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Formation of carbon monoxide gas is prevented by a linear of refractory material free of elemental carbon. For pressures above about 4 torr, silicon carbide can be used as refractory liner. The problem of carbide contamination can arise in crystal growth of any material that forms a carbide more stable than carbon monoxide. Prevention in such cases is possible by using noncarbon refractories in place of graphite.
Vertical access solar furnace experiments have produced refractory residues, condensates and chondrules that are similar to components of chondritic meteorites. In particular, Ca-Al-rich refractory residues similar in chemistry to inclusions in carbonaceous chondrites have been produced by partial evaporation of basaltic bulk rock samples. Fe-Mg-Si-rich condensates with distinctive microbotryoidal morphology have been collected from the same sample runs. Particle coatings and aggregates with virtually identical microbotryoidal morphology and major element chemistry have been identified in both the Allende and Murchison meteorites. Spattered drops from melt beads undergoing heating and partial evaporation resemble some meteoritic chondrules in their mineralogies, textures, grain size, and sorting. The spatter mechanism is highly efficient in the production of chondrules. If any of the refractory inclusions in chondrites are, in fact, partial evaporation residues, many meteoritic fluid drop chondrules must have been formed by this process. The hot central portion of the solar nebula, acting on a cloud of dust and gas, is the probable source of heat required to produce the fractionated chemistry and physical state of many of the components of chondritic meteorites.
Results are reported for a comprehensive petrographic survey of the refractory inclusions in the Allende and Mokoia CV3 chondrites. More than 600 refractory inclusions in 22 thin sections of the meteorites were studied by optical and scanning-electron microscopy. Olivine-rich inclusions and Ca, Al-rich inclusions (CAIs) are aggregates of various combinations of three fundamental petrographic constituents: rimmed concentric objects, Ca, Si-rich chaotic material, and mafic inclusion matrix. A new classification system for refractory inclusions is developed that is based on the size and abundance of these three fundamental constituents. The new classification system avoids several problems that are inherent in other classification systems, which use the term 'coarse-grained' too restrictively for many simple CAIs and inaccurately for most mililite-rich complex CAIs.
Space power requirements for future NASA and other U.S. missions will range from a few kilowatts to megawatts of electricity. Maximum efficiency is a key goal of any power system in order to minimize weight and size so that the Space Shuttle may be used a minimum number of times to put the power supply into orbit. Nuclear power has been identified as the primary power source to meet these high levels of electrical demand. One method to achieve maximum efficiency is to operate the power supply, energy conservation system, and related components at relatively high temperatures. For systems now in the planning stages, design temperatures range from 1300 K for the immediate future to as high as 1700 K for the advanced systems. NASA Lewis Research Center has undertaken a research program on advanced technology of refractory metal alloys and composites that will provide baseline information for space power systems in the 1900's and the 21st century. Special emphasis is focused on the refractory metal alloys of niobium and on the refractory metal composites which utilize tungsten alloy wires for reinforcement. Basic research on the creep and creep-rupture properties of wires, matrices, and composites are discussed.
Refractories - materials which are able to withstand extremely high temperatures - are sure to be an important part of any processing facility or human outpost which is built on Mars. Containers for processing lunar oxygen will need high temperature components. Fabrication of structural material from lunar resources need both containment vessels to hold high temperature melts and molds in which to form the final shapes. Certainly, it would be desirable to fabricate such vessels and molds on the Moon, rather than carrying them up from the Earth. At first glance, this might appear to be a trivial task, since the Moon's surface consists of a variety of refractory compositions. To turn the regolith into a useful fire brick or mold, however, will require water or other binders and additives which are likely to be in extremely short supply on the Moon. The steps needed to make fire bricks and molds for lunar-derived structural materials are examined, pointing out the critical steps and resources which will be needed. While these processes and applications may seem somewhat mundane, it is emphasized that it is precisely these rudimentary processes which must be mastered before discussing making aerobrakes, and other fancier refractories from lunar resources.
Silicon-base ceramics are promising candidate materials for high temperature structural applications such as heat exchangers, gas turbines and advanced internal combustion engines. Composites based on these materials are leading candidates for combustor materials for HSCT gas turbine engines. These materials possess a combination of excellent physical and mechanical properties at high temperatures, for example, high strength, high toughness, high thermal shock resistance, high thermal conductivity, light weight and excellent oxidation resistance. However, environmental durability can be significantly reduced in certain conditions such as when molten salts, H2 or water vapor are present. The oxidation resistance of silicon-base materials is provided by SiO2 protective layer. Molten salt reacts with SiO2 and forms a mixture of SiO2 and liquid silicate at temperatures above 800C. Oxygen diffuses more easily through the chemically altered layer, resulting in a catastrophic degradation of the substrate. SiC and Si3N4 are not stable in pure H2 and decompose to silicon and gaseous species such as CH4, SiH, SiH4, N2, and NH3. Water vapor is known to slightly increase the oxidation rate of SiC and Si3N4. Refractory oxides such as alumina, yttria-stabilized zirconia, yttria and mullite (3Al2O3.2SiO2) possess excellent environmental durability in harsh conditions mentioned above. Therefore, refractory oxide coatings on silicon-base ceramics can substantially improve the environmental durability of these materials by acting as a chemical reaction barrier. These oxide coatings can also serve as a thermal barrier. The purpose of this research program has been to develop refractory oxide chemical/thermal barrier coatings on silicon-base ceramics to provide extended temperature range and lifetime to these materials in harsh environments.
Rigid fibrous refractory insulations (TPS tiles) are integral components of many spacecraft thermal protection systems. These materials are composed of refractory fibers With diameters on the order of 1 to 15 micrometers. They are lightweight and have an open, highly porous microstructure. Typical densities are less than 500 kilograms per cubic meters, and porosities generally exceed 0.8. Because of their open porosity, these materials are permeable to gas glow. There are numerous instances in which internal gas transport in a thermal protection system could be important; examples include the penetration of hot boundary-layer gases into the insulation, the flow of decomposition (pyrolysis) products from the interior, the use of convective flows to mitigate ice formation caused by cryopumping, and the design of refractory vents for pressure equilibration during atmospheric entry. Computational analysis of gas flow through porous media requires values of permeability which have not previously been available for the rigid fibrous insulations used in thermal protection systems. This paper will document measurements of permeability for a variety of insulations from NASA's LI, FRCI, and AETB families of lightweight ceramic ablators. The directional anisotropy of permeability and its dependence on gas pressure and material density will be presented. It will be shown that rarified-flow effects are significant in the flow through such materials. Connections will be drawn between the insulation microstructure and permeability. The paper will also include representative computations of flow through rigid fibrous insulations.
An electrode having increased output with slower degradation is formed of a film applied to a beta-alumina solid electrolyte (BASE). The film comprises a refractory first metal M.sup.1 such as a platinum group metal, suitably platinum or rhodium, capable of forming a liquid or a strong surface adsorption phase with sodium at the operating temperature of an alkali metal thermoelectric converter (AMTEC) and a second refractory metal insoluble in sodium or the NaM.sup.1 liquid phase such as a Group IVB, VB or VIB metal, suitably tungsten, molybdenum, tantalum or niobium. The liquid phase or surface film provides fast transport through the electrode while the insoluble refractory metal provides a structural matrix for the electrode during operation. A trilayer structure that is stable and not subject to deadhesion comprises a first, thin layer of tungsten, an intermediate co-deposited layer of tungsten-platinum and a thin surface layer of platinum.
Much of Pluto's surface consists of N2 ice with smaller amounts of CH4 and CO ices. Despite the low temperature (approximately 45K), chemistry can be driven in the surface ices by radiation processing such as cosmic ray bombardment. When cosmic rays strike the surface, much of their energy is dispersed in the form of secondary electrons, which in turn drive much of the resulting chemical reactions. Laboratory experiments designed to simulate the conditions on these icy bodies may provide insight into this chemistry. Significant progress has been made in the laboratory toward understanding the smaller, simple compounds produced in the solid phase by radiation processing of (N2, CH4, CO) ices (Bohn et al. 1994; Moore & Hudson 2003; Hodyss et al. 2011; Kim and Kaiser 2012). Recently Materese et al. (2014) used a variety of techniques to better characterize the refractory materials produced from the UV photo-irradiation of N2:CH4:CO ices. However, because Pluto's atmosphere is optically thick to Lyman-alpha UV radiation it is important to re-examine the results using an alternate radiation source. Our latest work has consisted of the analysis of refractory materials produced from the electron bombardment of low temperature N2(‐), CH4(‐), and CO(‐)containing ices (100:1:1). The ice mixture was chosen to be analogous to the known surface ices on Pluto and the radiation source was chosen to mimic the secondary electrons produced by cosmic rays bombardment. The residues were studied using multiple chemical techniques including, infrared (IR) spectroscopy, X‐ray absorption near‐edge structure (XANES) spectroscopy, and gas chromatography coupled with mass spectrometry (GC‐MS). The organic residues produced in these experiments can be seen as an analog for the refractory component of the surface of Pluto, and are compared with the residues previously obtained from UV photo‐irradiation. UV and near‐ IR spectroscopy of the surfaces of Pluto and Charon during the encounter with NASA's New Horizons spacecraft in 2015, will give the first close‐up measurements of ices and their photoproducts. Laboratory measurements and experiments will provide a better context for the data returned by the spacecraft.
- NASA Refractory Alloy Projects: - STMD-GRC – Refractory Alloy Additive Manufacturing Build Optimization (RAAMBO) - Hypersonic Technology (HTP) Project. - Advance material characterization and prototypic testing allowing for critical data needed to demonstrate TRL advancement and for component flight qualification - Enable national supply chain for refractory alloy feedstock essential for production of historical to custom alloys for R&D to component fabrication. - Develop materials and processing for high performance in extreme environments enabling technologies for Moon to Mars missions.
Severe distortion is one of the four core effects in single-phase high-entropy alloys (HEAs) and contributes significantly to the yield strength. However, the connection between the atomic-scale lattice distortion and macro-scale mechanical properties through experimental verification has yet to be fully achieved, owing to two critical challenges: 1) the difficulty in the development of homogeneous single-phase solid-solution HEAs and 2) the ambiguity in describing the lattice distortion and related measurements and calculations. Here, a single-phase body-centered-cubic (BCC) refractory HEA, NbTaTiVZr, using thermodynamic modeling coupled with experimental verifications, is developed. Compared to the previously developed single-phase NbTaTiV HEA, the NbTaTiVZr HEA shows a higher yield strength and comparable plasticity. The increase in yield strength is systematically and quantitatively studied in terms of lattice distortion using a theoretical model, first-principles calculations, synchrotron X-ray/neutron diffraction, atom-probe tomography, and scanning transmission electron microscopy techniques. These results demonstrate that severe lattice distortion is a core factor for developing high strengths in refractory HEAs.
Extending the concept of complex concentrated alloys (CCAs) to the refractory alloys (solidus temperature over 2000 °C) space potentially facilitates the design of lightweight structural alloys with service temperatures that exceed those of Ni and Co‐based alloys. However, the room and elevated temperature tensile properties of the current refractory‐CCAs (R‐CCAs) are inferior to those of the Ni/Co‐based alloys. Furthermore, the manufacturing scalability of R‐CCAs remains challenging, in that cracks are prevalent in all R‐CCAs when processed using near‐net shape manufacturing processes, such as fusion‐based additive manufacturing (F‐BAM). Still, mechanisms governing the poor F‐BAM processability of R‐CCAs remain unexplored. Here, to this end, this work unveils the atomistic mechanisms underlying F‐BAM process‐induced cracking in a NbTiTaMoHfZrC R‐CCA. The implications of light elements’ presence for intrinsic ductility and grain boundary cohesion, and subsequently for F‐BAM processability and mechanical behavior, are revealed. Leveraging the insights, we accomplish what is, to the best of the knowledge, the first instance of crack‐free F‐BAM processing of any R‐CCA. Additionally, the R‐CCA exhibits over 20% tensile ductility and ≈160 MPa tensile yield strength at 1200 °C. In addition to facilitating the design of lightweight R‐CCAs, findings enable scalable manufacturing of these ultra‐high temperature alloys for structural applications.
Transition metal nitrides have recently gained attention in the fields of plasmonics, plasmon-enhanced photocatalysis, photothermal applications, and nonlinear optics because of their suitable optical properties, refractory nature, and large laser damage thresholds. Here we report comparative studies of the transient response of films of titanium nitride (TiN), zirconium nitride (ZrN), and gold (Au) under femtosecond excitation. Broadband transient optical characterization helps to adjudicate earlier, somewhat inconsistent reports regarding hot electron lifetimes based upon single wavelength measurements. These pump–probe experiments show sub-picosecond transient dynamics only within the epsilon-near-zero window of the refractory metals. The dynamics are dominated by photoinduced interband transitions resulting from ultrafast electron energy redistribution. The enhanced reflection modulation in the epsilon-near-zero window makes it possible to observe the ultrafast optical response of these films at low pump fluences. These results indicate that electron–phonon coupling in TiN and ZrN is 25–100 times greater than in Au. Strong electron–phonon coupling drives the sub-picosecond optical response and facilitates greater lattice heating compared to Au, making TiN and ZrN promising for photothermal applications. The spectral response and dynamics of TiN and ZrN are only weakly sensitive to pump fluence and pump excitation energy. However, the magnitude of the response is much greater at higher pump photon energies and higher fluences, reaching peak observed values of 15% in TiN and 50% in ZrN in the epsilon-near-zero window.
IntroductionTransarterial chemoembolisation (TACE) is the most widely used locoregional treatment for patients with an unresectable hepatocellular carcinoma (HCC). Transarterial radioembolisation (TARE) with yttrium-90 containing microspheres is an emerging interventional treatment that could be complementary or an alternative to TACE.AimTo evaluate the safety and efficacy of TARE in patients with HCC who are refractory to TACE with drug-eluting beads (DEB-TACE).MethodsWe identified all patients who received TARE for HCC following one or more sessions of DEB-TACE in the period 2007–2016. Grade ≥3 adverse events were graded according to Common Terminology Criteria for Adverse events. Response on MRI was determined on MRI by modified RECIST. Overall survival was estimated using the Kaplan–Meier method and was determined from the first TACE and from the TARE procedure.ResultsA total of 30 patients were included. Patients had a mean of 1.7 TACE procedures (range 1–4) prior to TARE. Grade 3 adverse events following TARE included: fatigue (20%), bilirubin increase (10%), cholecystitis (3.3%) and a gastric ulcer (3.3%). Response on MRI was achieved in 36.7%. Three patients (10%) were downstaged within the Milan criteria and received liver transplantation. The median overall survival after first TACE was 32.3 months (17.2–42.1 95% CI). The median overall survival after TARE was 14.8 months (8.33–26.5 95% CI).ConclusionTARE is safe and can be effective in patients with an intermediate or advanced stage HCC who are refractory to TACE. This treatment strategy has the potential to downstage to liver transplantation.
Recently, approximately 80% of participating laboratories failed to accurately determine uranium isotopes in soil samples in the U.S Department of Energy Mixed Analyte Performance Evaluation Program (MAPEP) Session 30, due to incomplete dissolution of refractory particles in the samples. Failing laboratories employed acid dissolution methods, including hydrofluoric acid, to recover uranium from the soil matrix. The failures illustrate the importance of rugged soil dissolution methods for the accurate measurement of analytes in the sample matrix. A new rapid fusion method has been developed by the Savannah River National Laboratory (SRNL) to prepare 1-2 g soil sample aliquots very quickly, with total dissolution of refractory particles. Soil samples are fused with sodium hydroxide at 600 ºC in zirconium crucibles to enable complete dissolution of the sample. Uranium and thorium are separated on stacked TEVA and TRU extraction chromatographic resin cartridges, prior to isotopic measurements by alpha spectrometry on cerium fluoride microprecipitation sources. Plutonium can also be separated and measured using this method. Batches of 12 samples can be prepared for measurement in <5 hours.
Cr (III)-containing refractories are widely used as electric-arc furnace cover because of their excellent corrosion resistance properties. However, the formation of hexavalent chromium [Cr(VI)] remains a matter of concern during the service and subsequent disposal of the spent refractories. Moreover, the Cr(VI) formation mechanism and total amount of Cr(VI) generated are not clearly understood. In this study, samples from different parts of a spent electric arc furnace cover were collected from a local integrated steel plant. The phase composition, microstructure, formation and leachability of Cr(VI) were investigated using X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy, and TRGS 613 leaching test (Technische Regeln für Gefahrstoffe-TRGS 613-October 2002)/multiple leaching tests. A Cr(VI)-containing phase namely CaCrO{sub 4} existed in the sample at a medium temperature range, while another Cr(VI)-containing phase namely hauyne (Ca{sub 4}Al{sub 6}CrO{sub 16}) and a Cr(III)-containing phase (Al{sub 2}O{sub 3}–Cr{sub 2}O{sub 3} solid solution) formed in the high temperature region. Concentrations of Cr(VI) in the leachates (as in the TRGS 613 procedure) exceeded the European permissible limit. During the leaching tests in an acid condition, Cr(VI) was reduced by Fe{sup 2+}, which was primarily derived from the dissolution of FeO in the samples, while more Cr(VI) leached out with distilled water. Formation of an Al{sub 2}O{sub 3}–Cr{sub 2}O{sub 3} solid solution can inhibit Cr(VI) generation.
S and As are common impurities in refractory gold ores and must be removed before gold extraction. Thermodynamic analyses show that it is possible to simultaneously remove S and As by an O{sub 2}-enriched single-stage roasting, which is confirmed with experimental results from roasting of a gold refractory ore. The range of optimal O{sub 2} requirement is narrow and varies with the S and As content in the ore. Both the extent of removal of S and As, and the subsequent recovery of gold achieved from the optimized single-stage roasting are comparable to those attained from two-stage roasting processes.
The interfacial reactions between liquid iron and MgO-based refractories were investigated based on the TiO{sub 2} concentration values. Substrates comprising MgO, MgO-TiO{sub 2} (MT), MgO-Al{sub 2}O{sub 3} (MA), and MgO-Al{sub 2}O{sub 3}, at loadings of 3, 6, 9, 12, and 15 wt pct TiO{sub 2} (MAT3-15), were reacted with liquid iron at 1823 K by using the sessile drop technique. Microscopic analysis by SEM/EDX and the associated thermochemical calculations by Factsage 7.0™ confirmed the reaction mechanisms of different refractory materials. MgO and MT showed higher resistance against liquid iron penetration compared with MA and MAT3-15, which was attributed to the formation of a magnesiowustite (MO (M = Fe, Mg)) layer formed at the interfaces. Increasing the levels of TiO{sub 2} up to 6 wt pct contributed to the denser microstructure of MA. However, the contact angle was lowest for 9 wt pct of TiO{sub 2} and then gradually increased up to 15 wt pct. Chemical reactions generating a liquid slag phase contributed to the fluctuations in contact angle with respect to TiO{sub 2}.