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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

GaAs Substrate Recycling Using in-situ Deposited NaCl Layers via Molecular Beam Epitaxy

This work presents an alternative method to conventional III-V substrate recycling methods via growth of NaCl on nearly-lattice matched GaAs (001) substrates. Reflection high energy electron diffraction and transmission electron microscopy confirm an epitaxial relationship between the NaCl layers and the underlying GaAs. If the sample is heated too much prior to GaAs deposition, the NaCl fully desorbs from the surface. The quality of the deposition of GaAs on NaCl ranges from amorphous at low temperature to polycrystalline at intermediate temperatures. Exposure to electron beams during growth results in larger and (001) textured grains. The substrate is separated from the GaAs film in seconds via submersion in water, revealing a substrate surface comparable to the original.

electron beams↗
DOE OSTI2021

Siloxane Deposition on the Ni-YSZ Solid Oxide Fuel Cell Anode Exposed to Bio-Syngas

Siloxane, a common contaminant present in biogas, is known for adverse effects on cogeneration prime movers. In this study, the siloxane deposition products and mechanism in the solid oxide fuel cell nickel-yttria stabilized zirconia (Ni-YSZ) anode are investigated analytically and experimentally. An SOFC with Ni-YSZ anode and pure Ni/YSZ pellets were exposed to a simulated biogas-reformate fuel with octamethylcyclotetrasiloxane (D4) contamination at 750 °C. The electrochemical characterization results show that the SOFCs performance degradation caused by D4 contamination is irreversible. Morphology and XRD results illustrate that silicon and carbon deposition can both be detected in the anode and pellets. Graphite, SiC and SiO2 are all possible products based on the results of XRD test. Here, according to the formation of graphite and SiC, the new mechanism suggests that carbon is also an essential factor in siloxane contamination of Ni-YSZ anodes besides silicon, which can be explained by the catalytic and electrochemical analysis.

25 ENERGY STORAGE↗
NASA NTRS1992

Composition variations in pulsed-laser-deposited Y-Ba-Cu-O thin films as a function of deposition parameters

The composition of pulsed-ultraviolet-laser-deposited Y-Ba-Cu-O films was examined as a function of position across the substrate, laser fluence, laser spot size, substrate temperature, target conditioning, oxygen pressure and target-substrate distance. Laser fluence, laser spot size, and substrate temperature were found to have little effect on composition within the range investigated. Ablation from a fresh target surface results in films enriched in copper and barium, both of which decrease in concentration until a steady state condition is achieved. Oxygen pressure and target-substrate distance have a significant effect on film composition. In vacuum, copper and barium are slightly concentrated at the center of deposition. With the introduction of an oxygen background pressure, scattering results in copper and barium depletion in the deposition center, an effect which increases with increasing target-substrate distance. A balancing of these two effects results in stoichiometric deposition.

Foote, M. C.↗
NASA NTRS2003

CuInS2 Films Deposited by Aerosol-Assisted Chemical Vapor Deposition Using Ternary Single-Source Precursors

Polycrystalline CuInS2 films were deposited by aerosol-assisted chemical vapor deposition using both solid and liquid ternary single-source precursors (SSPs) which were prepared in-house. Films with either (112) or (204/220) preferred orientation, had a chalcopyrite structure, and (112)-oriented films contained more copper than (204/220)-oriented films. The preferred orientation of the film is likely related to the decomposition and reaction kinetics associated with the molecular structure of the precursors at the substrate. Interestingly, the (204/220)-oriented films were always In-rich and were accompanied by a secondary phase. From the results of post-growth annealing, etching experiments, and Raman spectroscopic data, the secondary phase was identified as an In-rich compound. On the contrary, (112)-oriented films were always obtained with a minimal amount of the secondary phase, and had a maximum grain size of about 0.5 micron. Electrical and optical properties of all the films grown were characterized. They all showed p-type conduction with an electrical resistivity between 0.1 and 30 Omega-cm, and an optical band gap of approximately 1.46 eV +/- 0.02, as deposited. The material properties of deposited films revealed this methodology of using SSPs for fabricating chalcopyrite-based solar cells to be highly promising.

Jin, Michael↗
NASA NTRS2000

Depositional facies and aqueous-solid geochemistry of travertine-depositing hot springs (Angel Terrace, Mammoth Hot Springs, Yellowstone National Park, U.S.A.)

Petrographic and geochemical analyses of travertine-depositing hot springs at Angel Terrace, Mammoth Hot Springs, Yellowstone National Park, have been used to define five depositional facies along the spring drainage system. Spring waters are expelled in the vent facies at 71 to 73 degrees C and precipitate mounded travertine composed of aragonite needle botryoids. The apron and channel facies (43-72 degrees C) is floored by hollow tubes composed of aragonite needle botryoids that encrust sulfide-oxidizing Aquificales bacteria. The travertine of the pond facies (30-62 degrees C) varies in composition from aragonite needle shrubs formed at higher temperatures to ridged networks of calcite and aragonite at lower temperatures. Calcite "ice sheets", calcified bubbles, and aggregates of aragonite needles ("fuzzy dumbbells") precipitate at the air-water interface and settle to pond floors. The proximal-slope facies (28-54 degrees C), which forms the margins of terracette pools, is composed of arcuate aragonite needle shrubs that create small microterracettes on the steep slope face. Finally, the distal-slope facies (28-30 degrees C) is composed of calcite spherules and calcite "feather" crystals. Despite the presence of abundant microbial mat communities and their observed role in providing substrates for mineralization, the compositions of spring-water and travertine predominantly reflect abiotic physical and chemical processes. Vigorous CO2 degassing causes a +2 unit increase in spring water pH, as well as Rayleigh-type covariations between the concentration of dissolved inorganic carbon and corresponding delta 13C. Travertine delta 13C and delta 18O are nearly equivalent to aragonite and calcite equilibrium values calculated from spring water in the higher-temperature (approximately 50-73 degrees C) depositional facies. Conversely, travertine precipitating in the lower-temperature (< approximately 50 degrees C) depositional facies exhibits delta 13C and delta 18O values that are as much as 4% less than predicted equilibrium values. This isotopic shift may record microbial respiration as well as downstream transport of travertine crystals. Despite the production of H2S and the abundance of sulfide oxidizing microbes, preliminary delta 34S data do not uniquely define the microbial metabolic pathways present in the spring system. This suggests that the high extent of CO2 degassing and large open-system solute reservoir in these thermal systems overwhelm biological controls on travertine crystal chemistry.

Non-NASA Center↗
NASA NTRS2004

CuInS2 Films Deposited by Aerosol-Assisted Chemical Vapor Deposition Using Ternary Single-Source Precursors

Polycrystalline CuInS2 films were deposited by aerosol-assisted chemical vapor deposition using both solid and liquid ternary single-source precursors (SSPs) prepared in-house. Films with either (112) or (204/220) preferred orientation were obtained, and compositional analysis showed that (112)-oriented films contained more copper than (204/220)-oriented films. Using X-ray diffraction, the signature of chalcopyrite structure was often confirmed for (112)-oriented films. The preferred orientation of the film is likely related to the decomposition and reaction kinetics associated with the molecular structure of the precursors at the substrate. Interestingly, the (204/220)-oriented films were always accompanied by a secondary phase, which was identified as an unknown In-rich compound from the results of post-growth annealing, etching experiments, and Raman spectroscopic data. By increasing Cu to In ratio in the film, (112)-oriented films were obtained with a maximum grain size of about 0.5 micrometers, and their X-ray diffractions did not show any observable signature of the In secondary phase. Electrical and optical properties of all the films grown were characterized. They all showed p-type conduction with an electrical resistivity between 0.1 omega cm and 30 omega cm, and an optical band gap of 1.46eV +/- 0.02, as deposited. The material properties of deposited films revealed this methodology of using SSPs for fabricating chalcopyrite-based solar cells to be highly promising.

Jin, Michael H.-C.↗
DOE OSTI2026

Phase Transformation and Water Adsorption Behavior of As‐Deposited and Annealed Ru Metal Thin Films Prepared by Atomic Layer Deposition

ABSTRACT Surfaces play a central role in catalytic processes, and understanding the transformation of ruthenium metal into ruthenium oxide during annealing is essential for tailoring functional catalytic interfaces. In this study, we systematically investigate ≈22 nm thick Ru metal films deposited by atomic layer deposition (ALD) at 300°C, focusing on their chemical composition, structural evolution, and surface hydration behavior following post‐deposition annealing in air from 400 to 600°C. Lab‐based and synchrotron X‐ray photoelectron spectroscopy (XPS) reveal a gradual conversion from metallic Ru to fully oxidized Ru 4+ with increasing annealing temperature, accompanied by a corresponding increase in lattice oxygen. X‐ray diffraction (XRD) shows amorphous Ru oxide phases at 400°C and 500°C that evolve into crystalline RuO 2 at 600°C, while atomic force microscopy (AFM) indicates enhanced grain growth and surface roughening upon annealing. Ambient‐pressure XPS (AP‐XPS) under controlled H 2 O vapor environments (1–17 Torr) demonstrates that samples annealed at 400°C and 500°C exhibit initially high hydroxyl coverage that decreases with increasing water vapor pressure, concurrent with a rise in molecular H 2 O adsorption. In contrast, the crystalline RuO 2 surface formed at 600°C maintains stable hydroxylation and supports increased water uptake. Overall, this work provides fundamental insight into Ru oxide–H 2 O interactions and establishes design principles for engineering oxide surfaces optimized for electrocatalytic applications.

APXPS↗
DOE OSTI2021

Growth and characterization of uranium oxide thin films deposited by polymer assisted deposition

A thin film of uranium oxide was deposited by polymer assisted deposition on a single crystal lanthanum aluminate - strontium aluminum tantalate substrate. The deposition resulted in formation of epitaxial thin film of uranium oxide, which could be attributed to α-U 3 O 8 or α-UO 3 . X-ray diffraction revealed preferential orientation along (100) in case of α-U 3 O 8 or (001) for α-UO 3 for the thin film. A combination of x-ray and neutron reflectometry proved the sample to be α-U 3 O 8 . Furthermore, the film was of 17 nm thickness covered by a capping layer. The less dense capping layer could be a manifestation of surface water adsorbed on the sample.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Cold Spray Deposition of 304L Stainless Steel to Mitigate Chloride-Induced Stress Corrosion Cracking in Canisters for Used Nuclear Fuel Storage

A feasibility study of the cold spray deposition process of 304L stainless steel on 304L stainless steel substrates as a mitigation method for chloride-induced stress corrosion cracking (CISCC) has been investigated under various substrate conditions. The study is aimed at the application of this technology to mitigate CISCC that may potentially occur in or nearthe fusion welded regions of stainless steel canisters in Dry Cask Storage System (DCSS) for used nuclear fuels. Spherical gas-atomized 304L stainless steel powder, in the size range of 25 µm to 44 µm, was used as a feedstock powder for the cold spray process. The powder was deposited on four types of 304L substrates with various surface conditions: as-polished, oxidized, cold-rolled, plates with prototypical CISCC. The effects of cold spray parameters on quality of cold spray coatings were investigated. Thickness, porosity, and phases in the as-deposited materials were evaluated using scanning electron microscopy (SEM) and X-ray diffraction (XRD), and correlated with microhardness and adhesion strength measured via micro-indentation and ASTM C633 pulling test, respectively. XRD analysis of the coatings was also conducted to examine the effects of cold spray condition on residual stress state in the coating. Detailed cross-sectional examination of coating/substrate interfaces was performed with transmission electron microscopy (TEM) equipped with energy dispersive spectroscopy (EDS). Dense and continuous coatings with good adhesion strength and hardness were produced for the various substrate conditions by adjusting cold spray parameters. The results demonstrate that cold spray stainless steel coating is a viable option to provide a physical barrier against CISCC in fusion weld regions of stainless steel in corrosive chloride salt-bearing environments.

Dry Cask Storage Systems, cold spray, 304L stainle↗
DOE OSTI2024

Characterization of fluidized bed chemical vapor deposition ZrC coatings on PyC/YSZ kernels deposited under differing conditions

In this study, coated fuel particle architectures with ZrC coatings are candidate fuels for advanced power reactors and space nuclear propulsion (SNP) concepts. Owing to its relevance to SNP, the composition, microstructure, and mechanical properties of eight ZrC coatings prepared by fluidized bed chemical vapor deposition were evaluated. Evaluation by SEM and EBSD showed that all grains were columnar. Across the various examined samples, minor axis diameters varied between 0.3 and 1.1 μm, and major axis diameters varied between 0.4 and 2.3 μm. Major and minor diameters increased with thickness particularly at higher deposition temperatures in which the major grain axis (from an ellipse fit to the grain shape) increased by 2.5 μm over the entire coating. Coatings with higher reactive gas flows and Zr/C concentrations closer to 1 were observed to contain nanocrystalline graphite deposits. Reactive gas flow doubling led to increases in coating thickness from around 10–15 μm to around 22–27 μm.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Oxidation Temperature-Dependent Electrochemical Doping of WO 3 Deposited via Atomic Layer Deposition

Silicon-based photoelectrochemical devices show promise for the performance of light-driven CO 2 reduction but suffer from instability under photoelectrochemical conditions relevant to CO 2 reduction. Coating silicon electrodes with thin layers of metal oxides has shown promise to passivate unstable silicon surfaces, and many different metal oxides can be deposited on silicon using various techniques. In this study, we investigate the fundamental photoelectrochemical performance of WO 3 -coated silicon photoelectrodes, which were generated by oxidation of W-metal films deposited via atomic layer deposition on both degenerately doped (nSi + ) and low-doped (pSi) silicon. Two different oxidation temperatures were investigated (400 and 600 °C), and it was found that the monoclinic phase of WO 3 predominates at both temperatures but that more grain boundaries are present in the 600 °C film. From X-ray photoelectron spectroscopy, the stoichiometry of both films was found to be 1:3 W:O, and low electron energy loss experiments indicate band gaps of 3.0 and 3.1 eV for 400 and 600 °C films, respectively. Cyclic voltammetry experiments showed that the electron transfer kinetics increased after continued redox cycling, particularly for the material produced at 400 °C. X-ray photoelectron spectra suggest that the observed increase in electrode conductivity is due to the formation of oxygen vacancies in the film. Electrochemical impedance spectroscopy indicated that charge transport through the films was impacted by the grain boundaries that formed during oxidation of the film. Photoelectrochemical studies on pSi/WO 3 electrodes were highly variable, only producing a photocurrent and photovoltage with some samples. Our best sample, formed at 400 °C, produced a photovoltage of 180 mV, which is lower than what has previously been reported for WO 3 -coated silicon (500 mV). We hypothesize that the variability in photoelectrochemical experiments arose from a roughened WSiO x interface that is generated during film preparation. WO 3 shows promise as a metal oxide coating for silicon, but our results suggest that formation of a high-quality interface between Si and WO 3 is vital for best performance.

Charge transfer↗
DOE OSTI2022

Nb₃Sn Coating of a 2.6 GHz SRF Cavity by Sputter Deposition Technique

Nb₃Sn is of interest as a coating for SRF cavities due to its higher transition temperature Tc ~18.3 K and superheating field Hsh ~400 mT, both are twice that of Nb. Nb₃Sn coated cavities can achieve high-quality factors at 4 K and can replace the bulk Nb cavities operated at 2 K. A cylindrical magnetron sputtering system was built, commissioned, and used to deposit Nb₃Sn on the inner surface of a 2.6 GHz single-cell Nb cavity. With two identical cylindrical magnetrons, this system can coat a cavity with high symmetry and uniform thickness. Using Nb-Sn multilayer sequential sputtering followed by annealing at 950°C for 3 hours, polycrystalline Nb₃Sn films were first deposited at the equivalent positions of the cavity’s beam tubes and equator. The film’s composition, crystal structure, and morphology were characterized by energy dispersive spectroscopy, X-ray diffraction, and atomic force microscopy. The Tc of the films was measured by the four-point probe method and was 17.61 to 17.76 K. Based on these studies, ~1.2 micron thick Nb₃Sn was deposited inside a 2.6 GHz Nb cavity. We will discuss first results from samples and cavity coatings, and the status of the coating system.

43 PARTICLE ACCELERATORS↗
NASA NTRS1992

Deposition of adherent Ag-Ti duplex films on ceramics in a multiple-cathode sputter deposition system

The adhesion of Ag films deposited on oxide ceramics can be increased by first depositing intermediate films of active metals such as Ti. Such duplex coatings can be fabricated in a widely used three target sputter deposition system. It is shown here that the beneficial effect of the intermediate Ti film can be defeated by commonly used in situ target and substrate sputter cleaning procedures which result in Ag under the Ti. Auger electron spectroscopy and wear testing of the coatings are used to develop a cleaning strategy resulting in an adherent film system.

Honecy, Frank S.↗
NASA NTRS2014

High Temperature Multilayer Environmental Barrier Coatings Deposited Via Plasma Spray-Physical Vapor Deposition

Si-based ceramic matrix composites (CMCs) require environmental barrier coatings (EBCs) in combustion environments to avoid rapid material loss. Candidate EBC materials have use temperatures only marginally above current technology, but the addition of a columnar oxide topcoat can substantially increase the durability. Plasma Spray-Physical Vapor Deposition (PS-PVD) allows application of these multilayer EBCs in a single process. The PS-PVD technique is a unique method that combines conventional thermal spray and vapor phase methods, allowing for tailoring of thin, dense layers or columnar microstructures by varying deposition conditions. Multilayer coatings were deposited on CMC specimens and assessed for durability under high heat flux and load. Coated samples with surface temperatures ranging from 2400-2700F and 10 ksi loads using the high heat flux laser rigs at NASA Glenn. Coating morphology was characterized in the as-sprayed condition and after thermomechanical loading using electron microscopy and the phase structure was tracked using X-ray diffraction.

Plasma↗
NASA NTRS2017

CMAS Interactions with Advanced Environmental Barrier Coatings Deposited via Plasma Spray- Physical Vapor Deposition

Materials for advanced turbine engines are expected to have temperature capabilities in the range of 1370-1500C. At these temperatures the ingestion of sand and dust particulate can result in the formation of corrosive glass deposits referred to as CMAS. The presence of this glass can both thermomechanically and thermochemically significantly degrade protective coatings on metallic and ceramic components. Plasma Spray- Physical Vapor Deposition (PS-PVD) was used to deposit advanced environmental barrier coating (EBC) systems for investigation on their interaction with CMAS compositions. Coatings were exposed to CMAS and furnace tested in air from 1 to 50 hours at temperatures ranging from 1200-1500C. Coating composition and crystal structure were tracked with X-ray diffraction and microstructure with electron microscopy.

Coatings↗