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NASA NTRS1990

Simulation of Martian dust accumulation on surfaces

Future NASA space missions include the possibility of manned landings and exploration of Mars. Environmental and operational constraints unique to Mars must be considered when selecting and designing the power system to be used on the Mars surface. A technique is described which was developed to simulate the deposition of dust on surfaces. Three kinds of dust materials were studied: aluminum oxide, basalt, and iron oxide. The apparatus was designed using the Stokes and Stokes-Cunningham law for particle fallout, with additional consideration given to particle size and shape. Characterization of the resulting dust films on silicon dioxide, polytetrafluoroethylene, indium tin oxide, diamondlike carbon, and other surfaces are discussed based on optical transmittance measurements. The results of these experiments will guide future studies which will consider processes to remove the dust from surfaces under Martian environmental conditions.

Perez-Davis, Marla E.↗

NASA NTRS1981

Fracture toughness of brittle materials determined with chevron notch specimens

Short bar, short rod, and four-point-bend chevron-notch specimens were used to determine the plane strain fracture toughness of hot-pressed silicon nitride and sintered aluminum oxide brittle ceramics. The unique advantages of this specimen type are: (1) the production of a sharp natural crack during the early stage of test loading, so that no precracking is required, and (2) the load passes through a maximum at a constant, material-independent crack length-to-width ratio for a specific geometry, so that no post-test crack measurement is required. The plane strain fracture toughness is proportional to the maximum test load and functions of the specimen geometry and elastic compliance. Although results obtained for silicon nitride are in good mutual agreement and relatively free of geometry and size effects, aluminum oxide results were affected in both these respects by the rising crack growth resistance curve of the material.

Shannon, J. L., Jr.↗

NASA NTRS1989

A study of native oxides of beta-SiC using Auger electron spectroscopy

Thermal and anodic oxide films of beta-SiC are analyzed using Auger electron spectroscopy. Auger depth-composition profiles are obtained in order to determine the chemical composition of the oxide films. The position and shape of silicon spectral peaks are used to estimate the chemical bonding of the oxide constituents. It is found that the wet thermal oxide is almost stoichiometric but contains about 14 pct C. Dry oxide, on the other hand, has less than 3 pct C but is highly nonstoichiometric. The C content in the anodic oxide is 12 pct. Anodic oxide films, like dry-oxide films, are nonstoichiometric. A model of the SiC oxidation process is presented.

Chaudhry, M. Iqbal↗

NASA NTRS2014

Delta-Doping at Wafer Level for High Throughput, High Yield Fabrication of Silicon Imaging Arrays

Systems and methods for producing high quantum efficiency silicon devices. A silicon MBE has a preparation chamber that provides for cleaning silicon surfaces using an oxygen plasma to remove impurities and a gaseous (dry) NH3 + NF3 room temperature oxide removal process that leaves the silicon surface hydrogen terminated. Silicon wafers up to 8 inches in diameter have devices that can be fabricated using the cleaning procedures and MBE processing, including delta doping.

Hoenk, Michael E.↗

NASA NTRSDate not supplied

Assessing Degradation of Advanced Coatings for Carbon/Carbon Composites

Carbon/carbon (C/C) composites are a well-utilized material system for hot structures to enable hypersonic flight. However, C/C materials are susceptible to attack by environmental degradation mechanisms, notably oxidation, which can limit the durability of components resulting in premature failure. Environmental barrier coatings (EBCs) have been developed to mitigate deleterious oxidation. Coating compositions based on silicon carbide (SiC) offer promise as a protective coating material for C/C composites. Under particular hypersonic flight conditions, a passivating silica scale can form at the surface of the EBC, acting as a barrier that can protect the underlying coating and substrate. However, the transition from passive to active oxidation, which varies with temperature and pressure, causes the formation of gaseous SiO that volatilizes leading to detrimental consumption of the SiC coating. In this work, arc-jet testing of SiC-based coatings developed to protect Advanced C/C-6 (ACC-6) was performed under a range of conditions to replicate varying oxidation conditions. In-situ optical emission spectroscopic measurements of the gas-surface interactions were collected and evaluated to render compositional degradation of the coating and underlying composite during arc-jet testing. Specimens were evaluated before, during and after arc-jet testing using destructive and non-destructive materials characterization methods, including optical and scanning electron microscopy and energy dispersive spectroscopy.

Coatings, Hypersonics, Composites↗

NASA NTRS1982

RF sputtered silicon and hafnium nitrides: Properties and adhesion to 440C stainless steel

Silicon nitride and hafnium nitride coatings were deposited by reactive RF sputtering on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. Depositions were at two background pressures, 8 and 20 mtorr, and at two different fractions (f) of nitrogen in argon, 0.25 and 0.60, for hafnium nitride and at f = 0.25 for silicon nitride. The coatings and the interface between the coating and substrates were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. A Knoop microhardness of 1650 + or - 100 kg/sq mm was measured for hafnium nitride and 3900 + or - 500 kg/sq mm for silicon nitride. The friction coefficients between a 440C rider and the coatings were measured under lubricated conditions. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C.

Grill, A.↗

NASA NTRS1983

RF-sputtered silicon and hafnium nitrides - Properties and adhesion to 440C stainless steel

Silicon nitride and hafnium nitride coatings were deposited by reactive RF sputtering on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. Depositions were at two background pressures, 8 and 20 mtorr, and at two different fractions (f) of nitrogen in argon, 0.25 and 0.60, for hafnium nitride and at f = 0.25 for silicon nitride. The coatings and the interface between the coating and substrates were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. A Knoop microhardness of 1650 + or 100 kg/sq mm was measured for hafnium nitride and 3900 + or 500 kg/sq mm for silicon nitride. The friction coefficients between a 440C rider and the coatings were measured under lubricated conditions. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C.

Grill, A.↗

NASA NTRS1984

Development of improved coating for advanced carbon-carbon components

Reaction sintered silicon nitride (RSSN) was studied as a substitute coating material on the carbon-carbon material (RCC) presently used as a heat shield on the space shuttle, and on advanced carbon-carbon (ACC), a later development. On RCC, RSSN showed potential in a 538 C (1000 F) screening test in which silicon carbide coated material exhibits its highest oxidation rate; RSSN afforded less protection to ACC because of a larger thermal expansion mismatch. Organosilicon densification and metallic silicon sealing methods were studied as means of further increasing the oxidation resistance of the coating, and some improvement was noted when these methods were employed.

Yamaki, Y. R.↗

NASA NTRS2022

Natural Gas/Oxygen Burner Rig at The NASA Glenn Materials Research Laboratory

This technical memorandum describes the development of a new natural gas/oxygen (NG/O2) fueled burner rig to be used for high-temperature environmental durability studies of advanced materials and components at atmospheric pressure. The burner simulates the high-temperature, high-heat flux, and high-velocity thermal environments encountered in aerospace applications. It will be used to study environmental effects such as water vapor interactions relevant to advanced gas turbine engine materials such as ceramic matrix composites with protective environmental barrier coatings. The highest sample temperature achieved to date in a study of the oxidation and recession of monolithic silicon carbide is 3000 °F.

Burner Rig↗

NASA NTRS1975

Tunnel injection into gate oxide traps

An experimental method is described for measuring the density of oxide traps in the gate oxide of an MOS transistor as a function of energy and position near the silicon interface. Measurements are obtained from different oxide growth processes and after Co-60 irradiation. The results are related to long-term drift of threshold voltage.

Maserjian, J.↗

NASA NTRS1989

Sliding seal materials for low heat rejection engines

Sliding friction coefficients and wear rates of promising piston seal materials were measured under temperature, environmental, velocity, and loading conditions that are representative of the low heat rejection (LHR) diesel engine environment. These materials included carbides, oxides, and nitrides. In addition, silicon nitride and partially stablized zirconia disks (cylinder liners) were ion-implanted with TiNi, Ni, Co, and Cr, and subsequently run against carbide pins (piston rings), with the objective of producing reduced friction via solid lubrication at elevated temperature. Friction and wear measurements were obtained using pin-on-disk laboratory experiments and a unique engine friction test rig. Unmodified ceramic sliding couples were characterized at all temperatures by friction coefficients of 0.24 and above during the pin-on-disk tests. The coefficient at 800 C in an oxidizing environment was reduced to below 0.1, for certain material combination, by the ion-implantation of TiNi or Co. This beneficial effect was found to derive from the lubricious Ti, Ni, and Co oxides. Similar results were demonstrated on the engine friction test rig at lower temperatures. The structural integrity and feasibility of engine application with the most promising material combination were demonstrated during a 30-hour single-cylinder, direct-injection diesel engine test.

Beaty, Kevin↗

NASA NTRS1991

An empirical approach to predicting long term behavior of metal particle based recording media

Alpha iron particles used for magnetic recording are prepared through a series of dehydration and reduction steps of alpha-Fe2O3-H2O resulting in acicular, polycrystalline, body centered cubic (bcc) alpha-Fe particles that are single magnetic domains. Since fine iron particles are pyrophoric by nature, stabilization processes had to be developed in order for iron particles to be considered as a viable recording medium for long term archival (i.e., 25+ years) information storage. The primary means of establishing stability is through passivation or controlled oxidation of the iron particle's surface. Since iron particles used for magnetic recording are small, additional oxidation has a direct impact on performance especially where archival storage of recorded information for long periods of time is important. Further stabilization chemistry/processes had to be developed to guarantee that iron particles could be considered as a viable long term recording medium. In an effort to retard the diffusion of iron ions through the oxide layer, other elements such as silicon, aluminum, and chromium have been added to the base iron to promote more dense scale formation or to alleviate some of the non-stoichiometric behavior of the oxide or both. The presence of water vapor has been shown to disrupt the passive layer, subsequently increasing the oxidation rate of the iron. A study was undertaken to examine the degradation in magnetic properties as a function of both temperature and humidity on silicon-containing iron particles between 50-120 deg C and 3-89 percent relative humidity. The methodology to which experimental data was collected and analyzed leading to predictive capability is discussed.

Hadad, Allan S.↗

NASA NTRS2020

Influence of Thermally-Grown Oxide (TGO) Layer on the Driving Forces Associated with Failure in Environmental Barrier Coating (EBC) Systems

Environmental barrier coatings (EBC) is an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. Spallation of environmental barrier coating (EBC) induced by thermally grown oxide (TGO) layer is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from the silicon carbide (SiC) based substrate itself. Critical thickness of the TGO layer for failure is in the range of 20-30 microns but it can vary due to exposure temperature, microstructure etc. Current work at NASA Glenn Research Center, under the Revolutionary Tools and Methods (RTM) project is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers with or without damage on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. Initial results indicate that the presence of damage (vertical cracks caused by in-plane stresses) enhances the stresses that are present due to non-uniformity. However, the presence of non-uniformity itself is still the main factor influencing the magnitude of peel and shear stresses in the TGO layer.

Mital, Subodh K.↗

NASA NTRS1979

Study of high resistance inorganic coatings on graphite fibers

Coatings made of boron, silicon carbide, silica, and silica-like materials were studied to determine their ability to increase resistance of graphite fibers. The most promising results were attained by chemical vapor depositing silicon carbide on graphite fiber followed by oxidation, and drawing graphite fiber through ethyl silicate followed by appropriate heat treatments. In the silicon carbide coating studies, no degradation of the graphite fibers was observed and resistance values as high as three orders of magnitude higher than that of the uncoated fiber was attained. The strength of a composite fabricated from the coated fiber had a strength which compared favorably with those of composites prepared from uncoated fiber. For the silica-like coated fiber prepared by drawing the graphite fiber through an ethyl silicate solution followed by heating, coated fiber resistances about an order of magnitude greater than that of the uncoated fiber were attained. Composites prepared using these fibers had flexural strengths comparable with those prepared using uncoated fibers, but the shear strengths were lower.

Galasso, F. S.↗

NASA NTRS2012

Quantum-Well Infrared Photodetector (QWIP) Focal Plane Assembly

A paper describes the Thermal Infrared Sensor (TIRS), a QWIP-based instrument intended to supplement the Operational Land Imager (OLI) for the Landsat Data Continuity Mission (LDCM). The TIRS instrument is a far-infrared imager operating in the pushbroom mode with two IR channels: 10.8 and 12 microns. The focal plane will contain three 640x512 QWIP arrays mounted on a silicon substrate. The silicon substrate is a custom-fabricated carrier board with a single layer of aluminum interconnects. The general fabrication process starts with a 4-in. (approx.10-cm) diameter silicon wafer. The wafer is oxidized, a single substrate contact is etched, and aluminum is deposited, patterned, and alloyed. This technology development is aimed at incorporating three large-format infrared detecting arrays based on GaAs QWIP technology onto a common focal plane with precision alignment of all three arrays. This focal plane must survive the rigors of flight qualification and operate at a temperature of 43 K (-230 C) for five years while orbiting the Earth. The challenges presented include ensuring thermal compatibility among all the components, designing and building a compact, somewhat modular system and ensuring alignment to very tight levels. The multi-array focal plane integrated onto a single silicon substrate is a new application of both QWIP array development and silicon wafer scale integration. The Invar-based assembly has been tested to ensure thermal reliability.

Jhabvala, Murzy↗

NASA NTRS2012

Fabrication of a Cryogenic Terahertz Emitter for Bolometer Focal Plane Calibrations

A fabrication process is reported for prototype emitters of THz radiation, which operate cryogenically, and should provide a fast, stable blackbody source suitable for characterization of THz devices. The fabrication has been demonstrated and, at the time of this reporting, testing was underway. The emitter is similar to a monolithic silicon bolometer in design, using both a low-noise thermometer and a heater element on a thermally isolated stage. An impedance-matched, high-emissivity coat ing is also integrated to tune the blackbody properties. This emitter is designed to emit a precise amount of power as a blackbody spectrum centered on terahertz frequencies. The emission is a function of the blackbody temperature. An integrated resistive heater and thermometer system can control the temperature of the blackbody with greater precision than previous incarnations of calibration sources that relied on blackbody emission. The emitter is fabricated using a silicon- on-insulator substrate wafer. The buried oxide is chosen to be less than 1 micron thick, and the silicon device thickness is 1-2 microns. Layers of phosphorus compensated with boron are implanted into and diffused throughout the full thickness of the silicon device layer to create the thermometer and heater components. Degenerately doped wiring is implanted to connect the devices to wire-bondable contact pads at the edge of the emitter chip. Then the device is micromachined to remove the thick-handle silicon behind the thermometer and heater components, and to thermally isolate it on a silicon membrane. An impedance- matched emissive coating (ion assisted evaporated Bi) is applied to the back of the membrane to enable high-efficiency emission of the blackbody spectrum.

Chervenak, James↗

NASA NTRS2019

Modeling of the Influence of a Damaged Thermally Grown Oxide (TGO) Layer in an Environmental Barrier Coating System

Environmental barrier coatings (EBC) are an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. EBCs are susceptible to a number of failure modes including oxidation/delamination, recessions, chemical attack and dissolution, thermomechanical degradation, erosion, and foreign object impact damage in a combustion environment. Spallation of environmental barrier coating (EBC), induced by a thermally grown oxide (TGO) layer, is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from a silicon carbide (SiC) based substrate itself. The TGO layer evolves (i.e., thickness increases with time) as water vapor and oxygen gradually diffuse through the EBC, and the EBC spalls off once the TGO layer reaches some critical thickness. The critical thickness of the TGO layer for failure is in the range of 20-30 microns, but it can vary due to exposure temperature, microstructure etc. Current work at NASA Glenn Research Center, under the Revolutionary Tools and Methods (RTM) subproject is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. The effect of damage in the TGO layer on the resulting stress states is also assessed both in uniform and non-uniform TGO layers.

Mital, Subodh K.↗

NASA NTRS2021

Modeling of the Influence of Thermally Grown Oxide (TGO) Layers on the Driving Forces in Environmental Barrier Coating Systems

Environmental barrier coatings (EBC) are an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. EBCs are susceptible to several failure modes including oxidation/delamination, recession, chemical attack and dissolution, thermomechanical degradation, erosion, and foreign object impact damage in a combustion environment. Spallation of environmental barrier coating (EBC), induced by a thermally grown oxide (TGO) layer, is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from a silicon carbide (SiC) based substrate itself. The TGO layer evolves (i.e., thickness increases with time) as water vapor and oxygen gradually diffuse through the EBC, and the EBC spalls off once the TGO layer reaches some critical thickness. The critical thickness of the TGO layer for failure is in the range of 20-30 microns, with the actual value depending upon exposure temperature, microstructure, etc. Current work at NASA Glenn Research Center, under the Transformative Tools and Technology (TTT) subproject is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. The effect of damage in the TGO layer on the resulting stress states is also assessed both in uniform and non-uniform TGO layers.

Coatings↗