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At least 19 records

Reinforced Carbon Carbon (RCC) oxidation resistant material samples - Baseline coated, and baseline coated with tetraethyl orthosilicate (TEOS) impregnation

Reinforced carbon-carbon material specimens were machined from 19 and 33 ply flat panels which were fabricated and processed in accordance with the specifications and procedures accepted for the fabrication and processing of the leading edge structural subsystem (LESS) elements for the space shuttle orbiter. The specimens were then baseline coated and tetraethyl orthosilicate impregnated, as applicable, in accordance with the procedures and requirements of the appropriate LESS production specifications. Three heater bars were ATJ graphite silicon carbide coated with the Vought 'pack cementation' coating process, and three were stackpole grade 2020 graphite silicon carbide coated with the chemical vapor deposition process utilized by Vought in coating the LESS shell development program entry heater elements. Nondestructive test results are reported.

Gantz, E. E.↗

Reactions of calcium orthosilicate and barium zirconate with oxides and sulfates of various elements

Calcium orthosilicate and barium zirconate were evaluated as the insulation layer of thermal barrier coatings for air cooled gas turbine components. Their reactions with various oxides and sulfates were studied at 1100 C and 1300 C for times ranging up to 400 and 200 hours, respectively. These oxides and sulfates represent potential impurities or additives in gas turbine fuels and in turbine combustion air, as well as elements of potential bond coat alloys. The phase compositions of the reaction products were determined by X-ray diffraction analysis. BaZrO3 and 2CaO-SiO2 both reacted with P2O5, V2O5, Cr2O3, Al2O3, and SiO2. In addition, 2CaO-SiO2 reacted with Na2O, BaO, MgO, and CoO and BaZrO3 reacted with Fe2O3.

Zaplatynsky, I.↗

Anisotropic Optical-Response of Eu-doped Yttrium Orthosilicate

Eu-doped yttrium orthosilicate (Eu(3+) : Y2SiO5) had been a subject being investigated for coherent time-domain optical memory and information processing applications since its ultraslow optical dephasing was discovered several years ago. In this crystal the weakly allowed (7)F0 - (5)D0 transition of europium ions exhibits a sufficient long dephasing time and no spectral difli.usion on a time scale of several hours at low temperature, thus an information pattern or data can be stored as a population grating in the ground state hyperfine levels. On the other hand, the study on photon-echo relaxation shows that the dephasing time T2 of Eu (3+) and other rare-earth ions doped YAG, YAlO3 strongly depends on the intensity of the excitation pulses. In Eu (3+) :YAlO3, an exponential decay of photon-echo with T2 = 53 microseconds if the excitation pulses are weak (5 vJ/pulse) was observed. However, when the excitation pulses are strong (80 pJ/pulse) they observed a much shortened T2 with a highly nonexponential decay pattern. The conclusion they derived is that the intensity-dependent dephasing rate effects are quite general, and it depends on how much the excitation intensity varies. In this paper we use transient grating formation technique showing that a temporal lattice distortion may only occur along crystal c axis, caused by EU (3+) excitation. At high excitation level the produced exciton in conduction band may also couple to the dynamical lattice relaxation process, giving rise to an apparently much shortened dephasing time.

Liu, Huimin↗

Densification of porous refractory substrates

A hydrolyzed tetraethyl orthosilicate is applied to the surface of a porous refractory substrate following which the substrate is heated to a temperature and for a period of time sufficient to bond the silica released from the tetraethyl orthosilicate to the substrate. The surface is thus densified and strengthened.

Ecord, G. M.↗

Method of repairing surface damage to porous refractory substrates

A damaged porous refractory material coated with a glass coating is repaired by applying hydrolyzed tetraethyl orthosilicate to the damaged area and curing it. A pliable filler comprised of hydrolyzed tetraethyl orthosilicate and powdered refractory substrate is then applied to the area which is then heated.

Ecord, G. M.↗

Tile densification with TEOS

Densification process uses brushed or sprayed coating of tetraethyl orthosilicate. Liquid is applied and cured in three steps; tile weight increase averages 0.15 g per square centimeter. TEOS liquid is prepared by mixing TEOS with hydrochloric acid and adding marking dye. TEOS application provides variable stiffness, strength, and penetration. Surface of tile shows no buidup and is more durable for additional coatings.

Ecord, G. M.↗

Repairing high-temperature glazed tiles

Tetraethyl orthosilicate (TEOS) mixture fills chips and cracks in glazed tile surface. Filler is made by mixing hydrolyzed TEOS, silicon tetraboride powder, and pulverized tile material. Repaired tiles survived testing by intense acoustic emissions, arc jets, and intense heat radiation. Repair is reliable and rapid, performed in 1-1 1/2 hours with tile in any or orientation.

Ecord, G. M.↗

Mass loss of a TEOS-coated, reinforced carbon-carbon composite subjected to a simulted shuttle entry environment

Coated, reinforced carbon-carbon (RCC) is used for the leading edges of the space shuttle. The mass loss characteristics of RCC specimens coated with tetraethyl orthosilicate (TEOS) were determine for conditions which simulated the environment expected at the lug attachment area of the leading edge. Mission simulation included simultaneous application of load, temperature, and oxygen partial pressure. Maximum specimen temperature was 900 K (1160 F). Specimens were exposed for up to 80 simulated missions. Stress levels up to 6.8 MPa (980 psi) did not significantly affect the mass loss characteristics of the TEOS-coated RCC material. Mass loss was correlated with the bulk density of the specimens.

Stroud, C. W.↗

Comparative evaluation of insulating properties of plasma-sprayed ceramic coatings

A simple method for evaluating the thermal insulating capability of ceramic coatings was devised. It is based on monitoring the temperature of the uncoated back surface of a thin superalloy disk while its front surface, coated with the ceramic material, is exposed to the high-temperature environment of an electric muffle furnace. The results obtained indicate that zirconia containing 8 wt% Y2O3 is a better thermal insulator than barium zirconate or calcium orthosilicate.

Zaplatynsky, I.↗

Phase transformations in xerogels of mullite composition

Monophasic and diphasic xerogels have been prepared as precursors for mullite (3Al2O3-2SiO2). Monophasic xerogel was synthesized from tetraethyl orthosilicate and aluminum nitrate nanohydrate and the diphasic xerogel from colloidal suspension of silica and boehmite. The chemical and structural evolutions, as a function of thermal treatment, in these two types of sol-gel derived mullite precursor powders have been characterized by DTA, TGA, X-ray diffraction, SEM and infrared spectroscopy. Monophasic xerogel transforms to an Al-Si spinel from an amorphous structure at approximately 980 C. The spinel then changes into mullite on further heating. Diphasic xerogel forms mullite at approximately 1360 C. The components of the diphasic powder react independently up to the point of mullite formation. The transformation in the monophasic powder occurs rapidly and yields strongly crystalline mullite with no other phases present. The diphasic powder, however, transforms rather slowly and contains remnants of the starting materials (alpha-Al2O3, cristobalite) even after heating at high temperatures for long times (1600 C, 6 hr). The diphasic powder could be sintered to high density but not the monophasic powder in spite of its molecular level homogeneity.

Hyatt, Mark J.↗

Phase transformations in xerogels of mullite composition

Monophasic and diphasic xerogels have been prepared as precursors for mullite (3Al203-2Si02). Monophasic xerogel was synthesized from tetraethyl orthosilicate and aluminum nitrate nanohydrate and the diphasic xerogel from colloidal suspension of silica and boehmite. The chemical and structural evolutions, as a function of thermal treatment, in these two types of sol-gel derived mullite precursor powders have been characterized by DTA, TGA, X-ray diffraction, SEM and infrared spectroscopy. Monophasic xerogel transforms to an Al-Si spinel from an amorphous structure at approximately 980 C. The spinel then changes into mullite on further heating. Diphasic xerogel forms mullite at approximately 1360 C. The components of the diphasic powder react independently up to the point of mullite formation. The transformation in the monophasic powder occurs rapidly and yields strongly crystalline mullite with no other phases present. The diphasic powder, however, transforms rather slowly and contains remnants of the starting materials (alpha-Al203, cristobalite) even after heating at high temperatures for long times (1600 C, 6 hr). The diphasic powder could be sintered to high density but not the monophasic powder in spite of its molecular level homogeneity.

Hyatt, Mark J.↗

Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by sol-gel process

Calcium silicate glass compositions lying within the liquid-liquid immiscibility dome of the phase diagram, which could not have been prepared by the conventional melting method, were synthesized by the sol-gel process. Hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) solutions containing up to 20 mol percent calcium nitrate resulted in the formation of clear and transparent gels. The gel formation time decreased with increase in water:TEOS mole ratio, calcium content, and the reaction temperature. Smaller values of gel times in the presence of calcium nitrate are probably caused by lowering of the ionic charge on the sol particles by the salt present. The gelation activation energy, E(sub gel), was evaluated from temperature dependence of the gel time. Presence of Ca(2+) ions or the water:TEOS mole ratio did not have an appreciable effect on the value of E(sub gel). Presence of glycerol in the solution helped in the formation of crack-free monolithic gel specimens. Chemical and structural changes occurring in the gels, as a function of the heat treatments, have been monitored using DTA, TGA, IR-spectroscopy, x ray diffraction, surface area and pore size distribution measurements.

Bansal, Narottam P.↗

Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by the sol-gel process

Calcium silicate glass compositions lying within the liquid-liquid immiscibility dome of the phase diagram, which could not have been prepared by the conventional melting method, were synthesized by the sol-gel process. Hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) solutions containing up to 20 mol percent calcium nitrate resulted in the formation of clear and transparent gels. The gel formation time decreased with increase in water: TEOS mole ratio, calcium content, and the reaction temperature. Smaller values of gel times in the presence of calcium nitrate are probably caused by lowering of the ionic charge on the sol particles by the salt present. The gelation activation energy, E(sub gel), was evaluated from temperature dependence of the gel time. Presence of Ca(2+) ions or the water:TEOS mole ratio did not have an appreciable effect on the value of E(sub gel). Presence of glycerol in the solution helped in the formation of crack-free monolithic gel specimens. Chemical and structural changes occurring in the gels, as a function of the heat treatments, have been monitored using DTA, TGA, IR-spectroscopy, X-ray diffraction, surface area and pore size distribution measurements.

Bansal, N. P.↗

Compilation of reinforced carbon-carbon transatlantic abort landing arc jet test results

This document consists of the entire test database generated to support the Reinforced Carbon-Carbon Transatlantic Abort Landing Study. RCC components used for orbiter nose cap and wing leading edge thermal protection were originally designed to have a multi-mission entry capability of 2800 F. Increased orbiter range capability required a predicted increase in excess of 3300 F. Three test series were conducted. Test series #1 used ENKA-based RCC specimens coated with silicon carbide, treated with tetraethyl orthosilicate, sealed with Type A surface enhancement, and tested at 3000-3400 F with surface pressure of 60-101 psf. Series #2 used ENKA- or AVTEX-based RCC, with and without silicon carbide, Type A or double Type AA surface enhancement, all impregnated with TEOS, and at temperatures from 1440-3350 F with pressures from 100-350 psf. Series #3 tested ENKA-based RCC, with and without silicon carbide coating. No specimens were treated with TEOS or sealed with Type A. Surface temperatures ranged from 2690-3440 F and pressures ranged from 313-400 psf. These combined test results provided the database for establishing RCC material single-mission-limit temperature and developing surface recession correlations used to predict mass loss for abort conditions.

Milhoan, James D.↗

Orbiter Reinforced Carbon-Carbon Advanced Sealant Systems: Screening Tests

Oxidation protection for the Orbiter reinforced carbon-carbon (RCC consists of three components: silicon carbide coating, tetraethyl orthosilicate (TEOS) impregnated into the carbon substrate and a silicon based surface sealant (designated Type A). The Orbiter Type A sealant is being consumed each mission, which results in increased carbon-carbon substrate mass loss, which adversely impacts the mission life of the RCC components. In addition, the sealant loss in combination with launch pad contamination (salt deposit and zinc oxide) results in RCC pinholes. A sealant refurbishment schedule to maintain mission life and minimize affects of pin hole formation has been implemented in the Orbiter maintenance schedule. The objective of this investigation is to develop an advanced sealant system for the RCC that extends the refurbishment schedule by reducing sealant loss/pin hole formation and that can be applied to existing Orbiter RCC components. This paper presents the results of arc jet screening tests conducted on several sealants that are being considered for application to the Orbiter RCC.

Curry, Donald M.↗

Phosphorus Equilibria Among Mafic Silicate Phases

Phosphorus incorporation in major rock-forming silicate minerals has the following implications: (1) Reactions between phosphorus-hosting major silicates and accessory phosphates, which are also major trace element carriers, may control the stability of the latter and thus may affect the amount of phosphorus and other trace elements released to the coexisting melt or fluid phase. (2) Less of a phosphate mineral is needed to account for the bulk phosphorus of planetaty mantles. (3) During partial melting of mantle mineral assemblages or equilibrium fractional crystallization of basaltic magmas, and in the absence or prior to saturation with a phosphate mineral, silicate melts may become enriched in phosphorus, especially in the geochemically important low melt fraction regime, Although the small differences in the ionic radii of IVp5+, IVSi4+, and IV Al3+ makes phosphoms incorporation into crystalline silicates perhaps unsurprising, isostructural silicate and phosphate crystalline solids do not readily form solutions, e.g., (Fe, Mg)2SiO4 vs. LiMgPO4, SiO)2 VS. AlPO4. Nonetheless, there are reports of, poorly characterized silico-phosphate phases in angrites , 2-4 wt% P2O5 in olivine and pyroxene grains in pallasites and reduced terestrial basalts which are little understood but potentially useful, and up to 17 wt% P2O5 in olivine from ancient slags. However, such enrichments are rare and only underscore the likelihood of phosphoms incorporation in silicate minerals. The mechanisms that allow phosphorus to enter major rock-forming silicate minerals (e.g., Oliv, Px, Gt) remain little understood and the relevant data base is limited. Nonetheless, old and new high-pressure (5-10 GPa) experimental data suggest that P2O5 wt% decreases from silica-poor to silica-rich compositions or from orthosilicate to chain silicate structures (garnet > olivine > orthopyroxene) which implies that phosphorus incorporation in silicates is perhaps more structure-than site-specific. The data also indicate that DXVliQP2O5 decrease in the same order, but DOVLiQP2O5 and DOpx/LiQP205 are likely constant, respectively equal to 0.08(3) and 0.007(4), in contrast, DG1ILiQP205 increases from 0.15(3) to 0.36(10) as garnet becomes majoritic, thus silica-enriched, and may also depend on liquid composition (SiO2, P2O5 and Na2O wt%).

Berlin, Jana↗

Tailoring of Boehmite-Derived Aluminosilicate Aerogel Structure and Properties: Influence of Ti Addition

Aluminosilicate aerogels offer potential for extremely low thermal conductivities at temperatures greater than 900 C, beyond where silica aerogels reach their upper temperature limits. Aerogels have been synthesized at various Al:Si ratios, including mullite compositions, using Boehmite (AlOOH) as the Al source, and tetraethoxy orthosilicate as the Si precursor. The Boehmite-derived aerogels are found to form by a self-assembly process of AlOOH crystallites, with Si-O groups on the surface of an alumina skeleton. Morphology, surface area and pore size varies with the crystallite size of the starting Boehmite powder, as well as with synthesis parameters. Ternary systems, including Al-Si-Ti aerogels incorporating a soluble Ti precursor, are possible with careful control of pH. The addition of Ti influences sol viscosity, gelation time pore structure and pore size distribution, as well as phase formation on heat treatment.

Hurwitz, Frances I.↗