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DOE OSTI2012

Comprehensive computer model for magnetron sputtering. I. Gas heating and rarefaction

The complex interaction between several variables in magnetron sputtering discharges is a challenge in developing engineering design tools for industrial applications. For instance, at high pressures, rarefaction and gas heating should no longer be neglected for determining several parameters of the process. In this article, we use a comprehensive 3D reactor-scale simulator that incorporates most phenomena of interest in a self-consistent manner to simulate the transport of sputtered particles over a wide range of pressures and powers. Calculations of aluminum deposition rates and metal vapor densities are in reasonable agreement with experiments over a wide range of pressures and powers. Of the elements investigated (Al, Ti, and Cu), copper showed the greatest rarefaction (30%) due to its higher sputtering yield. Titanium, despite a slightly lower sputtering yield than Al, shows a greater rarefaction than aluminum as more particles are reflected from the target as high energy neutrals. In this case, a more efficient energy transfer process is responsible for the higher rarefaction observed in Ti sputtering when compared to Al. The authors also observed that by sputtering at a higher pressure, the probability of electron impact ionization of sputtered particles is increased and speculate about the role of this process in contrast to penning ionization, which is believed to be the dominant ionization mechanism in magnetron sputtering.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Kinetic and potential sputtering of an anorthite-like glassy thin film

In this paper, we present measurements of He + and He +2 ion-induced sputtering of an anorthite-like thin film at a fixed solar wind-relevant impact energy of ~0.5 keV/amu using a quartz crystal microbalance approach (QCM) for determination of total absolute sputtering yields. He +2 ions are the most abundant multicharged ions in the solar wind, and increased sputtering by these ions in comparison to equivelocity He + ions is expected to have the biggest effect on the overall sputtering efficiency of solar wind impact on the Moon. These measurements indicate an almost 70% increase of the sputtering yield for doubly charged incident He ions compared to that for same velocity He + impact (14.6 amu/ion for He +2 vs. 8.7 amu/ion for He+). Using a selective sputtering model, the new QCM results presented here, together with previously published results for Ar +q ions and SRIM results for the relevant kinetic-sputtering yields, the effect due to multicharged-solar-wind-ion impact on local near-surface modification of lunar anorthite-like soil is explored. It is shown that the multicharged-solar-wind component leads to a more pronounced and significant differentiation of depleted and enriched surface elements as well as a shortening of the timescale over which such surface-compositional modifications might occur in astrophysical settings. Additionally, to validate previous and future determinations of multicharged-ion-induced sputtering enhancement for those cases where the QCM approach cannot be used, relative quadrupole mass spectrometry (QMS)-based measurements are presented for the same anorthite-like thin film as were investigated by QCM, and their suitability and limitations for charge state-enhanced yield measurements are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Steady State Sputtering Yield and Surface Compositions of Depleted Uranium and Uranium Carbide bombarded by 16 and 30 keV Gallium or 16 keV Cesium Ions.

Depleted uranium that included carbide precipitates was sputtered with 30keV gallium ions or 16kev cesium ions to depths much greater than the ions’ range, i.e. using steady state sputtering. The recession of both the uranium’s and uranium carbide’s surfaces and the corresponding ion fluences were used to determine the steady state target sputtering yields of both uranium and uranium carbide. 6.3 and 6.02 atoms of uranium versus 2.4 and 1.45 units of uranium carbide were sputtered per gallium ion at 30 kV and 16 kV, respectively. 9.9 uranium atoms and 3.65 units of uranium carbide sputtered per cesium ion at 16 kV. The measured steady state sputtering coefficients for Ga at 30 keV and Cs at 16 keV are close to, but smaller than calculated sputtering coefficients for pure uranium. The steady state surface composition resulting from the simultaneous gallium or cesium implantation and sputter-erosion of uranium and uranium carbide were calculated to be U86Ga14, (UC) 70 Ga 30 and U 86 Ga 14 , (UC) 59 Ga 41 for Ga at 30keV and 16keV, respectively, and U 81 Cs 9 , (UC) 78 Cs 22 for Cesium at 16 keV,

36 MATERIALS SCIENCE↗
DOE OSTI2020

Modeling, analysis, and code/data validation of DIII-D tokamak divertor experiments on ELM and non-ELM plasma tungsten sputtering erosion

Abstract We analyzed recent DIII-D tokamak tungsten divertor probe experiments using advanced, coupled, sputter erosion/redeposition, plasma, and surface response code packages. Modeling is done for ELMing H-mode, and L-mode plasmas, impinging on various size tungsten deposits on Divertor Material Evaluation System (DiMES) carbon probes. The simulations compute 3D, full kinetic, sub-gyromotion, impurity sputtering and transport, including changes in tungsten surface composition and response due to mixed deuterium and carbon ions irradiation. Per our analysis, ELM (edge localized mode) plasma sputtering in DIII-D mostly involves free-streaming high energy (∼500–1000 eV) D + and C +6 ions, with high near-surface plasma density. L-Mode sputtering is due to impurity sputtering (C, W) only, with lower density. All cases show complete redeposition of tungsten on the divertor, with significant redeposition on the tungsten spots themselves, and low self-sputtering. Comparison of ELM plasma gross tungsten erosion simulation results with in-situ spectroscopic data is good, as are code/data comparisons of net erosion using post-exposure Rutherford backscattering (RBS) data for the L-mode probes. The analysis, extrapolated to a full tungsten divertor, implies low net erosion and negligible plasma contamination from sputtering. These results support the use of high-Z plasma facing surfaces in ITER and beyond.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2018

Optimization of sputtering NiOx films for perovskite solar cell applications

Highlights: • NiO{sub x} HTLs were fabricated by three kinds of magnetron sputtering techniques. • Chemical composition, lattice strain and energy levels of NiO{sub x} films were studied and compared. • PSCs based on sputtered NiO{sub x} HTL achieved highest PCE of 16.3% with negligible hysteresis. • Compared with PEDOT:PSS HTL, PSCs based on NiO{sub x} HTL exhibited enhanced stability in air. - Abstract: In this work, we systematically investigated the properties of three kinds of NiO{sub x} films prepared by magnetron sputtering either NiO or Ni target under direct current (DC) or radio frequency (RF) power without any preheating. Those NiO{sub x} films were found to be different in composition ratios, lattice strain and energy levels, thus showing different optical and carrier transport properties. By RF power source, sputtering Ni target in pure O{sub 2} atmosphere led to NiO{sub x} film with relatively good crystallization and surface properties compared with other two types of NiO{sub x} films. These NiO{sub x} films were further introduced into CH{sub 3}NH{sub 3}PbI{sub 3} based planar p-i-n heterojunction perovskite solar cells (PSCs) as the hole transport layers (HTL). It is revealed that PSCs based on NiO{sub x} HTL prepared by sputtering Ni target in pure O{sub 2} atmosphere achieved a highest power conversion efficiency of 16.3% with negligible hysteresis. Compared with devices with PEDOT:PSS HTL, PSCs based on magnetron sputtered NiO{sub x} HTL presented substantially improved stability in air. The results provide theoretical and experimental guidance on selecting NiO{sub x} HTLs fabricated by magnetron sputtering techniques.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

A new highly automated sputter equipment for in situ investigation of deposition processes with synchrotron radiation

HASE (Highly Automated Sputter Equipment) is a new mobile setup developed to investigate deposition processes with synchrotron radiation. HASE is based on an ultra-high vacuum sputter deposition chamber equipped with an in-vacuum sample pick-and-place robot. This enables a fast and reliable sample change without breaking the vacuum conditions and helps to save valuable measurement time, which is required for experiments at synchrotron sources like PETRA III at DESY. An advantageous arrangement of several sputter guns, mounted on a rotative flange, gives the possibility to sputter under different deposition angles or to sputter different materials on the same substrate. The chamber is also equipped with a modular sample stage, which allows for the integration of different sample environments, such as a sample heating and cooling device. The design of HASE is unique in the flexibility. The combination of several different sputtering methods like standard deposition, glancing angle deposition, and high pressure sputter deposition combined with heating and cooling possibil-ities of the sample, the large exit windows, and the degree of automation facilitate many different grazing incidence X-ray scattering experiments, such as grazing incidence small and wide angle X-ray scattering, in one setup. In this paper we describe in detail the design and the performance of the new equipment and present the installation of the HASE apparatus at the Micro and Nano focus X-ray Scattering beamline (MiNaXS) at PETRA III. Furthermore, we describe the measurement options and present some selected results. The HASE setup has been successfully commissioned and is now available for users.

43 PARTICLE ACCELERATORS↗
DOE OSTI2013

Chemical sputtering of graphite by low temperature nitrogen plasmas at various substrate temperatures and ion flux densities

We report measurements of chemical sputtering yields of graphite exposed to low temperature nitrogen plasmas. The influence of surface temperature and incoming ion energy on the sputtering yields has been investigated in two distinct ion flux density regimes. Sputtering yields grow consistently with increasing temperatures in experiments with low flux density (Γ{sub i}≈10{sup 20} m{sup −2}s{sup −1}−10{sup 21} m{sup −2}s{sup −1}) and high flux density (Γ{sub i}≈10{sup 23} m{sup −2}s{sup −1}). Moreover, empirical fitting of the data suggests that the temperature of 670 °C is optimal for chemical sputtering at high flux density. Negative biasing of the samples was used to vary the ion energy in the low flux density regime. The sputtering yield in this case increases from 0.07 atoms/ion for E{sub i} = 1.5 eV to 0.19 atoms/ion for E{sub i} = 35 eV. After taking into account the dependence of the yields on temperature and ion energy, we evidenced a flux dependence of sputtering, similar to that found for chemical sputtering of carbon by hydrogen.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Investigation of blister formation in sputtered Cu{sub 2}ZnSnS{sub 4} absorbers for thin film solar cells

Blister formation in Cu{sub 2}ZnSnS{sub 4} (CZTS) thin films sputtered from a quaternary compound target is investigated. While the thin film structure, composition, and substrate material are not correlated to the blister formation, a strong link between sputtering gas entrapment, in this case argon, and blistering effect is found. It is shown that argon is trapped in the film during sputtering and migrates to locally form blisters during the high temperature annealing. Blister formation in CZTS absorbers is detrimental for thin film solar cell fabrication causing partial peeling of the absorber layer and potential shunt paths in the complete device. Reduced sputtering gas entrapment, and blister formation, is seen for higher sputtering pressure, higher substrate temperature, and change of sputtering gas to larger atoms. This is all in accordance with previous publications on blister formation caused by sputtering gas entrapment in other materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

In-situ observation of sputtered particles for carbon implanted tungsten during energetic isotope ion implantation

Tungsten is a candidate for plasma facing materials in future fusion reactors. During DT plasma operations, carbon as an impurity will bombard tungsten, leading to the formation of tungsten-carbon (WC) layer and affecting tritium recycling behavior. The effect of carbon implantation for the dynamic recycling of deuterium, which demonstrates tritium recycling, including retention and sputtering, has been investigated using in-situ sputtered particle measurements. The C{sup +} implanted W, WC and HOPG were prepared and dynamic sputtered particles were measured during H{sub 2}{sup +} irradiation. It has been found that the major hydrocarbon species for C{sup +} implanted tungsten is CH{sub 3}, while for WC and HOPG (Highly Oriented Pyrolytic Graphite) it is CH{sub 4}. The chemical state of hydrocarbon is controlled by the H concentration in a W-C mixed layer. The amount of C-H bond and the retention of H trapped by carbon atom should control the chemical form of hydrocarbon sputtered by H{sub 2}{sup +} irradiation and the desorption of CH{sub 3} and CH{sub 2} are due to chemical sputtering, although that for CH is physical sputtering. The activation energy for CH{sub 3} desorption has been estimated to be 0.4 eV, corresponding to the trapping process of hydrogen by carbon through the diffusion in W. It is concluded that the chemical states of hydrocarbon sputtered by H{sub 2}{sup +} irradiation for W is determined by the amount of C-H bond on the W surface. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2026

Low-energy ion beam sputtering of polycrystalline diamond

Ion beam milling is a highly versatile and precise technique for the microfabrication of diamond films, enabling controlled material removal at both micrometer and sub-micrometer scales while accommodating complex geometries and surface features. Comprehensive sputtering yield data are essential for process optimization. In this work, we systematically measure the sputter yield of polycrystalline diamond bombarded with $\textrm{N}_2^+$, Ne + , Ar + , Kr + , and Xe + ions over an energy range of 300–900 eV and beam incidence angles of 0°−80°, providing data critical for precision machining applications. Results show that the sputter yield increases with both ion energy and the incidence angle and decreases with increasing ion mass. For $\textrm{N}_2^+$ ions, the sputter yield is largely insensitive to ion energy and exceeds values expected for pure physical sputtering. The concurrent formation of volatile C 2 N 2 molecules during $\textrm{N}_2^+$ ion bombardment suggests that the process is dominated by chemical sputtering. The absence of a peak in the dependence of the sputter yield on the beam incidence angle expected at oblique incidence angles is attributed to the effects of surface roughness.

Materials science↗
DOE OSTI2013

Structural and optical characterization of high-quality ZnO thin films deposited by reactive RF magnetron sputtering

Highlights: ► High-quality ZnO thin films were deposited at room temperature. ► Effect of O{sub 2} flow and RF sputtering voltages on properties of ZnO films were studied. ► O{sub 2}/Ar ratios played a key role in controlling optical properties of ZnO films. ► Photoluminescence intensity of the ZnO films strongly depended on O{sub 2}/Ar ratios. ► Crystallite size, stress and strain strongly depended on O{sub 2}/Ar ratios. - Abstract: ZnO thin films were deposited onto quartz substrates by radio frequency (RF) reactive magnetron sputtering using a Zn target. The structural and optical properties of the ZnO thin films were investigated comprehensively by X-ray diffraction (XRD), ultraviolet–visible and photoluminescence (PL) measurements. The effects of the oxygen content of the total oxygen–argon mixture and sputtering voltage in the sputtering process on the structural and optical properties of the ZnO films were studied systemically. The microstructural parameters, such as the lattice constant, crystallite size, stress and strain, were also calculated and correlated with the structural and optical properties of the ZnO films. In addition, the results showed that the crystalline quality of ZnO thin films improved with increasing O{sub 2}/Ar gas flow ratio from 2:8 to 8:2. XRD and PL spectroscopy revealed 800 V to be the most appropriate sputtering voltage for ZnO thin film growth. High-quality ZnO films with a good crystalline structure, tunable optical band gap as well as high transmittance could be fabricated easily by RF reactive magnetron sputtering, paving the way to obtaining cost-effective ZnO thin films transparent conducting oxides for optoelectronics applications.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Atomic insight into concurrent He, D, and T sputtering and near-surface implantation of 3C-SiC crystallographic surfaces

We present results from atomistic simulations of sputtering and near-surface implantation of concurrent He, D, and T bombardment of cubic silicon carbide (3C-SiC). This is achieved by first establishing a many-body interatomic potential parameter set to treat interactions of He and hydrogenic species in 3C-SiC informed by ab-initio calculations. To obtain sputtering yields we perform both classical molecular dynamics and binary collision approximation simulations for normal incident particles having energies ranging from 25 to 800 eV. We find that due to differences in species surface binding energy of various crystallographic surfaces in 3C-SiC, the sputtering yield of Si is significantly less than that of C, but sputtering yields show limited sensitivity to crystallographic surface orientation. An exception to this occurs when the terminating crystallographic surface plane is more rich in Si rather than C, resulting in comparable sputtering yields of Si and C. The influence of temperature on sputtering is explored and shows limited effect. Finally, the nature of implanted He, D, and T within 3C-SiC surfaces is investigated to understand implantation profiles and stability of defects.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Development of long-lived thick carbon stripper foils for high energy heavy ion accelerators by a heavy ion beam sputtering method

In the past decade, we have developed extremely long-lived carbon stripper foils of 1-50 {mu}g/cm{sup 2} thickness prepared by a heavy ion beam sputtering method. These foils were mainly used for low energy heavy ion beams. Recently, high energy negative Hydrogen and heavy ion accelerators have started to use carbon stripper foils of over 100 {mu}g/cm{sup 2} in thickness. However, the heavy ion beam sputtering method was unsuccessful in production of foils thicker than about 50 {mu}g/cm{sup 2} because of the collapse of carbon particle build-up from substrates during the sputtering process. The reproduction probability of the foils was less than 25%, and most of them had surface defects. However, these defects were successfully eliminated by introducing higher beam energies of sputtering ions and a substrate heater during the sputtering process. In this report we describe a highly reproducible method for making thick carbon stripper foils by a heavy ion beam sputtering with a Krypton ion beam.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Time-resolved temperature study in a high-power impulse magnetron sputtering discharge

The gas heating dynamics is studied in a high-power impulse magnetron sputtering discharge operating in Ar-N{sub 2} gas mixtures. The time-resolved rotational temperature analysis based on the spectral transition between the B{sup 2}{Sigma}{sub u}{sup +}-X{sup 2}{Sigma}{sub g}{sup +} energy levels in molecular nitrogen ion (N{sub 2}{sup +} First Negative Band) is undertaken for this purpose. The rotational temperature in the discharge is found to increase linearly during the plasma pulse being roughly independent on the nitrogen content in the examined range. Such a temperature increase is attributed to the bulk gas heating which is the result of collisions with the sputtered species. Two sputtered materials, Ti and W, are examined during the study. In the case of W sputtering, the gas heating is found to be more pronounced than in the Ti case, which is explained by more efficient energy exchange between the sputtered W atoms and the bulk gas atoms during the plasma on-time. The obtained temperature data are compared to the laser-induced fluorescence study of Ar metastable atoms performed recently in the same discharge in our group. The particularities related to gas thermalization as well as to validity of the utilized approach for characterization of the pulsed sputtering discharges are discussed.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2013

An (ultra) high-vacuum compatible sputter source for oxide thin film growth

A miniaturised CF-38 mountable sputter source for oxide and metal thin film preparation with enhanced high-vacuum and ultra-high-vacuum compatibility is described. The all home-built sputtering deposition device allows a high flexibility also in oxidic sputter materials, suitable deposition rates for preparation of films in the nm- and the sub-monolayer regime and excellent reliability and enhanced cleanliness for usage in UHV chambers. For a number of technologically important – yet hardly volatile – materials, the described source represents a significant improvement over thermal deposition techniques like electron-beam- or thermal evaporation, as especially the latter are no adequate tool to prepare atomically clean layers of refractory oxide materials. Furthermore, it is superior to commercially available magnetron sputter devices, especially for applications, where highly reproducible sub-monolayer thin film preparation under very clean UHV conditions is required (e.g., for studying phase boundary effects in catalysis). The device in turn offers the usage of a wide selection of evaporation materials and special target preparation procedures also allow the usage of pressed oxide powder targets. To prove the performance of the sputter-source, test preparations with technologically relevant oxide components, comprising ZrO{sub 2} and yttrium-stabilized ZrO{sub 2}, have been carried out. A wide range of characterization methods (electron microscopy, X-ray photoelectron spectroscopy, low-energy ion scattering, atomic force microscopy, and catalytic testing) were applied to demonstrate the properties of the sputter-deposited thin film systems.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Magnetic properties of in-plane oriented barium hexaferrite thin films prepared by direct current magnetron sputtering

In-plane c-axis oriented Ba-hexaferrite (BaM) thin films were prepared on a-plane (112{sup ¯}0) sapphire (Al{sub 2}O{sub 3}) substrates by DC magnetron sputtering followed by ex-situ annealing. The DC magnetron sputtering was demonstrated to have obvious advantages over the traditionally used RF magnetron sputtering in sputtering rate and operation simplicity. The sputtering power had a remarkable influence on the Ba/Fe ratio, the hematite secondary phase, and the grain morphology of the as-prepared BaM films. Under 80 W of sputtering power, in-plane c-axis highly oriented BaM films were obtained. These films had strong magnetic anisotropy with high hysteresis loop squareness (M{sub r}/M{sub s} of 0.96) along the in-plane easy axis and low M{sub r}/M{sub s} of 0.03 along the in-plane hard axis. X-ray diffraction patterns and pole figures revealed that the oriented BaM films grew via an epitaxy-like growth process with the crystallographic relationship BaM (101{sup ¯}0)//α-Fe{sub 2}O{sub 3}(112{sup ¯}0)//Al{sub 2}O{sub 3}(112{sup ¯}0)

36 MATERIALS SCIENCE↗
DOE OSTI2011

SPUTTERING FROM A POROUS MATERIAL BY PENETRATING IONS

Porous materials are ubiquitous in the universe and weathering of porous surfaces plays an important role in the evolution of planetary and interstellar materials. Sputtering of porous solids in particular can influence atmosphere formation, surface reflectivity, and the production of the ambient gas around materials in space. Several previous studies and models have shown a large reduction in the sputtering of a porous solid compared to the sputtering of the non-porous solid. Using molecular dynamics simulations we study the sputtering of a nanoporous solid with 55% of the solid density. We calculate the electronic sputtering induced by a fast, penetrating ion, using a thermal spike representation of the deposited energy. We find that sputtering for this porous solid is, surprisingly, the same as that for a full-density solid, even though the sticking coefficient is high.

36 MATERIALS SCIENCE↗
DOE OSTI2012

High power impulse magnetron sputtering discharge

The high power impulse magnetron sputtering (HiPIMS) discharge is a recent addition to plasma based sputtering technology. In HiPIMS, high power is applied to the magnetron target in unipolar pulses at low duty cycle and low repetition frequency while keeping the average power about 2 orders of magnitude lower than the peak power. This results in a high plasma density, and high ionization fraction of the sputtered vapor, which allows better control of the film growth by controlling the energy and direction of the deposition species. This is a significant advantage over conventional dc magnetron sputtering where the sputtered vapor consists mainly of neutral species. The HiPIMS discharge is now an established ionized physical vapor deposition technique, which is easily scalable and has been successfully introduced into various industrial applications. The authors give an overview of the development of the HiPIMS discharge, and the underlying mechanisms that dictate the discharge properties. First, an introduction to the magnetron sputtering discharge and its various configurations and modifications is given. Then the development and properties of the high power pulsed power supply are discussed, followed by an overview of the measured plasma parameters in the HiPIMS discharge, the electron energy and density, the ion energy, ion flux and plasma composition, and a discussion on the deposition rate. Finally, some of the models that have been developed to gain understanding of the discharge processes are reviewed, including the phenomenological material pathway model, and the ionization region model.

36 MATERIALS SCIENCE↗