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All sourcesNASA NTRSDOE OSTI
NASA NTRS2002

Oxidation Behavior of GRCop-84 Copper Alloy Assessed

NASA's goal of safe, affordable space transportation calls for increased reliability and lifetimes of launch vehicles, and significant reductions of launch costs. The areas targeted for enhanced performance in the next generation of reusable launch vehicles include combustion chambers and nozzle ramps; therefore, the search is on for suitable liner materials for these components. GRCop-84 (Cu-8Cr-4Nb), an advanced copper alloy developed at the NASA Glenn Research Center in conjunction with Case Western Reserve University, is a candidate. The current liner of the Space Shuttle Main Engine is another copper alloy, NARloy-Z (Cu-3Ag-0.1Zr). It provides a benchmark against which to compare the properties of candidate successors. The thermomechanical properties of GRCop-84 have been shown to be superior, and its physical properties comparable, to those of NARloy-Z. However, environmental durability issues control longevity in this application: because copper oxide scales are not highly protective, most copper alloys are quickly consumed in oxygen environments at elevated temperatures. In consequence, NARloy-Z and most other copper alloys are prone to blanching, a degradation process that occurs through cycles of oxidation-reduction as the oxide is repeatedly formed and removed because of microscale fluctuations in the oxygen-hydrogen fuel systems of rocket engines. The Space Shuttle Main Engine lining typically degraded by blanching-induced hot spots that lead to surface roughening, pore formation, and coolant leakage. Therefore, resistance to oxidation and blanching are key requirements for second-generation reusable launch vehicle liners. The rocket engine ambient includes H2 (fuel) and H2O (combustion product) and is, hence, under reduced oxygen partial pressures. Accordingly, our studies were expanded to include oxygen partial pressures as low as 322 parts per million (ppm) at the temperatures likely to be experienced in service. A comparison of 10-hr weight gains of GRCop-84, NARloy-Z, and pure copper in 0.032, 2.2, and 100 percent oxygen from 550 to 750 C is shown. In 2.2 vol% and higher oxygen content, GRCop-84 oxidation was slower than that of NARloy-Z or Cu, but that advantage was lost or diminished in 322-ppm O2. Over longer (50-hr) exposures in 1.0 atm O2, however, the advantage of GRCop-84 increased significantly, its oxidation rate becoming approximately 10 times slower than those of Cu and NARloy-Z from 500 to 700 C. Weight gains were moderate and the kinetics parabolic for all three materials in 2.2 vol% and higher oxygen content; however, in 322-ppm O2, the scales were nonprotective below about 650 C, as reflected in linear kinetics and large weight gains. The superior oxidation resistance of GRCop-84 is likely related to the kinetics of extra oxygen consumption to form the additional oxides of Cr and Nb detected beneath the GRCop-84 oxide layer. While we continue to evaluate the blanching resistance of GRCop-84 in other tests, these oxidation results indicate that GRCop-84 is suitable as a reusable launch vehicle liner, and in applications where it is desired to use a copper alloy but without the risk of oxidative failure. Three bar charts comparing overall specific weight gains by each of the three materials studied. The top chart is for oxidation in 1.0 atm of oxygen, the middle is for 2.2% oxygen (balance argon), and the bottom is for 0.0322% oxygen. GRCop-84 outperforms the other two materials, showing the least weight gain in nearly all cases.

Thomas-Ogbuji, Linus U.↗
NASA NTRS1985

Particle size distributions of several commonly used seeding aerosols

During the course of experimentation, no solid particle powder could be found which produced an aerosol with a narrow particle size distribution when fluidization was the only flow process used in producing the aerosol. The complication of adding particle size fractionation processes to the aerosol generation effort appears to be avoidable. In this regard, a simple sonic orifice is found to be effective in reducing the percentage of agglomerates in the several metal oxide powders tested. Marginally beneficial results are obtained for a 0.5/99.5 percent by weight mixture of the flow agent and metal oxide powder. However, agglomeration is observed to be enhanced when the flow agent percentage is increased to 5 percent. Liquid atomization using the Collison nebulizer as well as a version of the Laskin nozzle resulted in polydispersed aerosols with particle size distributions heavily weighted by the small particle end of the size spectrum. The aerosol particle size distributions produced by the vaporization/condensation seeder are closer to the ideal monodispersed aerosol than any of the other aerosols tested. In addition, this seeding approach affords a measure of control over particle size and particle production rate.

Crosswy, F. L.↗
NASA NTRS2004

Characterization of an Ultra-High Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment generated by an oxy-acetylene torch. The composite was prepared from a carbon fiber perform using ceramic particulates and a pre-cerns about microcracking due to thermal expansion mismatch between the matrix and the carbon fiber reinforcements, and about the oxidation resistance of the HfB2-SiC coating layer and the composite constituents. However, positive performance in the torch test warrants further study of this concept.

Levine, Stanley R.↗
NASA NTRS2004

Facility Activation and Characterization for IPD Oxidizer Turbopump Cold-Flow Testing at NASA Stennis Space Center

The Integrated Powerhead Demonstrator (IPD) is a 250K lbf (1.1 MN) thrust cryogenic hydrogen/oxygen engine technology demonstrator that utilizes a full flow staged combustion engine cycle. The Integrated Powerhead Demonstrator (IPD) is part of NASA's Next Generation Launch Technology (NGLT) program, which seeks to provide safe, dependable, cost-cutting technologies for future space launch systems. The project also is part of the Department of Defense's Integrated High Payoff Rocket Propulsion Technology (IHPRPT) program, which seeks to increase the performance and capability of today s state-of-the-art rocket propulsion systems while decreasing costs associated with military and commercial access to space. The primary industry participants include Boeing-Rocketdyne and GenCorp Aerojet. The intended full flow engine cycle is a key component in achieving all of the aforementioned goals. The IPD Program achieved a major milestone with the successful completion of the IPD Oxidizer Turbopump (OTP) cold-flow test project at the NASA John C. Stennis Space Center (SSC) E-1 test facility in November 2001. A total of 11 IPD OTP cold-flow tests were completed. Following an overview of the NASA SSC E-1 test facility, this paper addresses the facility aspects pertaining to the activation and the cold-flow testing of the IPD OTP. In addition, some of the facility challenges encountered during the test project are addressed.

Sass, J. P.↗
NASA NTRS2003

Characterization of a Ultra-high Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Levine, Stanley R.↗
NASA NTRS2011

The J-2X Oxidizer Turbopump - Design, Development, and Test

Pratt and Whitney Rocketdyne (PWR), a NASA subcontractor, is executing the Design, Development, Test, and Evaluation (DDT&E) of a liquid oxygen, liquid hydrogen two hundred ninety-four thousand pound thrust rocket engine initially intended for the Upper Stage (US) and Earth Departure Stage (EDS) of the Constellation Program Ares-I Crew Launch Vehicle (CLV). A key element of the design approach was to base the new J-2X engine on the heritage J-2S engine which was a design upgrade of the flight proven J-2 engine used to put American astronauts on the moon. This paper will discuss the design trades and analyses performed to achieve the required uprated Oxidizer Turbopump performance; structural margins and rotordynamic margins; incorporate updated materials and fabrication capability; and reflect lessons learned from legacy and existing Liquid Rocket Propulsion Engine turbomachinery. These engineering design, analysis, fabrication and assembly activities support the Oxidizer Turbopump readiness for J-2X engine test in 2011.

Brozowski, Laura A.↗
NASA NTRS1978

Adhesive/cohesive strength of a ZrO2.1-2 w/o Y2O3/NiCrAIY thermal barrier coating

The room temperature adhesive/cohesive strength of a 0.05 cm thick ZrO2.12w/oY2O3/0.013 cm thick NiCrAlY thermal barrier coating system (TBC) was investigated. The weakest link was the oxide/NiCrAlY interface region with a strength of 6.2 MN/sq m. The fracture was about half cohesive oxide failure, half oxide/NiCrAlY adhesive failure and 1 percent cohesive NiCrAlY failure. The TBC failed in a similar manner in 950 C tensile and compression tests. The oxide stripped from the TBC had a cohesive strength of 24.6 MN/sq m. The NiCrAlY had a cohesive strength of 25.1 MN/sq m. The NiCrAlY and oxide failed primarily at interparticle boundaries.

Levine, S. R.↗
NASA NTRS1975

Study of the thermal degradation mechanism of a composite propellant

The current experimental program was designed to systematically investigate the role of the oxidizer in the thermal degradation process of composite propellants. The scanning electron microscope (SEM) was used to examine the failure sites in thermally degraded propellant samples. The formulation variables tested were oxidizer purity, oxidizer particle size, and oxidizer to binder bonding agent. The binder, a saturated hydrocarbon, was kept constant throughout the experiments. The oxidizers were: AP, chlorate-doped AP, arsenate-doped AP, and phosphate-doped AP. The oxidizer particle size distribution was 60% of the large fraction and 40% of the small fraction. The bonding agent, when present, was used at the 0.15% level. The data showed that both the oxidizer purity and particle size had an important affect on the thermal degradation process. The affect of the oxidizer particle size was more noticeable at the higher temperature and stress levels. An examination of the failure site, by SEM, of propellants subject to these latter conditions indicated that the fracturing of the large oxidizer particles led to the propellant cracking.

Schmidt, W. G.↗
DOE OSTI2025

Testing piezoelectric sensors in a nuclear reactor environment

Several Department of Energy Office of Nuclear Energy (DOE-NE) programs, such as the Fuel Cycle Research and Development (FCRD), Advanced Reactor Concepts (ARC), Light Water Reactor Sustainability, and Next Generation Nuclear Power Plants (NGNP), are investigating new fuels, materials, and inspection paradigms for advanced and existing reactors. A key objective of such programs is to understand the performance of these fuels and materials during irradiation. In DOE-NE’s FCRD program, ultrasonic based technology was identified as a key approach that should be pursued to obtain the high-fidelity, high-accuracy data required to characterize the behavior and performance of new candidate fuels and structural materials during irradiation testing. The radiation, high temperatures, and pressure can limit the available tools and characterization methods. In this work piezoelectric transducers capable of making these measurements are developed. Specifically, three piezoelectric sensors (Bismuth Titanate, Aluminum Nitride, and Zinc Oxide) are tested in the Massachusetts Institute of Technology Research reactor to a fast neutron fluence of 8.65x1020 nf/cm2. It is demonstrated that Bismuth Titanate is capable of transduction up to 5 x1020 nf/cm2, Zinc Oxide is capable of transduction up to at least 6.27 x1020 nf/cm2 , and Aluminum Nitride is capable of transduction up to at least 8.65x x1020 nf/cm2.

T. Reinhardt, Brian↗
NASA NTRS1996

Cryogenic Brush Seal Test Results

Brush seals are compliant, contact seals that have long-life, low-leakage characteristics desirable for use in rocket engine turbopumps. 50.8-mm (2.0 inch) diameter brush seals with a nominal initial radial interference of 0.127-mm (0.005 inch) were tested in liquid nitrogen at shaft speeds up to 35,000 rpm and differential pressure loads up to 1.21 MPa (175 psi) per brush. The measured leakage rate of a single brush was 2-3 times less than that measured for a 12-tooth, 0.127-mm (0.005 inch) radial clearance labyrinth seal used as a baseline. Stage effects were studied and it was found that two brush seals with a large separation distance leaked less than two brushes tightly packed together. The maximum measured groove depth on the Inconel 718 rotor was 25.4 (mu)m (0.001 inch) after 4.31 hours of shaft rotation. The Haynes-25 bristles wore approximately 25.4-76.2 (mu)m (0.001-0.003 inch) under the same conditions. Three seal runner coatings, chromium carbide, Teflon impregnated chromium, and zirconium oxide, were tested in liquid hydrogen at 35,000 and 65,000 rpm with separate 50.8 mm diameter brush seals made of Haynes-25 bristles and having a nominal initial radial interference of 129 rpm. Two bare Inconel-718 rotors were also tested as a baseline. The test results revealed significant differences between the wear characteristics of the uncoated and coated seal runners. At both speeds the brush seal with the bare Inconel-718 seal runner exhibited significant bristle wear with excessive material transferring to the runner surface. In contrast, the coated seal runners inhibited the transfer and deposit of bristle material. The chromium carbide coating showed only small quantities of bristle material transferring to its surface. The Teflon impregnated chromium coating also inhibited material transfer and provided some lubrication. This coating, however, is self-sacrificing. The Teflon remained present on the low speed runner, but it was completely removed from the high speed brush seal, which was tested considerably longer. The tests of the Teflon coating revealed the importance of using a lubricating and low friction coating for brush seals to reduce bristle and seal runner wear. The zirconium oxide coating exhibited the greatest amount of coating wear, while the brushes incurred only slight wear. Further testing of ceramics is recommended before making a final judgement on the viability of ceramic coatings for brush seals because of the contrast between the results reported by Carlile and the results presented herein. Strictly based on the results presented hereinabove, the chromium carbide and Teflon impregnated chromium coatings were considered preferable to the uncoated Inconel-718 and zirconium oxide coatings because of their good wear resistance and characteristics to inhibit bristle material wear and transfer to the seal runner.

Proctor, Margaret P.↗
NASA NTRS2014

Simultaneous Laser-induced Fluorescence of Nitric Oxide and Atomic Oxygen in the Hypersonic Materials Environment Test System Arcjet Facility

Simultaneous nitric oxide (NO) and atomic oxygen (O) laser induced fluorescence (LIF) experiments were performed in the Hypersonic Materials Environmental Test System (HYMETS) facility at the NASA Langley Research Center. The data serves as an experimental database for validation for chemical and thermal nonequilibrium models used in hypersonic flows. Measurements were taken over a wide range of stagnation enthalpies (6.7 - 18.5 MJ/kg) using an Earth atmosphere simulant with a composition of 75% N2, 20% O2, and 5% Ar (by volume). These are the first simultaneous measurements of NO and O LIF to be reported in literature for the HYMETS facility. The maximum O LIF mean signal intensity was observed at a stagnation enthalpy of approximately 12 MJ/kg while the maximum NO LIF mean signal intensity was observed at a stagnation enthalpy of 6.7 MJ/kg. Experimental results were compared to simple fluorescence model that assumes equilibrium conditions in the plenum and frozen chemistry in the isentropic nozzle expansion (Mach 5). The equilibrium calculations were performed using CANTERA v2.1.1 with 16 species. The fluorescence model captured the correlation in mean O and NO LIF signal intensities over the entire range of stagnation enthalpies tested. Very weak correlations between single-shot O and NO LIF intensities were observed in the experiments at all of the stagnation enthalpy conditions.

Johansen, Craig↗
DOE OSTI2025

CO 2 Oxidative Ethane Dehydrogenation on CeO 2 /SiO 2 ‐Supported NiFe 3 Catalysts

CO 2 -assisted oxidative dehydrogenation of ethane is a sustainable alternative to steam cracking for ethylene production. In this study, a series of CeO 2 on SiO 2 supported NiFe 3 catalysts were synthesized by incipient wetness impregnation and tested for oxidative dehydrogenation performance. The CeO 2 /SiO 2 supported catalysts with high weight loading of CeO 2 (50%–75%) provided higher activity than the lower CeO 2 (0%–25%) loaded catalysts (with ethylene production rates of 0.62–0.98 µmol/g cat /s and 0.19–0.3 µmol/g cat /s, respectively) while maintaining high ethylene selectivity (43%–45%). In contrast, the NiFe 3 supported on only CeO 2 also exhibited high activity (ethylene production rate of 0.71 µmol/g cat /s), but the ethylene selectivity (16%) was greatly decreased compared to the mixed system. Temperature programmed reduction, X-ray diffraction, and Raman spectroscopy all indicate the creation of a solid solution of the Fe and Ni doped into the CeO 2 crystal structure in the catalysts with high CeO 2 loading/bulk CeO 2 support. Here, the high ethylene selectivity in the high CeO 2 loading catalysts indicates that the Fe is preferentially creating the solid solution, with the decrease in selectivity observed in the CeO 2 -only supported catalyst likely resulting from CeO 2 interacting directly with Ni, creating Ni-CeO X interfaces that are known active sites for the unwanted side reaction of dry reforming.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Non-catalytic gas phase NO oxidation in the presence of decane

In this study, experiments without a catalyst revealed that NO was oxidized in a diesel exhaust gas phase mixture due to the presence of n -C 10 H 22 (decane). This reaction was observed to occur following the low temperature oxidation catalyst test protocol (LTC-D) defined by U.S. DRIVE. The purpose of LTC-D conditions is to simulate an aftertreatment diesel combustion gas mixture in order to test candidate catalyst materials. 100% NO conversion was observed, without a catalyst, after beginning to react at 330 °C accompanied by consumption of decane. After experiments that isolated hydrocarbons, ethylene was also observed to facilitate NO oxidation to a lesser degree (>470 °C). Density functional theory (DFT) calculations were conducted to investigate thermodynamically-possible initiating elementary steps during n -C 10 H 22 consumption and NO oxidation. Two feasible intermediate radicals to oxidize NO to NO 2 are ·C 10 H 21 O 2 and ·HO

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2006

Space Shuttle Main Engine Low Pressure Oxidizer Turbo-Pump Inducer Dynamic Environment Characterization through Water Model and Hot-Fire Testing

The Low Pressure Oxidizer Turbopump (LPOTP) inducer on the Block II configuration Space Shuttle Main Engine (SSME) experienced blade leading edge ripples during hot firing. This undesirable condition led to a minor redesign of the inducer blades. This resulted in the need to evaluate the performance and the dynamic environment of the redesign, relative to the current configuration, as part of the design acceptance process. Sub-scale water model tests of the two inducer configurations were performed, with emphasis on the dynamic environment due to cavitation induced vibrations. Water model tests were performed over a wide range of inlet flow coefficient and pressure conditions, representative of the scaled operating envelope of the Block II SSME, both in flight and in ground hot-fire tests, including all power levels. The water test hardware, facility set-up, type and placement of instrumentation, the scope of the test program, specific test objectives, data evaluation process and water test results that characterize and compare the two SSME LPOTP inducers are discussed. In addition, dynamic characteristics of the two water models were compared to hot fire data from specially instrumented ground tests. In general, good agreement between the water model and hot fire data was found, which confirms the value of water model testing for dynamic characterization of rocket engine turbomachinery.

Patrick Arellano↗
DOE OSTI2023

Growth of titania and tin oxide from Ti 2 SnC via rapid thermal oxidation in air for lithium-ion battery application

Herein, we report the synthesis of TiO 2 –SnO 2 –C/carbide hybrid electrode materials for Li-ion batteries (LIBs) via two different methods of controlled oxidation of layered Ti 2 SnC. The material was partially oxidized in an open-air furnace (OAF) or using a rapid thermal annealing (RTA) approach to obtain the desired TiO 2 –SnO 2 –C/carbide hybrid material; the carbide phase encompassed both residual Ti 2 SnC and TiC as a reaction product. We tested the oxidized materials as an anode in a half cell to investigate their electrochemical performance in LIBs. Analysis of the various oxidation conditions indicated the highest initial lithiation capacity of 838 mAh/g at 100 mA/g for the sample oxidized in the OAF at 700°C for 1 h. Still, the delithiation capacity dropped to 427 mAh/g and faded over cycling. Long-term cycling demonstrated that the RTA sample treated at 800°C for 30 s was the most efficient, as it demonstrated a reversible capacity of around 270 mAh/g after 150 cycles, as well as a specific capacity of about 150 mAh/g under high cycling rate (2000 mA/g). Given the materials’ promising performance, this processing method could likely be applied to many other members of the MAX family, with a wide range of energy storage applications.

25 ENERGY STORAGE↗
NASA NTRS2001

Investigation into Spectroscopic Techniques for Thermal Barrier Coating Spall Detection

Spectroscopic methods are proposed for detection of thermal barrier coating (TBC) spallation from engine hot zone components. These methods include absorption and emission of airborne marker species originally embedded in the TBC bond coat. In this study, candidate marker materials for this application were evaluated. Thermochemical analysis of candidate marker materials combined with additional constraints such as toxicity and uniqueness to engine environment, provided a short list of four potential species: platinum, copper oxide, zinc oxide. and indium. The melting point of indium was considered to be too low for serious consideration. The other three candidate marker materials, platinum, copper oxide, and zinc oxide were placed in a high temperature furnace and emission and absorption properties were measured over a temperature range from 800-1400 C and a spectral range from 250 to 18000 nm. Platinum did not provide the desired response, likely due to the low vapor Pressure of the metallic species and the low absorption of the oxide species. It was also found, however. that platinum caused a broadening of the carbon dioxide absorption at 4300 nm. The nature of this effect is not known. Absorption and emission caused by sodium and potassium impurities in the platinum were found in the platinum tests. Zinc oxide did not provide the desired response, again, most likely due to the low vapor pressure of the metallic species and the low absorption of the oxide species. Copper oxide generated two strongly temperature dependent absorption peaks at 324.8 and 327.4 nm. The melting point of copper oxide was determined to be too low for serious consideration as marker material.

deGroot, Wim↗