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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Autonomous sputter synthesis of thin film nitrides with composition controlled by Bayesian optimization of optical plasma emission

Autonomous experimentation has emerged as an efficient approach to accelerate the pace of material discovery. Although instruments for autonomous synthesis have become popular in molecular and polymer science, solution processing of hybrid materials, and nanoparticles, examples of autonomous tools for physical vapor deposition are scarce yet important for the semiconductor industry. Here, we report the design and implementation of an autonomous workflow for sputter deposition of thin films with controlled composition, leveraging a highly automated sputtering reactor custom-controlled by Python, optical emission spectroscopy (OES), and a Bayesian optimization algorithm. We modeled film composition, measured by x-ray fluorescence, as a linear function of plasma emission lines monitored during co-sputtering from elemental Zn and Ti targets in an N 2 and Ar atmosphere. A Bayesian control algorithm, informed by OES, navigates the space of sputtering power to fabricate films with user-defined compositions by minimizing the absolute error between desired and measured optical emission signals. We validated our approach by autonomously fabricating Zn x Ti 1-x N y films that deviate from the targeted cation composition by a relative ±3.5%, even for 15 nm thin films, demonstrating that the proposed approach can reliably synthesize thin films with a specific composition and minimal human interference. Moreover, the proposed method can be extended to more difficult synthesis experiments where plasma intensity lines depend non-linearly on pressure, or the elemental sticking coefficients strongly depend on the substrate temperature.

36 MATERIALS SCIENCE↗
NASA NTRS2019

Molten Target Sputtering: Non-Conventional Method for High Mobility Si0.15Ge0.85 Growth at 500°C

Since electrons travel over 100 times faster in Silicon-Germanium (SiGe) than in pure Si due to the low effective masses associated with Ge and SiGe-based devices continue to replace Si-based solid-state electronic devices. SiGe thin film on sapphire was successfully grown at 890°C, using a magnetron sputtering system within heteroepitaxial framework. However, SiGe growth at 890oC is a costly and difficult process to produce as a uniform wafer for semiconductor device manufacturing due to thermal soak times, and geometric thermal shadowing from the wafer holder. To leverage the semiconducting capabilities of SiGe, novel processing techniques for SiGe film growth with decreased thermal loading are required. This paper introduces the Molten Target Sputtering (MTS) method that produces high mobility SiGe on sapphire below 500°C. This non-conventional method has the advantage of high kinetic energy, high-energy latency, and high flux density of sputtered atoms by combining benefits of both magnetron sputtering and thermal evaporation. For the MTS method, a 1~2 mm (depth and width) ring-shaped groove was cut between the center magnet and surrounded by electromagnets creating a circular cavity between the copper plate and source target materials that melt the target material. The SiGe grown from the MTS shows continuous morphology and 99.7% single crystal Si0.15Ge0.85 films. The Hall electron mobilities of the Si0.15Ge0.85 are 456 sq. cmV(exp -1)s(exp -1) and 123.9 sq. cmV(exp -1)s(exp -1) at 5.59 x 10(exp 18) cubic cm and 3.5 x 10(exp 20) cubic cm carrier concentration at 22.38°C, respectively. This is approximately 5.5 times higher than that of Si and similar to the Ge value at equivalent carrier concentrations and temperatures.

High mobility SiGe↗
DOE OSTI2019

Characterizations of Binary FeCr (AISI 430) Thin Films Deposited from a Single Magnetron Sputtering Under Easy Controllable Deposition Parameters

A series of 50-nm binary FeCr martensitic thin films were sputtered from a single source made of commercial AISI 430 ferritic stainless steel under the deposition rates gradually increased from 0.03 to 0.11 nm/s with 0.02 nm/s steps at stationary condition. And, under 0.09 nm/s deposition rate, a second series of the films were also deposited under the rotation speed of their substrates which was chosen at 0, 25, and 45 rpm. As far as we are concerned, this study is the first investigation of properties of the thin films produced from AISI 430. The atomic Fe content in the films increased from 79.3 to 98.6% while atomic Cr content decreased from 20.5 to 1.2% with the increase of deposition rate from 0.03 to 0.11 nm/s. According to compositional analysis, the Fe content increased while Cr content decreased with increasing deposition rate. The reason for this may be attributed to the relatively different bond energy/melting point of metals which have different contents sputtered from source material since this physical parameter is very significant for the sputtering process. And, the Fe content in the films decreased from 84.9 to 79.2 at. % while the Cr content increased from 14.9 to 20.6 at. % when the increase of rotation speed of substrate. The crystal structure of all films was observed to have a body-centered tetragonal phase and the intensity of (110) peak varied with the atomic Fe content. The surface observations of films performed by a scanning electron microscope exposed that the number of surface grains increased with the increase of deposition rate and decreased with the increase of rotation speed. According to surface roughness analysis done by an atomic force microscope, the roughness of the film surfaces increased as the deposition rate increased. And, the roughness of the film surfaces decreased as the rotation speed increased. This has been consistent with the grain size and roughness parameters. Thus, increasing deposition rate and decreasing rotation speed of the substrate caused an increase in grain size and roughness parameters. The magnetic measurements of the films achieved, by a vibrating sample magnetometer at room temperature, displayed that the saturation magnetization, M{sub s}, values increased from 820.1 to 1700.4 emu/cm{sup 3}, the remanence magnetization, M{sub r}, values increased from 293 to 817 emu/cm{sup 3}, and the coercivity, H{sub c}, value also increased from 38 to 107 Oe with the increasing of deposition rate. It is also seen that the magnetic easy axis are in the film plane due to the shape anisotropy. With the increase rotation speed, the values of M{sub s} and M{sub r} increased and the H{sub c} decreased. It was seen that variation of Fe content in the films influences the M{sub s} values and the H{sub c} values are consistent with the surface properties. It was concluded that the deposition rate and the rotation speed of the substrate play a considerable role on the structural and related magnetic properties of the sputtered FeCr thin films, and the properties of the films can be easily controlled by changing production parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Sputter-Coated Metal Screening for Small Molecule Analysis and High-Spatial Resolution Imaging in Laser Desorption Ionization Mass Spectrometry

Nanoparticles are efficient matrices in laser desorption/ionization (LDI) mass spectrometry (MS), especially for the profiling or imaging of small molecules. Recently, solvent-free physical vapor desorption (PVD), or sputter coating, was adopted as a homogenous method to rapidly apply metal nanoparticles (NPs) in situ to samples prior to LDI MS or MS imaging analysis. However, there has been no systematic study comparing different metal targets for the analysis of a variety of small molecule metabolites. Here, we present a screening and optimization of various sputter-coated metals, including Ag, Au, Cu, Pt, Ni, and Ti, for LDI analysis of small molecules in both positive and negative ion modes. Optimized sputter coating is then applied to high-spatial resolution LDI mass spectrometry imaging (MSI) of maize root and seed cross-sections. Noble metals, Ag, Au, and Pt, are found to be much more efficient than transition metals and organic matrices for most small metabolites. Sputter-coated metals are efficient for neutral lipids, such as triacylglycerols and diacylglycerols, but are very inefficient for most phospholipids. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Differences in Sb 2 Te 3 growth by pulsed laser and sputter deposition

High quality van der Waals chalcogenides are important for phase change data storage, thermoelectrics, and spintronics. Using a combination of statistical design of experiments and density functional theory, we clarify how out-of-equilibrium van der Waals epitaxial deposition methods can improve the crystal quality of Sb 2 Te 3 films. We compare films grown by radio frequency sputtering and pulsed laser deposition (PLD). The growth factors that influence the crystal quality for each method are different. For PLD grown films a thin amorphous Sb 2 Te 3 seed layer most significantly influences the crystal quality. In contrast, the crystalline quality of films grown by sputtering is rather sensitive to the deposition temperature and less affected by the presence of a seed layer. This difference is somewhat surprising as both methods are out-of-thermal-equilibrium plasma-based methods. Non-adiabatic quantum molecular dynamics simulations show that this difference originates from the density of excited atoms in the plasma. The PLD plasma is more intense and with higher energy than that used in sputtering, and this increases the electronic temperature of the deposited atoms, which concomitantly increases the adatom diffusion lengths in PLD. In contrast, the adatom diffusivity is dominated by the thermal temperature for sputter grown films. These results explain the wide range of Sb 2 Te 3 and superlattice crystal qualities observed in the literature. Finally, these results indicate that, contrary to popular belief, plasma-based deposition methods are suitable for growing high quality crystalline chalcogenides.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Molecular dynamics simulations of reflection and sputtering behavior of boron under deuterium ion irradiation

Boronization is a commonly used method of wall conditioning in fusion reactors. The application of boron films to the plasma-facing materials results in enhanced plasma performance due to the reduction of intrinsic impurities. This is primarily driven by a reduction in oxygen content that is chemically trapped in the boron film. The reactive nature of these boron films also raises questions concerning interactions with hydrogen isotopes. In this work, boron-deuterium interactions were studied using molecular dynamics (MD). Reactive force field potentials were used to model the chemical interactions between B and D. An amorphous boron substrate was irradiated by D atoms at varying incident energies, 10 eV < E i < 150 eV and angles, 0° < α < 85°. The reflection probability was calculated and compared to results from the commonly-used binary collision approximation (BCA) method. This comparison found that the BCA underestimated the reflection probability at E i < 35 eV and α > 45 ∘ . The source of this discrepancy was found to be the surface binding energy model. The BCA calculation with an isotropic surface binding energy model was more closely aligned to the MD result. This, in combination with a correction function based on the MD results allows for corrections to the reflection probability of deuterium impinging on boron surfaces. The sputtering of the substrate material was also studied. While this study did not contain sufficient events to quantitatively describe the sputtering behavior, some qualitative results emerged: namely, chemical sputtering of B and D-containing molecules (BD, BD 2 , BD 3 ) at low ( < 20 eV) incident deuterium energies. This result suggests that chemical sputtering could be a significant factor in limiting boron coating lifetime when exposed to lower ion energies, such as those in detached plasmas. The results show that chemical interactions should be taken into account when modeling the interactions between D ions and B surfaces.

Boron↗
DOE OSTI2024

Net lithium deposition and dominant self-sputtering in lithium tokamak experiment-β with a liquid lithium wall

We observed enhanced net lithium deposition and lithium erosion, possibly dominated by physical sputtering of lithium by lithium-ion bombardment, on the outer plasma-facing surface in the Lithium Tokamak eXperiment-β (LTX-β) during liquid lithium wall operations. Silicon crystal samples with micro-trenches (30 μm × 30 μm × 2–7 μm deep) were exposed to hydrogen plasmas in LTX-β for solid and liquid lithium wall operations. Post-mortem analysis using X-ray photoelectron spectroscopy combined with argon ion sputtering measured net lithium deposition of 8.2 or 21 nm on the silicon crystal surface exposed for ~ 50 repeated shots of ~ 50-ms hydrogen plasma discharges during the liquid lithium wall operations at a vessel temperature of 475 K. Energy dispersive X-ray spectroscopy measured oxygen concentration patterns on the micro-trench floors, which were due to oxidized lithium deposition. Using the inhomogeneous oxygen concentration pattern caused by an ion-shadowing effect associated with the micro-trench’s geometric structure, we determined a polar incident ion direction of 68.4 ± 1.6° referenced to the surface normal direction. This observation was well-explained by the hypothesis that self-sputtering of Li was a dominant lithium erosion source in addition to lithium sputtering by hydrogen bombardment.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2019

Impact of ELM control techniques on tungsten sputtering in the DIII-D divertor and extrapolations to ITER

The free-streaming plus recycling model (FSRM) has recently been developed to understand and predict tungsten gross erosion rates from the divertor during edge localized modes (ELMs). In this work, the FSRM was tested against the experimental measurements of W sputtering during ELMs, conducted via fast neutral tungsten (WI) spectroscopy. Good agreement is observed using a variety of controlling techniques, including gas puffing, neutral beam heating, and plasma shaping to modify the pedestal stability boundary and, thus, the ELM behavior. ELM mitigation by pellet pacing was observed to strongly reduce W sputtering by flushing C impurities from the pedestal and reducing the divertor target electron temperature. No reduction of W sputtering was observed during the application of resonant magnetic perturbations (RMPs), in contrast to the prediction of the FSRM. Potential sources of this discrepancy are discussed. Lastly, the framework of the FSRM is utilized to predict intra-ELM W sputtering rates in ITER. It is concluded that W erosion during ELMs in ITER will be caused mainly by free-streaming fuel ions, but free-streaming seeded impurities (N or Ne) may increase the erosion rate significantly if present in the pedestal at even the 1% level. Impurity recycling is not expected to cause critical W erosion in ITER due to the very low target electron temperature.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2019

Film Growth Dynamics During Pulsed Sputter Deposition (LDRD Final Report)

Novel materials synthesis and development using physical vapor deposition require our fundamental understanding of plasma conditions and film growth dynamics. A central theme is to control materials microstructure. Over the last few decades, the difficulty of thick heavy metal coatings has been one of the major bottlenecks limiting our studies of the important family of inertial-confinement-fusion (ICF) designs with colliding-shell targets. Our previous attempts to fabricate such coatings by conventional DC magnetron sputtering (DCMS) has had limited success due to the inherent complexity and our limited understanding of the deposition process. In this project, we have investigated the physics of a novel and promising pulsed sputter deposition process. We expanded the scientific foundation of sputter deposition processes through a combination of well-posed experiments and state-of-the-art characterizations. The following important scientific milestones have been achieved: (1) Successfully installed and tested a high-power impulse magnetron sputtering (HiPIMS) system; (2) Deployed a novel set of in-situ diagnostics during pulsed deposition, including a multibeam optical stress sensor (MOSS) system for real-time stress measurement, and Langmuir probe for the measurements of plasma physical properties. This allows us to monitor dynamically plasma conditions, ion flux and energy distributions, and film stress; (3) Investigated and obtained a fundamental understanding of HIPIMS on microstructure and stress control; (4) Successfully synthesized and demonstrated record-breaking strength nanocrystalline-nanotwinned (nnt) metals; (5) Successfully obtained high-quality, leak-proof Cr metal shells via HiPIMS method. The outcomes of this project could have transformational scientific and programmatic impacts, enabling novel materials synthesis and an experimental campaign with colliding shell target designs. The basic understanding of the deposition process has important implications to a broad range of industrial applications.

36 MATERIALS SCIENCE↗
NASA NTRS1972

Radiofrequency-sputtered coatings for lubrication system components and other complex surfaces

Irregularly shaped surfaces, such as lubrication system components (ball bearings, seals, gears, etc.), can be coated on all surfaces, including irregular shapes, when radiofrequency sputtering is used. When the specimen is properly located with respect to the sputtering target, the sputtered material covers the entire surface of the object irrespective of its geometrical configuration. An adherent, dense film is formed. The film thickness varies from 20 to 50 percent on, for example, a hearing cage or race depending on its geometry. When sputtered solid film lubricants such as molybdenum disulfide are used, a film thickness only of the order of 10 to the minus 7th power m (thousands of angstroms) is required at the contacting areas. It is only essential to determine the required film thickness at the critical areas in need of lubrication. The sections outside the areas to be lubricated fall within the thickness deviation range of 20 to 50 percent, which still constitutes a negligible change respect to tolerance requirements.

Spalvins, T.↗
NASA NTRS1972

Sputtering and ion plating

The proceedings of a conference on sputtering and ion plating are presented. Subjects discussed are: (1) concepts and applications of ion plating, (2) sputtering for deposition of solid film lubricants, (3) commercial ion plating equipment, (4) industrial potential for ion plating and sputtering, and (5) fundamentals of RF and DC sputtering.

Source record↗
NASA NTRS1972

Change in transmittance of fused silica as a means of detecting material sputtered from components on a 5-cm ion thruster

Two endurance tests of a 5-cm mercury bombardment thruster are reported. Both tests used a translational screen-grid system with the beam vectored 10 degrees. The first test lasted 141 hours and the second test operated for 2026 hours. In each test two fused silica samples (solar cell covers), 2.0 cm by 2.1 cm, were placed in shielded holders to detect materials sputtered from the thruster. Spectral optical properties between 0.398 and 2.16 microns were measured on each sample, both before and after the endurance tests. The deposition on each sample was spectrographically analyzed to determine the type of materials sputtered from the thruster. It was found that sputtering from the neutralizer is highly dependent on its position with respect to the beam edge. The sputtering from the accelerator grid of the translational screen-grid system of the 2026 hour test was sufficient to form an opaque film on the sample located in the direction opposite to the vectored beam.

Weigand, A. J.↗
NASA NTRS1973

Structure of molybdenum disulfide films sputtered on substrates at various temperatures

Molybdenum disulfide films 300 to 400 A thick were rf sputtered on aluminum and nickel surfaces at elevated, ambient, and liquid nitrogen temperatures. Electron transmission micrographs and electron diffraction patterns were taken to determine the structural growth. These transmission micrographs revealed that sputtered MoS2 films at ambient and elevated temperatures (320 and 150 C) formed an irregular network of ridges. The electron diffraction patterns of these films showed relatively sharp diffraction rings, indicating crystallinity. The transmission micrographs of sputtered films at liquid nitrogen temperatures revealed a continuous featureless film. The electron diffraction patterns showed broad, diffused rings indicating an amorphous film. The transmission micrographs of a post-annealed (425 C) MoS2 film sputtered at liquid-nitrogen temperature revealed the tendency for ridge formation. Electron diffraction patterns also showed increased sharpness of the diffraction rings. Friction tests showed that MoS2 films deposited at ambient and elevated temperatures exhibited good lubricating properties. The MoS2 films deposited at cryogenic temperatures had no lubricating characteristics.

Spalvins, T.↗
NASA NTRS1975

On the sputtering of binary compounds

A simple physical model is presented to describe some aspects of the sputtering of compound targets. In particular, expressions are developed for the partial sputtering yields for binary systems in terms of the elemental sputtering rates, the stoichiometric concentrations and surface binding energy. The partial yields depend non-linearly on the bulk target concentrations. Comparison of the theoretical predictions with the data on sputtering of PtSi, NiSi and Cu3Au indicates that the general features are well described.

Haff, P. K.↗
NASA NTRS1977

Microstructural and wear properties of sputtered carbides and silicides

Sputtered Cr3C2, Cr3Si2, and MoSi2 wear-resistant films (0.05 to 3.5 microns thick) were deposited on metal and glass surfaces. Electron transmission, electron diffraction, and scanning electron microscopy were used to determine the microstructural appearance. Strong adherence was obtained with these sputtered films. Internal stresses and defect crystallographic growth structures of various configurations within the film have progressively more undesirable effects for film thicknesses greater than 1.5 microns. Sliding contact and rolling element bearing tests were performed with these sputtered films. Bearings sputtered with a duplex coating (0.1-micron-thick undercoating of Cr3Si2 and subsequently 0.6-micron coating of MoS2) produced marked improvement over straight MoS2 films.

Spalvins, T.↗
NASA NTRS1977

X-Ray photoelectron spectroscopy study of radiofrequency-sputtered titanium, carbide, molybdenum carbide, and titanium boride coatings and their friction properties

Radiofrequency sputtered coatings of titanium carbide, molybdenum carbide and titanium boride were tested as wear resistant coatings on stainless steel in a pin on disk apparatus. X-ray photoelectron spectroscopy (XPS) was used to analyze the sputtered films with regard to both bulk and interface composition in order to obtain maximum film performance. Significant improvements in friction behavior were obtained when properly biased films were deposited on deliberately preoxidized substrates. XPS depth profile data showed thick graded interfaces for bias deposited films even when adherence was poor. The addition of 10 percent hydrogen to the sputtering gas produced coatings with thin poorly adherent interfaces. Results suggest that some of the common practices in the field of sputtering may be detrimental to achieving maximum adherence and optimum composition for these refractory compounds.

Brainard, W. A.↗
NASA NTRS1976

On the sputtering of binary compounds

A simple physical model is presented to describe some aspects of the sputtering of compound targets. In particular, expressions are developed for the partial sputtering yields for binary systems in terms of the elemental sputtering rates, the stoichiometric concentrations, and surface binding energy. The partial yields depend nonlinearly on the bulk target concentrations. Comparison of the theoretical predictions with the data on sputtering of PtSi, NiSi, and Cu3Au indicates that the general features are well described.

Haff, P. K.↗
NASA NTRS1978

Ion beam sputter etching and deposition of fluoropolymers

Fluoropolymer etching and deposition techniques including thermal evaporation, RF sputtering, plasma polymerization, and ion beam sputtering are reviewed. Etching and deposition mechanism and material characteristics are discussed. Ion beam sputter etch rates for polytetrafluoroethylene (PTFE) were determined as a function of ion energy, current density and ion beam power density. Peel strengths were measured for epoxy bonds to various ion beam sputtered fluoropolymers. Coefficients of static and dynamic friction were measured for fluoropolymers deposited from ion bombarded PTFE.

Banks, B. A.↗