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At least 73 records · Page 4

Evaluation of reusable surface insulation for space shuttle over a range of heat-transfer rate and surface temperature

Reusable surface insulation materials, which were developed as heat shields for the space shuttle, were tested over a range of conditions including heat-transfer rates between 160 and 620 kW/sq m. The lowest of these heating rates was in a range predicted for the space shuttle during reentry, and the highest was more than twice the predicted entry heating on shuttle areas where reusable surface insulation would be used. Individual specimens were tested repeatedly at increasingly severe conditions to determine the maximum heating rate and temperature capability. A silica-base material experienced only minimal degradation during repeated tests which included conditions twice as severe as predicted shuttle entry and withstood cumulative exposures three times longer than the best mullite material. Mullite-base materials cracked and experienced incipient melting at conditions within the range predicted for shuttle entry. Neither silica nor mullite materials consistently survived the test series with unbroken waterproof surfaces. Surface temperatures for a silica and a mullite material followed a trend expected for noncatalytic surfaces, whereas surface temperatures for a second mullite material appeared to follow a trend expected for a catalytic surface.

Chapman, A. J.↗

Chemical and morphological changes of reusable surface insulation coatings as a function of convectively heated cyclic testing

The effects of convective heating upon reusable surface insulation coatings were studied utilizing scanning electron microscopy, X-ray fluorescence, and X-ray diffraction. Samples of coated silica, mullite, and ceramic mullite fiber were cycled in an arc plasma stream up to 15 times for 15 minutes per cycle at surface temperatures simulating those on the space shuttle vehicle. The surfaces of ceramic mullite fiber and mullite coatings were roughened substantially by the convectively heated environment while the silica was significantly smoothed after testing. Scanning electron microscopy also showed surface cracking of varying degrees in all of the coatings. The surface chemistry of the coatings as examined by X-ray fluorescence revealed that significant changes in composition were occurring during cycling, particularly within the mullite coating.

Leiser, D. B.↗

Degradation Of Environmental Barrier Coatings (EBC) Due To Chemical and Thermal Expansion Incompatibility

Current environmental barrier coatings (EBCs) consist of multiple layers, with each layer having unique properties to meet the various requirements for successful EBCs. As a result, chemical and thermal expansion compatibility between layers becomes an important issue to maintaining durability. Key constituents in current EBCs are mullite (3Al2O3-2SiO2), BSAS (BaO(1-x)-SrO(x)-Al2O3-2SiO2), and YSZ (ZrO2-8 wt.% Y2O3). The mullite-BSAS combination appears benign although significant diffusion occurs. Mullite-YSZ and BSAS-YSZ combinations do not react up to 1500 C. Thermally grown SiO2- BSAS and mullite-BSAS-YSZ combinations are most detrimental, forming low melting glasses. Thermal expansion mismatch between YSZ and mullite or BSAS causes severe cracking and delamination.

Lee, Kang N.↗

Characterization of RSI coating

X-ray diffraction analyses on mullite, silica, and ceramic mullite fiber coating materials to investigate the effects of thermal cycling, show that ceramic mullite fiber coating porosity is little affected by cycling to 1250 C and that material pores are mostly smaller than 15 nm. Some mullite coatings experience a slight increase in crystobalite with somewhat increased porosity. Silica coatings show a marked tendency to precipitate cristobalite with increased porosity and dimensional instability.

Miller, A. D.↗

Reusable surface insulation thermal protection systems test evaluation status

Changes in coating morphology of mullite, silica, and ceramic mullite fiber at two heating rates are described followed by a discussion of the changes in surface chemistry that occur during convective heating tests. Subsequently, the surface chemistry changes observed are compared to similar data obtained from radiantly heated coatings and the significance of the difference between the results is discussed. Finally, the changes in chemistry of the coatings in cross section before and after convectively heated cyclic testing are discussed and the significance of surface chemistry changes are described. Results indicate that the thermal conductivity of mullite surface insulation is higher than that of silica insulation, based on thermal response data. Acoustic excitation of cracked silica tiles does not lead to catastrophic failure such as spallation or tile loss. Cracks in mullite material after thermal exposure lead to fracturing of the coating and surface insulation material after acoustic excitation.

Strouhal, G.↗

Emittance of RSI Coatings Determined from Radiation Measurements in Arc Jet Tests

Simultaneous measurements were made on three surface insulation coatings for total surface radiation and radiation at discrete wavelengths between 0.88 and 4.5 microns. The mullite coating radiated all the applied heat at convective heat rates of 204 and 295 kw/sq m. Radiation from the ceramic mullite fiber coating was 170 kw/sq m at a heat rate of 454 kw/sq m. Effective total emissivity and spectral emissivity values were evaluated; all three coatings were significantly non-grey. Effective total emissivity values were 0.79 for mullite, 0.50 for ceramic mullite fiber, and 0.78 for silica composite.

Wakefield, R. M.↗

Transformation toughened ceramics for the heavy duty diesel engine technology program, phase 2

The objective of this program is to develop an insulating structural ceramic for application in a heavy duty adiabatic diesel engine. The approach is to employ transformation toughening (TT) by additions of zirconia-hafnia solid solution (ZHSS). The feasibility of using ZHSS as a toughening agent in mullite and alumina has been demonstrated in Phase 1 of this work. Based on Phase 1 results, a decision was made to concentrate the Phase 2 effort on process optimization of the TT mullite. A strong factor in that decision was the low thermal conductivity and high thermal shock resistance of the mullite. Results of the Phase 2 effort indicate that optimum toughening of mullite by additions of ZHSS is difficult to achieve due to apparent sensitivity to morphology. The 48 ksi room temperature modulus-of-rupture (MOR) achieved in selected specimens is approximately 50% of the original strength target. The MOR deteriorated to 34 ksi at 800 C.

Musikant, S.↗

Environmental Barrier Coatings for Silicon-Based Ceramics

Silicon-based ceramics, such as SiC fiber-reinforced SiC (SiC/SiC ceramic matrix composites (CMC) and monolithic silicon nitride (Si3N4), are prime candidates for hot section structural components of next generation gas turbine engines. Silicon-based ceramics, however, suffer from rapid surface recession in combustion environments due to volatilization of the silica scale via reaction with water vapor, a major product of combustion. Therefore, application of silicon-based ceramic components in the hot section of advanced gas turbine engines requires development of a reliable method to protect the ceramic from environmental attack. An external environmental barrier coating (EBC) is considered a logical approach to achieve protection and CP long-term stability. The first generation EBC consisted of two layers, mullite (3Al2O3-2SiO2) bond coat and yttria-stabilized zirconia (YSZ, ZrO2-8 Wt.% Y2O3) top coat. Second generation EBCs, with substantially improved performance compared with the first generation EBC, were developed in the NASA High Speed Research-Enabling Propulsion Materials (HSR-EPM) Program. The first generation EBC consisted of two layers, mullite (3Al2O3-2SiO2) bond coat and yttria-stabilized zirconia (YSZ, ZrO2-8 wt.% Y2O3) top coat. Second generation EBCs, with substantially improved performance compared with the first generation EBC, were developed in the NASA High Speed Research-Enabling Propulsion Materials (HSR-EPM) Program (5). They consist of three layers, a silicon first bond coat, a mullite or a mullite + BSAS (BaO(1-x)-SrO(x)-Al2O3-2SiO2) second bond coat, and a BSAS top coat. The EPM EBCs were applied on SiC/SiC CMC combustor liners in three Solar Turbines (San Diego, CA) Centaur 50s gas turbine engines. The combined operation of the three engines has accumulated over 24,000 hours without failure (approximately 1,250 C maximum combustor liner temperature), with the engine in Texaco, Bakersfield, CA, accumulating about 14,000 hours. As the commercialization of Si-based ceramic components in gas turbines is on the horizon, a major emphasis is placed on EBCs for two reasons. First, they are absolute necessity for the protection of Si-based ceramics from water vapor. Second, they can enable a major enhancement in the performance of gas turbines by creating temperature gradients with the incorporation of a low thermal conductivity layer. Thorough understanding of current state-of-the-art EBCs will provide the foundation upon which development of future EBCs will be based. Phase stability and thermal conductivity of EPM EBCs are published elsewhere. This paper will discuss the chemical/environmental durability and silica volatility of EPM EBCs and their impact on the coating's upper temperature limit.

Lee, Kang N.↗

Radiant Heat Transfer in Reusable Surface Insulation

During radiant testing of mullite panels, temperatures in the insulation and support structure exceeded those predicted on the basis of guarded hot plate thermal conductivity tests. Similar results were obtained during arc tunnel tests of mullite specimens. The differences between effective conductivity and guarded hot plate values suggested that radiant transfer through the mullite was occurring. To study the radiant transport, measurements were made of the infrared transmission through various insulating materials and fibers of interest to the shuttle program, using black body sources over the range of 780 to 2000 K. Experimental data were analyzed and scattering coefficients were derived for a variety of materials, fiber diameters, and source temperature.

Hughes, T. A.↗

Phase transformations in 40-60-GPa shocked gneisses from the Haughton Crater (Canada): An Analytical Transmission Electron Microscopy (ATEM) study

In order to better understand phase transformations, chemical migration, and isotopic disequilibrium in highly shocked rocks, we have performed a microprobe and an ATEM study on gneisses shocked up to 60 GPa from the Haughton Crater. This study reveals the following chemical and structural characteristics: (1) SiO2 dominant areas are formed by a mixture of pure SiO2 polycrystalline quartz identified by electron diffraction pattern and chemical analysis and a silica-rich amorphous phase containing minor amounts of aluminium, potassium, and iron; (2) Areas with biotitelike composition are formed by less than 200-nm grains of iron-rich spinels embedded in a silica-rich amorphous phase that is very similar to the one described above; (3) Layers with feldsparlike composition are constituted by 100-200-nm-sized alumina-rich grains (the indexation of the crystalline structure is under progress) and the silica-rich amorphous phase; (4) Zones characterized by the unusual Al/Si ratio close to 1 are formed by spinel grains (200-nm-sized) embedded in the same silica-rich amorphous phase; and (5) The fracturated sillimanites contain domains with a lamellar structure, defined by the intercalation of 100-nm-wide lamellae of mullite crystals and of a silica-rich amorphous phase. These mullite crystals preserved the crystallographical orientation of the preshock sillimanite. All compositional domains, identified at the microprobe scale, can thus be explained by a mixture in different proportion between the following phases: (1) a silica-rich amorphous phase, with minor Al and K; (2) quartz crystals; (3) spinel crystals and alumina-rich crystals; (4) sillimanite; and (5) mullite. Such mixtures of amorphous phases and crystals in different proportions explain disturbed isotope systems in these rocks and chemical heterogeneities observed on the microprobe.

Martinez, I.↗

Controlled evolution of rare earth phosphate in coal ash slag

Coal ash slag as a waste by-product, is generated from commercial processes that include gasification facilities, power plants, and steelmaking industries. Some is recycled into construction materials, insulation fibers, and used as a soil neutralizer, but the majority is still discarded. Coal ash slag exhibit trace amounts of critical materials including rare earth elements (REEs). An economically viable extraction of REEs from the coal ash would lower the production costs, addressing the availability and environmental concerns. In nature, most REEs exist as phosphate such as monazite but its synthetic evolution in coal ash slag has never been reported. In industrial processes, P may originate from coal, additives, and/or refractory liners. REEs may be extracted by first concentrating REEs into phosphates, sulphide, or fluorides [1], or carbonates [2]. In this work, P-enriched coal ash slag bearing REEs was first melted above 1600 °C, then crystallization behaviors in the melt during controlled cooling was studied. REE phosphate coprecipitated with mullite and hematite with mullite being the first crystal to form on cooling. The REEs were rejected from the molten slag, mullite, and hematite, and tended to segregate only to the phosphate phase with REE concentration as high as 58 wt.% in the structure.

Nakano, Jinichiro↗

Controlled evolution of rare earth phosphate in coal ash slag

Coal ash slag as a waste by-product, is generated from commercial processes that include gasification facilities, power plants, and steelmaking industries. Some is recycled into construction materials, insulation fibers, and used as a soil neutralizer, but the majority is still discarded. Coal ash slag exhibit trace amounts of critical materials including rare earth elements (REEs). An economically viable extraction of REEs from the coal ash would lower the production costs, addressing the availability and environmental concerns. In nature, most REEs exist as phosphate such as monazite but its synthetic evolution in coal ash slag has never been reported. In industrial processes, P may originate from coal, additives, and/or refractory liners. REEs may be extracted by first concentrating REEs into phosphates, sulphide, or fluorides [1], or carbonates [2]. In this work, P-enriched coal ash slag bearing REEs was first melted above 1600 °C, then crystallization behaviors in the melt during controlled cooling was studied. REE phosphate coprecipitated with mullite and hematite with mullite being the first crystal to form on cooling. The REEs were rejected from the molten slag, mullite, and hematite, and tended to segregate only to the phosphate phase with REE concentration as high as 58 wt.% in the structure.

Nakano, Jinichiro↗

Characterization of SiO 2 Thermally Grown Oxide Stress Evolution of EBCs with Al-Containing Dopants

SiC/SiC ceramic matrix composites (CMCs) are desired for use in combustion environments to achieve higher turbine operating temperatures. However, CMCs require environmental barrier coatings (EBCs) for protection from the gas environment. EBC systems are known to primarily fail through coating delamination via growth of a thermally grown oxide (TGO) at the EBC—silicon bond coating interface when exposed to steam, which accelerates the TGO growth rate. The TGO undergoes a phase transformation during thermal cycling, which results in stresses that may encourage EBC spallation. Yb-silicate EBCs with mullite and yttrium aluminum garnet (YAG) dopant additions were deposited on SiC substrates with a Si intermediate bond coating and exposed to thermal cycling in steam at 1350 °C. The impact of Al dopant additions on the TGO growth rate and the SiO 2 phase transformation was assessed. Photo-stimulated luminescence spectroscopy (PSLS) was used to characterize the Al-containing phases and to measure stress evolution in the EBC following exposure using the stress-induced peak shift of the R-lines of mullite. Raman microscopy was used to map the stresses in the Si bond coating following exposure. It was found that the TGO phase transformation upon cooling increased compressive stress in the Si bond coating within 15 µm of the TGO.

Building Materials↗

Improvement of Reusable Surface Insulation (RSI) materials

The mullite fiber based hardened compacted fibers (HCF) type of reusable surface insulation was further developed for use in the Space Shuttle Program. Two hundred fifty formulations of fiber mixtures, fillers, binders, and organic processing aids were made using mullite fibers as the basic ingredient. Most of the work was accomplished on 15-lb/cu ft material. It was established that higher density materials are stronger with strength values as high as 250 lb/sq in. in tension. New measurement techniques and equipment were developed for accurate determination of strength and strain to failure. Room temperature to 2300 F stress-strain relationships were made. The room temperature tensile modulus of elasticity is 61,700 lb/sq in. and the strain at failure is 0.165 percent, typically, when measured longitudinally parallel to the long axes of the fibers. Thermal insulating effectiveness was increased 20 percent by reducing the diameter of some of the fibers in the material. Improvements were made in density uniformity and strength uniformity in a block of HCF by mixing improvements and by the use of organic additives. Specifications were established on the materials and processes used in making the insulation.

Blome, J. C.↗

Cyclic arc plasma tests of RSI materials using a preheater

The results of a test program are reported in which a preheater was used with an arc plasma stream to study the thermal response of samples of candidate reusable surface insulation materials for the space shuttle. The preheater simulated the shuttle temperature history during the first and last portions of the test cycle, which could not be simulated by the air arc plasma flow. Pre- and post-test data taken for each of the materials included magnified views, optical properties, and chemical analyses. The test results indicate that the mullite base samples experience higher surface temperatures than the other materials at heating rates greater than 225 kw/sq m. The ceramic fibrous mullite and silica coatings show noncatalytic wall behavior. Internal temperature response data for the materials are compared and correlated with analytical predictions.

Stewart, D. A.↗

Results of RSI Thermal-structural Analysis

Thermostructural comparisons of mullite and silica reusable surface insulation materials for space shuttle application show that mullite is much more subject to thermal stress failure than silica composite materials.

Pigg, O. E.↗

Thermal characterization of reusable external insulation for the space shuttle.

Thermal protection systems utilizing reusable ceramic external insulations are under study for application to the orbiter vehicle of NASA's space shuttle system which is to be launched by an expendable booster, remain in orbit for a week or two, reenter the earth's atmosphere, and land like a conventional aircraft. The required reuse capability is for 100 missions. The thermal characterization of the reusable external insulation (REI) is described. Thermal conductivity measurements are described for a series of mullite-based REIs with densities ranging from 100 to 300 kg/cu m, including opacified variations of the mullite material designed for reduction of the radiant component of heat transport. The results of thermal conductivity measurements performed on guarded-hot-plate equipment from 150 to above 1200 K in different vacuum and gaseous environments are described. Measurements were also made with exceptionally large temperature differences to detect transparency effects in the unopacified REIs. These measurements were made to provide design data for the flight conditions, and to aid in theoretical computations aimed at separating and optimizing the heat transport components.

Brazel, J. P.↗

Theoretical study of production of unique glasses in space

The potential of producing the glassy form of selected materials in the weightless, containerless nature of space processing is examined through the development of kinetic relationships describing nucleation and crystallization phenomena. Transformation kinetics are applied to a well-characterized system (SiO2), an excellent glass former (B2O3), and a poor glass former (Al2O3) by conventional earth processing methods. Viscosity and entropy of fusion are shown to be the primary materials parameters controlling the glass forming tendency. For multicomponent systems diffusion-controlled kinetics and heterogeneous nucleation effects are considered. An analytical empirical approach is used to analyze the mullite system. Results are consistent with experimentally observed data and indicate the promise of mullite as a future space processing candidate.

Larsen, D. C.↗