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At least 73 records · Page 4

Ultra high purity, dimensionally stable INVAR 36

An INVAR 36 material having long-term dimensional stability is produced by sintering a blend of powders of nickel and iron under pressure in an inert atmosphere to form an alloy containing less than 0.01 parts of carbon and less than 0.1 part aggregate and preferably 0.01 part individually of Mn, Si, P, S and Al impurities. The sintered alloy is heat treated and slowly and uniformly cooled to form a material having a coefficient of thermal expansion of less than 1 ppm/C and a temporal stability of less than 1 ppm/year.

Sokolowski, Witold M.↗

Ultra high purity, dimensionally stable INVAR 36

An INVAR 36 material having long-term dimensional stability is produced by sintering a blend of powders of nickel and iron under pressure in an inert atmosphere to form an alloy containing less than 0.01 parts of carbon and less than 0.1 part aggregate and preferably 0.01 part individually of Mn, Si, P, S and Al impurities. The sintered alloy is heat treated and slowly and uniformly cooled to form a material having a coefficient of thermal expansion of less than 1 ppm/C and a temporal stability of less than 1 ppm/year.

Sokolowski, Witold M.↗

Formation of porous surface layers in reaction bonded silicon nitride during processing

An effort was undertaken to determine if the formation of the generally observed layer of large porosity adjacent to the as-nitride surfaces of reaction bonded silicon nitrides could be prevented during processing. Isostatically pressed test bars were prepared from wet vibratory milled Si powder. Sintering and nitriding were each done under three different conditions:(1) bars directly exposed to the furnance atmosphere; (2) bars packed in Si powder; (3) bars packed in Si3N4 powder. Packing the bars in either Si of Si3N4 powder during sintering retarded formation of the layer of large porosity. Only packing the bars in Si prevented formation of the layer during nitridation. The strongest bars (316 MPa) were those sintered in Si and nitrided in Si3N4 despite their having a layer of large surface porosity; failure initiated at very large pores and inclusions. The alpha/beta ratio was found to be directly proportional to the oxygen content; a possible explanation for this relationship is discussed.

Shaw, N. J.↗

Silicon carbide sintered products and a method for their manufacturing

SiC based sinters are produced by pressureless sintering from a SiC-AlN solid solution containing Al2 to 20, N 0.2 to 10, O 0.2 to 5, a Group IIIB element 0 to 15 percent, the remainder being Si and C. Thus, a 90:10 mixture of SiC and AlN powders were cold pressed at 2000 kg/sq cm and sintered for 5 hours at 2100 C in a nitrogen atmosphere. The resulting product had density of 3.11 g/cu cm and bending strength at ambient and 1400 C at 68.5 and 66.3 kg/sq mm.

Suzuki, K.↗

Gas pressure sintering of Beta-Sialon with Z=3

An experiment conducted on beta-sialon in atmospheric pressure, using a temperature of 2000 C and 4 MPa nitrogen atmosphere, is described. Thermal decomposition was inhibited by the increase of the nitrogen gas pressure.

Tani, E.↗

Fluid transport on earth and aeolian transport on Mars

Experimental data on cohesion-free particle transport in fluid beds are applied, via a universal scaling relation, to atmospheric transport of fine grains on Mars. It may be that cohesion due to impact vitrification, vacuum sintering, and adsorbed thin films of water are absent on Mars - in which case the curve of threshold velocity versus grain size may show no turnup to small particle size, and one micron diameter grains may be injected directly by saltation into the Martian atmosphere more readily than 100 micron diameter grains. Curves for threshold and terminal velocities are presented for the full range of Martian pressures and temperatures. Suspension of fine grains is significantly easier at low temperatures and high pressures; late afternoon brightenings of many areas of Mars, and the generation of dust storms in such deep basins as Hellas, may be due to this effect.

Sagan, C.↗

Templated encapsulation of platinum-based catalysts promotes high-temperature stability to 1,100 °C

Stable catalysts are essential to address energy and environmental challenges, especially for applications in harsh environments (for example, high temperature, oxidizing atmosphere and steam). In such conditions, supported metal catalysts deactivate due to sintering-a process where initially small nanoparticles grow into larger ones with reduced active surface area-but strategies to stabilize them can lead to decreased performance. In this work, we report stable catalysts prepared through the encapsulation of platinum nanoparticles inside an alumina framework, which was formed by depositing an alumina precursor within a separately prepared porous organic framework impregnated with platinum nanoparticles. These catalysts do not sinter at 800 °C in the presence of oxygen and steam, conditions in which conventional catalysts sinter to a large extent, while showing similar reaction rates. Extending this approach to Pd-Pt bimetallic catalysts led to the small particle size being maintained at temperatures as high as 1,100 °C in air and 10% steam. This strategy can be broadly applied to other metal and metal oxides for applications where sintering is a major cause of material deactivation.

36 MATERIALS SCIENCE↗

U Metal Oxidation with Steam (U)

The Savannah Rive National Laboratory 9SRNL) is evaluating a method to produce uranium oxide (UO 2 ) from uranium metal using steam. The typical methods for making UO 2 yield powders with particle-size ranges of 1 to 50 micron. The goal of the steam oxidation is to produce a depleted uranium (DU) product with a larger particle size that can be used as a surrogate for testing physical and mechanical process techniques to refine uranium and/or plutonium bearing residues. Several studies in the literature indicated that reactions between uranium metal and steam will yield UO 2 as fine powders in the 160 to 500 °C range, but granular materials form above 500°C. Above 880 °C, a hard compact scale forms on the U metal. Furthermore, sintering of UO 2 occurs at about 1300 °C, but it has been stated that the presence of steam enhances the sintering characteristics of UO 2 . Initial studies into the oxidation of DU metal in an atmosphere of argon and steam have been completed. Oxidation of depleted uranium metal in Ar/steam at 600, 710, 700, and 830 °C yielded at UO 2 product with little or no impurity at each temperature. Although not enough sample was available to perform sieve analysis for particle size distribution, SEM images reveal that a significant volume fraction of the products at 710, 770, and 830 °C exceeds 100 microns. The material produced at 600 °C was too fine for programmatic needs. Questions associated with the UO 2 include morphology of product, mechanical strength of the particles, and performance in milling operations. The size of the samples produced in these tests did not allow for quantitative assessment of particle size of mechanical strength. A qualitative assessment of the particles formed at 710, 770, and 830 °C was that the samples produced at 710 and 770 °C were friable, and the sample produced 830 °C had more mechanical strength. Sintering of the samples in Ar/steam at 970 °C appeared to increase the strength of the particles without changing their general particle size characteristics. Due to the small sample sizes, the increase in strength could not be quantified. If the sintering at 970 °C is inadequate, higher sintering temperatures in Ar/steam can be evaluated. Future work will increase scale of the steam oxidation conditions which yield the most-favorable particle-size distributions with sufficient mechanical strength for programming usage. Further consideration will be given to oxidation temperature, steam addition to the reaction vessel, U metal pretreatment, and sintering conditions after oxidation. The UO 2 production could involve a two-step process where particles are formed in steam at lower temperatures (700-850 °C) and then sintered in Ar/steam at elevated temperatures (950-1200 °C). Larger samples (50-100 g each) will provide sufficient UO 2 product for sieve analysis and assessment of mechanical strength relatives to subsequent milling operations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Manufacture of dense sintered bodies containing silicon nitride

Sintered bodies containing 1-32.5 Si oxide and 1.5 wt.% SiC (Si oxide/SiC wt. ratio 3/2) are prepared and kept in a 10-3000 kg/2 sq. cm. N (g) atmosphere at 1500-2300 degrees, while simultaneously maintaining the CO (g) partial pressure around the body lower than the nitrogenation equil. pressure to give a dense sintered body. The prepared dense sintered body has high strength at high temperatures. Thus, SiC 40, oxide 30 and Si3N4 30 wt% were fired to a body which was kept in 1500 kg/sq. cm. N (g) for 20 h at 2000 degrees to give a dense sintered body having high bending strength at high temperatures.

Hirota, K.↗

Experimental and computational investigations on the SO 2 poisoning of (La 0.8 Sr 0.2 ) 0.95 MnO 3 cathode materials

To study the formation of detrimental phases under the sulfur gas impurity to the long-term degradation in the LSM cathode material, the classic cathode material, (La 0.8 Sr 0.2 ) 0.95 MnO 3 (LSM), was prepared, sintered, and annealed at 800, 900, and 1000°C in the sulfur-containing atmospheres, respectively. Through X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Transmission electron microscopy (TEM) techniques, as well as the CALPHAD (Computer Coupling of Phase Diagrams and Thermochemistry) methodology, the secondary phases, especially the detrimental ones, under different conditions were predicted and experimentally verified correspondingly. Furthermore, sulfur poisoning results indicate that the accelerated tests might have degradation mechanisms different from actual operation conditions. More importantly, comprehensive comparisons among various impurity-containing conditions were also made to recommend better operation parameters.

36 MATERIALS SCIENCE↗

Oxidation of porous stainless steel supports for metal-supported solid oxide electrolysis cells

Oxidation behavior of porous P434L ferritic stainless steel, used for the fabrication of metal-supported solid oxide electrolysis cells (MS-SOEC), is studied under oxygen-side and steam-side conditions. The impact of oxygen content on the oxygen side and steam:hydrogen ratio on the steam side is determined at 700°C for bare, as-sintered samples. For these conditions, oxidation is more aggressive in the steam-side atmosphere. Oxygen with 3% humidification and steam:hydrogen ratio of 90:10 are selected for further assessment with pre-oxidized, catalyst-coated, and CuMn1·8O4-coated samples. The rapid oxidation at 700°C and breakaway oxidation at 600 °C observed for bare stainless steel in 90:10 steam:hydrogen is mitigated by pre-oxidizing the sample in air before exposure. In oxygen, addition of the catalyst or CuMn 1·8 O 4 coatings moderately increases the oxidation rate, due to consumption of Cr via reaction between the coatings and Cr-oxide scale. In conclusion, the results for ex-situ controlled oxidation are similar to oxidation observed after 1000h operation of a full MS-SOEC. In general, the oxidation behavior at 700°C is found to be acceptable.

08 HYDROGEN↗

Wireless Passive Ceramic Sensor for Far-Field Temperature Measurement at High Temperatures

A passive wireless high-temperature sensor for far-field applications was developed for stable temperature sensing up to 1000 °C. The goal is to leverage the properties of electroceramic materials, including adequate electrical conductivity, high-temperature resilience, and chemical stability in harsh environments. Initial sensors were fabricated using Ag for operation to 600 °C to achieve a baseline understanding of temperature sensing principles using patch antenna designs. Fabrication then followed with higher temperature sensors made from (In, Sn) O2 (ITO) for evaluation up to 1000 °C. A patch antenna was modeled in ANSYS HFSS to operate in a high-frequency region (2.5–3.5 GHz) within a 50 × 50 mm2 confined geometric area using characteristic material properties. The sensor was fabricated on Al2O3 using screen printing methods and then sintered at 700 °C for Ag and 1200 °C for ITO in an ambient atmosphere. Sensors were evaluated at 600 °C for Ag and 1000 °C for ITO and analyzed at set interrogating distances up to 0.75 m using ultra-wideband slot antennas to collect scattering parameters. The sensitivity (average change in resonant frequency with respect to temperature) from 50 to 1000 °C was between 22 and 62 kHz/°C which decreased as interrogating distances reached 0.75 m.

47 OTHER INSTRUMENTATION↗

Rapid and Energy‐Efficient Synthesis of Disordered Rocksalt Cathodes

Abstract Lithium‐rich transition metal oxides with a cation‐disordered rocksalt structure (disordered rocksalt oxides or DRX) are promising candidates for sustainable, next‐generation Li‐ion cathodes due to their high energy densities and compositional flexibility, enabling Co‐ and Ni‐free battery chemistries. However, current methods to synthesize DRX compounds require either high temperature (≈1000 °C) sintering for several hours, or high energy ball milling for several days in an inert atmosphere. Both methods are time‐ and energy‐intensive, limiting the scale up of DRX production. The present study reports the rapid synthesis of various DRX compositions in ambient air via a microwave‐assisted solid‐state technique resulting in reaction times as short as 5 min, which are more than two orders of magnitude faster than current synthesis methods. The DRX compounds synthesized via microwave are phase‐pure and have a similar short‐ and long‐range structure as compared to DRX materials synthesized via a standard solid‐state route, resulting in nearly identical electrochemical performance. In some cases, microwave heating allows for better particle size and morphology control. Overall, the rapid and energy‐efficient microwave technique provides a more sustainable route to produce DRX materials, further incentivizes the development of next‐generation DRX cathodes, and is key to accelerating their optimization via high‐throughput studies.

25 ENERGY STORAGE↗

Novel High Temperature Carbide and Boride Ceramics for Direct Power Extraction Electrode Applications. Final report

The current project aims to develop new carbide and boride ceramic materials that incorporate different metal elements (e.g., (Hf 1-x Zr x )B 2 , also called ceramic solid solutions) and understand the fundamental composition-processing-structure-property relationships for such materials. Specifically, nano powders and related nano-composites for selected mixed metal carbide and boride materials are synthesized from nano-scale mixed precursors obtained from solution-based processing via heat treatment in inert atmosphere. The obtained fine powders were then consolidated into dense ceramics via a novel flash sintering process. The mechanical properties and thermal oxidation resistance for the obtained materials were evaluated for these materials. It was found that different synthesis routes produced powders with somewhat different characteristics in terms of composition and microstructure, which then led to different properties for the final ceramics. The synthesis and processing methods demonstrated in this study might be adopted for developing other similar high temperature ceramics, while the mixed metal or solid solution ceramic materials obtained from this study might be used as hot electrodes for direction power extraction and other energy-related applications.

20 FOSSIL-FUELED POWER PLANTS↗

Autonomous Aerosol and Plasma Co‐Jet Printing of Metallic Devices at Ambient Temperature

Abstract Additive manufacturing of metallic materials holds the potential to revolutionize the fabrication of functional devices unattainable via traditional methods. Despite recent advancements, printing metallic materials typically requires thermal processing at elevated temperatures to form dense structures with desired properties, which presents a major challenge for direct printing and integration with temperature‐sensitive materials. Herein, a unique co‐jet printing (CJP) method is reported integrating an aerosol jet and a non‐thermal, atmospheric pressure plasma jet to enable concurrent aerosol deposition of metal nanoparticle inks and in situ sintering at ambient temperature. A machine learning algorithm is integrated with the CJP to perform real‐time defect detection and autonomous correction, enhancing the yield of printed films with high electrical conductivity from 44% to 94%. Concurrent printing and sintering eliminate the need for post‐printing processing, reducing the overall manufacturing time by multiple folds depending on product size. CJP enables direct printing of functional devices on a variety of temperature‐sensitive materials including biological materials. Direct printing of hydration sensors on living plant leaves is demonstrated for long‐duration monitoring of hydration level in the plant. The versatile CJP method opens tremendous opportunities to harmoniously integrate abiotic and biotic materials for emerging applications in wearable/implantable devices and biohybrid systems.

Du, Yipu [Department of Aerospace and Mechanical E↗

Effects of 18 O Exchange on Neutron Emission Rates of Aging 238 PuO 2 LWRHUs

The Lightweight Radioisotope Heater Unit (LWRHU) provides about 1 Watt of thermal power to critical electrical and mechanical systems in the extreme temperatures of space, maintaining the operating temperature of the spacecraft’s scientific and general operating equipment. Los Alamos National Laboratory (LANL) designed and tested the LWRHU in the 1970s through early 1980s. The first production campaign at LANL was in the early 1980s in support of the Galileo mission in which over 100 LWRHUs were manufactured. In the mid-1990s, almost 200 LWRHUs were manufactured in support of the Cassini mission. After the primary Cassini manufacturing campaign, the Department of Energy (DOE) approved the fabrication of more than 10 additional LWRHUs as spares in 1998. The LWRHU assembly contains the following components: a fuel pellet, a vented capsule, a pyrolytic graphite insulator, and a fine-weave pierced fabric (FWPF) graphite aeroshell. The fuel pellet is a hot-pressed 238 PuO 2 cylindrical pellet that is sintered to create a ceramic pellet. The pellet is encapsulated in a platinum-rhodium encapsulation. The welded fueled clad is placed inside a pyrolytic graphite thermal insulation to protect the fuel from the heat produced in reentry events. The exterior layer of the LWRHU assembly is the FWPF aeroshell. Before sintering, PuO 2 granules are heated in a furnace at temperatures greater than or equal to 700°C under an enriched 16 O atmosphere in order to reduce trace quantities of 18 O. Because 18 O undergoes an (α,n) reaction, 18 O needs to be removed as much as possible to meet radiation emission requirements set by the Jet Propulsion Laboratory (JPL) and the National Aeronautics and Space Administration (NASA), as well as other agencies. The relative abundances of the oxygen isotopes are indicated by neutron emission rate (NER) measurements. LWRHUs are vented with a sintered platinum frit vent (George 1986). During extraterrestrial operation, the vent in the cladding allows helium from the decay of plutonium to escape and relieves pressure from the system while preventing the solids from escaping (Rinehart 1996, Tate 1982 & 1985). This vent is protected during manufacture by a platinum-30 rhodium cover. The capsule vent is activated by milling a 0.025-inch diameter hole through the protective cover to a nominal depth of 0.015 inches, generally immediately before the LWRHU is loaded into the aeroshell (George 1986). Prior to long-term storage, LWRHUs are vented and thus potentially allow infiltration of 18 O from the ambient atmosphere. Although NER decreases with age due to the reduction in emitted alpha particles, it might be expected that NER reduction is mitigated by the exchange of 18 O. However, this is not necessarily the case and no trend was observed relating NER to age other than the natural decay of 238 Pu (Mulford 2021). The most probable and dominant factor for determining specific NER was manufacturing discrepancies between individual units. It is important to understand the lack of observed 16 O- 18 O exchange and to compare LWRHU pellets as much as possible.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗