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NASA NTRS1997

Environmental Effects on Non-oxide Ceramics

Non-oxide ceramics such as silicon carbide (SiC) and silicon nitride (Si3N4) are promising materials for a wide range of high temperature applications. These include such diverse applications as components for heat engines, high temperature electronics, and re-entry shields for space vehicles. Table I lists a number of selected applications. Most of the emphasis here will be on SiC and Si3N4. Where appropriate, other non-oxide materials such as aluminum nitride (AlN) and boron nitride (BN) will be discussed. Proposed materials include both monolithic ceramics and composites. Composites are treated in more detail elsewhere in this volume, however, many of the oxidation/corrosion reactions discussed here can be extended to composites. In application these materials will be exposed to a wide variety of environments. Table I also lists reactive components of these environments.It is well-known that SiC and Si3N4 retain their strength to high temperatures. Thus these materials have been proposed for a variety of hot-gas-path components in combustion applications. These include heat exchanger tubes, combustor liners, and porous filters for coal combustion products. All combustion gases contain CO2, CO, H2, H2O, O2, and N2. The exact gas composition is dependent on the fuel to air ratio or equivalence ratio. (Equivalence ratio (EQ) is a fuel-to-air ratio, with total hydrocarbon content normalized to the amount of O2 and defined by EQ=1 for complete combustion to CO2 and H2O). Figure 1 is a plot of equilibrium gas composition vs. equivalence ratio. Note that as a general rule, all combustion atmospheres are about 10% water vapor and 10% CO2. The amounts of CO, H2, and O2 are highly dependent on equivalence ratio.

Jacobson, Nathan S.↗

NASA NTRS1979

High pressure sintering of non-oxide materials

Pure materials of AIN, alpha-Si3N4 and TiC, without additives were sintered at 800 C to 1400 C under the pressures of 30 kbar and 50 kbar for 0.5 hours. The maximum density of sintered bodies for the cited materials was nearly 100% for AIN, 98% for TiC and 96% for alpha-Si3N4.

Shimado, M.↗

NASA NTRS1999

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.

Sun, Z.↗

NASA NTRS1999

Corrosion of Ceramic Materials

Non-oxide ceramics are promising materials for a range of high temperature applications. Selected current and future applications are listed. In all such applications, the ceramics are exposed to high temperature gases. Therefore it is critical to understand the response of these materials to their environment. The variables to be considered here include both the type of ceramic and the environment to which it is exposed. Non-oxide ceramics include borides, nitrides, and carbides. Most high temperature corrosion environments contain oxygen and hence the emphasis of this chapter will be on oxidation processes.

Opila, Elizabeth J.↗

NASA NTRS1974

Oxide glass processing in space

The experimental work performed thus far has resulted in the preparation of new glass compositions not reported heretofore in the open literature. Recent experiments which have resulted in the formation of 1/4-inch-diameter glass samples from two compositions, suggest that containerless melting and cooling as envisioned for space operations is of real technological significance. To date studies of space glasses have by choice been confined to oxide glasses only. It is felt that the applications for such glasses are more readily predictable than for the other materials, and that many of the principles that will evolve from a study of oxide glasses, which can be melted in air, permit a more direct approach to non-oxide materials in the future. The compositions being studied are all very simple in terms of traditional glass practices, none of them containing more than three major constituents. Future efforts should be concerned with more complex compositions, both to cover a broader range of optical properties and to enhance glass-forming tendencies.

Happe, R. A.↗

NASA NTRS1976

Study of thermal stability and degradation of fire resistant candidate polymers for aircraft interiors

The thermochemistry of bismaleimide resins and phenolphthalein polycarbonate was studied. Both materials are fire-resistant polymers and may be suitable for aircraft interiors. The chemical composition of the polymers has been determined by nuclear magnetic resonance and infrared spectroscopy and by elemental analysis. Thermal properties of these polymers have been characterized by thermogravimetric analyses. Qualitative evaluation of the volatile products formed in pyrolysis under oxidative and non-oxidative conditions has been made using infrared spectrometry. The residues after pyrolysis were analyzed by elemental analysis. The thermal stability of composite panel and thermoplastic materials for aircraft interiors was studied by thermogravimetric analyses.

Hsu, M. T. S.↗

NASA NTRS1983

Organometalic carbosilane polymers containing vanadium and their preparation

The present invention concerns a new organometallic polymer material containing in part a vanadium-siloxane linkage (V-0-Si), which has excellent resistance to heat and oxidation and a high residue ratio after high temperature treatment in a non-oxidizing atmosphere, for example, nitrogen, argon, helium, ammonia, or hydrogen.

Yajima, S.↗

NASA NTRS1983

Electrodes for solid state devices

The invention relates to coated metal powders and to dispersions of such powders in liquid vehicles forming screenable, sinterable pastes for use in forming electrodes on photovoltaic devices. The primary nickel or copper metal particles are provided with a carrier of lower melting sintering metals such as 1-20% by weight, of a non-oxidizing metal such as lead or tin. The powdered metal systems operate on the basis of fusing together by way of eutectic alloying. As the paste is heated during firing the organic binder is first vaporized. An eutectic of the base metal (copper) and coating (tin) forms at the intersections of the base metal grains. This eutectic dissolves the grains and as the temperature is raised above the eutectic temperature, more of the base metal is dissolved. While the temperature is held at the higher value, the much smaller amount of sintering metal disappears as the eutectic dissolves and diffuses into the base metal until the composition of the eutectic is so enriched with base metal that it no longer has the eutectic properties and it solidifies. In this high temperature solidification, the base metal grains became thoroughly alloyed together and will not separate at the eutectic temperature (a lower temperature than their solidification by diffusion).

Bickler, D. B.↗

NASA NTRS1984

Petrologic model of the northern Mississippi Embayment based on satellite magnetic and ground-based geophysical data

A petrologic model of the northern Mississippi Embayment, derived from gravity, seismic and rift data, is evaluated by converting the model to a magnetization model which is compared with satellite magnetic anomaly models. A magnetization contrast of approximately -0.54 A/m, determined from the petrologic model of the embayment compares favorably to values of -0.62 A/m and -0.45 A/m from a Magsat United States Apparent Magnetization Contrast Map and a published POGO magnetization contrast model, respectively. The petrologic model suggests that the magnetic anomaly low associated with the Mississippi Embayment may be largely due to the intrusion under non-oxidizing conditions of low Curie temperature gabbroic material at the base of the crust of the embayment. Near-surface mafic plutons, bordering the Mississippi Valley Graben, appear from aeromagnetic data to have higher magnetizations than the deeper gabbroic material; however, it is impossible to ascertain if this is due to compositional differences or similar material at shallower (lower temperature) depths. These results indicate that variations in the Curie temperatures of intrusions accompanying rifting may account for a large part of the wide range of magnetic anomalies associated with presently inactive rifts with normal heat flow.

Thomas, H. H.↗

NASA NTRS1984

Friction and wear of ceramics

The adhesion, friction, wear and lubricated behaviors of both oxide and non-oxide ceramics are reviewed. Ceramics are examined in contact with themselves, other harder materials and metals. Elastic, plastic and fracture behavior of ceramics in solid state contact is discussed. The contact load necessary to initiate fracture in ceramics is shown to be appreciably reduced with tangential motion. Both friction and wear of ceramics are anisotropic and relate to crystal structure as with metals. Grit size effects in two- and three-body abrasive wear are observed for ceramics. Both free energy of oxide formation and the d valence bond character of metals are related to the friction and wear characteristics for metals in contact with ceramics. Surface contaminants affect friction and adhesive wear. For example, carbon on silicon carbide and chlorine on aluminum oxide reduce friction while oxygen on metal surfaces in contact with ceramics increases friction. Lubrication increases the critical load necessary to initiate fracture of ceramics both in indentation and with sliding or rubbing.

Buckley, D. H.↗

NASA NTRS1985

Thermal barrier coating life prediction model development

A methodology was established to predict thermal barrier coating life in an environment simulative of that experienced by gas turbine airfoils. Specifically, work is being conducted to determine failure modes of thermal barrier coatings in the aircraft engine environment. Analytical studies coupled with appropriate physical and mechanical property determinations are being employed to derive coating life prediction model(s) on the important failure mode(s). An initial review of experimental and flight service components indicates that the predominant mode of TBC failure involves thermomechanical spallation of the ceramic coating layer. This ceramic spallation involves the formation of a dominant crack in the ceramic coating parallel to and closely adjacent to the metal-ceramic interface. Initial results from a laboratory test program designed to study the influence of various driving forces such as temperature, thermal cycle frequency, environment, and coating thickness, on ceramic coating spalling life suggest that bond coat oxidation damage at the metal-ceramic interface contributes significantly to thermomechanical cracking in the ceramic layer. Low cycle rate furnace testing in air and in argon clearly shows a dramatic increase of spalling life in the non-oxidizing environments.

Sheffler, K. D.↗

NASA NTRS1986

Technology for satellite power conversion

The work performed in this reporting period has concentrated on the metal-oxide-metal (MOM) diode. The fabrication procedure begins with the deposition of gold probing pads to provide a non-oxidizing contact to test the dc characteristics to the diode accurately. A thin patch capped with an insulating SiO2 layer, is deposited next to form the first half of the diode. The other half of the diode, typically Ni, is deposited completing the conduction path from the oxidized edge of the Ni patch to the opposite gold probing pad. It is important in this step that the last metallization take place without exposing the newly oxidized surface to the atmosphere. Successful production of diodes has been achieved. Work on millimeter wave frequency rectennas incorporating known semiconductor diode technology has been initiated.

Gouker, M. A.↗

NASA NTRS1986

On the sintering of silicon carbide

This document deals with the sintering of silicon carbide using pressureless sintering. This technique makes it possible to sinter a primarily covalent material to usable densities up to over 98% thD without having to use a high amount of sinter additives as is the case with other non-oxide ceramic materials. The process takes place rapidly, and it is also possible to produce relatively thick-walled structural parts without major problems. This sheds more light on the true characteristics of silicon carbide in one structural part, since there is no second or nearly no second phase. Heat pressing has improved stability.

Gugel, E.↗

NASA NTRS1986

Friction and wear of ceramics

The adhesion, friction, wear, and lubricated behaviors of both oxide and non-oxide ceramics are reviewed. Ceramics are examined in contact with themselves, other harder materials, and metals. Elastic, plastic, and fracture behavior of ceramics in solid state contact is discussed. The contact load necessary to initiate fracture in ceramics is shown to be appreciably reduced with tangential motion. Both friction and wear of ceramics are anisotropic and relate to crystal structure as with metals. Grit size effects in two and three body abrasive wear are observed for ceramics. Both the free energy of oxide formation and the d valence bond character of metals are related to the friction and wear characteristics for metals in contact with ceramics. Surface contaminants affect friction and adhesive wear. For example, carbon on silicon carbide and chlorine on aluminum oxide reduce friction while oxygen on metal surfaces in contact with ceramics increases friction. Lubrication increases the critical load necessary to initiate fracture of ceramics both in indentation and with sliding or rubbing.

Buckley, Donald H.↗

NASA NTRS1992

Greenhouse warming by minor gases on early Mars

The early atmospheres of Earth and Mars were non-oxidizing mixtures likely derived from volcanic outgassing of a silicate mantle, with some fraction of the volatiles also contributed by impacting comets and meteorites. Here the authors investigate the potential of minor atmospheric constituents produced by ultraviolet and auroral chemistry to contribute to the thermal opacity of early Earth and Mars atmospheres. Using a very simple two-stream thermal opacity model, the authors show that HCN at 10 parts per million (ppm) and N2O at 100 ppm can each block radiation in thermal infrared windows sufficiently to increase the surface temperature by 7 K separately, or 14 K together. Small quantities of other species are also produced in such experiments. Some of these have especially complex infrared spectra and should be further investigated for their potential to help close windows in the CO2 + H2O infrared transmission. Enhancement of greenhouse warming by minor atmospheric species different from those present in today's atmosphere may have played important roles in the climate of early Earth and Mars.

Heinrich, M. N.↗

NASA NTRS1993

Ceramic fibers from Si-B-C polymer precursors

Non-oxide ceramics such as silicon carbide (SiC), silicon nitride (Si3N4), and silicon borides (SiB4, SiB6) have thermal stability, oxidation resistance, hardness, and varied electrical properties. All these materials can be prepared in a fiber form from a suitable polymer precursor. The above mentioned fibers, when tested over a temperature range from 25 to 1400 C, experience degradation at elevated temperatures. Past work in ceramic materials has shown that the strength of ceramics containing both carbides and borides is sustained at elevated temperatures, with minimum oxidation. The work presented here describes the formation of ceramic fibers containing both elements, boron and silicon, prepared via the polymer precursor route previously reported by the authors, and discusses the fiber mechanical properties that are retained over the temperature range studied.

Riccitiello, S. R.↗

NASA NTRS1995

A Porous Ceramic Interphase for SiC/Si(sub 3)N(sub 4) Composites

A suitable interphase material for non-oxide ceramic-matrix composites must be resistant to oxidation. This means it must exhibit a slow rate of oxidation, and its oxidation product must be such as to ensure that the system survives oxidation when it does occur. Because the current benchmark interphase materials, carbon and boron nitride, lack these qualities, a porous fiber coating was developed to satisfy both the mechanical and oxidative requirements of an interphase for the SiC/SiC and SiC/Si2N4 composites that are of interest to NASA. This report presents the interphase microstructure achieved and the resulting characteristics of fiber push-out from a matrix of reaction-bonded silicon nitride (RBSN), both as-fabricated and after substantial annealing and oxidation treatments.

Ogbuji, Linus U. J. T.↗

NASA NTRS1999

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

Two critical challenges facing the application of flames for synthesis of nanopowder materials are: (1) overcoming formation of agglomerates and (2) ensuring that the highly reactive nanopowders that are synthesized in flames can be produced in such a manner that their purity is maintained during subsequent processing. Agglomerates are produced in flames because particle formation occurs in a high temperature and high number density environment. They are undesirable in most advanced applications of powders. For example, agglomerates have a deleterious effect on compaction density, leading to voids when nanopowders are consolidated. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Powder purity must also be maintained during subsequent handling of nanopowders and this poses a significant challenge for any synthesis route because nanopowders, particularly metals and non-oxide ceramic powders, are inherently reactive. Impurities acquired during handling of nanopowders have slowed the advancement of the nanostructured materials industry. One promising approach that has been proposed to address these problems is nano-encapsulation. In this approach, the core particles are encapsulated in a removable material while they are within the flame but before excessive agglomeration has occurred. Condensation can be very rapid so that core particles are trapped within the condensed material and agglomeration is limited. Nano-encapsulation also addresses the handling concerns for post-synthesis processing. Results have shown that when nano-encapsulated powders are exposed to atmosphere the core particles are protected from oxidation and/or hydrolysis. Thus, handling of the powders does not require extreme care. If, for example, at the time of consolidation the encapsulation material is removed by vacuum annealing, the resulting powder remains unagglomerated and free of impurities. In this work, we described a novel aerosol model that has been developed to simulate particle encapsulation in flames. The model will ultimately be coupled to a one-dimensional spherical flame code and compared to results from microgravity flame experiments.

Sun, Z.↗