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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Thermoelectric Properties and Morphology of Si/SiC Thin-Film Multilayers Grown by Ion Beam Sputtering

Multilayers (MLs) of 31 bi-layers and a 10-nm layer thickness each of Si/SiC were deposited on silicon, quartz and mullite substrates using a high-speed, ion-beam sputter deposition process. The samples deposited on the silicon substrates were used for imaging purposes and structural verification as they did not allow for accurate electrical measurement of the material. The Seebeck coefficient and the electrical resistivity on the mullite and the quartz substrates were reported as a function of temperature and used to compare the film performance. The thermal conductivity measurement was performed for ML samples grown on Si, and an average value of the thermal conductivity was used to find the figure of merit, zT, for all samples tested. X-ray diffraction (XRD) spectra showed an amorphous nature of the thin films. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to study the film morphology and verify the nature of the crystallinity. The mobility of the multilayer films was measured to be only 0.039 to 1.0 cm 2 /Vs at room temperature. The samples were tested three times in the temperature range of 300 K to 900 K to document the changes in the films with temperature cycling. The highest Seebeck coefficient is measured for a Si/SiC multilayer system on quartz and mullite substrates and were observed at 870 K to be roughly -2600 μV/K due to a strain-induced redistribution of the states’ effect. The highest figure of merit, zT, calculated for the multilayers in this study was 0.08 at 870 K.

36 MATERIALS SCIENCE↗
NASA NTRS1973

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.↗
NASA NTRS1992

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.↗
DOE OSTI2020

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↗
DOE OSTI2021

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↗
DOE OSTI2018

Interface Analyses Between a Case-Hardened Ingot Casting Steel and Carbon-Containing and Carbon-Free Refractories

Corrosion tests of carbon-free and carbon-containing refractories were performed. The carbon-free crucibles corroded, whereas the carbon-containing crucibles were negligibly attacked. On them, inclusions were attached. This study investigates melt oxygen contents, interface properties, and steel compositions with their non-metallic inclusions in order to explore the inclusion formation and deposition mechanisms. The carbon-free crucibles were based on alumina, mullite, and zirconia- and titania-doped alumina (AZT). The carbon-containing (-C) ones were alumina-C and AZT-C. Furthermore, nanoscaled carbon and alumina additives (-n) were applied in an AZT-C-n material. In the crucibles, the case-hardened steel 17CrNiMo7-6 was remelted at 1580 °C. It was observed that the melt and steel oxygen contents were higher for the tests in the carbon-free crucibles. Into these crucibles, the deoxidizing alloying elements Mn and Si diffused. Reducing contents of deoxidizing elements resulted in higher steel oxygen levels and less inclusions, mainly of the inclusion group SiO 2 -core-MnS-shell (2.5 to 8 μm). These developed from smaller SiO 2 nuclei. The inclusion amount in the steel was highest after remelting in AZT-C-n for 30 minutes but decreased strongly with increasing remelting time (60 minutes) due to inclusions’ deposition on the refractory surface. The Ti from the AZT and the nanoadditives supported inclusion growth and deposition. Other inclusion groups were alumina and calcium aluminate inclusions. Their contents were high after remelting in carbon- or AZT-containing crucibles but generally decreased during remelting. On the AZT-C-n crucible, a dense layer formed from vitreous compositions including Al, Ca, Mg, Si, and Ti. To summarize, for reducing forming inclusion amounts, mullite is recommended as refractory material. For capturing formed inclusions, AZT-C-n showed a high potential.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Plasma electrolytic oxidation coating of synthetic Al-Mg binary alloys

The binary Al-Mg synthetic alloys were prepared in a vacuum/atmosphere controlled furnace with the addition of 0.5, 1, 2, 4, 7, and 15 wt.% pure Mg into pure aluminum as substrate material. The surfaces of the Al-Mg alloys and pure aluminum were coated for 120 min by plasma electrolytic oxidation in the same electrolyte of 12 g/L sodium silicate and 2 g/L KOH in distilled water. The coating was characterized by X-ray diffraction, scanning electron microscopy, profilometry and Vickers microhardness measurements. There regions of loose outer layer, dense inner layer with precipitate like particles of {alpha}-Al{sub 2}O{sub 3} and a thin transition layer were identified for the coated samples. The coating thickness increases from 85 to 150 {mu}m with Mg contents in the alloys. The surface morphology becomes more porous and consequently surface roughness tends to increase with plasma electrolytic oxidation treatment and further with Mg content. The increase in magnesium content reduces the formation of {alpha}-Al{sub 2}O{sub 3} and crystalline mullite phases in the coating and decreases microhardness of coating. The Mg concentration is constant throughout the other loose and dense regions of coating though it gradually decreases in the thin inner region. - Research Highlights: Black-Right-Pointing-Pointer The average thickness of PEO coating of Al-Mg alloys increases with Mg content. Black-Right-Pointing-Pointer The addition of Mg reduces and prevents the formation of {alpha}-Al{sub 2}O{sub 3} and mullite. Black-Right-Pointing-Pointer The surface roughness increases with Mg content in the Al-Mg alloys. Black-Right-Pointing-Pointer The hardness values of the coating decreases with the Mg amount in the substrate. Black-Right-Pointing-Pointer The Mg concentration is constant throughout the main regions of coating.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Transition-metal substitution in PbAlBO{sub 4}: Synthesis, structural and spectroscopic studies of manganese containing phases

Highlights: ► Synthesis of mullite-type PbAl{sub 1−x}Mn{sub x}BO{sub 4} by solid state and glycerin methods. ► Fundamental parameter approach describes the X-ray powder diffraction profiles. ► Cell parameters anisotropically change with increasing Mn in the structure. ► Bond valence sums of Pb{sup 2+} linearly correlates eccentricity parameter. ► FTIR spectra confirm the trigonal planar BO{sub 3}. -- Abstract: Mullite-type metal borates PbAlBO{sub 4} with planar BO{sub 3} groups are potential candidates for nonlinear optical properties. We successively substituted aluminum with manganese in the composition PbAl{sub 1−x}Mn{sub x}BO{sub 4}, which would help tuning the crystal chemistry and related physical properties. The end member PbAlBO{sub 4} was synthesized by conventional solid state reaction; the other members of the PbAl{sub 1−x}Mn{sub x}BO{sub 4} series were prepared by glycerin method. The fundamental parameter approach was applied in the Rietveld refinements to describe the X-ray powder diffraction profiles. The cell parameters and interatomic bond distances were studied with respect to the chemical composition x. The MO{sub 6} octahedral distortion linearly increased with the averaged M-O bond distance, which is correlated with the increasing amount of manganese atoms in the structure. The change of the average crystal size and microstrain were explained in terms of Al/Mn ratio in the solid solution. While the empirical bond-valence sums (BVS) of one oxygen atom, bridging the edge-sharing MO{sub 6} octahedron, were found to be under-bonded, the other one was over-bonded. The stereoactivity of the 6s{sup 2} lone electron pair of the Pb{sup 2+} cation was characterized in terms of the absolute value of eccentricity parameter (|Φ{sub i}|). Both bond valence parameter (r{sub 0i}) and BVS of Pb showed a linear correlation with |Φ{sub i}|. Deconvolution of the absorption feature of the infrared powder spectra between 1000 cm{sup −1} and 1400 cm{sup −1} required four fitted bands, which were assigned to B-O stretching vibrations of the trigonal planar BO{sub 3} groups. With increasing Al{sup 3+} dilution in PbAl{sub 1−x}Mn{sub x}BO{sub 4} almost all observed modes shifted toward lower wavenumbers confirming the solid solution. The absorptions caused by the vibrations of the heavy atom Pb were observed in the far-IR region.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Processing and characterization of multi-cellular monolithic bioceramics for bone regenerative scaffolds

Multicellular monolithic ceramic body is a ceramic material which has many gas or liquid passages partitioned by thin walls throughout the bulk material. There are many currently known advanced industrial applications of multicellular ceramics structures i.e. as supports for various catalysts, electrode support structure for solid oxide fuel cells, refractories, electric/electronic materials, aerospace vehicle re-entry heat shields and biomaterials for dental as well as orthopaedic implants by naming only a few. Multicellular ceramic bodies are usually made of ceramic phases such as mullite, cordierite, aluminum titanate or pure oxides such as silica, zirconia and alumina. What make alumina ceramics is excellent for the above functions are the intrinsic properties of alumina which are hard, wear resistant, excellent dielectric properties, resists strong acid and alkali attacks at elevated temperatures, good thermal conductivities, high strength and stiffness as well as biocompatible. In this work the processing technology leading to truly multicellular monolithic alumina ceramic bodies and their characterization are reported. Ceramic slip with 66 wt.% solid loading was found to be optimum as impregnant to the polyurethane foam template. Mullitic ceramic composite of alumina-sodium alumino disilicate-Leucite-like phases with bulk and true densities of 0.852 and 1.241 g cm{sup −3} respectively, pore linear density of ±35 cm{sup −1}, linear and bulk volume shrinkages of 7-16% and 32 vol.% were obtained. The compressive strength and elastic modulus of the bioceramics are ≈0.5-1.0 and ≈20 MPa respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2019

The Effect of Glass Chemistry on Caesium Volatility

The UK currently has 99,000 m3 of intermediate level waste (ILW). The current preferred treatment route is cementation. However, thermal treatment could offer a better long term option due to higher waste loading and lower storage costs. This project will focus on volatile retention in the vitrification process to make thermal treatment a more viable option. A series of iron phosphate base glasses were prepared with the nominal molar composition xM{sub y}O{sub z}(40 - x)Fe{sub 2}O{sub 3}-P{sub 2}O{sub 5} (M{sub y}O{sub z} = B{sub 2}O{sub 3}, MnO, ZnO with x = 5%). Samples are given names of the form IPG-1-X5 where X = B, Mn or Zn. For all batches, reagents were weighed and mechanically mixed to produce 150 g of glass. melted at 1150 deg. C for 3 h, Samples were immediately transferred to an annealing furnace and annealed at 450 deg. C for 1 h before being cooled to room temperature at 1 deg. C min{sup -1}. 75 g batches was produced with a target of 2 wt.% caesium oxide. Each batch was placed into a mullite crucible and placed in the sealed system seen below. Each canister was placed into a top-loading resistance furnace and ramped to 950 deg. C at a rate of 3 deg. C min{sup -1} under a nitrogen atmosphere with a flowrate of ∼0.9 L min{sup -1}. The samples were held at this temperature for 3 h before power to the furnace was removed and the system allowed to cool naturally. Once cool, the steel canister was opened and the entire apparatus (steel canister, mullite crucible and tubing) was washed through with ∼50 ml of 0.5 M HNO{sub 3} to allow for a complete mass balance of the caesium species. A series of Iron Phosphate glasses have been produced and characterised to investigate the influence of glass chemistry on the volatility of caesium. All glasses were doped with ∼2 wt.% Cs{sub 2}O and re-melted at 950 deg. C for 3 hours in a specially designed furnace set-up. Results of these experiments showed that the addition of 5 mol. % ZnO greatly increased the retention of Cs{sub 2}O whilst B{sub 2}O{sub 3} was detrimental to the Cs{sub 2}O retention. A series of iron phosphate based glasses have been produced with 5 mol.% additions of B{sub 2}O{sub 3}, MnO and ZnO, substituted in place of Fe{sub 2}O{sub 3}. All samples were analysed before and after being doped and re-melted with a 2 wt.% addition of Cs{sub 2}O. The effect of each additive on the base glass has been reported showing that both B{sub 2}O{sub 3} and ZnO increase the glass transition temperature, whilst MnO additions decrease the thermal stability of the glass. The Q-speciation of the glasses was investigated, and the results showed that the additives did not significantly influence the Q-speciation in comparison to the base glass. It has been shown that the addition of ZnO dramatically increases the retention of Cs during re-melting by almost a factor of 10 in comparison to the base glass, whilst the addition of MnO addition increased the caesium retention but only by a factor of ∼3. The addition of B{sub 2}O{sub 3} had a detrimental effect on the volatility in comparison to the 40Fe{sub 2}O{sub 3}-60P{sub 2}O{sub 5} base glass.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

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↗
DOE OSTI2012

Zr doped anatase supported reticulated ceramic foams for photocatalytic water purification

Highlights: ► Thick photocatalytic anatase films on macroporous reticulated ceramic foams. ► Alumina and alumina–mullite macroporous reticulated foams as photocatalyst support. ► Zr doping significantly improves the TiO{sub 2} film activity in phenol photomineralization. ► Comparison of photocatalytic activity of thick films and powder suspensions. -- Abstract: Titanium dioxide films were deposited on macroporous reticulated Al{sub 2}O{sub 3} and alumina–mullite foams with pore sizes of 15 ppi (pores per inch). Coatings were prepared from suspensions of precursor powders of Aeroxide{sup ®} P25 nanopowder and precipitated TiO{sub 2} by using a dip coating process. The TiO{sub 2} forms films with a thickness of ∼2–20 μm. The photocatalytic activity was characterized as the mineralization rate of an aqueous phenol solution under UVA irradiation by the TOC technique. Precipitated TiO{sub 2} films have nearly the same photocatalytic activity as a titania suspension, in which powder aggregates have a size comparable with the thickness of the films. Samples made of Aeroxide{sup ®} P25 nanopowder, in which the size of aggregates is ∼0.1 μm show higher efficiency of photodecomposition in suspensions with films. The doping of precipitated anatase with Zr(IV) in the atomic ratio Zr/Ti = 0.008 significantly improves the photocatalytic activity of the foam supported titania. Zr doped anatase films show better performance as the films prepared only from Aeroxide{sup ®} P25 nanopowder.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Feasible voltage-tap based quench detection in a Ag/Bi-2212 coil enabled by fast 3D normal zone propagation

For this study, small insert solenoids have been built using a commercial Ag/Bi-2212 multifilamentary round wire, insulated with a new thin TiO 2 – polymer coating insulation (thickness in ~20 μm versus ~100 μm for a commonly used mullite braided sleeve insulation), and characterized in background magnetic field up to 14 T at 4.2 K to explore the high-field performance and quench detection of Bi-2212 magnets. The coil has no visible leakage and no electrical shorts after reaction, and it carries 280 A/mm -2 in a background field 14 T and generates an additional 1.7 T. A notable result is that, despite normal zones propagate slowly along the conductor, the hot spot temperature upon detection increases only from 40 K to 60 K when the resistive quench detection voltage threshold increases from 0.1 V to 1 V for all operating current density investigated, showing that quench detection using voltage taps is feasible for this coil. This is in a strong contrast to a coil we previously built to the same specifications but from wires insulated with the mullite braided sleeve insulation, for which the hot spot temperature upon detection increases from ~80 K to ~140 K while increasing from the detection voltage threshold from 0.1 V to 1 V, and thus for which quench detection using voltage taps presents significant risks, consistent with the common belief that the effectiveness of quench detection using voltage taps for superconducting magnets built using high temperature superconductors is seriously compromised by their slow normal zone propagation. This striking difference is ascribed to the fast transverse quench propagation enabled by thin insulation and improved thermal coupling between conductor turns. Finally, this work demonstrates that quench detection for high-temperature superconducting magnets highly depends on the design and construction of the coils such as insulation materials used and this dependence should be factored into the overall magnet design.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterization of Rare Earth Element Minerals in Coal Utilization Byproducts

The United States currently produces over 100 million tons of coal utilization byproducts (CUB) per year in the form of fly ash, bottom ash, slag, and flue gas (American Coal Ash Association (ACCA), 2015). But this “waste material” also contains potentially useful levels of rare earth elements (REE). Rare earth elements are crucial for many existing and emerging technologies, but the U.S. lacks a domestic, sustainable REE source. Our project explored the possibility of developing a supply of REEs for U.S. technologies by extracting REEs from CUBs. This work offers the potential to reduce our dependence on other countries for supply of these critical elements (NETL, REE 2016 Project Portfolio). Geologic and diagenetic history, industrial preparation methods, and the specific combustion process all play major roles in the composition of CUB. During combustion, inorganic mineral phases of coal particles are fluidized at temperatures higher than 1400oC, so inorganic mineral materials are oxidized, fused, disintegrated, or agglomerated into larger spherical and amorphous (non-crystalline) particles. The original mineralogy of the coal-containing rock and heating/cooling of the material significantly affects the composition and morphology of the particles in the combustion byproduct (Kutchko and Kim, 2006). Thus, different types of coal/refuse/ash must be characterized to better understand mineral evolution during the combustion process. Our research focused on developing a working model to address how REE minerals behave during the combustion process: this research should help determine the most effective engineering methods for extracting REEs from CUBs. We used multimodal imaging and image processing techniques to characterize six rock and ash samples from different coal power plants with respect to morphology, grain size, presence of mineral phases, and elemental composition. The results of these characterization activities provided thresholds for realizing the occurrence of REE mineral phases in CUB and allowed us to calculate structural and volumetric estimates of REE. Collectively, the rock and coal ash samples contained minerals such as quartz, kaolinite, muscovite/illite, iron oxide (as hematite or magnetite), mullite, and clinochlore. Trace minerals included pyrite, zircon, siderite, rutile, diopside, foresterite, gypsum, and barite. We identified REE phosphate minerals monazite (Ce,La,Nd,Th)(PO 4 ,SiO 4 ), xenotime (YPO 4 ,SiO 4 ), and apatite (Ca 5 (PO 4 ) 3 (F,Cl,OH) via SEM and electron microprobe analysis: these materials generally occurred as 1-10 μm-long crystals in the rock and ash samples. As has been shown in other studies, amorphous material-aluminosilicate glass or iron oxyhydroxide-are the major components of coal fly and bottom ash. Trace amounts of amorphous calcium oxide and mixed element (e.g., Al-Si-Ca-Fe) slag are also present. Quartz, mullite, hematite, and magnetite are the crystalline phases present. We found that REEs are present as monomineralic grains dispersed within the ash, as well as fused to or encapsulated by amorphous aluminosilicate glass particles. Monazite and xenotime have relatively high melting points (>1800 °C) compared to typical combustion temperatures; our observations indicate that the REE-phosphates, which presumably contribute a large percentage of REE to the bulk ash REE pool, as measured by mass spectroscopy, are largely unaltered by the combustion. Our study shows that conventional coal combustion processes sequester REE minerals into aluminosilicate glass phases, which presents a new engineering challenge for extracting REE from coal ash. The characterization work summarized in this report provides a semi-quantitative assessments of REE in coal-containing rock and CUB. The data we obtained from 2- and 3-D imaging, elemental mapping, volumetric estimates, and advanced high-resolution pixel classification successfully identified the different mineral phases present in CUB. Further, our characterization results can guide techniques for extracting REEs from CUB, or other geologic and engineered materials. Whilst, interpretations will inform future REE separation and extraction techniques and technologies practical for commercial utilization of combustion byproducts generated by power plants.

01 COAL, LIGNITE, AND PEAT↗
NASA NTRS1972

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.↗
NASA NTRS1973

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.↗
NASA NTRS1973

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.↗