretical background optimum has to be found regarding the discharge pressure. The electron temperature is not as easily tunable as the electron density. It is predominantly determined by the production and loss mechanisms of the electrons which are necessary for the maintenance of the discharge. Since the main loss mechanism are collisions with the wall the discharge geometry sets the electron temperature (eq. (2.14), p. 17 and [14]). String formation The principles of the formation of dust particle strings and crystals are described e.g. in [42]45 . The ion flow within the sheath where the dust particles are situated leads to the formation of dust particle strings. A wake develops downstream a dust particle with a positive space charge directly below the particle. This positive space charge attracts the nearest downstream neighbour particle (sec. 2.4.7, p. 34). The dust particle strings are stabilised at higher pressures due to ion–neutral and dust–neutral collisions. The grain spacing is in the range of λD /3 to λD [42]. At strong vertical confinement the particles within a string are pushed closer together and a single particle can pop out. The string breaks into smaller strings. Thus long strings are formed in situations with only weak vertical confinement. Weak vertical confinement is achieved by lowering the input power (thus increasing the Debye length and sheath thickness) and increasing discharge pressure. The latter leads to a smoothing of the wake potential (through ion–neutral collisions) and thus to a decrease of the attractive force between vertically aligned dust grains. Furthermore the strings are susceptible to the so called “hose” instability. A wave-like motion of the string is seen when the string is unstable (Fig. 2.12, left, taken from [42]). This is essentially a two stream instability caused by the flowing ions. The grain spacing is not constant within a string but is bigger downstream a particle. This is due to the increasing ion velocity—ions are accelerated to the electrode. Therefore the attraction between the dust grains of a string decreases downstream. This leads to the hose instability with increasing amplitude downstream. Again the string is stabilised by increasing the discharge pressure. Crystal organisation When there are several strings the horizontally repulsive forces between the individual grains lead to horizontally hexagonal arrays. This can be seen through the 45 [42] Lampe: Structure and dynamics of dust in streaming plasma: Dust molecules, strings, and crystals, 2005 41 Fig. 2.12: Left: Simulation of the hose instability of a single string [42]. Right: Sketch of the change in crystal structure due to increased horizontal confinement. top window of the chamber. When the horizontal confinement is weak and the vertical confinement strong the strings arrange in a way that the individual particles are on an equal height in every string. When the horizontal confinement is strong and the vertical confinement weaker every second string moves to a higher or lower height so that the particles of one string are in the middle of the spacing of the particles of a neighbouring string (Fig. 2.12, right). The horizontal confinement can be adjusted in the presented experiment by applying a dc voltage to a stainless steel ring on the electrode (sec. 3.3, p. 74). The possible crystal structures are body-centred-cubic (bcc), face-centred-cubic (fcc), and hexagonal close-packed (hcp) [43]46 . Condensation At low pressures the dust cloud is in a gas-like or fluid-like state with a high kinetic dust temperature (10 to 100 eV). Such high dust kinetic temperatures result from an ion-dust two-stream instability [42, 44]47 . When the pressure is increased over a critical pressure pcond the dust cloud condensates abruptly. Ion–neutral and dust–neutral collisions then effectively damp the instability. The dust kinetic temperature is then approx. room temperature. Melting When the pressure is decreased again under a critical pressure pmelt the crystal melts 46 [43] Pieper: Experimental studies of two-dimensional and three-dimensional structure in a crystallized dusty plasma, 1996 47 [44] Joyce: Instability-triggered phase transition to a dusty-plasma condensate, 2002 42 Chapter 2 Theoretical background Fig. 2.13: Hysteresis loop traced out by the dust temperature as the pressure is varied up and then down (simulation) [42]. and the dust particles acquire a high kinetic temperature. The dust particle kinetic temperature describes a hysteresis loop when increasing the pressure over pcond and then decreasing the pressure below pmelt . That means pmelt < pcond as shown in Fig. 2.13 (taken from [42]). This figure shows a simulation of the dust particle kinetic temperature. But this behaviour is also seen in the presented experiment [45]48 . 48 [45] Aschinger: Struktur und Dynamik von Plasmakristallen, 2008 43 2.5 Light scattering by small particles The investigation of plasma crystal structures using scattering methods resembles X-ray diffraction techniques of solid state physics. Similar lattice types occur like body-centred-cubic (bcc) and face-centred-cubic (fcc). In order to calculate scattering intensities from a given structure the so called “structure factor” F is needed. This structure factor is the product of the so called “atomic form factor” f and a factor which is exclusively determined by the lattice type: F = N X j ~ fj exp (i~rj ◦ G) (2.43) Abbreviations: F : structure factor, N : number of atoms (for plasma crystals: particles) within a unit cell, f : atomic form factor, ~rj : distance vector from the point ~ reciprocal lattice vector. “ ◦ ” denotes the of origin to the atoms of a unit cell, G: scalar product of two vectors. In the case of identical atoms the atomic form factor can be written in front of the P ~ is sum. The latter factor (the geometrical structure factor Fg = N exp (i~rj ◦ G)) j the same for solid state physics and for the present case whereas the dimensionless atomic form factor has to be replaced by the so called “efficiency factor” Qsca . This efficiency factor is for spherical dust particles the scattering cross section Csca divided by the geometrical cross section: Qsca = Csca . πa2 (2.44) To understand this scattering cross section a description of the scattering of light by small particles seems appropriate. Here the word “light” is synonymic for electromagnetic radiation. The main focus of this section lies on the short discussion of scattering by particles which are smaller than the wavelength because this is the case of the experiment under consideration. This type of scattering is called Rayleigh scattering. For a complete and rigorous treatment see e.g. [46, 47, 48, 49]49 . Elastic and single scattering are assumed throughout this section. Elastic scattering means there is no change in wavelength through scattering. That implies 49 [46] van de Hulst: Light Scattering by Small Particles, 1981 [47] Bohren: Absorption and scattering of light by small particles, 1983 [48] Born: Principles of Optics, 1975 [49] Jackson: Klassische Elektrodynamik, 1985 44 Chapter 2 Theoretical background Optical Depth Scattering Type τ < 0.1 single scattering 0.1 < τ < 0.3 double scattering τ > 0.3 multiple scattering Table 2.4: Definition of single, double, and multiple scattering. that effects like Raman shifts or electronic excitations are excluded here. Single scattering means that a scattered wave directly leaves the particle cloud and is not scattered again. So multiple scattering is exluded as well and it is not necessary to find a radiation transfer function. There are two tests to decide if single scattering is dominant in a particle cloud: (i) Doubling of the particle concentration. Only single scattering is important if the scattered intensity is doubled as well. (ii) Measurement of the extinction. The extinction of a beam of light travelling through a particle cloud is described by exp(−τ ): I = I0 exp(−τ ). τ is the optical depth of the cloud. Three cases can be distinguished [46] as shown in table 2.4. 2.5.1 Some basics of scattering theory The 2 × 2 amplitude matrix relates the incoming fields to the scattered fields: Esca,|| Esca,⊥ ! exp(ik(r − z)) = −ikr S2 S3 S4 S1 ! E0,|| E0,⊥ ! (2.45) Fig. 2.14 shows the scattering geometry and defines the incoming (index 0) and scattered (index sca) electric fields parallel and perpendicular to the scattering plane. The scattering plane is defined by the direction of the incident beam and the direction of the scattered beam. In a real experiment only intensities can be measured. Therefore the scattering process needs to be described via incoming and scattered intensities. There are many possibilities to do this but using the Stokes vectors and the 4 × 4 scattering 45 z Esca, particle h y E0, Fig. 2.14: Scattering geometry. The electric Esca,|| E0,|| fields of the incident and scattered light are perpendicular (E⊥ ) to the scattering plane. scattering plane v divided into components parallel (E|| ) and x incident beam θ is the scattering angle. or Mueller matrix has shown to be very convenient: Isca Qsca U sca Vsca = 1 k2 r2 S11 S12 S13 S14 S21 S22 S23 S24 S 31 S32 S33 S34 S41 S42 S43 S44 I0 Q0 U . 0 V0 (2.46) The Stokes parameters are: Isca = Qsca = Usca = Vsca = k 2ωµ k 2ωµ k 2ωµ k i 2ωµ ∗ ∗ < Esca,|| Esca,|| + Esca,⊥ Esca,⊥ > ∗ ∗ < Esca,|| Esca,|| − Esca,⊥ Esca,⊥ > ∗ ∗ < Esca,|| Esca,⊥ + Esca,⊥ Esca,|| > ∗ ∗ < Esca,|| Esca,⊥ − Esca,⊥ Esca,|| > = b = b = b Intensity I|| − I⊥ I+45◦ − I−45◦ = b Iright circ. − Ilef t (2.47) circ. . The symbol < · · · > represents the time average and µ the permeability of the surrounding medium. The Stokes parameters can be measured using polarisers and λ/4 plates. Isca is the intensity of the scattered wave which is the sum of scattered parallel and perpendicular intensities. Qsca is the difference between scattered parallel and perpendicular intensity. (Not to confuse with the efficiency factor of eq. (2.44)!) Usca denotes the difference of scattered intensities with electric field components rotated by ±45◦ with respect to the scattering plane. Vsca is the difference between right circular and left circular polarised scattered intensities. 46 Chapter 2 Theoretical background Incident Polarisation Isca k2 r2 Qsca k2 r2 parallel |S2 |2 I0 |S2 |2 I0 perpendicular unpolarised |S1 |2 I0 −|S1 |2 I0 S11 I0 S12 I0 Table 2.5: Stokes parameters for spheres and different incident polarisations. Usca and Vsca are zero in these cases. Scattering by spheres The scattering amplitudes S3 and S4 are zero in the case of spheres: ! ! ! Esca,|| E0,|| exp(ik(r − z)) S2 0 = −ikr Esca,⊥ 0 S1 E0,⊥ (2.48) The scattering functions S1 and S2 write for spheres: X 2n + 1 (an πn + bn τn ) n(n + 1) n X 2n + 1 (an τn + bn πn ) = n(n + 1) n S1 = S2 (2.49) The scattering coefficients an and bn and the functions τn and πn are given in [47, chap. 4]50 . The stokes parameters follow from equations (2.48) and (2.47): Isca Qsca U sca Vsca S11 = S33 = = 1 k2 r2 1 (|S2 |2 2 1 (S2∗ S1 2 S11 S12 0 0 S12 S11 0 0 0 0 S33 S34 0 0 −S34 S33 + |S1 |2 ) , S12 = + S2 S1∗ ) , S34 = 1 2 i 2 I0 Q0 U . 0 V0 (|S2 |2 − |S1 |2 ) (S1 S2∗ − S2 S1∗ ) . (2.50) (2.51) The Mueller matrix elements for spheres fulfil the relation: 2 2 2 2 S11 = S12 + S33 + S34 . (2.52) Table 2.5 shows Stokes parameters of scattered light for spheres and different incident polarisations resulting from the equations above. 50 [47] Bohren: Absorption and scattering of light by small particles, 1983 47 Incident Polarisation parallel perpendicular unpolarised Isca 2 6 2 16π 4 a m −1 2 cos θ I0 r2 m2 + 2 λ4 2 6 16π 4 m2 − 1 a I0 2 2 r m +2 λ4 2 2 6 m −1 a 8π 4 2 (cos θ + 1) I0 2 2 r m +2 λ4 Table 2.6: Scattered intensities for different incident polarisations and spheres small compared with wavelength (Rayleigh scattering). The well known a6 /λ4 dependence is seen in the formulae. 2.5.2 Rayleigh scattering by one particle Assumptions underlying the theory of Rayleigh scattering as adopted here: 1. Spherical particles. 2. The external electric field of the light wave is considered to be seen as homogeneous by the particle. Therefore the particles must be small compared to the wavelength: 2πa ≪ λ. 3. The particles should build up a static polarisation in a short time compared to the period of the light wave. To meet this condition the size of the particle should be smaller than the wavelength inside the particle: 2πa ≪ λ/m. Here m is the refractive index of the dust particle. 4. Homogeneous particles with isotropic polarisability. The scattering functions S1 and S2 can be obtained using eq. (2.49) [47, chap. 4]51 : S1 = (3/2)a1 S2 = (3/2)a1 cos(θ) 2 m2 − 1 , a1 ∼ = −i x3 2 3 m +2 2πa x= λ (2.53) Inserting these equations into the formulae given in table 2.5 results in scattered intensities shown in table 2.6. 51 [47] Bohren: Absorption and scattering of light by small particles, 1983 48 Chapter 2 Theoretical background point P E r q p incoming wave Fig. 2.15: Dipole scattering. The corresponding Mueller matrix writes: 1 (cos2 θ + 1) 21 (cos2 θ − 1) 0 0 2 1 1 2 2 0 0 9|a1 |2 2 (cos θ − 1) 2 (cos θ + 1) 4k 2 r2 0 0 cos θ 0 0 0 0 cos θ (2.54) In the following the term “scattering cross section” is described in more detail. Energy can be removed out of a beam of light travelling through a sample in two different ways: scattering and absorption. The total energy scattered by a particle in all directions can be considered to be equal to the energy of the incident beam falling on an area Csca . This area is the scattering cross section. The absorption cross section is defined analogously: The total energy absorbed by a particle is by definition set equal to the energy of the incident beam falling on an area Cabs . This area is the absorption cross section. The sum of these effects—scattering and absorption—is called extinction and is described by the extinction cross section Cext : Cext = Csca + Cabs . (2.55) The efficiency factors are defined as described above by dividing the cross sections by the geometrical cross section of the particle. The formulae given above for scattered intensities can be derived differently with more physical insight. This is shown in the following. 49 The electric field of a scattered wave in an observation point P is in Gaussian units [46]: k2p ~ cos(θ) exp(−ikr)~e. (2.56) E= r ~ electric field, k = 2π/λ: wave number, p: dipole moment, r: disAbbreviations: E: tance between particle and view point, θ: scattering angle, ~e: unit vector perpendicular to the radius vector as shown in Fig. 2.15 (after [46]). Following assumptions 2, 3, and 4 at the beginning of this section (p. 47) the ~ 0 is proportional to the incoming electric field E0 where α is dipole moment p~ = αE the polarisability of the particle. Incoming and scattered intensities are given by the absolute value of the according Poyting vectors: I0,sca = c|E0,s |2 /8π (0: incoming, sca: scattered). Integration of Isca over the surface of a big sphere gives the total scattered power W = k 4 c|p|2 /3. Dividing this by the incoming intensity I0 results in the total scattering cross section: 8 Csca = πk 4 |α|2 . 3 (2.57) For a small sphere the polarisability is given by α = (m2 − 1)a3 /(m2 + 2) where m = n−iκ is the complex refractive index and a the sphere radius. Using k = 2π/λ in eq. (2.57) the total scattering cross section then writes: 2 6 128 5 m2 − 1 a Csca = π . 3 m2 + 2 λ4 (2.58) The a6 /λ4 dependence is seen again. Fig. 2.16 shows the well known polar diagram of Rayleigh scattered intensity for unpolarised incident radiation (taken from [46]52 ). From this figure it is clear that the parallel polarised component of the scattered intensity is not isotropically distributed over all angles. Under a scattering angle of 90◦ the scattered wave is linearly polarised perpendicular to the scattering plane (plane of drawing). The formula for the total scattered intensity Isca with unpolarised incident light reads [46]: Isca 8π 4 = 2 1 + cos2 θ r m2 − 1 m2 + 2 2 a6 I0 , λ4 (2.59) where r is the distance to the observation point (Fig. 2.15). This formula is identical to the one given in table 2.6 (p. 47). The cos2 θ contribution corresponds to the parallel component of the scattered light whereas the other term comes from the perpendicular component. 52 [46] van de Hulst: Light Scattering by Small Particles, 1981 50 Chapter 2 Theoretical background Fig. 2.16: Polar diagram for Rayleigh scattering. The scattered intensity is shown for the case of unpolarised incident radiation. 1 = scattered intensity polarised with electric field vector perpendicular to plane of drawing (perpendicular polarisation), 2 = scattered intensity polarised with electric field vector within plane of drawing (parallel polarisation), 1 + 2 = total scattered intensity. 2.5.3 Scattered radiant flux at the detector: particle clouds Section 2.5.2 gives the formulae necessary to calculate scattered intensities Isca for single spheres small compared with wavelength. Plasma crystals are considered in this section. Let N be the number of unit cells of a given plasma crystal and Fg the geometrical structure factor corresponding to the crystal structure. Now the scattered radiant flux by such a crystal is estimated. A bcc structure is assumed in the following. The radiant flux—which has the dimension of power—at the detector is given by: P det = Adet N Fg2 Isca (2.60) Abbreviations: P det : radiation power (radiant flux) reaching the detector, Adet : detector area, N : number of unit cells of the crystal under investigation, Fg : geometrical structure factor (eq. (2.43), p. 43), Isca : scattered intensity from a single particle. The input window diameter of the Golay detector is 6 mm and the geometrical structure factor for the bcc structure is zero or two [50]53 . The number of unit cells within the plasma crystal can be estimated with the crystal volume and the particle distances: 53 (20 mm)3 ∼ N= = 3 × 105 . 3 (0.3 mm) [50] Kittel: Einführung in die Festkörperphysik, 1993 (2.61) 51 The radiation power which reaches the detector can be estimated using table 2.6 (p. 47). To do this the following values are assumed: Particle radius a = 3.6 µm, real part of particle refractive index (MF particles) |m| = 1.68, distance particle cloud to detector: r = 220 mm, wavelength of FIR radiation λ = 118.83 µm, detector area: Adet = 28 mm2 , incoming intensity of FIR beam I0 ∼ = 0.05 mW/mm−2 , number of unit cells N ∼ = 3 × 105 , geometrical structure factor for bcc structure Fg = 2. For incident perpendicular polarisation this results in a radiation power of: P⊥det ∼ = 8 × 10−11 W , a = 3.6 µm. (2.62) a = 6 µm. (2.63) For particles with 6 µm radius this gives: P⊥det ∼ = 2 × 10−9 W , For an incident parallel polarised beam this value has to be multiplied by cos2 θ which reduces the radiation power at the detector. The incoming intensity of I0 ∼ = 0.05 mW/mm−2 for the expanded beam of diameter 1 cm at the plasma crystal corresponds to a FIR laser power density of 0.4 mW/mm2 at the FIR laser output (product of intensity and beam cross section is constant). This is a typical FIR laser beam intensity in the diffraction experiments as calibrated with Golay cell and Pyro detector (sec. 4.1, p. 84). This calculation does not include losses due to absorption and scattering by the plasma chamber walls. These effects reduce the radiation power at the detector by approximately 30% as measured with the Golay detector (see sec. 4.2, p. 90). Influence of the crystal temperature on the diffraction intensity The estimations of equations (2.62) and (2.63) do not include the temperature of the plasma crystal. This will be treated now. The so called Debye-Waller factor describes the dependence of the total diffraction intensity on the crystal temperature. It is described in [50]54 , appendix A. The total intensity J scattered by a crystal is: J= P det = N Fg2 Isca Adet (2.64) If the crystal has got a certain temperature T then J is reduced according to: 1 2 2 (2.65) J(T ) = J0 exp − < u(T ) > G . 3 54 [50] Kittel: Einführung in die Festkörperphysik, 1993 52 Chapter 2 Theoretical background Debye-Waller factor 1.0 J / J 0.9 2 0 = exp(-1/3 <u > 4 2 2 / d ) Fig. 2.17: The Debye-Waller factor. The relative diffracted intensity J/J0 is shown in J / J 0 0.8 dependence of the root-mean-square displace √ ment rms(u) = < u2 > in units of the 0.7 0.6 0.5 lattice plane distance d. J/J0 becomes ap- melting point after 0.4 prox. 0.88 at the melting point after Linde- Lindemann 0.3 0.2 0.00 0.05 0.10 0.15 0.20 rms(u) / d 0.25 0.30 0.35 mann (rms(u)/d ≥ 0.1). It decreases to 0.5 at rms(u)/d = 0.23. The exponential factor is the Debye-Waller factor. Abbreviations: J: total diffracted intensity, < u2(T ) >: mean square displacement of the particles from their lattice points, G2 : square of the reciprocal lattice vector. Now the Debye-Waller factor is estimated to clarify the temperature influence on the diffracted signals. Lindemann gave a criterion for the melting point of a 3D crystal: The root-meansquare displacement of the particles must be greater than 10 % of the inter particle distance: q < u2(T ) > = cb, (2.66) with b a typical inter particle distance and c ≥ 0.1. Approximating the typical particle distance b with the lattice plane distance d, substituting G = 2π/d, and applying then eq. (2.66) to eq. (2.65) gives: J(T ) 1 2 2 = exp − c 4π . J0 3 Fig. 2.17 shows this approximation of J/J0 in units of c = (2.67) √ < u2 >/d. The diffracted intensity decreases to ≈ 88 % at the melting point. This shows that even fluids can be investigated with scattering methods. Influence of crystal defects and domains on the diffraction intensity Defects within the crystal structure certainly reduce the diffraction peak intensity. Formally, a defect reduces the number of unit cells N of the crystal (see eq. (2.64)). The diffraction intensity therefore decreases linearly with an increasing number of crystal defects. The appearance of different crystal domains can lead to a significant reduction of the intensity of a certain diffraction peak. The Bragg condition is then met for certain domains only and the rest of the crystal does not contribute to the intensity 53 of the particular diffraction peak. Like defects the appearance of different domains is represented through the number of unit cells N that contribute to a particular diffraction peak. For example: If three different domains are present within the crystal, all with the same structure and lattice plane distances but with different spacial orientations then the number of unit cells that contribute to a particular diffraction peak is reduced by a factor of 1/3. The radiation power reaching the detector is now calculated including the extinction by the chamber walls, the temperature of the plasma crystal, crystal defects, and crystal domains: P det det N = TT P X A − NDef 2 1 2 2 Fg Isca exp − < u(T ) > G NDom 3 (2.68) Abbreviations: P det : radiation power reaching the detector, TT P X : transmission of the TPX chamber, Adet : detector area, N : total number of unit cells calculated with the crystal volume, NDef : number of defects, NDom : number of domains, Fg : geometrical structure factor, Isca : scattered intensity from a single particle, < u(T ) >: mean square displacement of the particles from their lattice points, G2 : square of the reciprocal lattice vector. Using eq. (2.68) and table 2.6 (p. 47) the total radiation power reaching the detector can be calculated. The parameter values inserted are listed in table 2.7. For incident perpendicular polarisation this results in a radiation power of: P det ∼ = 9.3 × 10−12 W ≈ 10−11 W. (2.69) This is too small to be detectable with the Golay cell detector, especially when allowing for a lower FIR power of e.g. only 0.01 mW instead of 0.1 mW at the plasma crystal. Such a small incident radiation power is possible when blocking parts of the FIR beam with an orifice to minimise background radiation. Thus the radiation power within a diffraction peak can easily be 10−12 W. Therefore a germanium detector cooled with liquid helium is used in some experiments. This germanium detector has a much higher sensitivity than the Golay cell (about four magnitudes better) and is occasionally provided as a loan by the work group of Prof. Dr. M. Havenith-Newen, Physikalische Chemie II, Ruhr-Universität Bochum. The estimations of this chapter imply the assumption that the incoming beam is a plain wave. This is certainly fulfilled for a single particle but not necessarily for 54 Chapter 2 Theoretical background Parameter Notation Transmission TPX TT P X Detector area Adet Number of unit cells N Number of defects NDef Number of domains NDom Geometrical structure factor Fg (bcc) Particle radius a Particle refractive index m Distance particles–detector r ∼ = 220 mm FIR wavelength λ 118.83 µm Intensity FIR beam I0 q < u2(T ) > Root-mean-square displacement Reciprocal lattice vector Value ∼ = 0.7 28 mm2 ∼ = 3 × 105 0.1 N ∼ = 3 × 104 ∼ = 10 2 3.6 µm 1.68 ∼ = 0.1 mW/mm−2 G 0.1 d 2π/d Table 2.7: Values for the calculation of the diffraction power. The transmission of the TPX chamber includes two walls to account for extinction of the incoming beam and the diffracted signal. The number of unit cells is calculated invoking crystal volume and volume of a unit cell. The numbers of defects and domains are roughly estimated from visual observation using a CCD camera. The value of the root-mean-square displacement of the particles is chosen to be like at the melting point after Lindemann. a hole plasma crystal. The FIR beam of the real experiment has a diameter of the order of one centimetre to assure the incoming wave to be plain. Chapter 3 Setup The optimum wavelength of the incident radiation lies in the range of the lattice plane distances for diffraction experiments on crystals. Therefore crystallography on solids uses X-rays. For plasma crystals these distances lie in the submm range (some hundred micrometre). Therefore a radiation source with submm wavelength is needed. Optically pumped far infrared (FIR) lasers are a well known source for this radiation [51]55 . They can produce monochromatic FIR radiation with power high enough for this application. Furthermore the design demands of FIR lasers are relatively easy to meet because the wavelength is so long. Mirror roughness for example is not a problem and high quality optical surfaces are not needed. Therefore it has been decided to build a FIR laser system. There are several diffraction methods to determine the structure of crystals including Debye–Scherrer for powders and the rotating crystal method for single crystals. The Debye–Scherrer method uses a monochromatic beam which is scattered by different crystalline domains of a powder. Beam and powder are not moved in this method and the diffraction peaks are usually recorded by a photographic film or plate. An equivalent two-dimensional detector is not available for the FIR. Special two-dimensional detectors are currently developed for specific wavelengths observed in astronomical investigations but are not available yet. A low cost and easy-to-handle FIR detector is the Golay cell [52]56 which works at room temperature and has a theoretical detection limit of 10−9 W. The Golay detector window has a diameter of 6 mm. Therefore the Golay cell has to be moved around the crystal very precisely to obtain angle resolved diffraction measurements. In the rotating crystal method the crystal is rotatable around all three axes with 55 [51] Douglas: Millimetre and submillimetre wavelength lasers, 1989 56 [52] Kimmit: Far-Infrared Techniques, 1970 55 56 Chapter 3 Setup the incident (white) beam fixed. However, 3D plasma crystals are hardly rotated without influencing structure and stability. Therefore a mirror system has been designed which allows to rotate the FIR beam and the detector around the chamber simultaneously. This mimics the rotating crystal method. The plasma chamber has to be transparent roundabout for the visible and the FIR. A material that meets this demand is the polymer TPX (poly-methylpentene). The chamber is made out of a TPX cylinder with stainless steel top and bottom parts. The setup of the laser system, mirror system, and plasma chamber is described in this chapter. The whole setup is built on two tables. The first one is for the laser system whereas the second one carries the mirror system and the plasma chamber. An overview of the experiment is shown in Fig. 3.1. 3.1 The laser system Setup and characterisation of the laser system is also described by S. Schornstein [9]57 in detail. The laser system is situated on an optical table58 . A sketch is shown in Fig. 3.1. The CO2 laser beam has a diameter of 7.5 mm (at the 1/e2 points) and a divergence of 8.5 mrad at the output coupler of the laser. The beam is deflected by a mirror (copper coated with gold), focussed by a ZnSe lens (Ø 25.1 mm, focal length: 600 mm), chopped with a frequency of 10.3 Hz, and again deflected by a second mirror into the FIR resonator. 3.1.1 The CO2 laser The CO2 laser PL5 by Edinburgh–Instruments Ltd. is used in this work. It produces 80 lines with wavelengths between 9 and 11 µm and a power of ≈ 50 W on the strongest line59 . Fig. 3.2 shows a sketch of the CO2 laser. The pyrex tube is 1.3 m long, double-walled for water cooling, and has a rippled inner surface to ensure power and stability. A gas flow mix of 7% CO2 , 18% N2 , and 75% He is established and a dc discharge is ignited between the electrodes and sustained using a voltage 57 [9] Schornstein: AUFBAU UND CHARAKTERISIERUNG EINES FERNIFRAROT-RESONATORS, 2006 58 Newport RP RelianceT M Sealed Hole Table Top, 2.4 × 1.2 m 59 measured with CO2 laser power head by Laser2000: PM30, 50W and FieldMaxII -TO, Coherent Waggon, Golay cell Laser diode Yolo telescope Mirror Pyro detector FIR resonator, 1900mm Chopper Lens CO2 laser, 2200mm Dump Beam splitter Tilted mirrors Laser and plasma chamber tables Guide rail Chamber, electrode, particles CCD camera, objective Fig. 3.1: The whole setup. The CO2 laser and the FIR laser are situated on the laser table (left). The CO2 laser beam is collimated by a zinc selenite(ZnSe) lens of focal length 600 mm, chopped with 10.3 Hz, and guided into the FIR resonator via two gold coated copper mirrors. The FIR laser beam is collimated via a Yolo telescope consisting of two spherical mirrors with diameters of 100 mm (1st mirror) and 120 mm (2nd mirror) and curvature radii of 850 and 1000 mm. A freezer bag foil serves as beam splitter and reflects ≈ 10% onto a pyro electric detector (Pyro). Two tilted mirrors guide the FIR beam to the plasma chamber table (right) to the plasma crystal. The Golay cell is placed on a waggon on a 360◦ guide rail. This waggon is motorised and can be positioned with an accuracy of 0.1◦ . The mirror system is shown in Fig. 3.11 (p. 67). 57 58 Chapter 3 Setup ZnSe mirror on piezo ZnSe window Golden grating 10 kV Pyrex pipe Fig. 3.2: Sketch of the CO2 laser. A gas flow mix of 7 % CO2 , 18 % N2 , and 75 % He is established within the pyrex tube (gas connections not shown) resulting in a pressure of 3000 Pa. A dc plasma is ignited between the electrodes with a voltage of about 10 kV and a current of 20 mA. A gold coated grating with 90 lines/mm and a plano-concave ZnSe window compose the resonator with a length of 1.83 m. of about 10 kV. A typical dc current of 20 mA is flowing through the discharge. The pyrex tube is sealed with two zinc selenite (ZnSe) Brewster windows. The output coupler is a plano-concave ZnSe lens with a radius of curvature of 6 m. A thermally compensated dual cylinder piezo ceramic is attached to the output coupler to allow fine tuning of the resonator length. A water cooled grating with 90 lines/mm which is gold coated and blazed for 10 µm serves as wavelength selective element. The cavity length is 1.83 m. The beam mode is specified by Edinburgh Instruments Ltd. to be TEM00 (> 90%) and M 2 < 1.25. This number is obtained computing: M2 = θL ω0,L , θG ω0,G (3.1) where θL and ω0,L are divergence and beam waist of the laser beam and θG and ω0,G are the corresponding values of a perfect Gaussian beam with the same wavelength. A real Gaussian beam therefore has M 2 = 1. Beam diameter and divergence are specified to 7.5 mm (at output coupler) and 3.5 mRad, respectively. A self made heat exchanger assures cooling of the pyrex tube. It consists of two copper pipes with different diameters which are fitted into each other. The inner one belongs to the closed cycle cooling system of the CO2 laser using water mixed with an anti-freezer for lower viscosity. The coolant is pumped through the system by a small commercial aquarium pump. The outer copper pipe is flushed by mains water which typically has a temperature of 16 ◦ C. The ZnSe Brewster windows got dirty after about one year of frequent CO2 laser operation (Fig. 3.3). The laser power then oscillated with an amplitude of about 59 Fig. 3.3: Dirty Brewster window of the CO2 laser. Dark orange areas are clearly visible. The circles mark areas that intercept the CO2 laser beam. These areas lower laser power and disturb the laser mode. The edge also shows such colouration. 5 W and a period of about 15 s. The FIR power got very low which hints to a mode change of the CO2 laser beam. Such colouration effects are known to be caused by oil vapour diffusing out of the rotary vane pump into the laser discharge tube [53]60 . The oil molecules can be cracked within the discharge and react with the ZnSe surface. The colouration occurred in spite of the use of an oil filter that should avoid oil vapour diffusion. Maybe the oil vapour got into the discharge tube during venting. The ZnSe Brewster windows were cleaned using lap foils. The contamination could be removed but some scratches remained on the windows. This is probably the reason for the lowered CO2 laser power after re-adjustment. A membrane pump has been tested but resulted in lower laser power due to the lower pumping speed compared with that of the rotary vane pump (only 2.2 m3 h−1 compared with 3.7 m3 h−1 ). Therefore the rotary vane pump was used again but with a different venting procedure which avoids oil vapour diffusion into the discharge tube. The lapping of the Brewster windows made a re-adjustment of the CO2 laser necessary. To do this the CO2 laser output coupler has to be replaced by a plate with a central alignment orifice to define the laser axis (part of the CO2 laser toolkit). A second orifice is mounted on the grating holder. A HeNe laser beam is adjusted to travel backwards through FIR resonator and CO2 laser as sketched in Fig. 3.4. This HeNe laser beam then travels the same path the CO2 laser beam goes after adjustment. The exact alignment procedure is described in the PL5 CO2 laser manual. The laser mode can be checked by placing the second mirror (near the FIR 60 [53] Bründermann: private communication 60 Chapter 3 Setup A:holder Mirrors, holders FIR resonator B:ground plate Dump Beam splitter CO2 laser HeNe laser and orifice Fig. 3.4: CO2 laser adjustment. A HeNe laser beam travels backwards through FIR resonator and CO2 laser. The photo shows a gold coated copper mirror on a special mirror holder and the third holder. resonator) onto a third holder (Fig. 3.4). The CO2 laser beam is then deflected parallel to but behind the FIR resonator onto a chamotte slab. This move of the mirror does not de-adjust the mirror. The power achieved is 20 W at the line 9P36 (λ = 9.695 µm). The CO2 laser is very stable after a warming up time of approximately one hour. 3.1.2 The FIR resonator A main part of this work was the design, fabrication, and characterisation of the FIR resonator. It is a wave guide resonator with plane mirrors which is described in [9] in detail. Fig. 3.5 shows an explicit drawing. The main item is a 1.5 m long Duran glass pipe of an inner diameter of 48 mm which is vacuum-sealed and fixed on each side in a stainless steel end piece. A smaller second pipe with inner diameter of 32 mm is placed into the bigger one using two ring spacers. The spacers are made of polyethylene and have holes to assure good pumping (Fig. 3.6). The end pieces have ports for gas inlet and vacuum pump and hold the entrance and output mirrors. The entrance side is water cooled to avoid refractive index variations of the ZnSe Brewster window (EF in Fig. 3.5). The stainless steel resonator mirrors (ES, AS) have concave drillings to minimise laser beam distortions. Different mirror configurations with different surface roughnesses and hole diame- water cooled quartz pipe Q A A D D C L B C spacer AF K duran glass pipes AS ES E water cooling EF H H D D A R A : main holder B : vacuum sealed resonator pipe C: mounting D: mirror holder adjustment A water cooled quartz pipe G : resonator length adjustm. H : entrance window mounting EF: entrance window AF: output window E F K L : bellows : support : output window mounting : gas inlet F G Q : port for pressure gauge R : pump port ES : entrance mirror AS : output mirror Fig. 3.5: FIR resonator. 61 62 Chapter 3 Setup outer pipe spacer with holes inner pipe Fig. 3.6: Cross section of resonator pipes and spacer. The spacers fix the inner pipe. Holes ensure good pumping. ters have been tested [9]. In the present work both mirrors are polished and have hole diameters of 2.5 mm (input) and 4 mm (output). The entrance mirror hole is drilled 3 mm off the centre to avoid back reflections of the CO2 laser beam. The CO2 laser beam is reflected at the output mirror of the FIR laser and can travel back into the CO2 laser if the entrance mirror hole is drilled centrally. This would lower the CO2 laser performance [54]61 . Two concave stainless steel mirrors have been manufactured with a radius of curvature of 1000 mm each. The entrance mirror hole diameter is again 2.5 mm and drilled 3 mm off the centre. The output mirror hole diameter is 4 mm. Both mirrors are polished as well. This concave mirror cavity is more stable (see e.g. [6]62 ) and provides better wavelength sensitivity than the plane mirror cavity (see sec. 4.1.1, p. 81). Three quartz glass pipes serve as spacers to assure a fixed distance between the two resonator mirrors. They are flushed by mains water at a constant temperature of 16 ◦ C. The whole resonator is supported by two triangular holders (A). One of these holders is not fixed at the table but allowed to slide lengthwise. This is done to fix the resonator length even when the length of the table changes due to temperature variations. The entrance end piece is mounted via two lengthwise ball bearings on two supports (F). This allows adjustment of the resonator length without changing the mirror tipping. Bellows on entrance and output side ensure mirror adjustments without vacuum breaks (E). Tipping of the mirrors is accomplished by three mi61 [54] Kuellmann: ENTWICKLUNG EINES OPTISCH GEPUMPTEN FERNINFRAROTLASERS FÜR DEN EINSATZ IN DER PLASMADIAGNOSTIK UND IN DER MOLEKÜLSPEKTROSKOPIE, 1989 62 [6] Kneubühl: Laser, 1991 63 Fig. 3.7: Bushings for screw screw nut quartz tube support. Left: Bushing with screw. quartz pipe quartz pipe Right: Bushing with screw nuts. main holder brass bushing main holder brass bushing crometer screws on each side (D). The output window (AF) is a 3 mm thick quartz plate glued into a polyethylene holder (K). This holder is also adjustable via two screws and a spring to avoid possible etalon effects inside the window which could lower the laser power. The FIR resonator is aligned using a HeNe laser beam as sketched in Fig. 3.8 (p. 65). Yolo telescope and tilted mirrors are not used for resonator adjustment but for FIR laser beam alignment. The resonator entrance mirror is replaced by a resonator output mirror with a central hole. The HeNe laser beam then travels straight through the resonator and is reflected at the output mirror. Observing the corresponding reflection and back-reflection spots on entrance and output mirror the mirrors can be adjusted with the micrometre screws (D in Fig. 3.5). The resonator Duran glass pipes have to be removed for the alignment procedure and the mirrors have to be of the polished type. If a rough output mirror is intended to be used during operation the alignment has to be done with a polished mirror first which is then replaced by the rough one. Alignment apertures can be placed on a straight rail which is centrally positioned along the resonator axis and fixed to the table. The fluids methyl alcohol (CH3 OH) and formic acid (HCOOH) are stored in polyethylene bottles. The vapours of these fluids are introduced into the resonator via a flexible polyethylene tube and a port on the entrance side (L in Fig. 3.5). The pumping is accomplished using a membrane pump63 and a turbo pump64 . A base pressure well below 5 × 10−3 Pa is achieved measured by a Leybold pressure gauge65 . The FIR resonator is operated with a small vapour flow to achieve better stability at pressures between 10 and 30 Pa. At the beginning of the experiments the water cooled quartz pipes broke due to disadvantageously designed holders. The tubes were glued into brass bushings which were attached to the main triangle holders using screws (Fig. 3.7, left). The 63 vacuubrand, 64 Pfeiffer, model MZ 2C model TMU 071 P 65 THERMOVAC TM22 64 Chapter 3 Setup screw exerted a pressure on brass bushing and quartz pipe which led to the failure of the pipe. The modified design (Fig. 3.7, right) with threads on the bushings and screw nuts exerts no pressure and functions very well. 3.1.3 The mirror system The CO2 laser beam pumps the FIR laser as described in sec. 2.1.3 (p. 9). The resulting FIR beam is divergent because of the resonator geometry (plane mirrors) and needs to be focussed onto the plasma crystal. A computer program has been developed to calculate beam diameters at the plasma crystal using the formulae of Gaussian beam optics (sec. 2.2, p. 13). The focussing is done by a Yolo telescope consisting of two home made spherical mirrors (Fig. 3.1, p. 57). The necessary mirror radii and positions were calculated using the computer program developed. First and second mirror have radii of curvature of 100 mm and 120 mm, respectively. The mirrors are made of aluminium and polished to have a low surface roughness. Therefore the mirrors reflect even optical light very well and a HeNe laser can be used for adjustment. To do this a plate with a central hole (e.g. a FIR resonator output mirror) is mounted in place of the FIR resonator entrance mirror and the HeNe laser beam is guided straightly into the resonator. The HeNe laser beam straightly leaves the FIR resonator through the output window and follows the beam path of the FIR beam. A sketch of this adjustment arrangement is shown in Fig. 3.8. A beam splitter is placed after the Yolo telescope to allow for the observation of the FIR beam during scattering experiments (Fig. 3.1, p. 57). This beam splitter is a freezer bag foil which transmits 90% of the FIR beam. About 5% are absorbed and 5% are reflected as measured with the Pyro detector. This reflected part of the FIR beam is sufficient to continuously observe the beam with the Pyro detector. The Pyro detector contains a pyro-electric (ionic) crystal which has a permanent electric polarisation. When heated the crystal axis parallel to the electric polarisation expands and the distances between the ions of the crystal change which leads to a charging according to the piezo effect. Furthermore the permanent electric polarisation changes with temperature. Both effects lead to the charging of the opposite crystal surfaces. The surface charges are not permanent but compensated by e.g. free electrons. Therefore only temperature changes induce (non-permanent) potential differences between the two opposite surfaces of the crystal. These voltages can be measured by contacting these surfaces. 65 A Mirrors FIR B Yolo telescope resonator E C Beam splitter CO2 laser D E HeNe laser and orifice (a) FIR resonator and laser beam adjustment. A HeNe laser (b) Photo showing FIR resonator output window beam travels through the FIR resonator. The entrance mirror (A), yolo telescope (B + C), beam splitter (D), and is replaced by an output mirror with central hole. tilted mirrors (E). The beam path is sketched. Fig. 3.8: Sketch of FIR laser beam adjustment and photo of the mirror system. Because of these Pyro detector characteristics only temperature changes can be detected and the FIR beam has to be chopped. This is accomplished by chopping the CO2 laser beam. The Pyro signal is then measured by an oscilloscope using the trigger signal of the chopper. Two tilted aluminium mirrors deflect the FIR beam to the plasma crystal. On the plasma chamber table a mirror system can be used to rotate the FIR laser beam around the plasma crystal. All the mirrors are home made and have a special design to maximise the mirror surface and to ease the production (Fig. 3.9). The mirror plate is directly mounted onto the holder and can be adjusted via two screws. The mirror system on the plasma chamber table is described in section 3.2. Fig. 3.10 shows reflection coefficients of aluminium for parallel and for perpendicular polarised light of a wavelength of 600 nm. These coefficients don’t differ much (only 0.06) at an incidence angle of 45◦ . The mirrors of the scattering arrangement are adjusted to angles around 45◦ . A beam deformation accompanied by a change Fig. 3.9: Aluminium mirrors. Left: Mirror with anodised surfaces. Right: Mirror components. 66 Chapter 3 Setup Fig. 3.10: Reflection coefficients of alu- Reflection coefficients of aluminium Reflection coefficient 1.00 minium for a wavelength of 600 nm. The re- = 600 nm, n = 1.2, k = 7.26 0.95 flection coefficients of parallel and perpendic- 0.90 ular polarised light differ by only 0.06 at an 0.85 angle of incidence of 45◦ which is the maximum incidence angle of the scattering ar- 0.80 parallel polarisation 0.75 rangement. Beam distortions due to angle perpendicular polarisation dependent reflection coefficients are thus not 0.70 0 10 20 30 40 50 60 70 Angle of incidence in degree 80 90 expected. of polarisation due to the reflection at the mirrors is thus not expected. 67 3.2 The scattering arrangement Fig. 3.11 shows a sketch of scattering arrangement and plasma chamber. The FIR beam is focussed as described in sec. 3.1.3 and guided to the plasma chamber table. Four additional mirrors can be used to rotate the FIR beam around the plasma chamber. The first one is fixed whereas the three remaining are mounted on a holder on a 360◦ guide rail. The Golay detector is placed on an additional waggon (not shown in the figure but sketched in Fig. 3.1). Both mirror system and Golay waggon can be motorised. This allows to rotate FIR beam and Golay cell quasi simultaneously around the chamber without changing the scattering angle. The rotating crystal diffraction method is mimicked with this configuration. The mirrors are adjusted using a HeNe laser beam travelling backwards along the FIR beam path. The HeNe laser beam spot is guided into the FIR resonator and observed at the FIR resonator entrance mirror while rotating the mirror system. The FIR beam can be guided to the plasma crystal straightly without using the mirrors and therefore with fixed direction. The powder diffraction method is 8 9 10 1 12 2 6 11 3 4 3 FIR laser 7 5 pump Fig. 3.11: Chamber and mirror system. 1: Dust dispenser, 2: Electrodes, 3: 360◦ guide rail, 4: Table, 5: Pressure gauge, 6: Mirror for camera observation, 7: Vacuum ports, 8: Tilted mirrors for FIR beam, 9: Mirror mount on guide rail, 10: fixed mirror mount, 11: TPX cylinder, 12: HeNe laser holder for adjustment. 68 Chapter 3 Setup Fig. 3.12: Waggon and guide rail with gear ring. Fig. 3.13: Scattering control scheme. Blue cables are data cables, black cables are for voltage supply. The dc voltage is modulated Golay cell Motor chopper signal by a pulse width control which generates rectangular pulses. The pulse width and thereby the motor speed is controlled with the com- Lock-In amplifier (2x) puter program “Cockpit”. The voltage polarity can be reversed by a computer controlled self-made switch. The Golay position is de- PC Pulse width control 9V termined via an incremental encoder conSwitch nected to the motor axle. The Golay signal voltage is recorded with two lock-in amplifiers (high and low sensitivity). applied when rotating only the Golay cell around the chamber. A 50 cm long glass tube with 15 mm inner diameter has been used in some experiments to guide the FIR beam to the chamber. The beam has been focused into the glass tube with the Yolo telescope. The glass tube serves as wave guide which results in a beam which is narrower at the plasma crystal than the beam without the glass tube. A waggon together with the 360◦ guide rail and its gear ring is shown in Fig. 3.12. The motorised angle resolved rotation, the Golay cell data storage, and the plasma control is accomplished via the computer program “Cockpit” developed in this work. Fig. 3.13 shows motorised rotation and data storage scheme. A dc voltage with an amplitude of 9 V or 16 V is modulated by a pulse width control. It generates rectangular dc pulses between 0 V and the maximum amplitude. The pulse width (the “ON” time) can be set by the computer. This determines the motor speed. The voltage polarity can also be controlled by a switch actuated by the computer. This polarity determines the motor speed direction. Pulse width control and switch are connected to the computer using the National Instruments Card66 and the connection panel NI BNC 2110. The incremental en66 National Instruments PCI-MIO-16E-1 69 Fig. 3.14: Angular velocity of the detector carriage against control voltage—with and without weight. The two upper curves are recorded with a supply voltage of 16 V and the lower curve is for a lower supply voltage of 9 V. The waggon has been loaded with a weight of 7.5 kg to obtain the red and blue Angular velocity in degree per second 5 Angular velocity vs. control voltage 4 3 2 1 no weight, 16 V 0 curves. with 7.5 kg, 16 V with 7.5 kg, 9 V 0 1 2 3 4 5 Control voltage in V Window Gas Reflective membrane Lenses Light source FIR Photo diode Absorber Mesh (a) Principle of the Golay cell. (b) Golay cell with aluminium optic adapter and orifice. Fig. 3.15: (a) Sketch of Golay principle. The FIR beam heats up absorber and gas. Heat induced changes of reflective membrane curvature change the photo diode signal. (b) Photo of Golay cell with optic mount and orifice. coder signal is recorded by an ADDI DATA card67 . Fig. 3.14 shows the dependence of the angular velocity of the detector waggon on the supply voltage and on the weight load of the waggon. The two upper curves show the angular velocity using a supply voltage of 16 V. This supply voltage is modulated by the pulse width control. This modulation is controlled by the control voltage which is the x-axis of the diagram. The angular velocity is independent of the weight load. The lower curve shows the angular velocity with a lower supply voltage of 9 V only. The Golay cell Fig. 3.15 shows the principle of a Golay cell detector (a) and a photo (b). The FIR radiation passes a HDPE (high density poly-ethylene) window and heats up an absorber plate. A gas (xenon) is thus heated and expands which 67 APCI 1710, 32 bit 70 Chapter 3 Setup Chopper-frequency response 300 of the Golay cell Golay signal in mV 250 200 Fig. 3.16: Dependence of the Golay sensi- 150 tivity on chopper frequency. The error bars 100 are smaller than the point size except of the 50 0 lowest frequency. The chopper frequency is 0 10 20 30 40 50 60 70 Chopper frequency in Hz 80 90 set to 10.3 Hz for the experiments with the Golay cell. leads to the bending of a flexible membrane. The membrane back side is reflective and illuminated by a light source. The light is focussed by a lens system and partly blocked by a mesh. When the reflected image of the mesh exactly matches the mesh itself then the photo diode signal is maximum. This signal changes because of heat induced changes of the curvature of the reflective membrane. Then the reflected mesh image does not exactly match the mesh itself. The changes of the photo diode signal are easily measured. The measurement signal has to be chopped to induce such changes of the photo diode signal. Fig. 3.16 shows the dependence of the Golay signal on the chopper frequency. A relatively big error occurs at the very low chopper frequency due to the unbalance of the chopper blade. The chopper frequency is set to 10.3 Hz for the experiments with the Golay cell. The Golay signal is recorded by means of two Lock-In amplifiers68 to increase the signal-to-noise ratio. One Lock-In amplifier is operated with high sensitivity to measure diffraction peaks. The 2nd is operated with low sensitivity to precisely determine the FIR beam forward direction. Noise reduction The Golay cell has a field of view of FWHM > 30◦ (FWHM: Full Width at Half Maximum). Therefore an orifice is needed to increase directional sensitivity and thereby to minimise background noise. An aluminium optic adapter has been manufactured and attached to the Golay cell. It has four holes to attach standard optic holders and components. Fig. 3.15 (b) shows a photo of the Golay cell with mounted optic adapter and orifice. A black low density polyethylene (LDPE) foil is placed directly in front of the Golay entrance window. It effectively suppresses IR and visible background radiation 68 Stanford Research Systems, Model SR830 DSP Lock-In Amplifier 71 and stems from the packaging of a laser printer toner. Three sides of the table and the mirror mounts of the mirror system are provided with board panels laminated with velours. Velours turned out to be a very good and cheap absorber material for FIR radiation because of its rough surface. This avoids background noise. The Golay cell was originally elastically supported but this turned out to be disadvantageous. The small shocks and vibrations during the movement of the Golay waggon and during stops of the waggon induced high signal peaks. Removing the elastic support eliminated these noise signals. The germanium detector Some experiments were carried out using a germanium detector in place of the Golay cell. This germanium detector is cooled with liquid helium and has a four orders of magnitude higher sensitivity than the Golay cell. Furthermore it can be operated at a frequency of some MHz which is a huge advantage regarding noise reduction and time resolution. This detector is occasionally borrowed from the work group of Prof. Dr. M. Havenith-Newen, Physikalische Chemie II, Ruhr-Universität Bochum. 72 Chapter 3 Setup 3.3 The plasma chamber Fig. 3.17 reproduces the plasma chamber already shown in Fig. 3.11 (p. 67). An argon plasma is ignited between two parallel aluminium electrodes (2). Dust particles are introduced into the plasma by a dust dispenser (1). This is a small stainless steel container with holes at the top (for good pumping) and a metal mesh at the bottom. It is mounted using a spring and can be shaken by knocking at the mount. The dust particles fall through a 8 mm hole within the upper electrode. Amplifier Match box 6 Power meter 1 2 13.56 MHz 5 3 PC 4 Valve control 7 dispenser, 2: Electrodes, 3: Plasma Pump Butterfly valve Fig. 3.17: Plasma chamber. 1: Dust crystal, 4: Vacuum ports, 5: TPX cylinder, 6: Mirror for CCD camera Gas flow observation, 7: Pressure gauge. Different dust particles can be used including melamine resin (melamine formaldehyde, MF) and polystyrene particles of diameters between 3 µm and 20 µm. They form a plasma crystal under certain plasma parameters (3). Vacuum ports (4) allow attachment of pressure gauge (7) and gas flow pipe. The gas flow is introduced near the butter fly valve far away from the chamber. This minimises gas streams inside the plasma volume which would disturb the plasma crystals. Butter fly valve and pressure gauge are controlled by a MKS controller69 via the computer program “Cockpit”. The system can be operated at constant pressure or fixed valve position. 69 MKS 600 Series Pressure Controller 73 A rotary vane pump70 with oil filter or a scroll pump71 pumps the chamber volume down to a base pressure of about 10 Pa. A turbo molecular pump72 can be used to obtain lower pressures. The argon gas flow is measured by a MKS mass flow meter73 and controlled by the MKS mass flow controller74 . Typically gas flows between 0.5 sccm and 2.0 sccm are used (sccm = b standard cubic centimetre per minute). A TPX cylinder (poly-methylpentene) is used as chamber wall. This polymer is transparent in the visible and in the FIR region of the spectrum. The cylinder allows roundabout optical access which is necessary both for camera observations in the visible and diffraction experiments in the FIR. Such a TPX cylinder is not easily bought from a supplier because usually suppliers want to sell big numbers of pieces. Therefore a 5 litre TPX measuring cup is used as plasma chamber which can be obtained from a chemical equipment supplier. The cup was cut at top and bottom to obtain a cylinder with precise edges. These cylinder edges were then glued into 1 cm deep grooves of aluminium flanges using silicone. The top of the plasma chamber has a central window and the upper electrode has a central hole for top view camera observations. The central hole within the electrode is closed by a metal mesh to minimise plasma sheath potential distortions. The top view observations are done using a tilted mirror to be able to place the CCD camera outside the 360◦ guide rail (Fig. 3.1, p. 57 and Fig. 3.17). Both electrodes can be powered but in most of the experiments the upper electrode is used. A frequency generator75 provides an rf signal (rf = b radio frequency) with frequency of 13.56 MHz and ≈ 2 V peak-to-peak amplitude. A rf amplifier76 amplifies this signal. Forward power and standing wave ratio (SWR) are measured with a NAP power meter77 directly before a matching network. In the experiments the forward power typically is 10 W with a standing wave ratio of typical 10 to 20. The matching network consists of a high pass filter followed by a blocking capacitor (Fig. 3.18). This means the electrical power is capacitively coupled to the 70 Pfeiffer 71 Varian Vacuum DUO 5 Model IDP3 72 Pfeiffer Vacuum TMU 261 73 MKS Instruments, 10 sccm N2 , Viton 74 MKS Type 247, 4 Channel Readout 75 Agilent 33120A 15MHz Function/Arbitrary Waveform Generator 76 Kalmus Wideband RF Power Amplifier, 0.001 – 100 MHz, 15 W, 43 dB gain 77 Power Reflection Meter – NAP 392.4017.02 74 Chapter 3 Setup blocking capacitor rf input rf output Fig. 3.18: low pass filter high pass filter self bias UDC Matching network consisting of high pass filter, blocking capacitor, and low pass filter for measuring self-bias or applying a dc voltage. electrode of the plasma chamber. The match box has a port to measure the self-bias (sec. 2.3, p. 17) through a low pass filter. The self-bias has a typical value of -100 V with an input power of 20 W and -10 V with an input power of 1 W (10 Vpp at a pressure of 30 Pa, measured with a voltage–current–probe near the chamber). The port for self-bias measurements also allows to apply an external dc voltage to the powered electrode. A positive dc voltage of about 1 to 10 V is applied to the powered electrode to stabilise the plasma crystals in some experiments. This voltage changes the sheath potential of the powered (upper) electrode. As a result the plasma crystals can be stretched vertically. Upper and lower aluminium electrodes are sketched in Fig. 3.19. The upper electrode has a central hole which is closed by a metal mesh to minimise sheath potential distortions. This hole allows top view observations as described earlier. A second hole allows to fill in dust particles. The lower electrode also has a central and outer mesh to allow dust particles to fall through. A trash can below the lower electrode stores such dust particles which were not levitated in the plasma or which fell through the meshes after switching off the plasma. Two integrated rings can be set to different potentials of up to Fig. 3.19: Electrodes of the plasma chamber. Both have a central and a lateral hole. In the upper electrode they serve as window and dust input hole. The holes in the lower electrode are for dust particle recycling. The lower electrode has two rings (red and blue in this figure) + + which can be biased separately. Both electrodes and the rings can be powered. 75 400 V (relative to ground). Such voltages deform the sheath potential to provide an effective particle trap. The body of the lower electrode is always grounded. The lower electrode surface profile is a crucial parameter in producing plasma crystals. Therefore the electrode was manufactured with a surface as flat as possible. It is made of aluminium (like the upper electrode) and the meshes are composed of several 1.5 mm holes drilled into the material. Nevertheless, this design turned out to be disadvantageous: The dust particles were pushed away from the centre. Therefore some modifications were applied including the usage of an stainless steel plate on top of the inner ring. The modifications are described in sec. 4.3.1 in more detail. A dressler rf generator78 can also be used to power the upper electrode. It is operated at about 40 W real power (forward minus reflected) and controlled via the computer program “Cockpit”. The power is damped down to about 5 W using three T-fittings and dummy loads. This allows to vary the power in 0.25 W steps and the generator operates at a favourable working point. 78 dressler CEASAR RF Power Generator, 13.56 MHz 76 Chapter 3 Setup 3.4 Setup for calibration scattering experiments Experiments have been conducted to calibrate the scattering arrangement. A golden mesh consisting of 40 µm × 40 µm gold squares with distances of 200 µm has been deposited onto a small GaAs wafer (≈ 2 cm ×1 cm, Fig. 3.20). The mesh properties were chosen to assure high diffraction signals and to cover the entire wavelength range. Therefore the gold squares are made relatively large: The geometrical cross section is about 15 to 40 times larger than that of the dust particles. The lattice distance was chosen to be 200 µm to separate the diffraction peaks of the 118.83 µm and of the 170.58 µm line for ease of detection. The GaAs wafer transmits about 80% of the FIR radiation. A standard lens holder by Linos has served as wafer holder. The holder has been placed onto the lower electrode near the position of the plasma crytals. Special care has been taken to minimise background noise and possible reflections of the incoming FIR beam at electrode and mirror holders. This has been achieved by masking electrode and holders with velours boards (Fig. 3.20). The FIR beam has been guided straightly to the gold mesh and diffraction peaks have been recorded with the Golay cell. Fig. 3.20: Gold mesh and holder. Left: Microscope image of the gold mesh. The golden squares (bright spots) are 40 µm × 40 µm and 200 µm apart. Right: Mesh holder on lower electrode of the plasma chamber. Electrode and chamber are covered with velours boards to minimise reflections of the FIR radiation. 77 3.5 CCD camera diagnostics and video analysis The dust particles are illuminated using a diode laser with a wavelength of 682 nm and a power of about 40 mW79 . An integrated optic produces a laser sheet with 8◦ apex angle and about 117 µm width (lateral Rayleigh length). The scattered light of the dust particles is observed using a Basler progressive scan CCD camera80 and a zoom objective81 . The videos are stored in an 8 bit format (Y8/Y800, 256 levels of brightness) using the free available program “Virtual VCR”82 . Video conversion from the Y8 to the RGB format is done with the program “Virtual Dub” and video analysis is accomplished using the software IDL83 . Several procedures for particle tracking and particle motion analysis have been provided by Uwe Konopka from the group of Prof. G. E. Morfill84 . They have been developed further in this project by Andreas Aschinger partly using and complementing the work of other programmers85 . The analysis software and first results of plasma crystal video analysis are extensively described in [45]86 . Therefore only a short summary and description is given here. Table 3.1 lists the working scheme of the analysis software. 1. Video processing and saving Several filters are applied to optimise the video quality for the particle tracking procedure. The “Avisynth Frame Server” is used for this task [55]87 . It provides several different filtering techniques and allows own filter development. Access to the “Video for Windows” application programming interface is needed for reading and writing AVI-files with the Avisynth Frame Server. A program package by Oleg Kornilov is used for this task [56]88 . A graphical preview interface developed in this project by Andreas Aschinger 79 Schäfter + Kirchhoff diode laser, P ≤ 40 mW, λ = 682 nm, cw, model: 5LM-8-S325-L + 25CM-660-40-M02-A8-2 80 BASLER 81 Nikon 82 Virtual 83 IDL: A622F, progressive scan, 1280 × 1024 pixel, 24 fps, up to 500 fps with 200 × 160 pixel field of view ED AF MIKRO NIKKOR 200 mm 1:4D VCR: Virtual Video Cassette Recorder Interactive Data Language 84 Max–Planck–Institut 85 David für extraterrestrische Physik – Theorie und komplexe Plasmen, Garching, Germany W. Fanning: “Coyote’s Guide to IDL”, Oleg Kornilov, Matthew W. Craig, NASA–Astronomy–Lib 86 [45] Aschinger: Struktur und Dynamik von Plasmakristallen, 2008 87 [55] Avisynth Frame Server, http://avisynth.org 88 [56] Kornilov: AVI, MPEG, QT reading, writing, and preprocessing, www.kilvarock.com/freesoftware/dlms/avi.htm 78 Chapter 3 Setup Task Methods 1. Video pro- Filtering using the “Avisynth Frame Server”: Gamma correc- cessing and tion, salt’n’pepper, cropping, spacial Gauss filter, saving in saving HDF file 2. Find particle Find optimum intensity threshold, eliminate pixel defects, de- coordinates termine intensity-weighted particle centre 3. Determine Track particles from frame to frame, find optimum search area particle trajec- with graphical interface developed, eventually use particle po- tories sition prediction 4. Data analysis Velocity distribution in x and y direction, distribution of |v| ⇒ and illustration crystal temperature, mean particle velocity against time, particle velocity against height above lower electrode, area density, pair correlation function ⇒ plane distances and crys- tallinity, Wigner–Seitz cells ⇒ defects Table 3.1: Working scheme of the analysis software. allows the application of different filters to selectable frame sequences of a video and the examination of the filtered video parts. The brightness and contrast filter is the main filter. It enhances high intensities via the so called Gamma correction. The bright dust particles are then clearly distinguishable from the background. The salt’n’pepper filter eliminates pixel defects and background noise. The cropping filter allows to cut out parts of the video image e.g. such parts in which no particles are visible. The Gauss filter changes the intensity distribution of a particle image to obtain a Gaussian brightness profile. The original intensity distribution is not smooth and exhibits a strong pixel effect: Neighbouring pixels of the CCD chip can measure very different intensities which leads to steps in the intensity distribution of a particle image. The Gauss filter smooths them out which improves the accuracy of the later determined particle coordinates and velocities. The data are stored in an HDF file [57]89 . This data format allows the successive processing of very large data amounts. It is possible e.g. to open a single frame out of a whole video without opening the video itself. It is also possible to save attributes together with the data. The applied filtering order or the frame rate of 89 [57] Hirachical Data Format, http://www.hdfgroup.org 79 the video can be saved for example. 2. Find particle coordinates The dust particles have to be identified within each frame of a video. They must be found within the 2D intensity distribution of each image. In order to separate the particles from the background noise an intensity threshold is determined with the graphical preview interface. Intensity values below the threshold are ignored in the following analysis. Care must be taken to obtain the right threshold value. The threshold value must be chosen so that background noise is suppressed but particles of the crystal plane of interest are still visible. The centre of intensity of each dust particle image is calculated analogously to the centre of mass of a given body in basic mechanics. This centre of intensity is the particle coordinate in the subsequent analysis. 3. Determine particle trajectories The dust particles must be followed and assigned from video frame to video frame to obtain particle trajectories. Different methods of particle tracking can be applied: “Simple–Search”, “Area–Search”, and “Educated Guess”. Simple–Search The particle search within the actual frame starts at the very same coordinate of the particle in the last frame. The first particle that is found is assigned to that particle of the last frame. Wrong assignments are very likely with this Simple–Search if the particle velocities are too high. Then the particle is too far away from the last position and a different particle is probably assigned. Area–Search A search area around the last position is defined. The particle is looked for only within this area in the next frame. This search area is actually a velocity limit because fast particles can move out of the search area and cannot be assigned. This leads to a cut-off at a certain velocity in the calculated velocity distribution. Furthermore the number of particle trajectories increases because a particle which cannot be assigned counts as new and additional particle. On the other hand particle trajectories can mix up if the search area is too large. Then particles are assigned wrongly and trajectories contain large jumps which are physically not meaningful. The search area size can be optimised using the already mentioned graphical interface with preview function. Educated Guess Using the velocity calculated from the last two frames a prediction for the particle position in the next frame is made. This is a big enhancement 80 Chapter 3 Setup in many cases. But if the particles perform only small oscillations around a fixed position this method can lead to a prediction which is too far away from the actual position. Then the particle cannot be assigned as well. This effect strongly depends on the ratio of the particle oscillation frequency to the frame rate of the CCD camera. A higher frame rate reduces this error. 4. Data analysis and illustration The velocity distribution in x and y direction and |v| can be plotted and analysed. The particles drift if the maximum of one or both of the 1D velocity distributions is not at velocity zero. A fit of the |v| distribution gives the crystal temperature if it is a Maxwell distribution. A diagram of the mean velocity against time shows the long term stability of the crystal against velocity (temperature) changes. Differences of the particle velocities in different heights above the lower electrode can also be seen in a separate diagram. The area density (number of particles divided by field of view) of the particles can be plotted as well. The pair correlation function can be calculated and fitted. The positions of the different peaks are unique to the possible crystal structures (e.g. hcp, bcc) and give the lattice plane distances. Height and width of the peaks give information about the crystallinity of the crystal. Smaller widths mean lower temperatures and smaller heights mean a worse structure. The ratio of peak height to peak width is the crystallinity. Defects in the crystal structure can be visualised with the Wigner–Seitz cells. E.g. each particle has six neighbours in a perfect hcp structure. The fraction of lattice points with less or more neighbours describes the quality of the crystal. Chapter 4 Results 4.1 Properties of the laser system Some properties of laser system and beam characteristics are already described in [9]90 . Here only the most important results are summarised and new results are presented. 4.1.1 FIR laser operation and beam characteristics Plane mirrors Fig. 4.1 shows the Pyro signal of the λ = 170.58 µm FIR line versus the methanol vapour pressure within the resonator for different mirror roughnesses and mirror hole diameters. The combination with polished mirrors and output mirror hole of 4 mm diameter shows the highest FIR signal. The input mirror hole diameter is 2.5 mm in any case. The highest FIR power with this configuration is achieved for a small pressure range around 15 Pa. Fig. 4.2 shows FIR laser beam profiles at 55 mm (a) and 1080 mm (b) distance to the output mirror. The profiles are obtained by precisely moving the Pyro detector laterally and reading the signal amplitude from the oscilloscope. Apertures of 1 mm diameter (at 55 mm distance) and 5 mm diameter (at 1080 mm distance) increased directional sensitivity of the Pyro and minimised background noise. Gauss fits reveal beam radii of w = 2.2 mm at 55 mm distance and w = 50.3 mm at 1080 mm distance. The beam diameter at 1080 mm distance gives a divergence of the FIR laser beam of about 5.3◦ . 90 [9] Schornstein: AUFBAU UND CHARAKTERISIERUNG EINES FERNIFRAROT-RESONATORS, 2006 81 82 Chapter 4 Results FIR power vs. pressure 6 Pyro signal in V 5 output output input mirror mirror mirror hole 4 3 2 1 roughness roughness 2mm rough 2mm polished rough rough 3mm polished rough 3mm rough 4mm polished polished 5mm polished polished 7mm polished rough rough 0 0.0 0.1 0.2 0.3 0.4 0.5 Pressure in mbar Fig. 4.1: FIR signal versus pressure for several mirror configurations. Waveguide diameter: 48 mm. The combination of both mirrors polished and a 4 mm output hole gives the highest FIR laser signal within a small pressure range around 15 Pa. (Input mirror hole diameter: 2.5 mm in any case.) 120 Beam profile at 55mm distance = 170.58 m Mirror hole: 3 mm 80 Mirror type: polished Pressure: 24 Pa 60 Beam profile at 1080 mm distance Aperture: 1 mm Beam radius w = 2.2 mm 40 Measurement Gauss fit Pyro signal in mV Pyro signal in mV 100 8 6 = 170.58 m Aperture: 5 mm 4 Mirror hole: 3 mm Mirror type: polished 2 Beam radius w = 50.27 mm 20 Measurement Gauss fit 0 90 92 94 96 98 100 102 104 106 108 x in mm (a) FIR beam profile at 55 mm distance. 40 60 80 100 120 140 x in mm (b) FIR beam profile at 1080 mm distance. Fig. 4.2: FIR laser beam profiles at 55 mm and 1080 mm distance to the output mirror of the FIR resonator. x denotes the lateral displacement of the Pyro. 1 mm and 5 mm apertures have been used to increase directional sensitivity of the Pyro. The output mirror has been of the polished type with a 3 mm hole. Gauss fits reveal FIR beam radii of 2.2 mm (a) and 50.3 mm (b). 83 B A A B Fig. 4.3: 3D visualisation of the FIR beam. Left: IR camera VarioCAM with HDPE lens and LDPE foil in front of the output side of the FIR resonator. The CO2 laser cover is visible in the background. Right: IR camera image without LDPE foil. The background (arrow A) results from the hot output window of the FIR resonator. This is heated by the CO2 laser beam leaking through the output mirror hole. Arrow B marks the FIR laser beam. The inset shows an image with LDPE foil. Setup and result of a 3D visualisation of the FIR laser beam are shown in Fig. 4.3. An infrared (IR) camera91 has been placed directly into the FIR laser beam near the output end of the FIR resonator. The IR optics has been replaced by a black low density polyethylene (LDPE) foil and a high density polyethylene (HDPE) lens with focal length of 50 mm. The LDPE foil stems from the packaging of a laser printer toner and effectively suppresses IR and visible background radiation. The HDPE lens has been glued onto the LDPE foil. It focusses the FIR beam onto the sensor chip of the IR camera. The experiments with the IR camera are published in [58]92 . Concave mirrors Two concave stainless steel mirrors have been manufactured and installed to further improve the stability of the FIR laser resonator. These mirrors are polished as well and they both have a radius of curvature of 1 m. This gives a stable concave resonator since the resonator length is 1.5 m. The entrance mirror has an offset hole of 2.5 mm diameter and the output mirror has a central 4 mm diameter hole like the plane mirrors. The FIR laser with concave mirrors shows a more stable operation 91 VarioCAM 92 by Jenoptik, exclusive distribution by InfraTec [58] Bründermann: Erste THz-Videos mit einer Silizium-basierten IR-Kamera, 2006 84 Chapter 4 Results Resonator scan 3 Pyro signal in mW Pyro signal in mW 3 2 1 118.83 m 170.58 m 2 1 118.83 m 170.58 m both lines both lines 0 0 200 400 600 Resonator position in 800 1000 0 600 700 m (a) Resonator scan with concave mirrors. 800 Resonator position in 900 1000 m (b) Right part of the left diagram. Fig. 4.4: Resonator scan with concave mirrors. A clear separation of the lines is not always possible. The resonator is more stable in the right part of the diagram. The entrance mirror is closer to the resonator pipe there which reduces losses. and a certain wavelength can be selected more easily. Fig. 4.4 shows the observed FIR laser lines during a resonator scan. Such resonator scans are shown in [9]93 for the plane mirror setup. The FIR resonator length is tuned to a value of 4.172 mm on the micrometer screw reading to obtain the 118.83 µm line. This corresponds to the resonator position of 883 µm in Fig. 4.4. The entrance mirror is very close to the resonator pipe at this position. This minimises radiation losses when the FIR radiation couples out of the resonator pipe to be reflected at the entrance mirror. This mirror position provides a stable laser signal. Fig. 4.5 shows pressure dependencies of both lines for plane and concave mirrors. The optimum working pressure for concave mirrors is higher than for plane mirrors and lies between 0.25 mbar and 0.35 mbar. The pressure profile of the 118.83 µm line is broader than that of the 170.58 µm line for concave mirrors. 4.1.2 The FIR laser power The Golay cell detector has been used to calibrate the FIR laser power. The sensitivity of the Golay cell is 32 kVW−1 . (The sensitivity of the Pyro detector is not known in the wavelength region used in this experiment.) Since the maximum radiation power permanently tolerable by the Golay cell is 10 µW the FIR laser radiation has to be damped. Therefore the procedure of the experiment was as 93 [9] Schornstein: AUFBAU UND CHARAKTERISIERUNG EINES FERNIFRAROT-RESONATORS, 2006 85 Fig. 4.5: Pressure dependence of the FIR lower signal amplitude with concave mir- 2.5 rors is due to the polishing of the CO2 laser Brewster windows (sec. 3.1.1, p. 59). For concave mirrors the optimum pressure is 8 2.0 6 1.5 4 1.0 2 higher and the laser can be operated be- 0.5 tween 0.25 mbar and 0.35 mbar for both 0.0 0.0 lines. 10 Pressure dependence Pyro signal in V 3.0 Pyro signal in mW signal with plane and concave mirrors. The 0.1 0.2 118.83 m, concave 170.58 m, concave 170.58 m, plane 0.3 0.4 0 0.5 0.6 Pressure in mbar follows: 1. Measurement of the FIR laser signal without damping using the Pyro detector. 2. Measurement of the FIR laser signal with damping (by a piece of paperboard) using the Pyro detector. The damping factor can be calculated from these measurements. 3. Measurement of the damped laser power using the Golay cell at the very same position. The damped laser power can be calculated in absolute numbers invoking the Golay cell sensitivity. Multiplying this damped laser power by the damping factor gives the undamped laser power. The undamped and damped FIR laser signals have been 643 mV ± 23 mV and 1.82 mV ± 0.02 mV measured with the Pyro and using a Lock-In amplifier and the PC program “Cockpit”. The statistical errors (one sigma) are due to laser fluctuations. These values give a damping factor of about 353.3 ± 13.2. The damped FIR laser signal has been 126.2 mV ± 2.6 mV measured with the Golay cell. Multiplying with the damping factor and invoking Golay cell sensitivity and error propagation this gives an undamped FIR laser power of about 1.39 mW ± 0.06 mW in this experiment. The Pyro signal was simultaneously recorded by the oscilloscope with a value of about 1.5 V. The sensitivity of the Pyro is therefore about 1 V(mW)−1 in this wavelength region. Typical Pyro signals are 4 to 5 V during diffraction experiments which gives a typical FIR laser power of 4 to 5 mW. This radiation power falls onto the Pyro detector placed directly at the FIR laser output. The FIR beam 86 Chapter 4 Results diameter is approximately 4 mm there. The laser power of 5 mW thus corresponds to an intensity of about 0.4 mW/mm2 . 4.1.3 Characteristics of the beam splitter A beam splitter can be used to record the FIR laser power during diffraction experiments (see Fig. 3.8, p. 65). The beam splitter consists of a freezer bag foil clamped onto an aluminium holder. It has a transmission of about 90 % measured with the Pyro detector. The FIR laser can produce the two wavelengths 118.83 µm and 170.58 µm simultaneously with certain resonator lengths set (see Fig. 4.4). If there is a difference in wavelength sensitivity between Golay and Pyro detector or if there is a strong wavelength sensitivity of the beam splitter then the recording of the FIR beam with the beam splitter can lead to wrong results. FIR laser beam signals deflected by the beam splitter have been measured with the Pyro and the Golay detector to exclude any wavelength sensitivity. Special care has been taken to operate the laser at only one single wavelength using the concave mirrors as resonator mirrors in this experiment. Both FIR lines (118.83 µm and 170.58 µm) are partly deflected by the beam splitter. The measured signals have the same values after correction for the different window diameters and window materials of Golay and Pyro (Fig. 4.6). Fig. 4.6: Calibration of the beam splitter. Signal in W 10 Calibration of the beam splitter The Pyro signal is corrected for window di- 9 ameter and window material. Golay win- 8 dow: HDPE, 6 mm diameter, Pyro win- 7 dow: Ge, 5 mm diameter. The beam split- 6 ter partly reflects both lines and the detec- 5 Golay, 118 m Golay, 170 m 4 Error bars: statistical error due to noise 3 + 4.3% error of the power calibration 1 2 3 Measurement Pyro, 118 m Pyro, 170 m 4 tors measure the reflected signals equally. The discrepancy between Golay and Pyro in measurement two results most probably from a slight misalignment of the Golay cell. The Golay window has a diameter of 6 mm and is made out of high density polyethylene (HDPE). One millimetre of HDPE has a transmission of about 90% in the wavelength region of interest [59]94 . The Pyro window has a diameter of 5 mm 94 [59] Fischbach: Eigenschaften optischer Materialien, 2004 87 and is made out of germanium (Ge). 1.5 millimetre of Ge have a transmission of about 42% [59]. The ratio of Golay window area to Pyro window area is 1.44. This is a first correction factor for the Pyro signal. The transmission of 42% of 1.5 mm of Ge corresponds to 56% transmission for 1 mm Ge roughly assuming a linear dependence (transmission of 1.0 mm = 4/3 × 0.42). The ratio of the transmissions of HDPE to Ge is then 90/56 = 1.61. The correction factor for the Pyro signal is therefore 1.44 × 1.61 ∼ = 2.3. The thickness of both windows is not known and a difference in this parameter could rise the need for a third correction. But even without this correction the deflected signals are equal within the error bars no matter if measured with the Golay cell or Pyro detector. Only measurement two in Fig. 4.6 shows a difference between the detectors which is likely due to a misalignment of the Golay cell. This shows that beam splitter and detectors have no significant wavelength sensitivity in the wavelength region of interest. 88 Chapter 4 Results 4.2 Results of calibration scattering experiments The setup described in sec. 3.4 (p. 76) has been used to perform calibration experiments to demonstrate the experimental procedure. The FIR beam has been guided straightly to a mesh consisting of golden squares (40 × 40 µm2 , 200 µm apart) deposited on a GaAs wafer. This wafer has been placed on the lower electrode of the plasma chamber and diffraction peaks have been recorded using the scattering arrangement described in sec. 3.2 (p. 67). The TPX plasma chamber has been removed in a first experiment. Fig. 4.7 shows the diffraction peaks obtained with this setup. The black curve shows the diffraction peaks and the main FIR 7 Scattering by golden mesh 6 7 Fig. 4.7: Diffraction peaks of the golden 6 mesh (black curve). Each peak is labelled 5 with diffraction angle, order, and corre- Signal in nW 5 dsin FIR beam = n 35° 4 4 n=1 3 2 -35° -57° n=1 1 118 m n=1 56° 3 n=1 170 m 118 m 170 m 0 -80 -40 -20 0 20 40 Scattering angle in degree 60 80 sponding wavelength. The 118.83 µm and the 170.58 µm lines are simultaneously 2 present within the FIR beam. The red 1 curve shows the main FIR beam recorded 0 -60 Signal in µW direct Maxima: with the Lock-In amplifier with lower sensitivity. beam (in forward direction) recorded with the Lock-In amplifier with high sensitivity (max. signal: 200 µV = b 6.25 nW). The diffraction peaks are distributed symmetrically around the forward direction. The diffraction angle of each peak can be calculated using the formula d sin θ = nλ for the diffraction of a planar wave incident on a mesh (d: lattice constant (200 µm); θ: diffraction angle; n: diffraction order; λ: wavelength). Two lines of 118.83 µm and 170.58 µm wavelength are simultaneously present within the FIR beam. Different amplitudes of the peaks of one wavelength result from a slight misalignment of the golden mesh which is not exactly perpendicularly aligned relative to the FIR beam. The shoulder of the main FIR beam at about -9◦ results from a reflection of the FIR beam by the mesh holder. It is also seen in the following diagrams. The red curve shows the FIR beam recorded with the Lock-In amplifier with low sensitivity (max. signal: 200 mV = b 6.25 µW). This curve has been used to determine the forward direction of the FIR beam and the zero point of the x-axis. A very small peak at -9◦ can be seen in this curve as well. 89 This result shows the principle of the experiment: A FIR diffraction pattern of a 2D lattice is recorded with a Golay cell. Here, the lattice constant of the golden mesh is comparable to that of plasma crystals. The size of the gold squares is larger than that of the dust particles of a plasma crystal. This is to enhance the diffraction signal of this 2D lattice with one plane only. Real plasma crystals consist of smaller dust particles (factor roughly 1/3 to 1/2 regarding radius a) but many planes. Invoking the a6 -dependence of the Rayleigh scattering intensity these smaller particles have scattering intensities 1/729 to 1/64 times the scattering intensity of the gold squares of the test wafer (neglecting the difference in refractive index). This smaller scattering intensity should be balanced by the higher number of particles contributing to a diffraction peak for the case of plasma crystals. The number of the gold squares constituting the mesh is roughly 2090 determined by simply counting them under a light microscope. A number of about 729 × 2090 = 1.5 × 106 dust particles with radii of 7 µm thus has to contribute to a diffraction peak in a real diffraction experiment to compensate for the smaller radius. Then a diffraction peak could be observed even with the Golay cell detector. In case of the germanium detector a much lower number of dust particles should be sufficient even invoking domains and temperature of the crystal. Scattering patterns of the golden mesh have been recorded with and without the TPX plasma chamber to study the influence of the TPX vessel on the diffraction signals. The diffraction patterns obtained are shown in Fig. 4.8. The most striking points in these diagrams are the absence of the 170.58 µm diffraction peak on the right side of the diagrams (only a small hump is observed at about 56◦ in (a)) and the appearance of a peak at -23◦ . The latter again stems from a reflection of the FIR beam by the mesh holder due to a slight misalignment and should be neglected. It arose after the re-adjustment of the mesh holder which was necessary to fit the holder into the TPX chamber. The absence of the 170.58 µm peak on the right is probably due to the misalignment as well: All peak intensities are lower on the right (Fig. 4.9). A further reason for the absence of the 170.58 µm peak on the right and for the angle dependent influence of the TPX chamber can be a change in the FIR laser 90 Chapter 4 Results 8 Maxima: dsin n=1 18 118 m 16 14 = n 12 10 6 8 -56° n=1 4 0 -60 -40 -20 0 20 40 60 18 n=1 Maxima: dsin Extinction by 118 m TPX cylinder = n not symmetric 8 36° 6 14 12 8 118 m n=1 6 170 m 4 2 0 80 16 10 n=1 2 0 -80 12 4 2 20 -35° 4 2 22 FIR beam -56° 6 170 m direct 14 10 24 with TPX 16 20 26 Scattering by golden mesh W 22 36° 118 m 12 FIR beam 18 Signal in n=1 24 W Signal in nW 14 direct Signal in without TPX -35° 10 26 Scattering by golden mesh 16 Signal in nW 18 0 -80 -60 -40 -20 0 20 40 60 80 Scattering angle in degree Scattering angle in degree (a) Diffraction by golden mesh without TPX chamber. (b) Diffraction by golden mesh with TPX chamber. Fig. 4.8: Influence of the TPX chamber on the diffraction pattern. The extinction caused by the TPX vessel is stronger on the right side. A slight misalignment of the mesh and FIR laser power variations cannot be excluded. Fig. 4.9: out/with TPX. Peak intensities measured Peak intensity ratio (without/with TPX) Ratio of peak intensities 3.0 Peak intensity ratios with- without and with TPX without TPX related to that measured with TPX (from Fig. 4.8). The 170.58 µm peak 2.5 at −56◦ is almost not attenuated whereas 2.0 the 118.83 µm peak at 36◦ is attenuated by a factor of 3. Possible reasons: Mis- 1.5 alignment of the mesh and/or variation of 1.0 laser power during the measurement time -60 -40 -20 0 20 Scattering angle in degree 40 of about 100 s. power during the measurement. The angular velocity of the Golay cell has been about 1.5 degree per second which corresponds to a measurement time of about 100 seconds. Variations of the FIR laser power on this time scale cannot be excluded because the beam splitter was not yet installed for these experiments. 91 4.3 The crystal Plasma crystals are produced by dropping dust particles of a defined size into the argon plasma in this experiment. The argon plasma is operated with a constant flow of about 1 sccm argon, a pressure between 5 Pa and 120 Pa and a power between 1 W and 20 W. A dust dispenser above the upper electrode drops the dust particles through a hole in the upper electrode (sec. 3.3, p. 72, 74). Thus the particles fall directly into the plasma and they are stored within the plasma due to their negative charge and the positive plasma potential. Particles of diameters between 3 µm and 20 µm are used in the experiments. The dust particles have high kinetic energies and they are in a gas-like state at low pressures with the upper electrode powered. Increasing the pressure leads to a sudden slowdown of the dust particle movement due to increased gas friction and the crystalline state is eventually reached. The exact pressure for this transition depends on input power, dust particle number density, dust particle size, and voltages applied to the rings of the lower electrode. An initially bad dust particle distribution made some changes in the electrode design necessary. These are described in the next section together with other minor modifications of the setup which led to more stable plasma crystals. The following sections describe the two major types of plasma crystals which can be created with this setup. 4.3.1 Design optimisations for producing plasma crystals A problem with the material TPX is its sensitivity to UV radiation. UV radiation causes material defects and makes the TPX more opaque. Because UV radiation is produced within the argon plasma the TPX chamber got more and more opaque and had to be changed. This is a principal problem which can only be solved by using a different chamber material. However, the only suitable material known is crystalline quartz glass (z–cut) which is also transparent in the visible and in the far infrared. A polygon chamber could be built out of several crystalline quartz glass windows. This has the major disadvantage that it would not provide roundabout optical access to the plasma. Furthermore the FIR transparency of such windows strongly decreases with increasing angle of incidence (apart from normal incidence). Therefore the material TPX has been chosen to built the plasma chamber. 92 Chapter 4 Results Fig. 4.10: Lower electrode configuration particles A and dust particle distribution. The regions above the meshes remain dust par- + + ticle free due to plasma–wall sheath deformations. Crystal Ring + Plate + Ring (a) Lower electrode configuration B with stainless steel (b) Corresponding photograph of the electrode with ring and plate. dust cloud. Fig. 4.11: Lower electrode configuration B and dust cloud—side view. The crystal from the right photo is inserted into the left sketch. Parameters: MF particle, diameter: 7.32 µm, power: 1.0 W, pressure: 83 Pa, outer ring voltage: −50 V, self bias adjusted to +8 V. The original lower electrode design turned out to be disadvantageous. The dust particles did not arrange themselves in the middle above the lower electrode but where pushed away from the middle to only one side of the chamber. Fig. 4.10 shows a sketch of this situation. Stopping the argon gas flow into the plasma chamber did not change the particle distribution. Thus it seems that potential maxima arose that pushed the particles away from the centre and away from the outer mesh. Several modifications of the lower electrode have been tested to optimise the dust particle distribution. Finally a stainless steel plate with a ring-shaped bottom side and an additional outer stainless steel ring were placed onto the lower electrode to cover the central mesh and to increase the radial confinement. This increased radial confinement reduces the influence of the outer mesh. Furthermore a negative dc voltage can be applied to the plate which lifts the particles and reduces the influence of the electrode roughness. A sketch of this new configuration is shown in Fig. 4.11 (a) and a photograph of the plasma crystal in Fig. 4.11 (b). The crystal arranges centrally and there are no observable distortions in the global dust particle distribution. Different outer ring sizes can be used to vary the lower electrode configuration: 93 The upper edge of the outer ring can be of the same height as the plate or higher. This varies the radial confinement of the plasma crystals. The radial confinement is weaker and higher confinement voltages are necessary when using a flat outer ring. The advantage of this configuration is that the outer ring does not disturb FIR beam and side view optical observations. A small funnel has been placed into the small hole of the upper electrode to improve the dust particle filling. The dust particles thus cannot disperse onto the upper electrode but fall straightly through the hole. A lens system consisting of two collecting lenses has been placed onto the upper electrode right above the central observation hole. The distance between the lenses is adjustable. A tenfold larger observation area is possible using this lens system. The electrical matching network is usually detuned to relatively high standing wave ratios (SWR) of about 20 to reduce dust particle oscillations. This detuning basically reduces the effective input power but a pure reduction of input power at the power generator does not have the same effect. The detuning changes the rf frequency characteristics of the complete electrical system as well. This leads to a more quiescent plasma which in turn results in more stable crystals in this setup. The home made match box has been replaced by a commercial one95 . The fine adjustment can be done more easily and the plasma runs more quiescent with this matching network. The electrical layout is basically the same as sketched in Fig. 3.18 but low pass filter and port for measuring or setting the self bias is not included. These are realised within a separate box which is connected in parallel to the output of the match box. Degeneration of gold coated particles Polystyrene (PS) particles coated with a 100 nm thick gold film have initially been used to produce plasma crystals for the diffraction experiments. The gold coating should enhance the diffraction signal expected because of its high refractive index. Fig. 4.12 displays a scanning electron microscope (SEM) image of such particles which have been used in a plasma crystal experiment. The particle surface is not smooth any more but exhibits a craggy structure. An argon ion etching process is most probably responsible for this surface change. These particles cannot be used for plasma crystal experiments because they lead to unstable crystals. Lower 95 PALSTAR, AT-2K Antennentuner, 1.8 MHz – 30 MHz, max. 2000 W power, distributed by Communication Systems Rosenberg e.K. 94 Chapter 4 Results Fig. 4.12: Degenerated gold coated micro particles. The particle surfaces are not smooth after being in the argon plasma but show a craggy structure. This is most probably the result of an etching process accomplished by the argon ions. The use of gold coated particles led to unstable plasma crystals. plasma crystal temperatures and thus more stable crystals can be reached using uncoated melamine resin (MF) particles. 4.3.2 Extended plasma crystals Two types of plasma crystals can be produced: extended and flat (21/2D) crystals. The plasma parameters differ in argon gas pressure and input power. First the extended crystals are described. The extended crystals are produced with the upper electrode powered and typically have dimensions of 3 cm × 3 cm × 2 cm. This size strongly depends on the ring voltages applied to the lower electrode. The crystals can be lifted in two ways: (i) By applying a constant positive dc voltage to the upper powered electrode or (ii) by applying a negative dc voltage to the inner ring of the lower electrode. In case (i) the average (positive) plasma potential is increased which pulls the dust particles into the centre of the discharge. In case (ii) the dust particles are pushed away from the lower electrode more strongly. This lifting by about 2 cm stabilises the crystals and the crystal temperature decreases. In case (ii) (applying a negative voltage to the ring of the lower electrode) the negative self bias of the upper powered electrode changes as well. This is shown in Fig. 4.13: The dependence of the self bias of the upper (powered) electrode on the ring voltages applied to the lower electrode. The self bias increases (gets more negative) with increasing negative ring voltages. The particles arrange in vertical strings one particle below another due to the wake field as already described in sec. 2.4.8 (p. 39). Fig. 4.14 shows an inverted photo of such a situation and the corresponding 2D pair correlation function of the 95 -5 Self bias against outer ring voltage -6 -6 -7 -7 Self bias in V Self bias in V -5 -8 -8 -9 -9 -10 -10 0 -20 -40 -60 -80 Self bias against inner ring voltage 0 -100 -20 -40 -60 -80 -100 Inner ring voltage in V Outer ring voltage in V Fig. 4.13: Self bias against ring voltages. The negative self bias increases with increasing negative ring voltages. Discharge power: 0.9 W video (side view). With increasing pressure the strings are stabilised but can break up at higher pressures due to the smoothing out of the wake potential. Depending on the outer ring voltage a structural phase transition can occur. Then the side view shows a transition from a quadratic to a hexagonal structure. Pair correlation function 2.5 Pair correlation function 2.0 Power: ~1 W Pressure: ~80 Pa Particle diameter: 7 1.5 Mean velocity: m 0.36 mm/s Particle distance: 0.47 mm 1.0 0.5 0.5 1.0 1.5 2.0 Particle distance in mm (a) Photo of strings in a plasma crystal. (b) Corresponding pair correlation function. Fig. 4.14: String formation in a plasma crystal. The particles are primarily ordered in strings one particle below another. 96 Chapter 4 Results These correspond to the hcp (hexagonal closed packed) and bcc (body centred cubic) structures in 3D [43]96 . Thus a transition from hcp to bcc can be observed during pressure increase in this experiment [45]97 . This transition is accompanied by a change of the plasma itself which resembles the so called α−γ transition [13]98 . Further investigations are necessary to clarify the exact nature of this transition in the plasma crystal structure. Fig. 4.15 shows particle positions and pair correlation functions of extended (4.15 A – D) and flat (4.15 E – H) crystals. The positions are shown for a time period of one second to illustrate the stability of the crystals. Only small parts (about 3 mm × 3 mm) of the observation area are shown to avoid overloading the pictures. The corresponding pair correlation functions are calculated including all visible particles within the observation area. The experimental parameters are given with the pair correlation functions. It becomes clear from Fig. 4.15 that the top view stability is better than the side view stability. This is also seen in the pair correlation functions: The top view gives higher peak intensities and higher long range correlations (more peaks). This can be seen by comparing Fig. 4.15 (B) with (D) for extended crystals and by comparing Fig. 4.15 (F) with (H) for flat crystals. Reviewing the pair correlation functions the extended crystals are in a fluid like state. Diffraction peaks from such crystals are expected to be very small and broad. A reduction of background noise of any kind is thus crucial. 4.3.3 Flat crystals Flat crystals, sometimes called 21/2D crystals, consist of a small number of horizontal planes only. Three to four planes are possible in this experiment. These crystals are produced using high pressure and power with the upper electrode powered. Only two planes are possible when the lower electrode is powered but in a wide pressure and power range. Then it is no longer possible to lift the crystals which is unfavourable for scattering experiments because reflections of the FIR beam at the electrode surface can occur. Fig. 4.15 (E) – (H) show particle positions and corresponding pair correlation 96 [43] Pieper: Experimental studies of two-dimensional and three-dimensional structure in a crystallized dusty plasma, 1996 97 [45] Aschinger: Struktur und Dynamik von Plasmakristallen, 2008 98 [13] Raizer: Radio-Frequency Capacitive Discharges, 1995 97 3.0 10.0 extended crystal, top view Pair correlation function 9.5 9.0 y-position in mm (B) Pair correlation function (A) Particle positions over 1 second 8.5 8.0 7.5 extended crystal, top view 2.5 2.0 1.5 1.0 2.9 W Pressure: 66.6 Pa Particle diameter: 7 0.5 7.0 Power: Mean velocity: m 0.4 mm/s Particle distance: 0.33 mm 0.0 6.5 6.5 7.0 7.5 8.0 8.5 9.0 9.5 0.2 10.0 0.4 0.6 7.5 1.8 (C) Particle positions over 1 second 7.0 extended crystal, side view 1.0 1.2 1.4 1.6 1.8 2.0 (D) Pair correlation function Pair correlation function 1.6 6.5 y-position in mm 0.8 Particle distances in mm x-position in mm 6.0 5.5 5.0 4.5 4.0 extended crystal, side view 1.4 1.2 1.0 0.8 0.6 0.4 Power: 2.9 W Pressure: 67.4 Pa Particle diameter: 7 Mean velocity: 0.2 m 0.36 mm/s Particle distance: 0.34 mm 3.5 3.5 0.0 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 0.0 0.2 0.4 0.6 x-position in mm 13.5 (E) Particle positions over 1 second 1.4 1.6 1.8 12.5 12.0 11.5 11.0 6 5 4 Power: 23.3 W Pressure: 99 Pa Particle diameter: 7 Mean velocity: 3 m 0.13 mm/s Particle distance: 0.29 mm 2 1 10.5 0 13.5 14.0 14.5 15.0 15.5 16.0 16.5 17.0 17.5 0.0 x-position in mm 0.5 1.0 1.5 2.0 Particle distance in mm 1.8 (G) Particle positions over 1 second 3.5 flat crystal, side view 1.6 (H) Pair correlation function flat crystal, side view 1.4 y-position in mm 3.0 2.5 2.0 1.5 1.0 1.2 1.0 0.8 0.6 0.4 Power: 23.3 W Pressure: 99 Pa Particle diameter: 7 0.5 0.2 Mean velocity: m 0.13 mm/s Particle distance: 0.44 mm 0.0 5.0 2.0 flat crystal, top view Pair correlation function y-position in mm 1.2 (F) Pair correlation function 7 13.0 y-position in mm 1.0 Particle distance in mm flat crystal, top view 4.0 0.8 0.0 5.5 6.0 6.5 7.0 7.5 x-position in mm 8.0 8.5 9.0 0.0 0.5 1.0 1.5 2.0 x-position in mm Fig. 4.15: Particle positions and pair correlation functions of crystals—extended and flat, side and top view. 98 Chapter 4 Results functions of a flat crystal. The particles don’t move very far within one second (E) compared to extended crystals (A). The peaks of the top view pair correlation function (F) are much higher and more peaks are found than in the case of extended crystals (B). The crystalline state is clearly reached in this situation. But the side view of this crystal exhibits more particle movement and thus a much worse pair correlation function. The side view of flat crystals also exhibits a worse statistics since only a few particles are seen. This also degrades the pair correlation function. Fig. 4.16 shows the top view trajectories of the dust particles of the whole observation area of a flat crystal over five seconds. The crystal has been illuminated by two sheets of laser light to increase the observation area. This has the disadvantage that the crystal is not homogeneously illuminated. This explains the parts within the figure without particle trajectories. It is clearly seen that the crystal is not isotropic. The crystal has different regions with different degrees of stability. E.g. the right part of the picture exhibits longer trajectories which means more particle movements than the left part. The movement directions differ as well which can be seen from the orientation of the trajectories. A more or less stable region has been chosen to obtain Fig. 4.15 (E) but the corresponding pair correlation function (F) includes the whole observation area. Fig. 4.16: Particle trajectories of a flat crystal over 5 seconds—top view. 99 4.4 Scattering by the crystal Diffraction experiments have been conducted using extended crystals and the Golay cell as well as the germanium detector. The germanium detector is much more sensitive and has a higher time resolution than the Golay cell (best: µs instead of 0.1 s). This is necessary as can be inferred from Fig. 4.16: Several crystal domains are visible and the crystal exhibits regions of higher temperature. These effects reduce the scattering intensity as described in section 2.5.3 (p. 52). Fig. 4.17 shows particle positions over one second and the corresponding pair correlation function of the crystal of the actual diffraction experiment. The crystal was comparably bad regarding structure and stability. Unfortunately no better crystal could be established that very day when the germanium detector could be lend. Fig. 4.18 shows the result of the plasma crystal diffraction experiment on the crystal shown in Fig. 4.17 using the germanium detector. An orifice within a piece of paper board has been used to obtain a narrow beam at the plasma crystal and to reduce unwanted background radiation. The black curve (upper curve) is the measurement signal obtained by a motorised scan with the germanium detector. The scan direction has been from positive angles to negative angles as indicated by the black (upper) arrow in (a). The large signal between −5◦ and +5◦ is the direct FIR beam. Several small peaks are visible at negative angles. The red curve (middle curve) shows the detector signal without plasma crys0.5 2.0 B Particle positions over 1 second Pair correlation function extended crystal, side view Pair correlation function y-position in mm extended crystal, side view 0.4 1.5 1.0 0.5 Power: ~2 W Pressure: ~50 Pa Particle diameter: 7 Mean velocity: m 0.25 mm/s Particle distance: 0.35 mm 0.3 0.7 0.0 0.8 0.9 1.0 x-position in mm (a) Particle positions over one second. 1.1 0.00 0.25 0.50 0.75 1.00 1.25 1.50 Particle distance in mm (b) Corresponding pair correlation function. Fig. 4.17: Particle positions and pair correlation function of the diffraction experiment crystal. Structure and stability have been very bad in this experiment. Chapter 4 Results 3.0 10 insensitive lock-in 8 Scan direction 6 insensitive lock-in with crystal, sensitive 4 without crystal, sensitive Diffraction peak? 2 2.5 2.0 with crystal, sensitive without crystal, sensitive Diffraction peak? 1.5 1.0 0.5 0.0 0 -20 Germanium detector signal in a.u. Germanium detector signal in a.u. 100 -15 -10 -5 0 5 10 15 20 Angle in degree (a) The scan direction of the detector is indicated by -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 Angle in degree (b) Detail of the left figure. the black and red arrows. Fig. 4.18: Diffraction experiment with the germanium detector. The blue curves show the signal of the insensitive lock-in amplifier. The black curve is the measured signal with plasma crystal and the red curve is measured without crystal. There seems to be a diffraction peak at −12.7 degree. tal. Some peaks are visible here as well but with lower amplitudes. The peak at −12.7◦ seems to be missing. This is a hint that this peak could be a real diffrac- tion peak originating from the plasma crystal. Fig. 4.18 (b) shows a detail of part (a) which magnifies the peaks. The differences between the diffraction signals with crystal (black, upper curve) and without crystal (red, lower curve) are clearly seen. The right peak structure between −3◦ and −10◦ is quite comparable between the two curves and thus cannot originate from the plasma crystal. However, the peak at −12.7◦ could be a real plasma crystal diffraction signal. The scan direction has been reversed for the measurement without plasma crystal as indicated by the red (lower) horizontal arrow in (a). This led to a small error in the angle measurement of about 0.4◦ due to a small mechanical tolerance of motor and gear box. For this reason scans were performed in one and the same direction only in later experiments. The blue curves (lowest curves) show the signal recorded with the insensitive lock-in amplifier. They serve for fixing the zero point of the angle scale. The angle error of about 0.4◦ is visible comparing the positions of the maxima of these two blue curves. Both curves exhibit side shoulders which result from diffraction by the orifice. The amplitude difference between the two measurements (with and without crystal) can result from a drift of the FIR laser beam intensity to lower values. The signals therefore have been normalised to a certain peak to eliminate such an effect. 101 Fig. 4.19: Normalised diffraction signals. The signals have been normalised to the peak marked with the arrow because the corresponding peak structure clearly originates from the scattering arrangement and should not depend on the plasma crystal. Germanium detector signal in a.u. Analysis of the measurement 1.5 with crystal without crystal normalised to this peak 1.0 0.5 0.0 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 Angle in degree The result of the normalisation is shown in Fig. 4.19. The peak at −5.8◦ has been chosen to normalise to because the corresponding peak structure of three close peaks seems to clearly originate from the scattering arrangement (e.g. from the orifice). It should not change when dropping down the plasma crystal. This peak structure (between −4◦ and −7◦ ) appears almost identical for both cases after the normalisation. The difference in the curves between −7◦ and −10◦ are mainly due to the angle measurement error after changing the scan direction as already mentioned. The amplitude difference at −7.8◦ seems to be of minor importance and is not much larger than that at −6.5◦ . The amplitude difference at −12.7◦ is now negligible. This shows that this peak is not a diffraction peak originating from the plasma crystal. A possible but not observed diffraction peak of this experiment could have had a maximum radiation power below 10−14 W since no diffraction peak could be measured with the germanium detector. The negative outcome of this very experiment reveals some important points: (1) It is very difficult but essential to get the different experimental parts running at their optimum at the very same time: FIR laser beam, scattering arrangement, plasma crystal, and data storage. (2) Wavelength stability and intensity of the FIR laser have to be further improved. This could probably be done by replacing the stainless steel, hole output mirror by a mesh output mirror (gold squares on a multi layer film system on a quartz substrate). This would make a different input mirror necessary with a radius of curvature larger than the resonator length. Such a mesh output mirror and concave input mirror could not be manufactured and have to be bought. Additionally a 102 Chapter 4 Results different stabilising system for the whole FIR laser system including the CO2 laser should be installed. Such a system is available from Edinburgh Instruments Ltd. The beam splitter concept should be improved to reliably correct the measured data points for FIR intensity drifts. Different time resolutions of the Pyro, germanium, and Golay cell detectors complicate this and prevented the development of an automatic data correction program. (3) The focussing of the FIR beam has to be improved e.g. using an additional focussing mirror near the plasma chamber. This would make an orifice obsolete. (4) An adjustment of the FIR beam into the plasma chamber during the experiment is difficult and should be avoided. This is so because additional background radiation can occur due to e.g. reflections at the electrodes. These then will most probably be more intense than any diffraction peak. A later calibration is thus useless. (5) It is necessary to have an in situ evaluation of the plasma crystals to decide if structure and stability are good or not. This could not be realised so far: The video analysis takes too much time to meet experimental needs. (6) Flat crystals could be an alternative for the scattering experiments because they are more stable and exhibit a better structure (Fig. 4.15 (E,F)). But then the adjustment of the FIR beam is more difficult because of the closeness to the lower electrode. This favours reflections which would cover real diffraction peaks. The FIR laser beam of 118.83 µm wavelength cannot exactly be focussed to the plasma crystal because the mirrors of the Yolo telescope have limited radii of curvature. Larger radii would be preferable but could not be manufactured by the in-house workshop. Therefore the FIR beam has been relatively broad at the plasma crystal and an orifice has been used to obtain a more narrow beam. But this reduces the FIR radiation power reaching the plasma crystal. To eliminate such losses due to an orifice a 50 cm long pyrex glass tube of inner diameter of 15 mm has been installed to guide the FIR beam to the TPX plasma chamber. The FIR beam has been focussed into the glass tube which serves as wave guide and avoids a broadening of the FIR beam. This narrows the beam and increases the radiation power at the plasma crystal. But the glass tube has to be adjusted very carefully to avoid a diffraction pattern originating from the tube itself. Furthermore only the powder diffraction method can be applied with this setup and not the pendant of the rotating crystal method because the direction of 103 40 FIR beam profile at the plasma chamber 35 Pyro signal in W 30 Fig. 4.20: FIR beam profile at the lower electrode. The beam width is about 7.1 mm 25 20 width = 7.1 mm 15 10 Measurement Gauss fit 5 with a peak intensity of about 36 µW mea- 0 -12 -10 sured with the Pyro detector. -8 -6 -4 -2 0 2 4 6 8 10 12 Horizontal position in mm the incoming FIR beam cannot be changed. Fig. 4.20 shows the FIR beam profile 2 cm above the lower electrode when using the glass tube. This beam profile has been recorded with the Pyro detector without any orifice to avoid lowering the signal. Thus the directional sensitivity has not been very good. A Gaussian fit of the measurement curve gives a width of about 7.1 mm and a peak power of 36 µW is reached in this experiment. The measured curve is not perfectly symmetric which hints to a slight misalignment of the glass tube. 1.0 10 0.9 sensitive insensitiv (a.u.) reference signal 0.8 5 0.7 0 0.6 -15 -10 -5 0 5 10 Angle in degree (a) Scan with de-adjusted glass tube. 1.0 Adjusted glass tube 30 Golay signal in nW Golay signal in nW 1.1 15 35 0.9 25 0.8 20 0.7 15 sensitive insensitive (a.u.) 10 0.6 reference signal 0.5 5 0 Pyro reference signal in a.u. 1.2 De-adjusted glass tube Pyro reference signal in a.u. 20 0.4 -15 -10 -5 0 5 10 Angle in degree (b) Scan with adjusted glass tube. Fig. 4.21: Calibration scans for glass tube adjustment. Precise adjustment of FIR beam and glass tube are necessary to avoid perturbing parasitic peaks. The blue curve (with circles) shows the Pyro reference signal recorded using the beam splitter right after the FIR laser output. The FIR laser intensity fluctuations of about 10 to 20 % cannot explain the parasitic peaks. Fig. 4.21 shows calibration scans with the Golay cell detector for the glass tube adjustment. The difference between (a) and (b) is a different focussing of the FIR beam into the glass tube. In (a) there are several peaks visible besides the main FIR beam. A careful adjustment of glass tube and FIR beam eliminates such parasitic 104 Chapter 4 Results peaks as shown in (b). This experiment shows the necessity of a careful adjustment of FIR beam and glass tube to avoid perturbing reflections. Thus beam and glass tube cannot be adjusted during an actual diffraction experiment but beforehand. This is a major disadvantage when using the glass tube and it is doubtful if the enhancement of the FIR beam intensity due to the glass tube is such a big improvement. However, using only flat crystals for the scattering experiments should ease the situation because they are more stable. Thus FIR beam adjustments during the scattering experiments should not be necessary when using flat crystals. Chapter 5 Conclusion The aim of this work was the development and qualification of a setup for the analysis of 3D plasma crystals using FIR (far infrared) diffraction signals. During the progress of this project the realisation of several elements of the undertaking turned out to be much more challenging than initially expected. Significant design and development effort had to be invested in each part of the system starting with the FIR laser system and ending with the plasma crystals and their control procedures. Large 3D plasma crystals had initially been produced in a stainless steel plasma chamber with four glass windows. This chamber resembles the well known GEC reference cell (GEC: Gaseous Electronic Conference) but it is smaller and has a segmented electrode which allows the application of different electric fields. These crystals had been very stable with volumes of about 3 × 3 × 3 cm3 containing millions of dust particles. The mono disperse micro particles used have been gold coated because of the higher refractive index of gold compared to polymer particles. This gold coating increases scattering intensities expected from these particles. The power of the incoming radiation necessary to measure diffraction peaks from those crystals has been calculated using the scattering theory described in this work. The use of gold coated micro particles has been assumed in this calculation. A CO2 laser that pumps the FIR resonator has been purchased based on this estimation and a FIR resonator has been developed. A Golay cell detector has been purchased which is operated at room temperature and has a minimum signal limit well above the diffraction intensities estimated. However, it turned out that the gold coated dust particles could not be used in actual scattering experiments because they degenerate most probably due to an argon ion etching process. The surface of the dust particles becomes craggy and long 105 106 Chapter 5 Conclusion term stable plasma crystals could not be produced using these particles. Therefore, uncoated mono disperse melamine resin (MF) and polystyrene (PS) particles could be used only, decreasing the diffraction signal intensities below those expected. The FIR laser system built in this work consists of a commercial CO2 pump laser and a home made FIR wave guide resonator. The FIR resonator design allows an easy change of the wave guide radius, input and output stainless steel mirrors, and of the laser gas. The FIR laser provides a Gaussian beam of up to 5 mW power and a wavelength of 118.83 µm and 170.58 µm when using methyl alcohol as laser medium. The FIR laser system has carefully been characterised and tested. This includes e.g. the variation of input and output plane mirror roughness and their hole diameters, the variation of the resonator pipe radius, and the change from plane mirrors to concave mirrors. The wavelength selectivity and the stability of the resonator has been improved using the concave instead of plane mirrors. The CO2 laser Brewster windows got dirty after about one year of frequent operation due to oil vapour originating from the rotary vane pump and diffusing back into the CO2 laser plasma. The zinc selenite (ZnSe) Brewster windows therefore had to be removed, cleaned, polished using lap foils, and reinstalled again. This procedure worked quite well but some scratches remained on the windows which could not be removed by polishing. These are probably responsible for the somewhat reduced CO2 laser power after the readjustment of the laser. The CO2 laser power is stabilised by an opto–galvanic stabiliser. It measures changes of the laser current which are induced by changes of the laser power to readjust the laser resonator length. However, it turned out that the long term stability of the whole FIR laser system has to be further improved by enhancing the frequency stability of the CO2 laser with a feedback system that measures directly the FIR beam intensity through a beam splitter. The development of a new plasma vacuum chamber has been a challenging task of this project. The chamber should provide optical and FIR access to the plasma crystals—if possible roundabout. Only a few materials suitable for vacuum vessels meet the requirement to be transparent in the visible and in the far infrared region of the spectrum. Crystalline quartz windows of the z-cut type fulfil the transparency demand. But a polygon chamber does not provide roundabout access to the crystals which is necessary to assure the detection of every possible diffraction peak from plasma crystals. The polymer poly-methylpentene (TPX) is a mechanically stable material which 107 meets the demand of roundabout optical and FIR transparency. Thus a plasma vacuum chamber has been built using a TPX cylinder which is glued into grooves of aluminium flanges using silicone rubber. This chamber is smaller than the one previously mentioned and it has a larger window area which means more floating walls. This changes plasma characteristics and thereby plasma crystal properties compared to the other chamber. The material TPX turned out to be sensitive to UV radiation which is produced by the plasma. It becomes more and more opaque due to microscopically small imperfections of the material. Furthermore, TPX is elastic to a certain extent but at the same time prudish. Forces due to repetitive venting and pumping stressed the material enormously and led to failures of the chamber. Although TPX is not the perfect material for the plasma chamber it is still used because of the lack of alternatives. Several electrode geometries and electrical wirings have been examined to produce plasma crystals. These include the powering of upper, lower, and parts of the lower electrode as well as the application of different DC and AC electric fields to the powered as well as to parts of the grounded electrode. Two different plasma crystal types have thereby been found: extended and flat crystals. The extended crystals have volumes up to 3 × 3 × 2 cm3 and are not fully stationary. They still show relatively high mean particle velocities of e.g. 0.36 mms−1 . The flat crystals are produced using higher power or by powering the lower electrode. They consist of three to four layers only but are extended over almost the whole electrode area of 10 cm in diameter. They are more stable (mean particle velocity e.g. 0.13 mms−1 ) and exhibit a better defined crystal with less structural domains. Various control procedures have been developed to stabilise the crystals and to optimise their structure by reducing their defects and the structural domain density. The crystal temperature could be reduced through lifting the plasma crystal to about two centimetres above the lower electrode by applying DC voltages to the electrodes. This lifted crystal position is not only advantageous for the crystal quality but also for the diffraction experiment. It eases the FIR beam adjustment and disturbing reflections from the lower electrode can easily be minimised. A scattering arrangement has been developed to guide the FIR laser beam into the plasma chamber and to record diffraction peaks. It consists of a Yolo telescope, several tilted mirrors, and a motorised circular positioning system to move mirrors and detector around the chamber. All mirrors and mirror holders have been made 108 Chapter 5 Conclusion of aluminium and they have been manufactured and polished by the in house workshop. The Yolo telescope is composed of two spherical mirrors and focusses the FIR beam. Two tilted mirrors deflect the beam from the laser table to the plasma chamber table where it can straightly reach the plasma chamber. Incoming beam and plasma crystal are not moved and diffraction signals are expected from single structure domains of the crystals. A second diffraction method is an analogy to the rotating crystal recording. But since 3D plasma crystals can not easily be rotated in a well defined way, the incoming laser beam has to be rotated around the crystal together with the detector. A mirror system consisting of four mirrors mounted on a circular rail way accomplishes this beam rotation around the chamber and the detector is placed on a separate waggon. Several computer programs have been written e.g. the program “Cockpit” by which it is possible to control the plasma parameters like pressure and power, to move the detector waggon and monitor its position, to calculate diffraction peak positions for different crystal structures and lattice plane distances, and to do the complete data storage. The program “Beam calculator” has been developed to calculate beam diameters of the FIR beam on its way along the scattering arrangement. Position and focal distances of the Yolo telescope mirrors have been determined using this program which applies the formulae of Gaussian beam optics. A significant effort has been put into the design, the improvement, and the testing of the video analysis software. Existing procedures have been adapted, refined, and customised to ensure the correct analysis of videos taken by laser sheet illumination and a CCD (Charge Coupled Device) camera. The production of plasma crystals has been evaluated and refined by judging structure and stability with the video analysis software. A 2D mesh that consists of about 2090 golden squares with edge lengths of 40 µm and distances of 200 µm has been deposited on a GaAs wafer (courtesy of Nadine Vitteriti, Chair for Applied Solid State Physics, Prof. Dr. A. D. Wieck, Ruhr–University Bochum). Diffraction signals from this golden mesh have successfully been recorded and the influence of the TPX wall and chamber structure has been analysed. Detailed estimations have been given for the diffraction peak intensities expected from real plasma crystals on the basis of these results. They suggest that a more sensitive and fast germanium detector should be used in diffraction 109 experiments and that the number of different domains within a plasma crystal has to be minimised to achieve enough intensity in one diffraction peak. The presence of several structural domains within the extended 3D plasma crystals remains an unsolved problem. It prevented the recording of a diffraction peak of an actual plasma crystal. Flat crystals consisting of only three or four planes may be an alternative to large 3D crystals. They are located nearer to the lower electrode, however. The adjustment of the FIR beam becomes more critical when using flat crystals because beam reflections from the near electrode may increase the incoherent background. The basis for FIR diffraction experiments on plasma crystals has been developed in this work. Further refinements of the FIR laser system and the plasma crystal production and control are necessary to obtain diffraction signals. 110 Chapter 5 Conclusion List of Figures 2.1 The CO2 molecule and its vibration modes . . . . . . . . . . . . . . 7 2.2 Energy level and excitation scheme for the CO2 laser . . . . . . . . 8 2.3 Molecules within the FIR resonator . . . . . . . . . . . . . . . . . . 9 2.4 Energy levels of the FIR active molecules . . . . . . . . . . . . . . . 10 2.5 Propagation of a Gaussian beam . . . . . . . . . . . . . . . . . . . . 13 2.6 Focussing of a Gaussian beam by a lens . . . . . . . . . . . . . . . . 14 2.7 Sheath and presheath near a wall . . . . . . . . . . . . . . . . . . . 18 2.8 Dust particle charge vs. ion drift velocity . . . . . . . . . . . . . . . 25 2.9 Contour plot of the ion density . . . . . . . . . . . . . . . . . . . . 26 2.10 Interparticle forces in a dust molecule . . . . . . . . . . . . . . . . . 34 2.11 Comparison of ion drag forces . . . . . . . . . . . . . . . . . . . . . 37 2.12 Dust particle strings and crystal organisation . . . . . . . . . . . . . 41 2.13 Hysteresis loop of dust temperature during pressure variation . . . . 42 2.14 Scattering geometry . . . . . . . . . . . . . . . . . . . . . . . . . . . 45 2.15 Dipole scattering. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 2.16 Polar diagram for Rayleigh scattering . . . . . . . . . . . . . . . . . 50 2.17 The Debye-Waller factor . . . . . . . . . . . . . . . . . . . . . . . . 52 3.1 The whole setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57 3.2 Sketch of the CO2 laser . . . . . . . . . . . . . . . . . . . . . . . . . 58 3.3 Dirty Brewster window . . . . . . . . . . . . . . . . . . . . . . . . . 59 3.4 CO2 laser adjustment . . . . . . . . . . . . . . . . . . . . . . . . . . 60 3.5 FIR resonator. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 3.6 Cross section of resonator pipes and spacer . . . . . . . . . . . . . . 62 3.7 Bushings for quartz tube support . . . . . . . . . . . . . . . . . . . 63 3.8 Sketch of FIR laser beam adjustment and photo of the mirror system 65 3.9 Aluminium mirrors . . . . . . . . . . . . . . . . . . . . . . . . . . . 65 3.10 Reflection coefficients of aluminium . . . . . . . . . . . . . . . . . . 66 111 112 List of Figures 3.11 Chamber and mirror system . . . . . . . . . . . . . . . . . . . . . . 67 3.12 Waggon and guide rail with gear ring. . . . . . . . . . . . . . . . . . 68 3.13 Scattering control scheme . . . . . . . . . . . . . . . . . . . . . . . 68 3.14 Angular velocity of the detector carriage against control voltage . . 69 3.15 Sketch of Golay principle and photo . . . . . . . . . . . . . . . . . . 69 3.16 Dependence of the Golay sensitivity on chopper frequency . . . . . 70 3.17 Plasma chamber. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72 3.18 Matching network . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74 3.19 Electrodes of the plasma chamber . . . . . . . . . . . . . . . . . . . 74 3.20 Gold mesh and holder . . . . . . . . . . . . . . . . . . . . . . . . . 76 4.1 FIR signal versus pressure . . . . . . . . . . . . . . . . . . . . . . . 82 4.2 FIR laser beam profiles at 55 mm and 1080 mm distance . . . . . . 82 4.3 3D visualisation of the FIR beam . . . . . . . . . . . . . . . . . . . 83 4.4 Resonator scan with concave mirrors . . . . . . . . . . . . . . . . . 84 4.5 Pressure dependence of the FIR signal . . . . . . . . . . . . . . . . 85 4.6 Calibration of the beam splitter . . . . . . . . . . . . . . . . . . . . 86 4.7 Diffraction peaks of the golden mesh . . . . . . . . . . . . . . . . . 88 4.8 Influence of the TPX chamber on the diffraction pattern . . . . . . 90 4.9 Peak intensity ratios without/with TPX . . . . . . . . . . . . . . . 90 4.10 Lower electrode configuration A and dust particle distribution . . . 92 4.11 Lower electrode configuration B and dust cloud—side view . . . . . 92 4.12 Degenerated gold coated micro particles . . . . . . . . . . . . . . . 94 4.13 Self bias against ring voltages . . . . . . . . . . . . . . . . . . . . . 95 4.14 String formation in a plasma crystal . . . . . . . . . . . . . . . . . . 95 4.15 Particle positions and pair correlation functions of crystals . . . . . 97 4.16 Particle trajectories of a flat crystal over 5 seconds—top view. . . . 98 4.17 Particle positions and pair correlation function of the diffraction experiment crystal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99 4.18 Diffraction experiment with the germanium detector . . . . . . . . . 100 4.19 Normalised diffraction signals . . . . . . . . . . . . . . . . . . . . . 101 4.20 FIR beam profile at the lower electrode . . . . . . . . . . . . . . . . 103 4.21 Calibration scans for glass tube adjustment . . . . . . . . . . . . . . 103 List of Tables 2.1 Grain charge for different mechanisms not included in OML theory 31 2.2 Ion currents and grain potentials for different effects 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[58] Erik Bründermann, Jens Ränsch, Matthias Krauß, and Johannes Kunsch. Erste THz-Videos mit einer silizium-basierten IR-Kamera. Photonik, 6:60–63, 2006. [59] Jürgen Fischbach. Eigenschaften optischer Materialien. LOT-Oriel Gruppe Europa, 2004. 120 Bibliography Danksagung Mein herzlicher Dank geht an Herrn Prof. Dr. Jörg Winter, der mir die Durchführung dieser Arbeit ermöglichte. Seinen Ideen und seiner enthusiastischen Überzeugungskraft ist das Zustandekommen weiter Teile des Aufbaus zu verdanken. Seit ich an diesem Lehrstuhl für Experimentalphysik II arbeite, unterstützt mich Herr Winter, wo er kann. Er gab mir besonders in den persönlich schwierigen Zeiten der letzten Jahre, in denen mein Bruder und mein Vater starben, den für mich notwendigen Freiraum und uneingeschränkte Rückendeckung. Dafür danke ich Herrn Winter sehr. Bei dem gesamten Team des Lehrstuhls für Experimentalphysik II möchte ich mich bedanken für die freundliche und fröhliche Atmosphäre. Der lockere Umgang miteinander erleichtert das Arbeiten ungemein. Besonders bedanke ich mich bei Andreas Aschinger für die Zusammenarbeit in allen Bereichen der Arbeit und insbesondere für die Umsetzung der Konzepte zur Videoanalyse. Stefanie Schornstein danke ich für die Mitarbeit bei der Charakterisierung des FIR Resonators. Beide haben das Projekt entscheidend vorangetrieben. Die Techniker des Lehrstuhls haben wesentlich dazu beigetragen, den Aufbau zu realisieren. Ich danke deshalb Herrn Karl Brinkhoff für die Hilfe bei der Entwicklung des FIR Resonators und der Plasmakammer. In vielen Diskussionen haben wir diese entworfen und immer wieder verbessert. Herrn Kai Fiegler danke ich für die Hilfe bei der Entwicklung des Spiegelsystems zur Lenkung des FIR Strahls in die Plasmakammer und für die weitere Betreuung des Aufbaus. Er hat auch einen erheblichen Teil seiner Freizeit in diese Arbeit investiert. Herrn Axel Lang danke ich für die gesamte und umfassende Betreuung des Labors und die Hilfe bei allen möglichen Problemen. Herrn Wilhelm Winterhalder und Herrn Michael Konkowski danke ich für die Anfertigung verschiedenster elektrischer und elektronischer Komponenten, die zur Steuerung des Experiments und zur Datenaufnahme unerlässlich sind. Eine solche Arbeit wäre ohne die Anstrengungen der Techniker nicht möglich – vielen herzlichen Dank! Frau Margot Ocklenburg möchte ich danken für vielfache Hilfen in jeglichen organisatorischen und verwaltungstechnischen Dingen. Es ist oft schwer, den Überblick zu behalten und ich war stets froh, jemanden zu haben, der sich auskennt. Herrn Dr. Erik Bründermann gilt mein Dank für zahlreiche Tipps bezüglich der Detektion der FIR Strahlung und für das Ausleihen und Bedienen des Germanium Detektors. Durch die Zusammenarbeit mit ihm habe ich viel gelernt. Ebenso danke ich Herrn Prof. Dr. Henning Soltwisch und Herrn Dr. Carsten Pargmann für die Beratung und die Tipps beim Aufbau des FIR Resonators. Ihre Erfahrungen halfen mir beim meiner Arbeit sehr. Weiterhin danke ich Herrn Soltwisch für die Übernahme des Koreferates. Mein herzlicher Dank geht auch an Herrn Dr. Uwe Konopka für die Einführung in das Feld der komplexen Plasmen während meines Besuches in Garching und die Bereitstellung einiger Routinen zur Auswertung der Partikelbewegungen. Darauf aufbauend konnte die Videoanalyse weiterentwickelt werden. Ebenso danke ich Herrn Dr. habil. Dietmar Block für die zahlreichen Diskussionen während meines Besuchs in Kiel und während der vielen Tagungen, auf denen wir uns begegneten. Seine Kommentare und Ratschläge waren immer sehr erhellend. Frau Nadine Viteritti danke ich für die Anfertigung des Goldgitters, welches sie nach mehreren Versuchen auf einen Wafer gebracht hat. Mit diesem Goldgitter konnte das Arbeitsprinzip des Aufbaus demonstriert werden. Bei Frau Dr. Janine–Christina Schauer und Herrn Dr. Suk-Ho Hong bedanke ich mich herzlich für ihre Freundschaft und die unendlichen physikalischen und teils philosophischen Diskussionen. Unsere gegenseitige Unterstützung hat mir sehr geholfen und mir viel Rückhalt gegeben. Zu guter Letzt bedanke ich mich herzlich bei meiner Familie. Bei meiner Frau Liudmila, die mir mit Ihrer Liebe jederzeit ihre volle Unterstützung gibt. Bei meiner Mutter, die mir trotz schwieriger Zeiten immer zur Seite Stand und auch bei meinem Vater, der nie seinen Humor verlor. Er hat mir gezeigt, wie man mit Mut und Lebensfreude Wunder vollbringen kann. Lebenslauf Persönliche Daten Name Jens Ränsch Anschrift An der Maarbrücke 41 44973 Bochum Geburtstag 31.01.1978 Geburtsort Bernburg (Sachsen–Anhalt) Familienstand verheiratet, 1 Kind Hochschulausbildung 10.2003 – heute Wissenschaftlicher Mitarbeiter am Lehrstuhl für Experimentalphysik II an der Ruhr–Universität Bochm, Promotion in experimenteller Plasmaphysik 10.1998 – 10.2003 Studium der Physik an der Ruhr–Universität Bochum, Diplomarbeit Untersuchungen zu Wechselwirkungen zwischen flüssigen Galliumoberflächen und kapazitiv gekoppelten HF–Plasmen, Abschlussnote: “mit Auszeichnung” Wehrdienst 07.1997 – 05.1998 Wehrdienst in Düsseldorf als Richtfunker und Kraftfahrer Schulausbildung 08.1992 – 07.1997 Ingeborg-Drewitz-Gesamtschule in Gladbeck, Abiturnote: 1.0 08.1991 – 08.1992 Gymnasium Süd-Ost in Bernburg 08.1989 – 08.1991 7. Oberschule “Wilhelm Pieck” in Bernburg 09.1984 – 08.1989 Allgemeinbildende polytechnische Oberschule “Karl Liebknecht” in Bernburg Preise 05.2003 Studienabschlussstipendium der Ruth und Gert Massenberg-Stiftung für die Studienleistung 02.2004 “ROTARY-UNIVERSITÄTSPREIS 2003 für herausragende Studienleistungen” für die Diplomarbeit, verliehen vom Rotary-Club Bochum-Hellweg Tätigkeiten neben Studium und Promotion 01.2005 – heute Mitarbeit im Vorstand des Sportvereins “Biriba Brasil de Bochum e.V.” als Schriftführer, Organisation diverser Sportveranstaltungen und Vereinsfahrten, Abwicklung sämtlicher schriftlicher Korrespondenz 10.2000 – 02.2008 Leitung von Seminaren, Übungsgruppen und Praktika an der Ruhr–Universität Bochum 10.2003 – 08.2006 Leitung des Physikunterrichts für die MTA-Ausbildung am Bergmannsheil-Krankenhaus in Bochum Ränsch, Jens ......................................................... Name, Vorname Versicherung gemäß § 7 Abs. 2 Nr. 5 PromO 1987 Hiermit versichere ich, dass ich meine Dissertation selbstständig angefertigt und verfasst und keine anderen als die angegebenen Hilfsmittel und Hilfen benutzt habe. Meine Dissertation habe ich in dieser oder ähnlicher Form noch bei keiner anderen Fakultät der Ruhr-Universität Bochum oder bei einer anderen Hochschule eingereicht. Bochum, den ............................................ .......................................................... Unterschrift