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NASA NTRS2004

Final Summary of Research Report to the National Aeronautics and Space Administration Cosmochemistry Program

The discovery of presolar grains in meteorites is one of the most exciting recent developments in meteoritics. Six types of presolar grain have been discovered: diamond, Sic, graphite, Si3N4, Al2O3 and MgAl2O4. These grains have been identified as presolar because their isotopic compositions are very different from those of Solar System materials. Comparison of their isotopic compositions with astronomical observations and theoretical models indicates most of the grains formed in the envelopes of highly evolved stars. They are, therefore, a new source of information with which to test astrophysical models of the evolution of these stars. In fact, because several elements can often be measured in the same grain, including elements that are not measurable spectroscopically in stars, the grain data provide some very stringent constraints for these models. Our primary goal is to create large, unbiased, multi-isotope databases of single presolar Sic, Si,N,, oxide and graphite grains in meteorites, as well as any new presolar grain types that are identified in the future. These will be used to: (i) test stellar and nucleosynthetic models, (ii) constrain the galactic chemical evolution (GCE) paths of the isotopes of Si, Ti, 0 and Mg, (iii) establish how many stellar sources contributed to the Solar System, (iv) constrain relative dust production rates of various stellar types and (v) assess how representative of galactic dust production the record in meteorites is. The primary tool for this project is a highly automated grain analysis system we have developed for the Carnegie 6f ion probe.

O'D.Alexander, Conel↗
NASA NTRS2003

Final Summary of Research Report to the National Aeronautics and Space Administration Cosmochemistry Program

The discovery of presolar grains in meteorites is one of the most exciting recent developments in meteoritics. Six types of presolar grain have been discovered: diamond, Sic, graphite, Si3N4, Al2O3 and MgAl2O4. These grains have been identified as presolar because their isotopic compositions are very different from those of Solar System materials. Comparison of their isotopic compositions with astronomical observations and theoretical models indicates most of the grains formed in the envelopes of highly evolved stars. They are, therefore, a new source of information with which to test astrophysical models of the evolution of these stars. In fact, because several elements can often be measured in the same grain, including elements that are not measurable spectroscopically in stars, the grain data provide some very stringent constraints for these models. Our primary goal is to create large, unbiased, multi-isotope databases of single presolar Sic, Si,N,, oxide and graphite grains in meteorites, as well as any new presolar grain types that are identified in the future. These will be used to: (i) test stellar and nucleosynthetic models, (ii) constrain the galactic chemical evolution (GCE) paths of the isotopes of Si, Ti, O and Mg, (iii) establish how many stellar sources contributed to the Solar System, (iv) constrain relative dust production rates of various stellar types and (v) assess how representative of galactic dust production the record in meteorites is. The primary tool for this project is a highly automated grain analysis system on the Carnegie 6f ion probe.

O'D. Alexander, Conel↗
NASA NTRS2004

Planetary Regolith Microstructure: An Unexpected Opposition Effect Result

The Opposition Effect (OE) is the non-linear increase in the intensity of light scattered from a surface as phase angle approaches 0 deg. It is seen in laboratory experiments and in remote sensing observations of planetary surfaces. Understanding the OE is a requirement to fitting photometric models which will produce meaningful results about regolith texture. Our previous laboratory studies are consistent with the hypothesis that the OE in particulate materials is due to two processes, Shadow Hiding (SHOE) and Coherent Backscattering (CBOE). SHOE arises because, as phase angle approaches zero, shadows cast by regolith grains on other grains become invisible to the observer. CBOE results from constructive interference between rays traveling the same path but in opposite directions. In this study we measured the angular scattering properties of 9 mixtures of Aluminum Oxide and Boron Carbide powders of the same particle diameter (25 microns). The reflectance of the materials ranged from 7% (pure B4C) to 91% (pure Al2O3). Along with the reflectance phase curve we measured the circular polarization ratio (CPR) - the ratio of the intensity of the light returned with the same helicity as the incident light to that with the opposite helicity. An increase in CPR with decreasing phase angle indicates increased multiple scattering and is consistent with CBOE (Hapke, 1993). Popular conceptions of CBOE (Belskaya et al, 2003) hold that materials of higher albedo would exhibit increased multiple scattering and that the contribution of CBOE to the OE would increase as albedo increases. Remarkably, we find the highest albedo samples did not have the strongest CBOE opposition peaks. Instead, the maximum CBOE contribution is observed in samples with reflectance between 15 and 40%.

Nelson, R. M.↗
NASA NTRS2004

Micro-XANES Measurements on Experimental Spinels and the Oxidation State of Vanadium in Spinel-Melt Pairs

Spinel can be a significant host phase for V as well as other transition metals such as Ni and Co. However, vanadium has multiple oxidation states V(2+), V(3+), V(4+) or V(5+) at oxygen fugacities relevant to natural systems. We do know that D(V) spinel/melt is correlated with V and TiO2 content and fO2, but the uncertainty of the oxidation state under the range of natural conditions has made elusive a thorough understanding of D(V) spinel/melt. For example, V(3+) is likely to be stable in spinels, based on exchange with Al in experiments in the CaO-MgO-Al2O3-SiO2 system. On the other hand, it has been argued that V(4+) will be stable across the range of natural oxygen fugacities in nature. In order to gain a better understanding of D(V) spinel/melt we have equilibrated spinel-melt pairs at controlled oxygen fugacities, between HM to NNO, where V is present in the spinel at natural levels (approx. 300 ppm V). These spinel-melt pairs were analyzed using micro-XANES at the Advanced Photon Source at Argonne National Laboratory. The new results will be used together with spinel compositional data (Ti, V content) and oxygen fugacity, to unravel the effects of these variables on D(V) spinel/melt.

Righter, K.↗
NASA NTRS2000

Remote query measurement of pressure, fluid-flow velocity, and humidity using magnetoelastic thick-film sensors

Free-standing magnetoelastic thick-film sensors have a characteristic resonant frequency that can be determined by monitoring the magnetic flux emitted from the sensor in response to a time varying magnetic field. This property allows the sensors to be monitored remotely without the use of direct physical connections, such as wires, enabling measurement of environmental parameters from within sealed, opaque containers. In this work, we report on application of magnetoelastic sensors to measurement of atmospheric pressure, fluid-flow velocity, temperature, and mass load. Mass loading effects are demonstrated by fabrication of a remote query humidity sensor, made by coating the magnetoelastic thick film with a thin layer of solgel deposited Al2O3 that reversibly changes mass in response to humidity. c2000 Elsevier Science S.A. All rights reserved.

NASA Discipline Life Sciences Technologies↗
NASA NTRS2001

Mid-infrared trace gas detection using continuous-wave difference frequency generation in periodically poled RbTiOAsO4

A tunable mid-infrared continuous-wave (cw) spectroscopic source in the 3.4-4.5 micrometers region is reported, based on difference frequency generation (DFG) in a quasi-phase-matched periodically poled RbTiOAsO4 (PPRTA) crystal. DFG power levels of 10 microW were generated at approximately 4 micrometers in a 20-mm long PPRTA crystal by mixing two cw single-frequency Ti:Al2O3 lasers operating near 713 nm and 871 nm, respectively, using a laser pump power of 300 mW. A quasi-phase-matched infrared wavelength-tuning bandwidth (FWHM) of ~ 12 cm-1 and a temperature tuning rate of 1.02 cm-1/degree C were achieved. Experimental details regarding the feasibility of trace gas detection based on absorption spectroscopy of CO2 in ambient air using this DFG radiation source are also described.

NASA Discipline Life Sciences Technologies↗
NASA NTRS1997

Geochemistry of approximately 1.9 Ga sedimentary rocks from northeastern Labrador, Canada

Fifty-eight rock chips from fifteen samples of sedimentary rocks from the Ramah Group (approximately 1.9 Ga) in northeastern Labrador, Canada, were analyzed for major and minor elements, including C and S, to elucidate weathering processes on the Earth's surface about 1.9 Ga ago. The samples come from the Rowsell Harbour, Reddick Bight, and Nullataktok Formations. Two rock series, graywackes-gray shales of the Rowsell Harbour, Reddick Bight and Nullataktok Formations, and black shales of the Nullataktok Formation, are distinguishable on the basis of lithology, mineralogy, and major and trace element chemistry. The black shales show lower concentrations than the graywackes-gray shales in TiO2 (0.3-0.7 wt% vs. 0.7-1.8 wt%), Al2O3 (9.5-20.1 wt% vs. 13.0-25.0 wt%), and sigma Fe (<1 wt% vs. 3.8-13.9 wt% as FeO). Contents of Zr, Th, U, Nb, Ce, Y, Rb, Y, Co, and Ni are also lower in the black shales. The source rocks for the Ramah Group sediments were probably Archean gneisses with compositions similar to those in Labrador and western Greenland. The major element chemistry of source rocks for the Ramah Group sedimentary rocks was estimated from the Al2O3/TiO2 ratios of the sedimentary rocks and the relationship between the major element contents (e.g., SiO2 wt%) and Al2O3/TiO2 ratios of the Archean gneisses. This approach is justified, because the Al/Ti ratios of shales generally retain their source rock values; however, the Zr/Al, Zr/Ti, and Cr/Ni ratios fractionate during the transport of sediments. The measured SiO2 contents of shales in the Ramah Group are generally higher than the estimated SiO2 contents of source rocks by approximately 5 wt%. This correction may also have to be applied when estimating average crustal compositions from shales. Two provenances were recognized for the Ramah Group sediments. Provenance I was comprised mostly of rocks of bimodal compositions, one with SiO2 contents approximately 45 wt% and the other approximately 65 wt%, and was the source for most sedimentary rocks of the Ramah Group, except for black shales of the Nullataktok Formation. The black shales were apparently derived from Provenance II that was comprised mostly of felsic rocks with SiO2 contents approximately 65 wt%. Comparing the compositions of the Ramah Group sedimentary rocks and their source rocks, we have recognized that several major elements, especially Ca and Mg, were lost almost entirely from the source rocks during weathering and sedimentation. Sodium and potassium were also leached almost entirely during the weathering of the source rocks. However, significant amounts of Na were added to the black shales and K to all the rock types during diagenesis and/or regional metamorphism. The intensity of weathering of source rocks for the Ramah Group sediments was much higher than that of typical Phanerozoic sediments, possibly because of a higher PCO2 in the Proterozoic atmosphere. Compared to the source rock values, the Fe3+/Ti ratios of many of the graywackes and gray shales of the Ramah Group are higher, the Fe2+/Ti ratios are lower, and the sigma Fe/Ti ratios are the same. Such characteristics of the Fe geochemistry indicate that these sedimentary rocks are comprised of soils formed by weathering of source rocks under an oxygen-rich atmosphere. The atmosphere about 1.9 Ga was, therefore, oxygen rich. Typical black shales of Phanerozoic age exhibit positive correlations between the organic C contents and the concentrations of S, U, and Mo, because these elements are enriched in oxygenated seawater and are removed from seawater by organic matter in sediments. However, such correlations are not found in the Ramah Group sediments. Black shales of the Ramah Group contain 1.7-2.8 wt% organic C, but are extremely depleted in sigma Fe (<1 wt% as FeO), S (<0.3 wt%), U (approximately l ppm), Mo (<5 ppm), Ni (<2 ppm), and Co (approximately 0 ppm). This lack of correlation, however, does not imply that the approximately 1.9 Ga atmosphere-ocean system was anoxic. Depletion of these elements from the Ramah Group sediments may have occurred during diagenesis.

Non-NASA Center↗
NASA NTRS1989

The Flin Flon paleosol and the composition of the atmosphere 1.8 BYBP

Within the 1800 to 1900 my old Flin Flon-Snow Lake greenstone belt, Amisk Group volcanics are overlain by Missi Group fluvial sediments. Several localities along the Missi-Amisk contact, the volcanics show evidence of subaerial weathering. Field relationships, mineralogical evidence, and chemical analyses confirm that this alteration zone is a paleosol. Pedogenic fabrics and mineralogy were somewhat obscured by greenschist-grade metamorphism associated with the Hudsonian orogeny (1750 my). This is especially true in the upper meter of the paleosol, where metamorphic paragonite and sericitic micas developed in a crenulated fabric. This metamorphism did not, however, obliterate the imprint of weathering on the Amisk volcanics. Features characteristic of well-drained modern soils are evident in the paleosol. Corestones of spheroidally weathered pillow lavas occur at depth within the paleosol (Cr horizon). The corestones decrease in size upward and eventually disappear into a hematite-rich horizon at the top of the paleosol. These macroscopic changes are accompanied by a decrease in CaO and MgO and by an increase in Al2O3, TiO2, and total iron toward the paleosol-Missi contact. Ferrous iron decreases upward toward the contact; FeO was apparently oxidized to ferric iron and retained within the paleosol during weathering. The oxidation and retention of iron within the Flin Flon paleosol indicates that PO2 was probably > or = 10(-2) P.A.L. at the time of weathering. The behavior of iron in the Flin Flon paleosol contrasts sharply with its behavior in the 2200 my Hekpoort paleosol, which is strongly depleted in iron. This difference suggests that a significant increase in the ratio of PO2/PCO2 in the atmosphere took place between 2200 and 1800 mybp.

Non-NASA Center↗
NASA NTRS2004

Discovery of Presolar Corundum (and SiC?) in an Interplanetary Dust Particle

This work is part of an ongoing investigation [1-3] of isotopically anomalous phases in interplanetary dust particles (IDPs) on a scale of 100 nm. Previously, such NanoSIMS studies have found sub-micrometer sized, isotopically distinct presolar grains in IDPs at higher abundances than in primitive meteorites [1-5], which demonstrates the unique and primitive nature of IDPs. Although not all presolar grains found so far in IDPs have been chemically or petrographically characterized, the majority appear to be silicate stardust. Conspicuously absent from the presolar grain inventory in IDPs have been other grain types, which are commonly found in primitive meteorites, such as SiC and corundum (Al2O3).

Stadermann, F. J.↗
NASA NTRS2005

Micro-XANES Measurements on Experimental Spinels and the Oxidation State of Vanadium in Coexisting Spinel and Silicate Melt

Spinel can be a significant host phase for V which has multiple oxidation states V(sup 2+), V(sup 3+), V(sup 4+) or V(sup 5+) at oxygen fugacities relevant to natural systems. The magnitude of D(V) spinel/melt is known to be a function of composition, temperature and fO2, but the uncertainty of the oxidation state under the range of natural conditions has made elusive a thorough understanding of D(V) spinel/melt. For example, V(sup 3+) is likely to be stable in spinels, based on exchange with Al in experiments in the CaO-MgO-Al2O3-SiO2 system. On the other hand, it has been argued that V(sup 4+) will be stable across the range of natural oxygen fugacities in nature. In order to build on our previous work in more oxidized systems, we have carried out experiments at relatively reducing conditions from the FMQ buffer to 2 log fO2 units below the IW buffer. These spinel-melt pairs, where V is present in the spinel at natural levels (approx. 300 ppm V), were analyzed using an electron microprobe at NASA-JSC and micro- XANES at the Advanced Photon Source at Argonne National Laboratory. The new results will be used together with previous results to understand the valence of V in spinel-melt systems across 12 orders of magnitude of oxygen fugacity, and with application to natural systems.

Righter, K.↗
NASA NTRS1997

Oxidation Resistance and Critical Sulfur Content of Single-Crystal Superalloys

The high-temperature components of a jet turbine engine are made from nickel-base superalloys. These components must be able to withstand high stresses, fatigue, and corrosive reactions with high-temperature gases. Such oxidation resistance is associated with slow-growing Al2O3 scales that remain adherent to superalloy components after many thermal cycles. Historically, good oxidation resistance has been obtained by coating these components with Ni-Cr-Al-Y coatings, where small additions of yttrium (Y) were necessary for scale adhesion. Subsequently, it was found that the Y aids scale adhesion by preventing sulfur from segregating to the scale metal interface and thus preventing the sulfur from weakening the oxide-metal bonds. Y is a difficult element to incorporate in single-crystal superalloy castings, but it was shown in early work at the NASA Lewis Research Center that good adhesion could be obtained for low-sulfur, uncoated, singlecrystal superalloys, without Y additions. Low sulfur contents for these uncoated superalloys were achieved in the laboratory by a high-temperature hydrogen annealing process. This process allows segregation and surface cleaning of sulfur monolayers in a reducing environment. Another approach is to remove sulfur from the alloy in the melting process. The present study was designed to establish a guideline for the minimum level of desulfurization needed to achieve maximum performance. Coupons of various thicknesses of the superalloy PWA 1480 were hydrogen annealed at various times (8 to 100 hr) and temperatures (1000 to 1300 C), resulting in coupons with sulfur contents ranging from about 0.05 to 5 ppm. Cyclic oxidation tests at 1100 C were then used to assess adhesion and spalling. The weight change of one set of 20-mil (0.5-mm) samples, annealed for 20 hr at 1000, 1100, 1200, and 1300 C, is shown in the following figure. Clearly, the effect of the annealing temperature is quite dramatic in that the higher temperatures produced scales that spalled very little, whereas the lower temperatures resulted in severe weight losses comparable to those for the as-received, unannealed sample.

Smialek, James L.↗
NASA NTRS2005

Materials Chemistry Issues in the Development of a Single-Crystal Solar/Thermal Refractive Secondary Concentrator

A translucent crystal concentrates and transmits energy to a heat exchanger, which in turn heats a propellant gas, working gas of a dynamic power system, or a thermopile. Materials are the limiting issue in such a system. Central is the durability of the crystal, which must maintain the required chemical, physical/optical, and mechanical properties as it is heated and cooled. This report summarizes available data to date on the materials issues with this system. We focus on the current leading candidate materials, which are sapphire (Al2O3) for higher temperatures and silica (SiO2) for lower temperatures. We use data from thermochemical calculations; laboratory coupon tests with silica and sapphire; and system tests with sapphire. The required chemical properties include low-vapor pressure and interfacial stability with supporting structural materials. Optical properties such as transmittance and index of refraction must be maintained. Thermomechanical stability is a major challenge for a large, single-crystal ceramic and has been discussed in another report. In addition to the crystal, other materials in the proposed system include refractory metals (Nb, Ta, Mo, W, and Re), carbon (C), and high-temperature ceramic insulation. The major issue here is low levels of oxygen, which lead to volatile refractory metal oxides and rapid consumption of the refractory metal. Interfacial reactions between the ceramic crystal and refractory metal are also discussed. Finally, high-temperature ceramic insulating materials are also likely to be used in this system. Outgassing is a major issue for these materials. The products of outgassing are typically reactive with the refractory metals and must be minimized.

Jacobson, Nathan S.↗
NASA NTRS2004

Research Report to the National Aeronautics and Space Administration Cosmochemistry Program

The discovery of presolar grains in meteorites is one of the most exciting recent developments in meteoritics. Six types of presolar grain have been discovered: diamond, Sic, graphite, Si3N4, Al2O3 and MgAl2O4 (NIITLER, 2003). These grains have been identified as presolar because their isotopic compositions are very different from those of Solar System materials. Comparison of their isotopic compositions with astronomical observations and theoretical models indicates that most of the grains formed in the envelopes of highly evolved stars. They are, therefore, a new source of information with which to test astrophysical models of the evolution of these stars. In fact, because several elements can often be measured in the same grain, including elements that are not measurable spectroscopically in stars, the grain data provide some very stringent constraints for these models. Our primary goal is to create large, unbiased, multi-isotope databases of single presolar Sic, Si3N4, oxide and graphite grains in meteorites, as well as any new presolar grain types that are identified in the future. These will be used to: (i) test stellar and nucleosynthetic models, (ii) constrain the galactic chemical evolution (GCE) paths of the isotopes of Si, Ti, O and Mg, (iii) establish how many stellar sources contributed to the Solar System, (iv) constrain relative dust production rates of various stellar types and (v) assess how representative of galactic dust production the record in meteorites is. The primary tool for this project is a highly automated grain analysis system on the Carnegie 6f ion probe. This proposal was part of a long-standing research effort that is still ongoing.

Alexander, Conel O'D.↗
NASA NTRS2005

Evolution of the Electron Yield Curves of Insulators as a Function of Impinging Electron Fluence and Energy

Electron emission and concomitant change accumulation near the surface of insulators in central to understanding spacecraft charging. We present a study of changes in electron emission yields as a result of internal charge build up due to electron dose. Evolution of total, backscattered and secondary yield results over a broad range of incident energies are presented for two representative insulators, Kapton(trademark) and Al2O3. Reliable yield curves for uncharged insulators are measured and quantifiable changes in yield are observed due to < 100 fC/sq mm fluences. We find excellent agreement with a phenomenological argument based on insulator charging predicted by the yield curve; this includes a decrease in the rate of change of the yield as incident energies approach the crossover energies and as accumulated internal charge reduces the landing energy to asymptotically approach a steady state surface charge and unity yield. We also find that the exponential decay of yield curves with fluence exhibit an energy dependent decay constant, alpha(E). Finally, we discuss physics based models for this energy dependence. To understand fluence and energy dependence of these charging processes requires knowledge of how charge is deposited within the insulator, the mechanisms for charge trapping and transport within the insulator, and how the profile of trapped charge affects the transport and emission of charges from insulators.

Sim, Alec↗
NASA NTRS2004

Increasing the Thermal Stability of Aluminum Titanate for Solid Oxide Fuel Cell Anodes

Solid-oxide fuel cells (SOFCs) show great potential as a power source for future space exploration missions. Because SOFCs operate at temperatures significantly higher than other types of fuel cells, they can reach overall efficiencies of up to 60% and are able to utilize fossil fuels. The SOFC team at GRC is leading NASA's effort to develop a solid oxide fuel cell with a power density high enough to be used for aeronautics and space applications, which is approximately ten times higher than ground transport targets. layers must be able to operate as a single unit at temperatures upwards of 900'C for at least 40,000 hours with less than ten percent degradation. One key challenge to meeting this goal arises from the thermal expansion mismatch between different layers. The amount a material expands upon heating is expressed by its coefficient of thermal expansion (CTE). If the CTEs of adjacent layers are substantially different, thermal stresses will arise during the cell's fabrication and operation. These stresses, accompanied by thermal cycling, can fracture and destroy the cell. While this is not an issue at the electrolyte-cathode interface, it is a major concern at the electrolyte-anode interface, especially in high power anode-supported systems. electrolyte are nearly identical. Conventionally, this has been accomplished by varying the composition of the anode to match the CTE of the yittria-stabilized zirconia (YSZ) electrolyte (approx.10.8x10(exp -6/degC). A Ni/YSZ composite is typically used as a base material for the anode due to its excellent electrochemical properties, but its CTE is about 13.4x10(exp -6/degC). One potential way to lower the CTE of this anode is to add a small percentage of polycrystalline Al2TiO5, with a CTE of 0.68x10(exp -6/degC, to the Ni/YSZ base. However, Al2TiO5 is thermally unstable and loses its effectiveness as it decomposes to Al2O3 and TiO2 between 750 C and 1280 C. be used as additives to increase the thermal stability of Al2TiO5 in SOFC operating conditions without adversely affecting the electrochemical properties of the SOFC anode. Three candidate materials were chosen through an extensive literature review: MgO, Fe2O3, and ZrTiO4. Although all three have been shown to prevent Al2TiO5 decomposition under various conditions, their effectiveness in the temperature range and atmosphere of the SOFC has not yet been evaluated. Several batches of Al2TiO5 with varying amounts of additives were prepared, exposed to reducing and oxidizing atmospheres at elevated temperatures, and the resulting decomposition of Al2TiO5 was measured. The most promising additives were further evaluated with the goal of ultimately preparing low CTE anodes that are chemically compatible to current systems. Adding minor constituents to stabilize Al2TiO5 could ultimately preserve its low CTE for the life of the fuel cell and improve the cell's long-term performance without a drop in anode conductivity. Further, these low CTE filler additions could allow the use of new sulfur tolerant anode materials, improving the viability of SOFCs for future aeronautics and space applications. Every SOFC consists of a cathode and an anode separated by an electrolyte, These three One way to avoid this problem is to design the cell such that the CTEs of the anode and The objective of this summer research project was to evaluate several materials that could

Bender, Jeffrey B.↗
NASA NTRS1999

Thermal Mechanical Stability of Single-Crystal-Oxide Refractive Concentrators Evaluated for High-Temperature Solar-Thermal Propulsion

Recently, refractive secondary solar concentrator systems were developed for solar thermal power and propulsion (ref. 1). Single-crystal oxides-such as yttria-stabilized zirconia (Y2O3-ZrO2), yttrium aluminum garnet (Y3Al5O12, or YAG), magnesium oxide (MgO), and sapphire (Al2O3)-are candidate refractive secondary concentrator materials. However, the refractive concentrator system will experience high-temperature thermal cycling in the solar thermal engine during the sun/shade transition of a space mission. The thermal mechanical reliability of these components in severe thermal environments is of great concern. Simulated mission tests are important for evaluating these candidate oxide materials under a variety of transient and steady-state heat flux conditions. In this research at the NASA Lewis Research Center, a controlled heat flux test approach was developed for investigating the thermal mechanical stability of the candidate oxide. This approach used a 3.0-kW continuous-wave (wavelength, 10.6 mm) carbon dioxide (CO2) laser (ref. 2). The CO2 laser is especially well-suited for single-crystal thermal shock tests because it can directly deliver well-characterized heat energy to the oxide surfaces. Since the oxides are opaque at the 10.6-mm wavelength of the laser beam, the light energy is absorbed at the surfaces rather than transmitting into the crystals, and thus generates the required temperature gradients within the specimens. The following figure is a schematic diagram of the test rig.

Jacobson, Nathan S.↗
NASA NTRS1999

10 000-hr Cyclic Oxidation Behavior of 68 High-Temperature Co-, Fe-, and Ni- Base Alloys Evaluated at 982 deg. C (1800 deg. F)

Power systems with operating temperatures in the range of 815 to 982 C (1500 to 1800 F) frequently require alloys that can operate for long times at these temperatures. A critical requirement is that these alloys have adequate oxidation resistance. The alloys used in these power systems require thousands of hours of operating life with intermittent shutdown to room temperature. Intermittent power plant shutdowns, however, offer the possibility that the protective scale will tend to spall (i.e., crack and flake off) upon cooling, increasing the rate of oxidative attack in subsequent heating cycles. Thus, it is critical that candidate alloys be evaluated for cyclic oxidation behavior. It was determined that exposing test alloys to ten 1000-hr cycles in static air at 982 10 000-hr Cyclic Oxidation Behavior of 68 High-Temperature Co-, Fe-, and Ni-Base Alloys Evaluated at 982 C (1800 F) could give a reasonable simulation of long-time power plant operation. Iron- (Fe-), nickel- (Ni-), and cobalt- (Co-) based high-temperature alloys with sufficient chromium (Cr) and/or aluminum (Al) content can exhibit excellent oxidation resistance. The protective oxides formed by these classes of alloys are typically Cr2O3 and/or Al2O3, and are usually influenced by their Cr, or Cr and Al, content. Sixty-eight Co-, Fe-, and Ni-base high-temperature alloys, typical of those used at this temperature or higher, were used in this study. At the NASA Lewis Research Center, the alloys were tested and compared on the basis of their weight change as a function of time, x-ray diffraction of the protective scale composition, and the physical appearance of the exposed samples. Although final appearance and x-ray diffraction of the final scale products were two factors used to evaluate the oxidation resistance of each alloy, the main criterion was the oxidation kinetics inferred from the specific weight change versus time data. These data indicated a range of oxidation behavior including parabolic (typical of isothermal oxidation), paralinear, linear, and mixed-linear kinetics.

Barrett, Charles A.↗
NASA NTRS2000

Erosion Coatings for High-Temperature Polymer Composites: A Collaborative Project With Allison Advanced Development Company

The advantages of replacing metals in aircraft turbine engines with high-temperature polymer matrix composites (PMC's) include weight savings accompanied by strength improvements, reduced part count, and lower manufacturing costs. Successfully integrating high-temperature PMC's into turbine engines requires several long-term characteristics. Resistance to surface erosion is one rarely reported property of PMC's in engine applications because PMC's are generally softer than metals and their erosion resistance suffers. Airflow rates in stationary turbine engine components typically exceed 2.3 kg/sec at elevated temperatures and pressures. In engine applications, as shown in the following photos, the survivability of PMC components is clearly a concern, especially when engine and component life-cycle requirements become longer. Although very few publications regarding the performance of erosion coatings on PMC's are available particularly in high-temperature applications the use of erosion-resistant coatings to significantly reduce wear on metallic substrates is well documented. In this study initiated by the NASA Glenn Research Center at Lewis Field, a low-cost (less than $140/kg) graphite-fiber-reinforced T650 35/PMR 15 sheet-molding compound was investigated with various coatings. This sheet-molding compound has been compression molded into many structurally complicated components, such as shrouds for gas turbine inlet housings and gearboxes. Erosion coatings developed for PMC s in this study consisted of a two-layered system: a bondcoat sprayed onto a cleaned PMC surface, followed by an erosion-resistant, hard topcoat sprayed onto the bondcoat as shown in following photomicrograph. Six erosion coating systems were evaluated for their ability to withstand harsh thermal cycles, erosion resistance (ASTM G76 83 "Standard Practice for Conducting Erosion Tests by Solid Particle Impingement Using Gas Jets") using Al2O3, and adhesion to the graphite fiber polyimide composite (ASTM D 4541 95 "Pull Off Strength of Coatings"). Glenn and Allison Advanced Development Company collaborated to optimize erosion coatings for gas turbine fan and compressor applications. All the coating systems survived aggressive thermal cycling without spalling. During erosion tests (see the final photo), the most promising coating systems tested had Cr3C2-NiCr and WC-Co as the hard topcoats. In all cases, these coating systems performed significantly better than that with a TiN hard topcoat. When material depth (thickness) loss is considered, the Cr3C2-NiCr and WC-Co coating systems provided, on average, an erosion resistance 8.5 times greater than that for the uncoated PMR 15/T650 35 composite. Similarly, Cr3C2-NiCr and WC-Co coating systems adhered to the PMC substrate during tensile tests significantly better than systems containing a TiN topcoat. Differences in topcoats of Cr3C2-NiCr and WC-Co were determined by considering issues such as cost and environmental impact. The preferred erosion-resistant coating system for PMR 15/T650 35 has WC-Co as the hard topcoat. This system provides the following benefits in comparison to the coating system with Cr3C2-NiCr topcoat: lower powder material cost (15 to 20 percent), environmentally friendly materials (Cr3C2-NiCr is hazardous), and higher deposition yield (10 to 15 percent), which results in less waste.

Sutter, James K.↗