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Results for “Thermal oxidation”

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 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS2020

Progress of Coating Stress Compensation of Silicon Mirrors for Lynx X-ray Telescope Mission Concept Using Thermal Oxide Patterning Method

A thermal oxide patterning method has proven to be effective for correcting coating-stress-induced distortion on flat silicon wafers. We report progress on developing this method for correcting curved silicon mirrors distorted by front-side iridium coatings. Owing to the difference in geometry, a finite element model has been established to calculate the appropriate duty cycle maps in thermal oxide hexagon patterns used for compensation. In addition, a photolithographic process, along with three-dimensional printed equipment, has been developed for creating patterns precisely on the back side of curved mirrors. The developed method has been used to recover the original surface shape of two silicon mirrors which are 100-mm long, 0.5-mm thick, having 312-mm radius of curvature, and 30 deg in azimuthal span (Wolter-I geometry). These mirrors’ front sides are sputter-coated by 20-nm iridium layers with ∼-70 N∕m integrated stress. Measurement results show that the developed method can mitigate coating-induced distortion by a factor of ∼5 in RMS height and ∼4 in RMS slope error, corresponding to ∼0.5 arc sec RMS slope error. Residual errors after correction are dominated by midfrequency ripples created during the annealing process, which will be resolved in the future. The presented method is precise and inexpensive and a potential candidate for resolving the coating stress issue for Lynx optics in the future.

x-ray↗
DOE OSTI2022

Effect of thermal oxidation on helium implanted 316L stainless steel

The effect of thermal oxide layer on He implanted 316L stainless steel was studied to evaluate experimentally how thermal oxidation affects the diffusion and distribution of He in the material. In the case of thermal oxidation of a He implanted sample, with an increase in oxidation time, the max swelling height increases logarithmically as a function of time and finally saturates for all samples except for the lowest dose of implanted He. Concerning TEM results, two void regions are identified. Similar to the calculation, the total irradiated depth was around 250 nm and the large void region was formed around 100–150 nm depth. On the other hand, the small void region was observed immediately under oxide layer from the thermal oxidation. In contrast, there were no voids in the altered zone near the metal/oxide interface in the non-thermal oxidized/He implanted sample. This description of the phenomena was justified using the Kirkendall effect and the Point Defect Model.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Multi–length scale characterization of point defects in thermally oxidized, proton irradiated iron oxides

A key for the success of safe nuclear power generation system is to consider structural materials that are economical, meet mechanical property needs, possess good corrosion resistance, and are radiation tolerant. Nevertheless, fundamental insights that elucidate the details of radiation damage on materials corrosion performance are lacking. This includes the behavior of surface oxides which often regulate corrosion. For example, it is unclear how non-equilibrium point defects, oxide structure, mass transport in oxides, and subsequent oxidation behavior are altered by the radiation. Here, in this work, some of the effects of proton irradiation on the attributes of point defects, iron oxide microstructures, and the physical nature of the oxidation product were correlated with corrosion behavior. Iron oxides, fabricated by thermal oxidation in air at 400°C and 800°C for 1 h, were subjected to 200 keV, 0.03 dpa (displacements per atom) of proton irradiation, and subjected to corrosion reactivity assessment using AC and DC electrochemical methods. Experimental methods that target materials information at different length scales, such as positron annihilation spectroscopy (atomistic), transmission electron microscopy (mesoscopic), and electrochemical methods (macroscopic), were coupled to shed light on the impact of radiation-induced defect modifications and structural changes in oxides on corrosion reactivity which ultimately affects durability in harsh environments.

36 MATERIALS SCIENCE↗
NASA NTRS1994

Thermal-oxidative Pretreatment and Evaluation of Poly (hexafluoropropene Oxide) Fluids

Two commercial poly(hexafluoropropene oxide) fluids were thermally pretreated at 343 C in pure oxygen. IR and NMR spectra indicate that this pretreatment was effective in removing hydrogen end-capped impurities. Decrease in the quantity of volatile material produced during thermal oxidative decomposition and increase in the thermal decomposition temperature indicated improvement in the stability of the fluids. However, this pretreatment failed to render the fluids completely stable in oxidizing atmospheres at 316 C in the presence of metal alloys.

Paciorek, K. J. L.↗
NASA NTRS1995

Thermal-oxidative pretreatment and evaluation of poly(hexafluoropropene oxide) fluids

Two commercial poly(hexafluoropropene oxide) fluids were thermally pretreated at 343 C in pure oxygen. IR and nuclear magnetic resonance(NMR) spectra indicate that this pretreatment was effective in removing hydrogen end-capped impurities. A decrease in the quantity of volatile material produced during thermal oxidative decomposition and increase in the thermal decomposition temperature indicated improvement in the stability of the fluids. However, this pretreatment failed to render the fluids completely stable in oxidizing atmospheres at 316 C in the presence of metal alloys.

Paciorek, K. J. L.↗
DOE OSTI2025

Effect of thermal oxidation on helium implanted pure iron

The impact of thermal oxidation on Helium (He) implanted pure iron (Fe) was investigated to experimentally evaluate how thermal oxidation influences the diffusion and distribution of He within the material. In case of the sample with the lowest dose (2 × 10 17 ions/cm 2 ), the thinnest oxide layer was observed compared to the non-implanted pure Fe. It is due to He nano bubbles implanted in the material, which hinder the diffusion of Fe ions necessary for forming the oxide layer. For the medium dose sample (5 × 10 17 ions/cm 2 ), the oxide layer was slightly thicker than that of the lowest dose, however it had more porous structure due to the numerous nano He bubbles. In addition, a large bubble region around 150–200 nm depth was generated. Here, the highest dose sample (1 × 10 18 ions/cm 2 ) was observed that the escape of He was accelerated by the large amount of nano He bubbles from within the metal, forming a porous Fe matrix on the top surface and an oxide layer that is very porous but thicker than those of lower doses.

He implantation↗
DOE OSTI2021

Operando Study of Thermal Oxidation of Monolayer MoS 2

Abstract Monolayer MoS 2 is a promising semiconductor to overcome the physical dimension limits of microelectronic devices. Understanding the thermochemical stability of MoS 2 is essential since these devices generate heat and are susceptible to oxidative environments. Herein, the promoting effect of molybdenum oxides (MoO x ) particles on the thermal oxidation of MoS 2 monolayers is shown by employing operando X‐ray absorption spectroscopy, ex situ scanning electron microscopy and X‐ray photoelectron spectroscopy. The study demonstrates that chemical vapor deposition‐grown MoS 2 monolayers contain intrinsic MoO x and are quickly oxidized at 100 °C (3 vol% O 2 /He), in contrast to previously reported oxidation thresholds (e.g., 250 °C, t ≤ 1 h in the air). Otherwise, removing MoO x increases the thermal oxidation onset temperature of monolayer MoS 2 to 300 °C. These results indicate that MoO x promote oxidation. An oxide‐free lattice is critical to the long‐term stability of monolayer MoS 2 in state‐of‐the‐art 2D electronic, optical, and catalytic applications.

2-dimensional material↗
NASA NTRS1988

Temperature stability of Al(x)Ga(1-x)As (x = 0-1) thermal oxide masks for selective-area epitaxy

The use of thermal oxides of Al(x)Ga(1-x)As (x = 0-1) as masking materials for selective-area epitaxy by a organometallic chemical-vapor deposition has been investigated. It was found that the thermal oxide of GaAs is only applicable for low growth temperatures (less than or equal to 600 C), and the addition of aluminum significantly improves the thermal stability of the oxide. The oxide of Al(0.4)Ga(0.6)As is suitable for high-temperature deposition, but there are criteria for the thickness and oxidation temperature. Thin layers of AlAs oxidized at 475 C are excellent masks and allow precise thickness control. Promising results of selective-area deposition using these aluminum oxide masks have been obtained. High-quality single crystal grew in mask openings uniformly surrounded by dense and fine-grain polycrystalline deposits, producing a planar duplication of the original pattern.

Jones, Stephen H.↗
NASA NTRS1981

Thermal oxidative degradation reactions of perfluoroalkylethers

The mechanisms operative in thermal oxidative degradation of Fomblin Z and hexafluoropropene oxide derived fluids and the effect of alloys and additives upon these processes are investigated. The nature of arrangements responsible for the inherent thermal oxidative instability of the Fomblin Z fluids is not established. It was determined that this behavior is not associated with hydrogen end groups or peroxy linkages. The degradation rate of these fluids at elevated temperatures in oxidizing atmospheres is dependent on the surface/volume ratio. Once a limiting ratio is reached, a steady rate appears to be attained. Based on elemental analysis and oxygen consumption data, CF2OCF2CF2O2, no. CF2CF2O, is one of the major arrangements present. The action of the M-50 and Ti(4 Al, 4 Mn) alloys is much more drastic in the case of Fomblin Z fluids than that observed for the hexafluoropropene derived materials. The effectiveness of antioxidation anticorrosion additives, P-3 and phospha-s-triazine, in the presence of metal alloys is very limited at 316 C; at 288 C the additives arrested almost completely the fluid degradation. The phospha-s-triazine appears to be at least twice as effective as the P-3 compound; it also protected the coupon better. The Ti(4 Al, 4 Mn) alloy degraded the fluid mainly by chain scission processes this takes place to a much lesser degree with M-50.

Paciorek, K. L.↗
NASA NTRS1985

Pretreatment effects on the morphology and properties of aluminum oxide thermally grown on NiCoCrAlY

The effect of pretreatments on the morphology and properties of aluminum oxide thermally grown from NiCoCrAlY was investigated. The goal was to optimize process steps to produce a highly adherent, continuous, and insulating aluminum oxide. Two pretreatments were carried out, one in vacuum (about 0.0001 Torr) at 1350 K for 5 h, and the other consisting of deposition of a 1-micron thick Al2O3 film by activated reactive evaporation. Samples were subsequently oxidized thermally at 1000 C for 50 h at 0.5 Torr oxygen pressure. The two pretreatments were carried out on electron-beam evaporation NiCoCrAlY, about 120 microns thick, deposited on a superalloy turbine blade substrate. The results showed that the thermally grown oxide was significantly different in microstructure, surface topography and in its adherence to the NiCoCrAlY for the two pretreatments. Optimum results were obtained by combining the two pretreatments to produce an adherent, continuous, and insulating oxide film on the NiCoCrAlY-coated superalloy substrate.

Prakash, S.↗
DOE OSTI2021

Insights into the Enhanced Oxidative Thermal Stability of Nanoparticle Organic Hybrid Materials Developed for Carbon Capture and Energy Storage

Due to the growing need for Direct Air Capture (DAC) and integrated carbon capture and conversion technologies, CO 2 capture materials that can withstand a wide range of environmental conditions, including fluctuating ambient temperatures and high concentrations of oxidizing agents (i.e., oxygen and moisture), are critically needed. Liquid-like Nanoparticle Organic Hybrid Materials (NOHMs) have been proposed as candidates for DAC and electrolyte additives enabling sustainable energy storage (i.e., integrated CO 2 capture and conversion and flow batteries). Liquid-like NOHMs functionalized with an ionic bond have been shown to display greatly enhanced oxidative thermal stability compared to the untethered polymer. However, these studies were limited in terms of reaction conditions and the detailed mechanisms of the oxidative thermal degradation were not reported. In this work, a kinetic thermal degradation analysis was performed on NOHM-I-HPE and the neat polymer, Jeffamine M2070 (HPE), in both non-oxidative and oxidative conditions. NOHM-I-HPE displayed similar thermal stability to the untethered polymer in a nitrogen environment, but interestingly, the thermal stability of the ionically tethered polymer was significantly enhanced in the presence of air. This observed enhancement of oxidative thermal stability is attributed to the orders of magnitude larger viscosity of the liquid-like NOHMs compared to untethered polymer and the bond stabilization of the ionically tethered polymer in the NOHMs canopy. Further, spectroscopic analyses of the liquid residue revealed that in the presence of oxygen, the degradation of HPE and NOHM-I-HPE occurs through the formation of trace amounts of carbonyls. This study illustrated that NOHMs can serve as functional materials for sustainable energy storage applications because of their excellent oxidative thermal stability.

25 ENERGY STORAGE↗
NASA NTRS1983

The effects of metals and inhibitors on thermal oxidative degradation reactions of unbranched perfluoroalkylethers

Thermal oxidative degradation studies were performed on unbranched perfluoroalkylethers at 288 C in oxygen. Metals and alloys studied included Ti, Al, and Ti (4 Al, 4 Mn). The mechanism of degradation was by chain scission. Ti and Al promoted less degradation than Ti (4 Al, 4 Mn). The two inhibitors investigated (a perfluorophenyl phosphine and a phosphatriazine) reduced degradation rates by several orders of magnitude. Both inhibitors were effective for the same duration (75 to 100 hours). The phosphatriazine appeared to provide more surface protection.

Jones, W. R., Jr.↗
DOE OSTI2026

A Comparative Study of Thermal Oxidization Resistance of a High-Entropy Metal Boride and a High-Entropy Metal Carbide

We present a systematic study of thermal oxidation resistance of transition metal borides and carbides up to 1300 °C in a dry air environment. A High-Entropy Metal Boride (HEMB), of composition (Hf 0.2 , Mo 0.2 , Nb 0.2 , Ta 0.2 , Zr 0.2 )B 2 , and a similar High-Entropy Metal Carbide (HEMC) (Hf, Mo, Nb, Ta, Zr)C 5 were synthesized from precursor mixtures, under 30 MPa of pressure at a temperature of 1800 °C using a Spark Plasma Sintering Device. The synthesized phases were confirmed via X-ray Diffraction analysis, which showed a pure hexagonal AlB 2 -type structure for HEMB and a face-centered cubic (FCC) structure for HEMC, with lattice parameters, a = 3.10 Å and c = 3.37 Å for HEMB and a = 4.524 Å for HEMC. Oxidation resistance was evaluated using a simultaneous thermogravimetric analysis and differential scanning calorimetry (TGA/DSC) stage in which HEMB and HEMC were heated up to 1300 °C at a rate of 2 °C/min in a dry air environment. Scanning electron microscopy (SEM) was used to analyze the resulting oxidized material. Our study demonstrates that HEMB shows better thermal oxidation resistance as compared to a similar metal composition HEMC at high temperatures.

36 MATERIALS SCIENCE↗
NASA NTRS1983

Thermal oxidative degradation reactions of perfluoroalklethers

The objective of this contract was to investigate the mechanisms operative in thermal and thermal oxidative degradation of Fomblin Z and hexafluoropropene oxide derived fluids and the effect of alloys and additives upon these processes. The nature of arrangements responsible for the inherent thermal oxidative instability of the Fomblin Z fluids has not been established. It was determined that this behavior was not associated with hydrogen end-groups or peroxy linkages. The degradation rate of these fluids at elevated temperatures in oxidizing atmospheres was found to be dependent on the surface/volume ratio. Once a limiting ratio was reached, a steady rate appeared to be attained. Based on elemental analysis and oxygen consumption data, -CF2OCF2CF2O-, not -CF2CF2O-, is one of the major arrangements present. The action of the M-50 and Ti(4 Al, 4 Mn) alloys was found to be much more drastic in the case of Fomblin Z fluids than that observed for the hexalfuoropropane oxide derived materials. The effectiveness of antioxidation/anticorrosion additives, P-3 and phospha-s-triazine, in the presence of metal alloys was very limited at 316 C; at 288 C the additives arrested almost completely the fluid degradation. The phospha-s-triazine appeared to be at least twice as effective as the P-3 compound; it also protected the coupon better. The Ti(4 Al, 4 Mn) alloy degraded the fluid mainly by chain scission processes; this took place to a much lesser degree with M-50.

Paciorek, K. L.↗
NASA NTRS1982

Thermal oxidative degradation reactions of linear perfluoroalky lethers

Thermal and thermal oxidative stability studies were performed on linear perfluoro alkyl ether fluids. The effect on degradation by metal catalysts and degradation inhibitors are reported. The liner perfluoro alkylethers are inherently unstable at 316 C in an oxidizing atmosphere. The metal catalysts greatly increased the rate of degradation in oxidizing atmospheres. In the presence of these metals in an oxidizing atmosphere, the degradation inhibitors were highly effective in arresting degradation at 288 C. However, the inhibitors had only limited effectiveness at 316 C. The metals promote degradation by chain scission. Based on elemental analysis and oxygen consumption data, the linear perfluoro alkylether fluids have a structural arrangement based on difluoroformyl and tetrafluoroethylene oxide units, with the former predominating.

Jones, W. R., Jr.↗
NASA NTRS1983

Thermal oxidative degradation reactions of linear perfluoroalkyl ethers

Thermal and thermal oxidative stability studies were performed on linear perfluoroalkyl ether fluids. The effect on degradation by metal catalysts and degradation inhibitors is reported. The linear perfluoroalkyl ethers are inherently unstable at 316 C in an oxidizing atmosphere. The metal catalysts greatly increased the rate of degradation in oxidizing atmospheres. In the presence of these metals in an oxidizing atmosphere, the degradation inhibitors were highly effective in arresting degradation at 288 C. However, the inhibitors had only limited effectiveness at 316 C. The metals promote degradation by chain scission. Based on elemental analysis and oxygen consumption data, the linear perfluoroalkyl ether fluids have a structural arrangement based on difluoroformyl and tetrafluoroethylene oxide units, with the former predominating. Previously announced in STAR as N82-26468

Jones, W. R., Jr.↗
NASA NTRS1985

The effects of metals and inhibitors on thermal oxidative degradation reactions of unbranched perfluoroalkyl ethers

Thermal oxidative degradation studies were performed on unbranched perfluoroalkylethers at 288 C in oxygen. Metals and alloys studied included Ti, Al, and Ti (4 Al, 4 Mn). The mechanism of degradation was by chain scission. Ti and Al promoted less degradation than Ti (4 Al, 4 Mn). The two inhibitors investigated (a perfluorophenyl phosphine and a phosphatriazine) reduced degradation rates by several orders of magnitude. Both inhibitors were effective for the same duration (75 to 100 hours). The phosphatriazine appeared to provide more surface protection.

Jones, W. R., Jr.↗