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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
NASA NTRS1979

Effect of nitrogen-containing plasma on adherence, friction, and wear of radiofrequency-sputtered titanium carbide coatings

Friction and wear experiments on 440C steel surfaces that were rf sputtered with titanium carbide when a small percentage of nitrogen was added to the plasma were conducted. Both X-ray photoelectron spectroscopy and X-ray diffraction were used to analyze the resultant coatings. Results indicate that the small partial pressure of nitrogen (approximately 0.5 percent) markedly improves the adherence, friction, and wear properties when compared with coatings applied to sputter-etched surfaces, oxidized surfaces, or in the presence of a small oxygen partial pressure. The improvements are related to the formation of an interface containing a mixture of the nitrides of titanium and iron, which are harder than their corresponding oxides.

Brainard, W. A.↗
NASA NTRS1979

Use of a nitrogen-argon plasma to improve adherence of sputtered titanium carbide coatings on steel

Friction and wear experiments on 440-C steel surfaces that had been RF-sputtered with titanium carbide when a small percentage of nitrogen was added to the plasma were conducted. X-ray photoelectron spectroscopy and X-ray diffraction were used to analyze the resultant coatings. Results indicate that a small partial pressure of nitrogen (about 0.5%) markedly improves the adherence, friction, and wear properties when compared with coatings applied on sputter-etched oxidized surfaces or in the presence of a small oxygen partial pressure. The improvements are related to the formation of an interface containing a mixture of the nitrides of titanium and iron, which are harder than their corresponding oxides.

Brainard, W. A.↗
NASA NTRS1980

Improved adherence of T1C coatings to steel

Modified process for RF sputtering of titanium carbide coatings onto 440-C steel has resulted in improved adherence. Small partial pressure of nitrogen, approximately 0.5 percent, during first minutes of deposition markedby improved adherence, friction, and wear properties when compared with coatings applied on sputter-etched surfaces, or oxidized surfaces or in presence of small oxygen partial pressure. X-ray photoelectron spectroscopy and X-ray diffraction were used to characterize resultant coatings.

Brainard, W. A.↗
NASA NTRS1982

Surface chemistry, microstructure and friction properties of some ferrous-base metallic glasses at temperatures to 750 C

X-ray photoelectron spectroscopy analysis, transmission electron microscopy, diffraction studies, and sliding friction experiments were conducted with ferrous-base metallic glasses in sliding contact with aluminum oxide at temperatures from room to 750 C in a vacuum of 30 nPa. The results indicate that there is a significant temperature influence on the friction properties, surface chemistry, and microstructure of metallic glasses. The relative concentrations of the various constituents at the surface of the sputtered specimens were very different from the normal bulk compositions. Contaminants can come from the bulk of the material to the surface upon heating and impart boric oxide and silicon oxide at 350 C and boron nitride above 500 C. The coefficient of friction increased with increasing temperature to 350 C. Above 500 C the coefficient of friction decreased rapidly. The segregation of contaminants may be responsible for the friction behavior.

Miyoshi, K.↗
NASA NTRS1992

LDEF thermal control coatings post-flight analysis

The optical, physical, and chemical properties of selected spacecraft thermal control coatings, exposed for 10 months and 5.8 years on the leading edge (Row 9) of the LDEF, are reported. The following coatings were used: quartz/silver optical solar reflector; silvered FEP Teflon; S-13GLO, YB-71, and A-276 white paints; black paint; and sputter deposited coatings over graphite-epoxy composite substrates. The solar absorptance, total normal emittance, scanning electron and X-ray photoelectron microscopy, and X-ray diffraction analyses will be compared for the control, the 10 month exposed, and the 5.8 year exposed specimens. Data suggests that the high atomic flux over the last 6 months of the LDEF mission may have influenced the results from from this coatings experiment.

Slemp, Wayne S.↗
NASA NTRS1994

Friction and Wear Properties of As-deposited and Carbon Ion-implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 ke V ion energy, resulting in a dose of 1.2310(exp 17) carbon ions/cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, x-ray photoelectron spectroscopy, and x-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40 percent relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and were properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to 10(exp -8)mm(exp 3)/N-m) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4)mm(exp 3/N-m) in ultrahigh vacuum. The carbon ion implanation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, nondiamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine- and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7)mm(exp 3/N-m). Even in ultrahigh vacuum, the presence of the nondiamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6)mm(exp 3)/N-m. Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum. The wear mechanism of diamond films is that of small fragments chipping off the surface. The size of wear particles is related to the extent of wear rates.

Miyoshi, Kazuhisa↗
NASA NTRS1996

Friction and Wear Properties of As-Deposited and Carbon Ion-Implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 keV ion energy, resulting in a dose of 1.2 x 10(exp 17) carbon ions per cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40% relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and wear properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to lO(exp -8) mm(exp 3) N(exp -1) m(exp -1)) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4) mm(exp 7) N(exp -1) m(exp -1)) in ultrahigh vacuum. The carbon ion implantation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, non-diamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7) mm(exp 3) N(exp -1) m(exp-1)). Even in ultrahigh vacuum, the presence of the non-diamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6) mm(exp 3) N(exp -1) m(exp -1). Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum.

Miyoshi, Kazuhisa↗
DOE OSTI2025

Steam-Assisted Ammonolysis of MoO2 as a Synthetic Pathway to Oxygenated δ-MoN

A common route for the synthesis of molybdenum nitrides is through the temperature-programmed reaction of molybdenum oxides with NH3, or ammonolysis. In this work, the role of precursor phase, gas phase chemistry (impact of H2O), and temperature profile on the reaction outcome (700 °C) was examined, which resulted in varying amounts of MoO2, H2MoO5, and the nitride phases—cubic γ (nominally Mo2N) and hexagonal δ (nominally MoN). The phase fraction of the δ phase increased with precursor in the sequence MoO2 > MoO3 > H2MoO5. Steam in the reaction gas also favored the production of δ over γ, but with too much steam, MoO2 was obtained in the product. Synthesis conditions for obtaining nearly phase-pure δ were identified: MoO2 as the precursor, 2% H2O in the gas stream, and a moderate heating rate (3 °C/min). In situ X-ray diffraction provided insights into the reaction pathway. Extensive physico-chemical analysis of the δ phase, including synchrotron X-ray and neutron diffraction, electron microscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy, and prompt gamma activation analysis, revealed its stoichiometry to be MoO0.108(8)N0.892(8)H0.012(5), indicating non-trivial oxygen incorporation. The presence of N/O ordering and an impurity phase Mo5N6 were also revealed, detectable only by neutron diffraction. Notably, a computationally predicted MoON phase (doi: 10.1103/PhysRevLett.123.236402), of interest due to its potential to display a metal-insulator transition, did not appear under any reaction condition examined.

Pandey, Shobhit↗
DOE OSTI2023

Revealing the Chemical State of Palladium in Operating In 2 O 3 Gas Sensors: Metallic Pd Enhances Sensing Response and Intermetallic In x Pd y Compound Blocks It

The sensing response of metal oxides activated with noble metal nanoparticles is significantly influenced by changes to the chemical state of corresponding elements under operating conditions. Here, a PdO/rh-In 2 O3 consisting of PdO nanoparticles loaded onto rhombohedral In 2 O 3 was studied as a gas sensor for H 2 gas (100–40000 ppm in an oxygen-free atmosphere) in the temperature range of 25–450 °C. The phase composition and chemical state of elements were examined by resistance measurements combined with synchrotron-based in situ X-ray diffraction and ex situ X-ray photoelectron spectroscopy. As found, PdO/rh-In 2 O 3 undergoes a series of structural and chemical transformations during operation: from PdO to Pd/PdH x and finally to the intermetallic In x Pd y phase. The maximal sensing response (R N2 /R H2 ) of ~5 · 10 7 towards 40000 ppm (4 vol %) H 2 at 70 °C is correlated with the formation of PdH 0.706 /Pd. The In x Pd y intermetallic compounds formed around 250 °C significantly decrease the sensing response.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Atomic Layer Deposition of Nickel Using Ni(dmamb)2 and ZnO Adhesion Layer Without Plasma

Abstract In this study, a novel deposition technique that utilizes diethylzinc (C 4 H 10 ZnO) with H 2 O to form a ZnO adhesion layer was proposed. This technique was followed by the deposition of vaporized nickel(II) 1-dimethylamino-2-methyl-2-butoxide (Ni(dmamb) 2 ) and H 2 gas to facilitate the deposit of uniform layers of nickel on the ZnO adhesion layer using atomic layer deposition. Deposition temperatures ranged from 220 to 300 °C. Thickness, composition, and crystallographic structure results were analyzed using spectroscopic ellipsometry, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD), respectively. An average growth rate of approximately 0.0105 angstroms per cycle at 260 °C was observed via ellipsometry. Uniform deposition of ZnO with less than 1% of Ni was displayed by utilizing the elemental analysis function via SEM, thereby providing high-quality images. XPS revealed ionizations consistent with nickel and ZnO through the kinetic and binding energies of each detected electron. XRD provided supplemental information regarding the validity of ZnO by exhibiting crystalline attributes, revealing the presence of its hexagonal wurtzite structure.

Baker, Kaiya↗
DOE OSTI2025

Scalable thin graphene oxide membranes enabled by polydopamine gutter layer

Two-dimensional (2D) nanosheets have been widely used to fabricate thin-film composite membranes for dye desalination. However, they often need to be thick to mitigate the defects resulting from their random stacking and rough support surface. Herein, bio-adhesive polydopamine (PDA) is used as a gutter layer to prepare graphene oxide (GO)-based membranes by improving the adhesion between the GO and porous support and providing a smooth surface to form thin, highly selective layers. For example, the PDA priming reduces the GO layer thickness by 57 %, from 447 to 190 nm, while achieving similar dye desalination properties. The effect of the dopamine concentration, exposure time, and GO layer thickness on the membrane structure and desalination performance are thoroughly investigated using various techniques, such as scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS), and x-ray diffraction (XRD). The PDA gutter layer is also applied for hollow fiber membranes, achieving water permeance of 79 L m -2 h −1 bar−1 and rejection of ∼99 % for Direct red 80. The membranes were challenged by simulated dye/salt mixtures to elucidate the complicated effect of the compositions on the desalination performance. Furthermore, this study unveils a new avenue to improve separation performance and large-scale manufacturability of 2D material-based membranes.

Dye desalination↗
DOE OSTI2025

Unsupported and carbon-supported silver catalysts for oxygen reduction reaction in alkaline media

Quick and easy Ag catalysts preparation via wet chemical synthesis method using only reducing agent (pure-Ag); reducing agent and citric acid as the capping agent (Ag-CA); and carbon support (KetjenBlack 600J), capping agent, and the reducing agent (Ag/C) is demonstrated. The Ag-based electrocatalysts are characterized by high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) with energy-dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD) analysis, and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of Ag catalysts for O 2 reduction reaction (ORR) in 1 M KOH is evaluated using the rotating (ring)-disc electrode method. SEM and HAADF-STEM results show that the unsupported pure-Ag and Ag-CA catalysts consist mainly of big agglomerates, and Ag/C has the smallest agglomerates and some sub-3 nm Ag nanoparticles. The XPS results reveal that Ag in all the catalysts is in the metallic form (Ag 0 ). Despite consisting of big agglomerates, the Ag-CA catalyst exhibits similar ORR electrocatalytic activity to that of Ag/C. Ag-CA (unsupported) shows the lowest hydrogen peroxide yield. These results are of great importance for the development of Ag-based catalysts that can be prepared in a fast, simple and easily up scalable fashion, for anion exchange membrane fuel cells.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

MOCVD Surface Preparation of V-Groove Si for III-V Growth

V-groove nanopatterning of Si substrates has recently demonstrated promise for achieving high-quality III-V-on-Si epitaxy while providing a lower-cost processing route than chemo-mechanical polishing to produce epi-ready planar wafers. A key factor in determining the crystalline quality of III-V buffer layers is the Si surface structure and its chemical composition. Unlike planar Si surfaces, the surfaces of V-grooves prior to growth have not been studied in detail. Here, we study the surface of V-groove Si prepared for GaP nucleation via X-ray photoelectron spectroscopy and low-energy electron diffraction. We identify several pretreatments, using both 830 and 1000 annealing under an As background pressure, as being suitable for deoxidizing and cleaning the V-groove Si surface. The V-groove Si was found to behave similarly to reference Si(0 0 1) and Si(1 1 1) planar samples, demonstrating that in situ techniques such as reflection anisotropy spectroscopy can be used on reference samples to infer the state of the V-groove surface, and indicating that the extensive research on planar Si surfaces can be directly applied to V-grooves.

III-V epitaxy↗
DOE OSTI2025

Xerogel-Derived Ni Electrocatalysts for the Hydrogen Evolution Reaction in Alkaline Media

Anion exchange membrane water electrolyzers (AEMWEs) represent a promising technology for hydrogen production. The big advantage of the technology is that it allows for the use of platinum group metal-free (PGM-free) electrocatalysts at both electrodes, including catalysts for the hydrogen evolution reaction (HER) at the cathode. In addition to fulfilling the cost requirement, PGM-free HER catalysts need to meet the activity and durability targets of the AEMWEs. Here, in this work, we developed several carbon-supported, xerogel-derived nickel (Ni) HER electrocatalysts and evaluated the effect of various synthesis conditions, such as the type of carbon support, Ni-to-carbon ratio, and heat-treatment temperature and time, on their performance. Scanning transmission electron microscopy combined with energy-dispersive X-ray spectroscopy (STEM-EDS), X-ray diffraction spectroscopy (XRD), and X-ray photoelectron spectroscopy (XPS) revealed the formation of Ni nanoparticles with an oxygen-rich layer on the outside. Durability of the best-performing catalyst was assessed via a constant-current hold at 10 mA cm –2 over 100 h. This catalyst was found to be more active and durable than the reference PGM-free material, a commercial Ni catalyst supported on a Vulcan XC-72. The catalyst was also tested in the cathode of a fully PGM-free AEMWE, allowing to reach 1.90 V (1.84 V HFR-free) at 1 A cm –2 at 80 °C.

08 HYDROGEN↗
DOE OSTI2024

Determining the oxidation stability of SnSe under atmospheric exposure

Abstract Understanding surface stability becomes critical as 2D materials like SnSe are developed for piezoelectric and optical applications. SnSe thin films deposited by molecular beam epitaxy showed no structural changes after a two-year exposure to atmosphere, as confirmed by X-ray diffraction and Raman spectroscopy. X-ray photoelectron spectroscopy and reflectivity show a stable 3.5 nm surface oxide layer, indicating a self-arresting oxidative process. Resistivity measurements show an electrical response dominated by SnSe post-exposure. This work shows that SnSe films can be used in ambient conditions with minimal risk of long-term degradation, which is critical for the development of piezoelectric or photovoltaic devices. Graphical Abstract

Chin, Jonathan R. (ORCID:0000000273205678)↗
DOE OSTI2024

Functionalization of nitrogen vacancy-containing nanodiamonds with a metal-organic framework for quantum sensing applications

Nitrogen vacancy (NV)-containing nanodiamonds (NDs) are an important material in applications such as biological imaging, catalysis, and, in particular, quantum sensing. Careful manipulation of the surface coating on NV NDs is essential for both enhancing quantum sensor performance and for tuning selectivity towards specific sensing targets. Here, we demonstrate a simple synthetic approach for functionalizing NV NDs with the zeolitic imidazole framework-8 (ZIF-8) metal–organic framework (MOF), providing a well-ordered, porous scaffold for immobilizing target analytes near the NV ND surface. The composites were structurally characterized by x-ray diffraction, electron microscopy, and X-ray photoelectron spectroscopy, and these results were all consistent with NV NDs fully encapsulated by ZIF-8. Critically, the luminescent properties of the NV NDs, which are vital for quantum sensing experiments such as optically detected magnetic resonance (ODMR), are unchanged by the MOF coating. Moreover, spin relaxometry experiments indicate that the ZIF-8 coating significantly enhances the NV ND spin longitudinal relaxation time T1, a critical quantum parameter for sensing applications. Given the tremendous structural diversity of MOFs, the NV ND@MOF composites are an exciting material class with exciting implications for the development of high-performance quantum sensors.

Crawford, Scott↗
DOE OSTI2022

Effect of Cationic (Na + ) and Anionic (F – ) Co-Doping on the Structural and Electrochemical Properties of LiNi 1/3 Mn 1/3 Co 1/3 O 2 Cathode Material for Lithium-Ion Batteries

Elemental doping for substituting lithium or oxygen sites has become a simple and effective technique to improve the electrochemical performance of layered cathode materials. Compared with single-element doping, this work presents an unprecedented contribution to the study of the effect of Na + /F – co-doping on the structure and electrochemical performance of LiNi 1/3 Mn 1/3 Co 1/3 O 2 . The co-doped Li 1-z Na z Ni 1/3 Mn 1/3 Co 1/3 O 2-z F z (z = 0.025) and pristine LiNi 1/3 Co 1/3 Mn 1/3 O 2 materials were synthesized via the sol–gel method using EDTA as a chelating agent. Structural analyses, carried out by X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy, revealed that the Na + and F – dopants were successfully incorporated into the Li and O sites, respectively. The co-doping resulted in larger Li-slab spacing, a lower degree of cation mixing, and the stabilization of the surface structure, which substantially enhanced the cycling stability and rate capability of the cathode material. The Na/F co-doped LiNi 1/3 Mn 1/3 Co 1/3 O 2 electrode delivered an initial specific capacity of 142 mAh g –1 at a 1C rate (178 mAh g –1 at 0.1C), and it maintained 50% of its initial capacity after 1000 charge–discharge cycles at a 1C rate.

25 ENERGY STORAGE↗
DOE OSTI2023

Diesel Particulate Filter Durability Performance Comparison Using Metals Doped B20 vs. Conventional Diesel Part II: Chemical and Microscopic Characterization of Aged DPFs

This project's objective was to generate experimental data to evaluate the impact of metals doped B20 on diesel particle filter (DPF) ash loading and performance compared to that of conventional petrodiesel. The effect of metals doped B20 vs. conventional diesel on a DPF was quantified in a laboratory controlled accelerated ash loading study. The ash loading was conducted on two DPFs - one using ULSD fuel and the other on B20 containing metals dopants equivalent to 4 ppm B100 total metals. Engine oil consumption and B20 metals levels were accelerated by a factor of 5, with DPFs loaded to 30 g/L of ash. Details of the ash loading experiment and on-engine DPF performance evaluations are presented in the companion paper (Part I). The DPFs were cleaned, and ash samples were taken from the cleaned material. X-ray Fluorescence (XRF), X-Ray Photoelectron Spectroscopy (XPS) and X-Ray Diffraction (XRD) were conducted on the ash samples. Core samples were taken from the cleaned DPF and were subjected to scanning electron microscope energy dispersive x-ray spectroscopy (SEM-EDS) and XRF analysis. A comparison of the data from the two DPFs is presented. The XRD and XPS analysis showed that the compounds present in the ash from the two DPFs were nearly identical, though differing in concentrations. CaSO4 was the biggest component of the ash from both DPFs. The metals doped B20 fuel resulted in ash with similar characteristics to that deposited by the lube oil and did not appear to have any deleterious physical effects on the DPF substrate (did not penetrate the substrate).

ADVANCED PROPULSION SYSTEMS,BIOMASS FUELS↗