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All sourcesNASA NTRSDOE OSTI
NASA NTRS2002

Molecular Level Coating of Metal Oxide Particles

Polymer encapsulated metal oxide particles are prepared by combining a polyamide acid in a polar osmotic solvent with a metal alkoxide solution. The polymer was imidized and the metal oxide formed simultaneously in a refluxing organic solvent. The resulting polymer-metal oxide is an intimately mixed commingled blend, possessing, synergistic properties of both the polymer and preceramic metal oxide. The encapsulated metal oxide particles have multiple uses including, being useful in the production of skin lubricating creams, weather resistant paints, as a filler for paper. making ultraviolet light stable filled printing ink, being extruded into fibers or ribbons, and coatings for fibers used in the production of composite structural panels.

Patricia R McDaniel↗
NASA NTRS2002

Oxidation and Volatilization of Silica-Formers in Water Vapor

At high temperatures SiC and Si3N4 react with water vapor to form a silica scale. Silica scales also react with water vapor to form a volatile Si(OH)4 species. These simultaneous reactions, one forming silica and the other removing silica, are described by paralinear kinetics. A steady state, in which these reactions occur at the same rate, is eventually achieved, After steady state is achieved, the oxide found on the surface is a constant thickness and recession of the underlying material occurs at a linear rate. The steady state oxide thickness, the time to achieve steady state, and the steady state recession rate can all be described in terms of the rate constants for the oxidation and volatilization reactions. In addition, the oxide thickness, the time to achieve steady state, and the recession rate can also be determined from parameters that describe a water vapor-containing environment. Accordingly, maps have been developed to show these steady state conditions as a function of reaction rate constants, pressure, and gas velocity. These maps can be used to predict the behavior of silica formers in water-vapor containing environments such as combustion environments. Finally, these maps are used to explore the limits of the paralinear oxidation model for SiC and Si3N4

Opila, E. J.↗
NASA NTRS2002

A Deterministic Interfacial Cyclic Oxidation Spalling Model: Algebraic Approximation, Descriptive Parameters, and Normalized Universal Curve - Part 2

A cyclic oxidation interfacial spalling model has been developed in Part 1. The governing equations have been simplified here by substituting a new algebraic expression for the series (Good-Smialek approximation). This produced a direct relationship between cyclic oxidation weight change and model input parameters. It also allowed for the mathematical derivation of various descriptive parameters as a function of the inputs. It is shown that the maximum in weight change varies directly with the parabolic rate constant and cycle duration and inversely with the spall fraction, all to the 1/2 power. The number of cycles to reach maximum and zero weight change vary inversely with the spall fraction, and the ratio of these cycles is exactly 1:3 for most oxides. By suitably normalizing the weight change and cycle number, it is shown that all cyclic oxidation weight change model curves can be represented by one universal expression for a given oxide scale.

Smialek, James L.↗
NASA NTRS2003

Switching Oxide Traps

We consider radiation-induced charge trapping in SiO2 dielectric layers, primarily from the point of view of CMOS devices. However, SiO2 insulators are used in many other ways, and the same defects occur in other contexts. The key studies, which determined the nature of the oxide charge traps, were done primarily on gate oxides in CMOS devices, because that was the main radiation problem in CMOS at one time. There are two major reviews of radiation-induced oxide charge trapping already in the literature, which discuss the subject in far greater detail than is possible here. The first of these was by McLean et al. in 1989, and the second, ten years later, was intended as an update, because of additional, new work that had been reported. Basically, the picture that has emerged is that ionizing radiation creates electron-hole pairs in the oxide, and the electrons have much higher mobility than the holes. Therefore, the electrons are swept out of the oxide very rapidly by any field that is present, leaving behind any holes that escape the initial recombination process. These holes then undergo a polaron hopping transport toward the Si/SiO2 interface (under positive bias). Near the interface, some fraction of them fall into deep, relatively stable, long-lived hole traps. The nature and annealing behavior of these hole traps is the main focus of this paper.

Oldham, Timothy R.↗
NASA NTRS2003

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi-component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma-sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), electron energy-loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia- yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging from 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗
NASA NTRS2003

Oxidation-Reduction Resistance of Advanced Copper Alloys

Resistance to oxidation and blanching is a key issue for advanced copper alloys under development for NASA's next generation of reusable launch vehicles. Candidate alloys, including dispersion-strengthened Cu-Cr-Nb, solution-strengthened Cu-Ag-Zr, and ODS Cu-Al2O3, are being evaluated for oxidation resistance by static TGA exposures in low-p(O2) and cyclic oxidation in air, and by cyclic oxidation-reduction exposures (using air for oxidation and CO/CO2 or H2/Ar for reduction) to simulate expected service environments. The test protocol and results are presented.

Greenbauer-Seng, L.↗
NASA NTRS2003

Fe-Ti-Cr-Oxides in Martian Meteorite EETA79001 Studied by Point-counting Procedure Using Raman Spectroscopy

Fe-Ti-Cr-Oxide minerals contain much information about rock petrogenesis and alteration. Among the most important in the petrology of common intrusive and extrusive rocks are those of the FeO-TiO2-Cr2O3 compositional system chromite, ulv spinel-magnetite, and ilmenite-hematite. These minerals retain memories of oxygen fugacity. Their exsolution into companion mineral pairs give constraints on formation temperature and cooling rate. Laser Raman spectroscopy is anticipated to be a powerful technique for characterization of materials on the surface of Mars. A Mars Microbeam Raman Spectrometer (MMRS) is under development. It combines a micro sized laser beam and an automatic point-counting mechanism, and so can detect minor minerals or weak Raman-scattering phases such as Fe- Ti-Cr-oxides in mixtures (rocks & soils), and provide information on grain size and mineral mode. Most Fe-Ti-Cr-oxides produce weaker Raman signals than those from oxyanionic minerals, e.g. carbonates, sulfates, phosphates, and silicates, partly because most of them are intrinsically weaker Raman scatters, and partly because their dark colors limit the penetration depth of the excitation laser beam (visible wavelength) and of the Raman radiation produced. The purpose of this study is to show how well the Fe-Ti-Cr-oxides can be characterized by on-surface planetary exploration using Raman spectroscopy. We studied the basic Raman features of common examples of these minerals using well-characterized individual mineral grains. The knowledge gained was then used to study the Fe-Ti-Cr-oxides in Martian meteorite EETA79001, especially effects of compositional and structural variations on their Raman features.

Wang, Alian↗
NASA NTRS2003

Oxidation of Ultra-High Temperature Ceramics in Water Vapor

Ultra high temperature ceramics (UHTCs) including HfB2 + SiC (20% by volume), ZrB2 + SiC (20% by volume) and ZrB2 + SiC (14% by volume) + C (30% by volume) have historically been evaluated as reusable thermal protection systems for hypersonic vehicles. This study investigates UHTCs for use as potential combustion and aeropropulsion engine materials. These materials were oxidized in water vapor (90%) using a cyclic vertical furnace at 1 atm. The total exposure time was 10 hours at temperatures of 1200, 1300, and 1400 C. CVD SiC was also evaluated as a baseline comparison. Weight change measurements, X-ray diffraction analyses, surface and cross-sectional SEM and EDS were performed. These results will be compared with tests ran in static air at temperatures of 1327, 1627, and 1927 C. Oxidation comparisons will also be made to the study by Tripp. A small number of high pressure burner rig (HPBR) results at 1100 and 1300 C will also be discussed. Specific weight changes at all three temperatures along with the SIC results are shown. SiC weight change is negligible at such short duration times. HB2 + SiC (HS) performed the best out of all the tested UHTCS for all exposure temperatures. ZrB2 + Sic (ZS) results indicate a slightly lower oxidation rate than that of ZrBl + SiC + C (ZCS) at 1200 and 1400 C, but a clear distinction can not be made based on the limited number of tested samples. Scanning electron micrographs of the cross-sections of all the UHTCs were evaluated. A representative area for HS is presented at 1400 C for 26 hours which was the composition with the least amount of oxidation. A continuous SiO2 scale is present in the outer most edge of the surface. An image of ZCS is presented at 1400 C for 10 hours, which shows the most degradation of all the compositions studied. Here, the oxide surface is a mixture of ZrSiO4, ZrO2 and SO2.

Nguyen, QuynhGiao N.↗
NASA NTRS2003

Process for Nitrogen Oxide Waste Conversion to Fertilizer

The present invention describes a process for converting vapor streams from sources containing at least one nitrogen-containing oxidizing agent therein to a liquid fertilizer composition comprising the steps of: a) directing a vapor stream containing at least one nitrogen-containing oxidizing agent to a first contact zone; b) contacting said vapor stream with water to form nitrogen oxide(s) from said at least one nitrogen-containing oxidizing agent; c) directing said acid(s) as a second stream to a second contact zone; d) exposing said second stream to hydrogen peroxide which is present within said second contact zone in a relative amount of at least 0.1% by weight of said second stream within said second contact zone to convert at least some of any nitrogen oxide species or ions other than in the nitrate form present within said second stream to nitrate ion; e) sampling said stream within said second contact zone to determine the relative amount of hydrogen peroxide within said second contact zone; f) adding hydrogen peroxide to said second contact zone when a level of hydrogen peroxide less than 0.1 % by weight in said second stream is determined by said sampling; g) adding a solution comprising potassium hydroxide to said second stream to maintain a pH between 6.0 and 11.0 within said second stream within said second contact zone to form a solution of potassium nitrate; and h) removing said solution of potassium nitrate from said second contact zone.

Lueck, Dale E.↗
NASA NTRS2003

Development of Oxidation Protection Coatings for Gamma Titanium Aluminide Alloys

Metallic material systems play a key role in meeting the stringent weight and durability requirements for reusable launch vehicle (RLV) airframe hot structures. Gamma titanium aluminides (gamma-TiAl) have been identified as high-payoff materials for high-temperature applications. The low density and good elevated temperature mechanical properties of gamma-TiAl alloys make them attractive candidates for durable lightweight hot structure and thermal protection systems at temperatures as high as 871 C. However, oxidation significantly degrades gamma-TiAl alloys under the high-temperature service conditions associated with the RLV operating environment. This paper discusses ongoing efforts at NASA Langley Research Center to develop durable ultrathin coatings for protecting gamma-TiAl alloys from high-temperature oxidation environments. In addition to offering oxidation protection, these multifunctional coatings are being engineered to provide thermal control features to help minimize heat input into the hot structures. This paper describes the coating development effort and discusses the effects of long-term high-temperature exposures on the microstructure of coated and uncoated gamma-TiAl alloys. The alloy of primary consideration was the Plansee alloy gamma-Met, but limited studies of the newer alloy gamma-Met-PX were also included. The oxidation behavior of the uncoated materials was evaluated over the temperature range of 704 C to 871 C. Sol-gel-based coatings were applied to the gamma-TiAl samples by dipping and spraying, and the performance evaluated at 871 C. Results showed that the coatings improve the oxidation resistance, but that further development is necessary.

Wallace, T. A.↗
NASA NTRS1998

Abundances of ethylene oxide and acetaldehyde in hot molecular cloud cores

We have searched for millimetre-wave line emission from ethylene oxide (c-C2H4O) and its structural isomer acetaldehyde (CH3CHO) in 11 molecular clouds using SEST. Ethylene oxide and acetaldehyde were detected through multiple lines in the hot cores NGC 6334F, G327.3-0.6, G31.41+0.31, and G34.3+0.2. Acetaldehyde was also detected towards G10.47+0.03, G322.2+0.6, and Orion 3'N, and one ethylene oxide line was tentatively detected in G10.47+0.03. Column densities and rotational excitation temperatures were derived using a procedure which fits the observed line intensifies by finding the minimum chi 2-value. The resulting rotational excitation temperatures of ethylene oxide and acetaldehyde are in the range 16-38 K, indicating that these species are excited in the outer, cooler parts of the hot cores or that the excitation is significantly subthermal. For an assumed source size of 20", the deduced column densities are (0.6-1)x10(14) cm-2 for ethylene oxide and (2-5)x10(14) cm-2 for acetaldehyde. The fractional abundances with respect to H2 are X[c-C2H4O]=(2-6)xl0(-10), and X[CH3CHO]=(0.8-3)x10(-9). The ratio X[CH3CHO]/X[c-C2H4O] varies between 2.6 (NGC 6334F) and 8.5 (G327.3-0.6). We also detected and analysed multiple transitions of CH3OH, CH3OCH3, C2H5OH, and HCOOH. The chemical, and possibly evolutionary, states of NGC 6334F, G327.3-0.6, G31.41+0.31, and G34.3+0.2 seem to be very similar.

Non-NASA Center↗
NASA NTRS2004

Volatility of Common Protective Oxides in High-Temperature Water Vapor: Current Understanding and Unanswered Questions

Many structural materials rely on the formation of chromia, silica or alumina as a protective layer when exposed in high temperature oxidizing environments. The presence of these oxide layers provides a protective diffusion barrier which slows down further oxidation. In atmospheres containing water vapor, however, reactions to form volatile hydroxide species occur which remove the surface oxide, thus, lowering the protective capability of the oxide scale. This paper summarizes the current understanding of volatility of chromia, silica and alumina in water vapor containing combustion environments. In addition unanswered questions in each system are discussed. Th current paper represents an update on the considerable information learned in the past five years for these systems.

Opila, Elizabeth J.↗
NASA NTRS2000

Oxidant damage during and after spaceflight

The objectives of this study were to assess oxidant damage during and after spaceflight and to compare the results against bed rest with 6 degrees head-down tilt. We measured the urinary excretion of the F(2) isoprostane, 8-iso-prostaglandin (PG) F(2alpha), and 8-oxo-7,8-dihydro-2 deoxyguanosine (8-OH DG) before, during, and after long-duration spaceflight (4-9 mo) on the Russian space station MIR, short-duration spaceflight on the shuttle, and 17 days of bed rest. Sample collections on MIR were obtained between 88 and 186 days in orbit. 8-iso-PGF(2alpha) and 8-OH DG are markers for oxidative damage to membrane lipids and DNA, respectively. Data are mean +/- SE. On MIR, isoprostane levels were decreased inflight (96. 9 +/- 11.6 vs. 76.7 +/- 14.9 ng. kg(-1). day(-1), P < 0.05, n = 6) due to decreased dietary intake secondary to impaired thermoregulation. Isoprostane excretion was increased postflight (245.7 +/- 55.8 ng. kg(-1). day(-1), P < 0.01). 8-OH DG excretion was unchanged with spaceflight and increased postflight (269 +/- 84 vs 442 +/- 180 ng. kg(-1). day(-1), P < 0.05). On the shuttle, 8-OH DG excretion was unchanged in- and postflight, but 8-iso-PGF(2alpha) excretion was decreased inflight (15.6 +/- 4.3 vs 8.0 +/- 2.7 ng. kg(-1). day(-1), P < 0.05). No changes were found with bed rest, but 8-iso-PGF(2alpha) was increased during the recovery phase (48.9 +/- 23.0 vs 65.4 +/- 28.3 ng. kg(-1). day(-1), P < 0.05). The changes in isoprostane production were attributed to decreased production of oxygen radicals from the electron transport chain due to the reduced energy intake inflight. The postflight increases in the excretion of the products of oxidative damage were attributed to a combination of an increase in metabolic activity and the loss of some host antioxidant defenses inflight. We conclude that 1) oxidative damage was decreased inflight, and 2) oxidative damage was increased postflight.

Mir Project↗
NASA NTRS2003

Advanced Multi-Component Defect Cluster Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

The advantages of using ceramic thermal barrier coatings in gas turbine engine hot sections include increased fuel efficiency and improved engine reliability. However, current thermal barrier coatings will not have the low thermal conductivity and necessary sintering resistance under higher operating temperatures and thermal gradients required by future advanced ultra efficient and low emission aircraft engines. In this paper, a novel oxide defect cluster design approach is described for achieving low thermal conductivity and excellent thermal stability of the thermal barrier coating systems. This approach utilizes multi-component rare earth and other metal cluster oxide dopants that are incorporated in the zirconia-yttna based systems, thus significantly reducing coating thermal conductivity and sintering resistance by effectively promoting the formation of thermodynamically stable, essentially immobile defect clusters and/or nanoscale phases. The performance of selected plasma-sprayed cluster oxide thermal barrier coating systems has been evaluated. The advanced multi-component thermal barrier coating systems were found to have significantly lower initial and long-term thermal conductivities, and better high temperature stability. The effect of oxide cluster dopants on coating thermal conductivity, sintering resistance, oxide grain growth behavior and durability will be discussed.

Zhu, Dongming↗
NASA NTRS1990

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi- component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma- sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia-yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging fiom 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗
NASA NTRS1990

Advanced Multi-Component Defect Cluster Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

The advantages of using ceramic thermal barrier coatings in gas turbine engine hot sections include increased fuel efficiency and improved engine reliability. However, current thermal barrier coatings will not have the low thermal conductivity and necessary sintering resistance under higher operating temperatures and thermal gradients required by future advanced ultra-efficient and low-emission aircraft engines. In this paper, a novel oxide defect cluster design approach is described for achieving low thermal conductivity and excellent thermal stability of the thermal barrier coating systems. This approach utilizes multi-component rare earth and other metal cluster oxide dopants that are incorporated in the zirconia-yttria based systems, thus significantly reducing coating thermal conductivity and sintering resistance by effectively promoting the formation of thermodynamically stable, essentially immobile defect clusters and/or nanoscale phases. The performance of selected plasma-sprayed cluster oxide thermal barrier coating systems has been evaluated. The advanced multi-component thermal barrier coating systems were found to have significantly lower initial and long-term thermal conductivities, and better high temperature stability. The effect of oxide cluster dopants on coating thermal conductivity, sintering resistance, oxide grain growth behavior and durability will be discussed.

Zhu, Dongming↗
NASA NTRS2003

Universal Responses of Cyclic-Oxidation Models Studied

Oxidation is an important degradation process for materials operating in the high-temperature air or oxygen environments typical of jet turbine or rocket engines. Reaction of the combustion gases with the component material forms surface layer scales during these oxidative exposures. Typically, the instantaneous rate of reaction is inversely proportional to the existing scale thickness, giving rise to parabolic kinetics. However, more realistic applications entail periodic startup and shutdown. Some scale spallation may occur upon cooling, resulting in loss of the protective diffusion barrier provided by a fully intact scale. Upon reheating, the component will experience accelerated oxidation due to this spallation. Cyclic-oxidation testing has, therefore, been a mainstay of characterization and performance ranking for high-temperature materials. Models simulate this process by calculating how a scale spalls upon cooling and regrows upon heating (refs. 1 to 3). Recently released NASA software (COSP for Windows) allows researchers to specify a uniform layer or discrete segments of spallation (ref. 4). Families of model curves exhibit consistent regularity and trends with input parameters, and characteristic features have been empirically described in terms of these parameters. Although much insight has been gained from experimental and model curves, no equation has been derived that can describe this behavior explicitly as functions of the key oxidation parameters.

Smialek, James L.↗
NASA NTRS2003

High-Temperature Oxidation-Resistant and Low Coefficient of Thermal Expansion NiAl-Base Bond Coat Developed for a Turbine Blade Application

Many critical gas turbine engine components are currently made from Ni-base superalloys that are coated with a thermal barrier coating (TBC). The TBC consists of a ZrO2-based top coat and a bond coat that is used to enhance the bonding between the superalloy substrate and the top coat. MCrAlY alloys (CoCrAlY and NiCrAlY) are currently used as bond coats and are chosen for their very good oxidation resistance. TBC life is frequently limited by the oxidation resistance of the bond coat, along with a thermal expansion mismatch between the metallic bond coat and the ceramic top coat. The aim of this investigation at the NASA Glenn Research Center was to develop a new longer life, higher temperature bond coat by improving both the oxidation resistance and the thermal expansion characteristics of the bond coat. Nickel aluminide (NiAl) has excellent high-temperature oxidation resistance and can sustain a protective Al2O3 scale to longer times and higher temperatures in comparison to MCrAlY alloys. Cryomilling of NiAl results in aluminum nitride (AlN) formation that reduces the coefficient of thermal expansion (CTE) of the alloy and enhances creep strength. Thus, additions of cryomilled NiAl-AlN to CoCrAlY were examined as a potential bond coat. In this work, the composite alloy was investigated as a stand-alone substrate to demonstrate its feasibility prior to actual use as a coating. About 85 percent of prealloyed NiAl and 15 percent of standard commercial CoCrAlY alloys were mixed and cryomilled in an attritor with stainless steel balls used as grinding media. The milling was carried out in the presence of liquid nitrogen. The milled powder was consolidated by hot extrusion or by hot isostatic pressing. From the consolidated material, oxidation coupons, four-point bend, CTE, and tensile specimens were machined. The CTE measurements were made between room temperature and 1000 C in an argon atmosphere. It is shown that the CTE of the NiAl-AlN-CoCrAlY composite bond coat is lower than that of the commercially used coating alloy 16-6. To examine the potential of NiAl-AlN-CoCrAlY as a bond coat, we subjected two samples to cyclic furnace testing. The furnace cycle consisted of 45 min at 1163 C (2125 F ) followed by 15 min of cooling out of the furnace. The current NASA baseline TBC is a NiCrAlY bond coat below the 7YSZ top coat. The average TBC life for this baseline coating on Ren N5 is 188 plus or minus 19 cycles. NiAl-AlN-CoCrAlY specimens coated with the same 7YSZ top coat were still intact even after 1000 cycles. Therefore, the NiAl-AlN-CoCrAlY as a bulk substrate material, exhibits more than 5 times the life of the current state-of-the-art material. The next step is to evaluate this material as a coating on the same superalloy substrate.

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