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NASA NTRS1977

In situ oxidation studies on /001/ copper-nickel alloy thin films

High-resolution transmission electron microscopy studies are reported of (001)-oriented single crystalline thin films of Cu-3%Ni, Cu-4.6%Ni, and Cu-50%Ni alloy which were prepared by vapor deposition onto (001) NaCl substrates and subsequently annealed at around 1100 K and oxidized at 725 K at low oxygen partial pressure. At all alloy concentrations, Cu2O and NiO nucleated and grew independently without the formation of mixed oxides. The shape and growth rates of Cu2O nuclei were similar to rates found earlier. For low-nickel alloy concentrations, the NiO nuclei were larger and the number density of NiO was less than that of Cu-50%Ni films for which the shape and growth rates of NiO were identical to those for pure nickel films. Phenomena involving a reduced induction period, surface precipitation, and through-thickness growth are also described. The results are consistent with previously established oxidation mechanisms for pure copper and pure nickel films.

Heinemann, K.↗

NASA NTRS1978

The friction and wear properties of sputtered hard refractory compounds

The friction and wear properties of several refractory silicides, borides, and carbide coatings were examined. The coatings were applied to type 440C steel surfaces by radio-frequency sputtering. The friction and wear properties of the coatings were found to be related to stoichiometry and impurity content of the bulk coating as well as the degree of interfacial adherence between coating and substrate. Bulk coating stoichiometry could to large extent be controlled by the application of a negative bias voltage during deposition. Adherence was promoted by the formation of an oxidized layer at the interface. Deliberate preoxidizing of the 440C produced enhanced adherence for many compounds which is related to the formation of a mixed oxide transition region.

Brainard, W. A.↗

NASA NTRS2010

Oxidation Characterization of Hafnium-Based Ceramics Fabricated by Hot Pressing and Electric Field-Assisted Sintering

Ceramic borides, such as hafnium diboride (HfB2) and zirconium diboride (ZrB2), are members of a family of materials with extremely high melting temperatures referred to as Ultra High Temperature Ceramics (UHTCs). UHTCs constitute a class of promising materials for use in high temperature applications, such as sharp leading edges on future-generation hypersonic flight vehicles, because of their high melting points. The controlled development of microstructure has become important to the processing of UHTCs, with the prospect of improving their mechanical and thermal properties. The improved oxidation resistance of HfB2 has also become important if this material is to be successfully used at temperatures above 2000 C. Furthermore, the use of UHTCs on the leading edges of vehicles traveling at hypersonic speeds will mean exposure to a mixed oxidation environment comprised of both molecular and atomic oxygen. The current study has investigated the high-temperature oxidation behavior of HfB2-based materials in a pure O2 environment, as well as in environments containing different levels of dissociated oxygen (O/O2). Materials were processed by two techniques: conventional hot pressing (HP) and electric field-assisted sintering (FAS). Their oxidation behavior was evaluated in both a tube furnace at 1250 C for 3 hours and in a simulated re-entry environment in the Advanced Heating Facility (AHF) arcjet at NASA Ames Research Center, during a 10-minute exposure to a cold wall heat flux of 250W/sq cm and stagnation pressure of 0.1-0.2 atm. The microstructure of the different materials was characterized before and after oxidation using scanning electron microscopy (SEM).

Gasch, Matt↗

NASA NTRS1986

Corrosion of metals and alloys in sulfate melts at 750 C

The corrosion of Ni, Co, Ni-10Cr, Co-21Cr, and IN738 was studied at 750 C in the presence of molten sulfate mixtures (Na2SO4-Li2SO4 and Na2SO4-CoSO4) and in an atmosphere consisting of O2 + 0.12 percent SO2-SO3. The corrosion was observed to be similar for both Na2SO4-Li2SO4 and Na2SO4-CoSO4 melts. The corrosion of Ni and Co took place by the formation of a mixed oxide plus sulfide scale, very similar to the corrosion in SO2 or SO3 alone. The initial stage for the corrosion of Ni-10Cr involved the formation of a thick NiO + Ni3S2 duplex scale, and Cr sulfide was formed during the later stages. A pitting type of morphology was observed for both Co-21Cr and IN738. The pit was Cr sulfide at the beginning, and subsequently the sulfides oxidized to Cr2O3. A base-metal oxide layer was present above the pit, and this was observed to be formed very early in the corrosion process. A mechanism is proposed to explain this. In general, the formation of sulfides appears to be the primary mode of degradation in mixed sulfide melts.

Misra, A. K.↗

NASA NTRS1987

High-temperature oxidation/corrosion of iron-based superalloys

The oxidation and sulfidation of several novel iron-base superalloys were evaluated in high-temperature cyclic tests. The experimental austenitic alloys examined were modifications of NASAUT-4GA which were developed for Stirling-engine application. The weight gains and resulting surface scales were measured and analyzed. Mixed oxide scales were found to form on all specimens exposed above 871 C. The build-up of these scales led to a depletion of Mn and Cr in a zone adjacent to the oxides. In addition, the initial oxidation of the Fe-rich alloy was inhibited by a thin but tenacious Si layer which formed at the interface between oxides and the parent layer. Sulfidation tests using Na2SO4 coatings resulted in the formation of a protective spinel and alpha-Fe2O3 phases. Preferential attack of the carbide phase by hydrogen was not observed after 350 h at 871 C.

Lemkey, F. D.↗

NASA NTRS2007

High-Temperature Desulfurization of Heavy Fuel-Derived Reformate Gas Streams for SOFC Applications

Desulfurization of the hot reformate gas produced by catalytic partial oxidation or autothermal reforming of heavy fuels, such as JP-8 and jet fuels, is required prior to using the gas in a solid oxide fuel cell (SOFC). Development of suitable sorbent materials involves the identification of sorbents with favorable sulfidation equilibria, good kinetics, and high structural stability and regenerability at the SOFC operating temperatures (650 to 800 C). Over the last two decades, a major barrier to the development of regenerable desulfurization sorbents has been the gradual loss of sorbent performance in cyclic sulfidation and regeneration at such high temperatures. Mixed oxide compositions based on ceria were examined in this work as regenerable sorbents in simulated reformate gas mixtures and temperatures greater than 650 C. Regeneration was carried out with dilute oxygen streams. We have shown that under oxidative regeneration conditions, high regeneration space velocities (greater than 80,000 h(sup -1)) can be used to suppress sulfate formation and shorten the total time required for sorbent regeneration. A major finding of this work is that the surface of ceria and lanthanan sorbents can be sulfided and regenerated completely, independent of the underlying bulk sorbent. This is due to reversible adsorption of H2S on the surface of these sorbents even at temperatures as high as 800 C. La-rich cerium oxide formulations are excellent for application to regenerative H2S removal from reformate gas streams at 650 to 800 C. These results create new opportunities for compact sorber/regenerator reactor designs to meet the requirements of solid oxide fuel cell systems at any scale.

Flytzani-Stephanopoulos, Maria↗

NASA NTRS1991

Laser induced spark ignition of methane-oxygen mixtures

The use of laser-induced spark ignition in liquid-propellant rocket engines is investigated by studying the ignition of mixtures of methane and oxygen. Specific attention is given to minimum ignition energy, spark efficiency, the effect of ignition energy on flame kernels, the effect of laser wavelength, and comparisons with electrode-spark ignition. A pulsed frequency-doubled Nd:YAG laser is tested at atmospheric pressure and 296 K under both laminar-premixed and turbulent-incompletely-mixed conditions. Laser sparks of 10 and 40 mJ and an electrode spark of 6 mJ are measured for flame-kernel radius as a function of time with pulsed laser shadowgraphy. Initially, the flame-kernel size is similar to those predicted by the Taylor spherical-blast-wave model, and subsequent growth is characterized by rapid acceleration. The growth rate is significantly affected by the effect of incomplete fuel-oxidizer mixing.

Lee, T. W.↗

NASA NTRS1997

An Insidious Mode of Oxidative Degradation in a SiC-SiC Composite

The oxidative durability of a SiC-SiC composite with Hi-Nicalon fiber and BN interphase was investigated at 800 C (where pesting is known to occur in SiC-SiC composites) for exposure durations of up to 500 hours and in a variety of oxidant mixes and flow rates, ranging from quasi-stagnant room air, through slow flowing O2 containing 30-90% H2O, to the high-velocity flame of a burner rig. Degradation of the composite was determined from residual strength and fracture strain in post-exposure mechanical tests and correlated with microstructural evidence of damage to fiber and interphase. The severest degradation of composite behavior was found to occur in the bumer rig, and is shown to be connected with the high oxidant velocity and substantial moisture content, as well as a thin sublayer of carbon indicated to form between fiber and interphase during composite processing.

Ogbuji, Linus U. J. T.↗

NASA NTRS1991

Laser induced spark ignition of methane-oxygen mixtures

Results from an experimental study of laser induced spark ignition of methane-oxygen mixtures are presented. The experiments were conducted at atmospheric pressure and 296 K under laminar pre-mixed and turbulent-incompletely mixed conditions. A pulsed, frequency doubled Nd:YAG laser was used as the ignition source. Laser sparks with energies of 10 mJ and 40 mJ were used, as well as a conventional electrode spark with an effective energy of 6 mJ. Measurements were made of the flame kernel radius as a function of time using pulsed laser shadowgraphy. The initial size of the spark ignited flame kernel was found to correlate reasonably well with breakdown energy as predicted by the Taylor spherical blast wave model. The subsequent growth rate of the flame kernel was found to increase with time from a value less than to a value greater than the adiabatic, unstretched laminar growth rate. This behavior was attributed to the combined effects of flame stretch and an apparent wrinkling of the flame surface due to the extremely rapid acceleration of the flame. The very large laminar flame speed of methane-oxygen mixtures appears to be the dominant factor affecting the growth rate of spark ignited flame kernels, with the mode of ignition having a small effect. The effect of incomplete fuel-oxidizer mixing was found to have a significant effect on the growth rate, one which was greater than could simply be accounted for by the effect of local variations in the equivalence ratio on the local flame speed.

Santavicca, D. A.↗

NASA NTRS1972

Cathode for use with low density gases

Method for preventing deterioration of mixed oxide cathodes in low density gas tubes caused by ion bombardment is discussed. Construction of cathode is described and illustration is furnished. Electron emission through space charge to neutralize ion-filled regions is basic process.

Bennett, W. H.↗

NASA NTRS1977

Analytical model of the combustion of multicomponent solid propellants

Multiple flame models derived for simple composite propellants are extended to describe the combustion of propellants containing multimodal particle sizes, mixed oxidizers and monopropellant binders. Models combining the component contributions to propellant surface structure, flame structure and energy distribution are based in part upon experimental observations and in part upon hypotheses constrained to provide reasonable agreement with measured burning rate characteristics. The methods employed consist of superposition, interaction and iteration. The computerized model is applied to explain the effects of multiple ingredients and to discuss burning rate tailoring problems of current interest.

Cohen, N. S.↗

NASA NTRS1979

Review of composite propellant burn rate modeling

Steady-state combustion modeling of composite solid propellants is discussed with emphasis on the Beckstead-Derr-Price (BDP) model. The BDP model and some revisions are considered with respect to the analysis of monomodal ammonium perchlorate/inert binder propellants: topics examined include continuity relations, surface area relations, characteristic surface dimension, flame heights, and energy balance. Application of the BDP model to more complicated propellants containing multiple active ingredients is described. These propellants include multimodal, mixed oxidizer, active binder, aluminized, catalyzed, and nitramine propellants. Example cases of modeling (with comparison to experimental data) are presented, and strengths and weaknesses of current modeling approaches are evaluated.

Cohen, N. S.↗

NASA NTRS1982

Improved Ceramic for Heat Exchangers

Most promising composition developed in investigation consisted of mixed oxides described generically as ZrMAS. Has been commercially designated as GE-7808. Material was obtained from low-cost clay/talc mixture. Overall assessment of ZrMAS indicates it is a viable candidate for heat-exchanger application in automotive gas-turbine engines and possibly other areas that require dielectric materials of moderate refractoriness, good corrosion resistance, and excellent thermal-shock resistance.

Herbell, T. P.↗

NASA NTRS1982

Extraterrestrial materials processing

The first year results of a multi-year study of processing extraterrestrial materials for use in space are summarized. Theoretically, there are potential major advantages to be derived from the use of such materials for future space endeavors. The types of known or postulated starting raw materials are described including silicate-rich mixed oxides on the Moon, some asteroids and Mars; free metals in some asteroids and in small quantities in the lunar soil; and probably volatiles like water and CO2 on Mars and some asteroids. Candidate processes for space materials are likely to be significantly different from their terrestrial counterparts largely because of: absence of atmosphere; lack of of readily available working fluids; low- or micro-gravity; no carbon-based fuels; readily available solar energy; and severe constraints on manned intervention. The extraction of metals and oxygen from lunar material by magma electrolysis or by vapor/ion phase separation appears practical.

Steurer, W. H.↗

NASA NTRS1990

Processing Bi-Pb-Sr-Ca-Cu-O superconductors from amorphous state

Researchers produced superconducting ceramics of the Bi-Pb-Sr-Ca-Cu-O system started from a glass. To form the glass, the mixed oxide powder was melted at 1200 C in air. The liquid was quenched rapidly by pouring it onto an aluminum plate and rapidly pressing with another plate. The quenched compound was in the form of black amorphous solid, whose x-ray powder pattern has no crystalline peaks. After heat treatment at high temperatures, the glass crystallized into a superconductor. The crystalline phases in the superconductor identified using x-ray diffraction patterns. These phases were that associated with the superconducting phases of T(sub c) = 80 K (Bi2Ca1Sr2Cu2Ox) and of T(sub c) = 110 K (Bi2Ca2Sr2Cu3Ox). The dc resistivity and the ac susceptibility of these superconductors were studied.

Chiang, C. K.↗

NASA NTRS1991

Droplet-turbulence interactions in subcritical and supercritical evaporating sprays

The objective of this research is to obtain an improved understanding of droplet turbulence interactions in vaporizing liquid sprays under conditions typical of those encountered in liquid fueled rocket engines. The interaction between liquid droplets and the surrounding turbulent gas flow affects droplet dispersion, droplet collisions, droplet vaporization and gas-phase, fuel-oxidant mixing, and therefore has a significant effect on the engine's combustion characteristics. An example of this is the role which droplet-turbulence interactions are believed to play in combustion instabilities. Despite their importance, droplet-turbulence interactions and their effect on liquid fueled rocket engine performance are not well understood. This is particularly true under supercritical conditions, where many conventional concepts, such as surface tension, no longer apply. Our limited understanding of droplet-turbulence interactions, under both subcritical conditions, represents a major limitation in our ability to design improved liquid previously unavailable information and valuable new insights which will directly impact the design of future liquid fueled rocket engines, as well as, allow for the development of significantly improved spray combustion models, making such models useful design tools.

Santavicca, Domenic A.↗

NASA NTRS1990

A Planar-Fluorescence Imaging Technique for Studying Droplet-Turbulence Interactions in Vaporizing Sprays

Droplet turbulence interactions directly affect the vaporization and dispersion of droplets in liquid sprays and therefore play a major role in fuel oxidizer mixing in liquid fueled combustion systems. Proper characterization of droplet turbulence interactions in vaporizing sprays require measurement of droplet size velocity and size temperature correlations. A planar, fluorescence imaging technique is described which is being developed for simultaneously measuring the size, velocity, and temperature of individual droplets in vaporizing sprays. Preliminary droplet size velocity correlation measurements made with this technique are presented. These measurements are also compared to and show very good agreement with measurements made in the same spray using a phase Doppler particle analyzer.

Santavicca, Dom A.↗

NASA NTRS1991

Advanced Materials Center, Battelle

The goal of the Mixed Oxide Program is to determine the results obtained by using microgravity processing on a commercially significant catalyst - V-P-O System. The topics are presented in viewgraph form and include the following: (1) reasons for using microgravity; (2) the synthesis process; (3) novel results of the earth based program; and (4) Dupont interests.

Bellis, Harold↗