Influence of the bias voltage on the formation of beryllium films by a thermionic vacuum arc method

Beryllium is intended to be used as suggested material for the first wall in the thermonuclear power plants. Some tiles of the first wall will be of inconel coated by a beryllium layer that must be adherent to the substrate and have a compact structure in order to resist as much as possible the dramatic interaction with the high energetic plasma particles, ions, electrons and neutrons. Applying bias voltages (−200 to + 700 V) on the substrates, the morphology of the prepared Be layers using the original thermionic vacuum arc method developed at NILPRP was controlled in order to obtain smooth surfaces, free of holes and lamellar structures. The prepared films were studied and characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Auger spectroscopy (AES). The films prepared using negative bias voltages were found to be more compact and smooth with an average roughness (R_ms) of 7 nm.     

Modelling the erosion of beryllium carbide surfaces

Redeposition of beryllium eroded from main chamber plasma facing components of ITER onto the divertor material carbon creates a mixed material, beryllium carbide Be₂C, whose interaction with the plasma is not well known. In this study, we have investigated the erosion of Be₂C by deuterium using molecular dynamics simulations and ERO impurity modelling. We found that beryllium sputters preferentially over carbon and identified the sputtering mechanism in the ion energy range 10-100 eV to be both physical and swift chemical sputtering. In addition to single atoms, different types of small molecules/clusters were sputtered, the most frequently occurring molecules being BeD, Be₂D, and CD. The sputtering threshold was found to lie between 10 and 15 eV. The MD sputtering yields were used in plasma impurity simulations, serving as a replacement for input data obtained with TRIM. This changes the accumulation rate of impurity Be in the divertor region compared to previous estimates.     

Argon plasma immersion ion implantation of polystyrene films

Plasma immersion ion implantation (PIII), using bias voltages of 5, 10, 15 and 20 kV in an argon plasma and fluences in the range of 2 × 10¹⁴-2 × 10¹⁶ ions/cm², was applied to 100 nm polystyrene films coated on silicon wafer substrates. The etching kinetics and structural changes induced in the polystyrene films were investigated with ellipsometry, Raman and FTIR spectroscopies, optical and scanning electron microscopies, atomic force microscopy and contact angle measurements. Effects such as carbonisation, oxidation and cross-linking were observed and their dependence on the applied bias voltage is reported. Variations in the etching rate during the PIII process and its relationship to carbonisation of the modified surface layer are explored.     

First tests of diagnostic mirrors in a tokamak divertor: An overview of experiments in DIII-D

Mirrors will be used in ITER in all optical diagnostic systems observing the plasma radiation in the ultraviolet, visible and infrared ranges. Diagnostic mirrors in ITER will suffer from electromagnetic radiation, energetic particles and neutron irradiation. Erosion due to impact of fast neutrals from plasma and deposition of plasma impurities may significantly degrade optical and polarization characteristics of mirrors influencing the overall performance of the respective diagnostics. Therefore, maintaining the best possible performance of mirrors is of the crucial importance for the ITER optical diagnostics. Mirrors in ITER divertor are expected to suffer from deposition of impurities. The dedicated experiment in a tokamak divertor was needed to address this issue. Investigations with molybdenum diagnostic mirrors were made in DIII-D divertor. Mirror samples were exposed at different temperatures in the private flux region to a series of ELMy H-mode discharges with partially detached divertor plasmas. An increase of temperature of mirrors during the exposure generally led to the mitigation of carbon deposition, primarily due to temperature-enhanced chemical erosion of carbon layers by D atoms. Finally, for the mirrors exposed at the temperature of ∼160 °C neither carbon deposition nor degradation of optical properties was detected.     

Preparation of Al thin films charged with helium by DC magnetron sputtering

Helium atoms, up to 6.9 at.%, were introduced into Al films by DC magnetron sputtering in a He/Ar mixed atmosphere and distributed evenly in it. The relation between the He/Ar flux ratio, bias voltage, substrate temperature and helium concentration is studied. The helium concentration can be easily controlled by change of the process parameters and it greatly affects the morphology of film. TEM analysis suggests that small helium bubbles with a diameter of 1 nm are formed in the grain.     

Change in magnetic properties of MgB2 thin films after irradiation by 200 MeV Au ion beam

The SHI irradiation induced effects on magnetic properties of MgB₂ thin films are reported. The films having thickness 300-400 nm, prepared by hybrid physical chemical vapor deposition (HPCVD) were irradiated by 200 MeV Au ion beam (S_e ∼ 23 keV/nm) at the fluence 1 × 10¹² ion/cm². Interestingly, increase in the transition temperature T_c from 35.1 K to 36 K resulted after irradiation. Substantial enhancement of critical current density after irradiation was also observed because of the pinning provided by the defects created due to irradiation. The change in surface morphology due to irradiation is also studied.     

Structural investigation of re-deposited layers in JET

JET Mk-II Gas Box divertor tiles exposed in 1998-2001 have been analysed with various ion beam techniques, secondary ion mass spectrometry (SIMS) and Raman spectroscopy. Inner divertor wall tiles removed in 2001 were covered with a duplex film. The inner layer was very rich in metallic impurities, with Be/C ∼ 1 and H-isotopes only present at low concentrations. The outer layer contained higher concentrations of D than normal for plasma-facing surfaces in JET (D/C ∼ 0.4), and Be/C ∼ 0.14. Raman and SIMS analyses show that the deposited films on inner divertor tiles are hydrogenated amorphous carbon with low sp³ fractions. The deposits have polymeric structure and low density. Both Raman scattering and SIMS indicate that films on inner divertor wall Tiles 1 and 3, and on floor Tile 4 have some differences in the chemical structure of the deposited films     

Middle-frequency magnetron sputtering for GaN growth

A middle-frequency magnetron sputtering system was designed and constructed for GaN growth, in which a pair of back cooled pool-shaped twin magnetrons were used for Ga metal targets. GaN films were prepared using this system under various gas pressure (0.5-3.0 Pa) in a mixture of N₂ and Ar with N₂/Ar ratio of 6:1. X-ray diffraction showed that the GaN films had a strong (0 0 0 2) orientation, and the film deposited at 1.5 Pa had two more weak peaks attributed to and . The full width at half maximum (FWHM) of the (0 0 0 2) peak for the GaN film deposited at 1.5 Pa and 0.5 Pa is ∼721 and ∼986 arcsec, respectively. The deposition rate was in the range of 43.5-87.8 nm/min and was mainly influenced by the deposition pressure. The films deposited at higher pressures are columnar in structure. A root-mean-square roughness of 4.4 nm was obtained from the atomic force microscopy (AFM) surface morphology of the film deposited at 0.5 Pa.     

Nanoscratch study of ZnO thin films deposited using radio frequency magnetron sputtering

In this study, a radio frequency magnetron sputtering system was used to deposit zinc oxide (ZnO) thin films onto langasite substrates. The thickness of the ZnO film increased from 0.3 to 1.2 μm upon increasing the deposition power from 100 to 200 W. The predominant growth orientation was along the c-axis (0 0 2); the intensities of the signals in the X-ray diffraction spectrum increased significantly upon increasing the film thickness. Scanning electron microscopy images revealed columnar structures in the ZnO films and the morphology of ZnO grains is found to be continuous and dense. It is attributed that oxygen chemisorbs on the target and cases a surface layer of adsorbed oxygen. We suggest that the more neutral ion bombardment on the growing film which induces the higher sputtering rate of the growing film. From in situ imaging of scratched tracks, measurement of the coefficient of friction was an effective means of detecting the occurrence of structural defects in the microstructures. We also found that the chemical compositions of ZnO films prepared under various deposition powers could be investigated using X-ray photoelectron spectroscopy.     

Studies of effect of deposition parameters on the ZnO films prepared by PLD

Thin films of zinc oxide (ZnO), having different thicknesses were prepared by pulsed laser deposition (PLD) technique onto silicon Si(1 1 1) and quartz (SiO₂) substrates at different partial pressures of oxygen. Rutherford back scattering (RBS) analysis was carried out in order to investigate effect of deposition parameters on thickness of films. Quality of the films was investigated by X-ray diffraction (XRD) and atomic force microscopy (AFM) analyses. The thickness of the film was found to increase with oxygen partial pressure for both Si and SiO₂ substrates.     

Super X divertors for solving heat and neutron flux problems of fusion devices

We present a new magnetic geometry, called the Super X divertor (SXD), that could potentially solve the enormous heat exhaust problem of next-generation high power-density experiments and fusion reactors. With only small changes in net coil currents, the axisymmetric SXD modification of the standard divertor (SD) coils greatly increases the divertor radius, the line length, and the plasma-wetted area. The lower B at large R decreases parallel heat flux and hence lowers the plasma temperature at SXD plates to below 10 eV, allowing higher divertor radiation fractions. The SXD could safely exhaust five times more heat than an SD, is unique in allowing adequate shielding of divertor target from neutron damage, and can enable much improved, reactor-relevant core plasma performance.     

A direct current glow discharge plasma source for inner surface modification of metallic tube

A dc glow discharge plasma source was developed for inner surface modification of metallic tubes with an inner diameter of 10 mm. A tungsten wire of 30 μm thick was stretched inside the tube to form coaxial electrodes. DC glow discharge plasma was generated inside the tube by applying a negative high dc voltage to the tube. It was found that the length of the cylindrical plasma bulk depends linearly on the applied voltage. The electron excitation temperature of Ar plasma was measured as 12830 ± 550 K by optical emission spectroscopy method. As a preliminary application, diamond-like carbon (DLC) films were deposited onto the inner surface of stainless steel tube of 100 mm in length and 10 mm in inner diameter by using CH₄/Ar mixture with 40% CH₄ at 40 Pa pressure. The chemical structure of the DLC film deposited on the substrate was analyzed by Raman spectroscopy. The integrated intensity ratio (I_D:I_G) was obtained as 1.62 from the Raman spectra. The thickness of the DLC film deposited on the substrate was estimated as 1.5 μm by scanning electron microscopy (SEM) observation.     

MeV-ion beam analysis of the interface between filtered cathodic arc-deposited a-carbon and single crystalline silicon

Amorphous carbon (a-C) films were deposited on Si(1 0 0) wafers by a filtered cathodic vacuum arc (FCVA) plasma source. A negative electrical bias was applied to the silicon substrate in order to control the incident energy of carbon ions. Effects of the electrical bias on the a-C/Si interface characteristics were investigated by using standard Rutherford backscattering spectrometry (RBS) in the channeling mode with 2.1-MeV He²⁺ ions. The shape of the Si surface peaks of the RBS/channeling spectra reflects the degree of interface disorder due to atomic displacement from the bulk position of the Si crystal. Details of the analysis method developed are described. It was found that the width of the a-C/Si interface increases linearly with the substrate bias voltage but not the thickness of the a-C film.     

Formation of Au nanoparticles in silica by post-irradiation and thermal annealing

SiO₂ + Au thin films were prepared on SiO₂ substrates using ion beam assisted deposition (IBAD). The film was annealed at different temperatures. After each annealing, the optical absorption spectrum was taken to monitor the gold nanocluster formation in the thin film. By using Doyle’s formula, the size of the nanoclusters was determined and plotted as a function of the annealing temperature. Separately, other identical films were bombarded with ions of different energies and different fluence to monitor the nanoclusters forming during the bombardments. We have compared the effect of electronic energy deposition of the energetic ions with the effect of annealing at various temperatures.     

Ion beam characterization of rf-sputter deposited AlN films on Si(1 1 1)

Aluminum nitride (AlN) thin films have been deposited on Si(1 1 1) substrates by using reactive-rf-magnetron-sputtering at 250 °C. The crystalline quality and orientation of the films have been studied by X-ray diffraction (XRD). We have observed that the films grow with c- or a-axis orientation. The composition, film thickness, impurities and stress are considered to be factors affecting the orientation and have been analyzed by Rutherford backscattering spectroscopy (RBS), nuclear reaction analysis (NRA) and XRD. Their effects on the film growth will be discussed. Surface morphology of the films will be also presented.     

Surface roughness of ion-bombarded Si(1 0 0) surfaces: Roughening and smoothing with the same roughness exponent

We have carried out scanning tunneling microscopy experiments under ultrahigh vacuum condition to study the roughness of pristine as well as ion-bombarded Si(1 0 0) surfaces and of ultrathin Ge films deposited on them. One half of a Si(1 0 0) sample (with native oxide layer) was irradiated at room temperature using 45 keV Si⁻ ions at a fluence of 4 × 10¹⁵ ions/cm² while the other half was masked. STM measurements were then carried out on the unirradiated as well as the irradiated half of the sample. Root-mean-square (rms) roughness of both the halves of the sample has been measured as a function of STM scan size. Below a length scale of ∼30 nm we observe surface smoothing and surface roughening is observed for length scales above this value. However, the surface is self-affine up to length scales of ∼200 nm and the observed roughness exponent of 0.46 ± 0.04 is comparable to earlier cases of ion sputtering studies where only roughening [J. Krim, I. Heyvart, D.V. Haesendonck, Y. Bruynseraede, Phys. Rev. Lett. 70 (1993) 57] or only smoothing [D.K. Goswami, B.N. Dev, Phys. Rev. B 68 (2003) 033401] was observed. Preliminary results involving morphology for Ge deposition on clean ion-irradiated and pristine Si(1 0 0) surfaces are presented.     

Studies on the high electronic energy deposition in polyaniline thin films

We report here the physico-chemical changes brought about by high electronic energy deposition of gold ions in HCl doped polyaniline (PANI) thin films. PANI thin films were synthesized by in situ polymerization technique. The as-synthesized PANI thin films of thickness 160 nm were irradiated using Au⁷⁺ ion of 100 MeV energy at different fluences, namely, 5 × 10¹¹ ions/cm² and 5 × 10¹² ions/cm², respectively. A significant change was seen after irradiation in electrical and photo conductivity, which may be related to increased carrier concentration, and structural modifications in the polymer film. In addition, the high electronic energy deposition showed other effects like cross-linking of polymer chains, bond breaking and creation of defect sites. AFM observations revealed mountainous type features in all (before and after irradiation) PANI samples. The average size (diameter) and density of such mountainous clusters were found to be related with the ion fluence. The AFM profiles also showed change in the surface roughness of the films with respect to irradiation, which is one of the peculiarity of the high electronic energy deposition technique.     

Study on deposition of Al2O3 films by plasma-assisted atomic layer with different plasma sources

In this paper,A12O3 thin films are deposited on a hydrogen-terminated Si substrate by using two home-built electron cyclotron resonance (ECR) and magnetic field enhanced radio frequency plasma-assisted atomic layer deposition (PA-ALD) devices with Al(CH3)3 (trimethylaluminum,TMA) and oxygen plasma used as precursor and oxidant,respectively.The thickness,chemical composition,surface morphology and group reactions are characterized by in situ spectroscopic ellipsometer,x-ray photoelectric spectroscopy,atomic force microscopy,scanning electron microscopy,a high-resolution transmission electron microscope and in situ mass spectrometry (MS),respectively.We obtain that both ECR PA-ALD and the magnetic field enhanced PA-ALD can deposit thin films with high density,high purity,and uniformity at a high deposition rate.MS analysis reveals that the A12O3 deposition reactions are not simple reactions between TMA and oxygen plasma to produce alumina,water and carbon dioxide.In fact,acetylene,carbon monoxide and some other by-products also appear in the exhaustion gas.In addition,the presence of bias voltage has a certain effect on the deposition rate and surface morphology of films,which may be attributed to the presence of bias voltage controlling the plasma energy and density.We conclude that both plasma sources have a different deposition mechanism,which is much more complicated than expected.     

New separator prepared by electron beam irradiation for high voltage lithium secondary batteries

Grafted separators, for which poly(ethylene glycol) borate acrylate (PEGBA) was grafted onto polyethylene (PE) separator, were newly prepared by electron beam irradiation. The grafted separators were characterized by FT-IR, energy dispersive X-ray spectrometer (EDS). The morphological changes of the grafted separators were investigated by scanning electron microscopy (SEM). The degree of grafting was increased with irradiation doses. The ionic conductivity of the grafted separator showed the highest value of 6.24 × 10⁻⁴ S cm⁻¹ at 10 kGy. In addition, its lithium ion transference number and electrochemical stability were enhanced to 0.53 and 4.8 V, respectively owing to anion trapping effect of the grafted unit. The Li ion cells using the grafted separator showed better cycle performances than that using conventional PE separator at various C-rates and high voltage operation conditions. It is suggested that this grafted separator can be a promising candidate for high voltage operation of lithium secondary batteries.