Lithium leaching recovery and mechanisms from density fractions of an Illinois Basin bituminous coal
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Energy & Fuels↗
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Reticulated porous lanthanum strontium manganite structures for solar thermochemical hydrogen production
Porous ceramic foams are utilized in various fields and applications due to their advantageous properties such as high porosity, high specific surface area, and controlled permeability. Non-stoichiometric oxide foams are of particular interest for the solar thermochemical production of hydrogen in directly irradiated solar receivers due to their enhanced heat transfer capabilities and structural integrity. Here we report the fabrication of lanthanum strontium manganite replica foams and their solar thermochemical water splitting performance. Highly porous (>80%) foams were produced with controlled structure and tested in a high temperature water splitting furnace to demonstrate stability and overall performance. The temperature profile of the burnout and sintering of the foam structure were altered based on simultaneous differential scanning calorimetry and thermal gravimetry analysis. Two-step sintering was used both to retain micron-sized pores (D50 = 0.4 μm) on the foam's struts and to limit grain growth to a grain size of ~1 μm. The structural characteristics were confirmed by porosimetry and scanning electron microscopy. The foams were repeatedly cycled, producing approximately 200 μmol/g of H 2 per cycle. Water splitting performance was tested for 50 cycles and approximately 35 h at 1400 °C. No statistical difference in the effective hydrogen production per cycle was observed, which is promising for long-term redox cycle stability.
08 HYDROGEN↗
Enhancing the Chemical Energy Flux in a High-Temperature Tubular Counterflow Solid Fuel Synthesis Reactor Using a Bypass
Redox reactions of metal oxides offer a path towards using intermittent renewable resources for high-density thermochemical energy storage. Thermochemical energy storage often involves the flow of a particulate media. We describe a novel method to increase the throughput in a gravity-driven high-temperature thermochemical storage reactor flowing pelletized MgMnO. The moving bed reactor operates under counter-flow conditions and encounters particle flowability problems at temperatures of 1500 °C leading to sintering of the bed. Inertial forces of a counter-flowing gas can overcome the gravitational forces on the particles and limit the chemical energy storage rate of the reactor. We found that the insertion of a gas bypass (a slotted tube) into the reactor results in a 100% increase of the flow rates and achieved a 50% higher chemical energy storage flux compared to the operation without a bypass tube while mitigating the effects of sintering on the particles. As a result, the higher solid flow rates require a longer heated zone to reach a comparable residence time and extent of reduction compared to the lower flow rates.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
The Triple Component Interface of Ni–Co–Ce: Growth, Chemical State, and Stability of NiCo Bimetallic Particles on Reducible CeO 2 (111) Thin Films
The growth of NiCo particles at low coverages over reducible CeO 2 (111) thin films producing a triple interface between Ni-Co-Ce was investigated by scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS), which was compared to that of monometallic Ni and Co particles. XPS data show that deposition of either Ni or Co on CeO 2 at 300 K causes a partial reduction of Ce 4+ cations to Ce 3+ ions. At 0.3 monolayer (ML), XPS detects Co 2+ on CeO 2 . However, both Ni 0 and Ni 2+ are present as major species at 300 K and annealing causes a significant increase of Ni 2+ in Ni particles. Deposition of 0.3 ML Co over 0.3 ML Ni on CeO 2 at 300 K induces reduction of Ni 2+ to metallic Ni and Ni 0 was found as predominant species. Unlike for Co/CeO 2 , metallic Co was also present over the Co-Ni/CeO 2 surface in addition to Co 2+ . Further, this behavior indicates the formation of NiCo bimetallic particles with the possibility of Co diffusion to the interface of Ni/ceria. With heating, the intermixing of Ni and Co atoms in bimetallic particles on CeO 2 was facilitated. Furthermore, oxidation of both metals and ceria occurred as a result of the diffusion of lattice oxygen from the bulk of ceria to the surface. A slight increase in Ni 2+ was observed after heating Co-Ni/CeO 2 to 500 K or higher. Co became Co 2+ with heating to 800 K. Our STM results confirm the formation of NiCo bimetallic particles on CeO 2 at 300 K and further suggest that the addition of Co can help inhibit the sintering of Ni particles at higher temperatures. Bimetallic particles were also obtained by depositing Ni over existing Co particles on CeO 2 . However, our XPS data demonstrate that the deposition order of Co and Ni plays a role in the chemical state of these two metals in bimetallic particles, likely attributed to the difference in their compositions at the bimetallic particle surface as well as the metal-support interface.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Chemical bond and phase stability of Ga-doped Sm2Fe17Cx magnet
Sm2Fe17C3 phase (2:17) is metastable and exhibits excellent intrinsic hard magnetic properties. Doping elements such as Ga facilitate the formation of a single-phase 2:17 structure in arc-melted Sm2Fe17Cx alloys, which opens a promising route for fabricating fully dense bulk Sm2Fe17Cx magnets via high-temperature techniques such as melting and sintering. First-principles electronic structure calculation indicates that Ga prefers to partially replace Fe at the 9d and 18h crystallographic sites in Sm2Fe17C3 and Sm2Fe17, respectively. This difference in site preference is attributed to the distinct chemical environments surrounding the Fe atoms in the two compounds. Ga substitution favors the Sm–Ga bonding formation while avoiding Ga–C interactions. Doped Ga atoms result in more negative formation energy in Sm2(Fe, Ga)17C3, indicating improved structural stability. Crystal Orbital Hamilton Population analysis reveals that carbon insertion weakens the bonding of Sm-Fe (18h) and Sm-Fe (18f) in Sm2Fe17C3. Ga doping facilitates electron redistribution across chemical bonds, thereby reinforcing Fe(18h)–Sm and Fe(18f)–Sm interactions and stabilizing the carbon-centered octahedral local structure. This synergistic effect contributes significantly to the observed enhancement in phase stability of Sm2(Fe, Ga)17Cx. These findings suggest that chemical bond engineering through the selective doping of Ga can enhance phase stability and facilitate the synthesis of Sm2Fe17C3, providing a viable strategy for developing advanced magnets.
Liu, Xubo [Critical Materials Innovation Hub, Divi↗
A Rapid Sintering Method for Cerium Nitride Pellet: A Uranium Mononitride Surrogate
Uranium mononitride (UN) is a candidate fuel material for light water reactors with higher uranium (U) loading and thermal conductivity than uranium dioxide (UO 2 ). However, the sintering of UN pellets is challenging as the UN powder particles oxidize rapidly at high temperatures unless the oxygen concentration is extremely low. Oxidation during sintering either reduces the relative density of the sintered UN pellet or disintegrates the sintered UN pellet to powder. To address this problem, the present work developed a rapid sintering method for producing highly densified UN surrogate pellets with minimal oxidation. Cerium nitride (CeN) is used as a surrogate for UN to reduce radiation hazards. With the custom-developed fast-heating system, the sintering process was completed within 150 s. The sintering atmosphere was flowing nitrogen (N 2 ). The sintered CeN pellet density was 95% of the theoretical density (TD) or higher. The microstructure was uniform with a 10–25 µm grain size as demonstrated by scanning electron microscopy (SEM) and contained trivial levels of oxides as demonstrated by X-ray diffraction (XRD). The resultant pellets indicate that the rapid sintering method is a promising method to make UN fuel pellets with equivalent or higher density to pellets made by conventional sintering methods, while also being more efficient in time and costs.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Electron petrography of Apollo 14 and 15 rocks.
Comparative optical and high-voltage electron petrographic analyses of igneous rocks and several types of breccias the Fra Mauro and Apennine sites of Apollo 14 and 15 are reported and interpreted. The crystalline rocks are found to differ substantially from the Apollo 11 and 12 basalts. Substructures in the Apollo 14 breccias are complex. At least two bonding mechanisms can be discerned from the electron petrographic examination: (a) 'shock sintering' due to high pressures and temperatures associated with the shock waves of meteoritic impacts; and (b) lithification by glass bonding.
Lally, J. S.↗
Hydrometeor development in cold clouds in FIRE
The microphysical characteristics of cold clouds were examined using aircraft. The clouds investigated ranged in temperature from minus 20 to minus 46 C. Liquid water was detected in these clouds at minus 35 C and may exist at even colder temperatures. Aircraft patterns in the form of Lagrangian spirals were used to interpret particle growth processes. Significant broadening of the particle size spectra is observed with minor changes in the spectra at small sizes. Virtually all of the broadening observed is attributable to ice particle aggregation which occurs at all temperatures. The crystals comprising the aggregates are of comparable size, joined either at tips or edges, and are usually 2 in number at temperatures lower than minus 25 C, increasing to 3 or more at warmer temperatures. The data strongly suggest that sintering is the mechanism through which the crystals aggregate. Aggregation appears to be important in the transfer of water mass from upper to lower levels in clouds.
Heymsfield, Andrew J.↗
Consortium for materials development in space
During fiscal 1993, the Consortium for Materials Development in Space (CMDS) maintained the organizational structure and project orientation established in prior years. The commercial objectives are improved materials, biomedical applications, and infrastructure and support hardware. Projects include nonlinear optical materials; space materials (specifically polymer foam/films, atomic oxygen and high temperature superconductors); alloyed and blended materials: sintered and alloyed materials; polymer and carbonate blends; electrodeposition; organic separation; materials dispersion and biodynamics; space carriers: Consort, COMET support, Spacehab utilization; and flight services: accelerometers, CMIX, USEC, ORSEP, and Space Experiment Facility (SEF).
Source record↗
Evaluation of an Alternate Method for Determining Yield Strength Offset Values for Selective Laser Sintered Polymeric Materials
Due to the unique characteristics of Additively Manufactured (AM) polymeric materials, typical mechanical strength characterization methods such as those commonly used for traditionally-processed polymers or composite materials can produce results that do not accurately represent material capabilities. In order to characterize mechanical properties of these materials, new test and analysis methods are required. As part of the National Aeronautics and Space Administration (NASA) Advanced Composites Project (ACP), Boeing has evaluated true yield testing as an alternative or complimentary test to 0.2% offset yield testing for determining appropriate yield strength values of polymer materials. Previous testing has shown high strain, low modulus polymer materials such as selective laser sintered (SLS) Nylon 11 at elevated temperatures produce large variations in yield strength. The true yield test method was successful in finding the applied strain level when yield commences and appears to offer an increase in data robustness.
Henry, Chelsey↗
Manufacture of sintered silicon nitrides
Sintered silicon nitrides are manufactured by sintering Si3N powder containing 2 to 15% in wt of a powder mixture composed of nitride powder of lanthanide or Y 100 parts and AIN powder less than 100 parts at 1500 to 1900 deg. temperature under a pressure of less than 200 Kg/sq. cm. The sintered Si3N has high mechanical strength in high temperature. Thus, Si3N4 93.0, Y 5.0 and AlN 2.0% in weight were wet mixed in acetone in N atom, molded and sintered at 1750 deg. and 1000 Kg/sq. cm. to give a sintered body having high hardness.
Iwai, T.↗
Indirect additive manufacturing process for fabricating bonded soft magnets
A bonded soft magnet object comprising bonded soft magnetic particles of an iron-containing alloy having a soft magnet characteristic, wherein the bonded soft magnetic particles have a particle size of at least 200 nm and up to 100 microns. Also described herein is a method for producing the bonded soft magnet by indirect additive manufacturing (IAM), such as by: (i) producing a soft magnet preform by bonding soft magnetic particles with an organic binder, wherein the magnetic particles have an iron-containing alloy composition with a soft magnet characteristic, and wherein the particles of the soft magnet material have a particle size of at least 200 nm and up to 100 microns; (ii) subjecting the preform to an elevated temperature sufficient to remove the organic binder to produce a binder-free preform; and (iii) sintering the binder-free preform at a further elevated temperature to produce the bonded soft magnet.
Paranthaman, Mariappan Parans↗
Development of Advanced Thermal and Environmental Barrier Coatings Using a High-Heat-Flux Testing Approach
The development of low conductivity, robust thermal and environmental barrier coatings requires advanced testing techniques that can accurately and effectively evaluate coating thermal conductivity and cyclic resistance at very high surface temperatures (up to 1700 C) under large thermal gradients. In this study, a laser high-heat-flux test approach is established for evaluating advanced low conductivity, high temperature capability thermal and environmental barrier coatings under the NASA Ultra Efficient Engine Technology (UEET) program. The test approach emphasizes the real-time monitoring and assessment of the coating thermal conductivity, which initially rises under the steady-state high temperature thermal gradient test due to coating sintering, and later drops under the cyclic thermal gradient test due to coating cracking/delamination. The coating system is then evaluated based on damage accumulation and failure after the combined steady-state and cyclic thermal gradient tests. The lattice and radiation thermal conductivity of advanced ceramic coatings can also be evaluated using laser heat-flux techniques. The external radiation resistance of the coating is assessed based on the measured specimen temperature response under a laser- heated intense radiation-flux source. The coating internal radiation contribution is investigated based on the measured apparent coating conductivity increases with the coating surface test temperature under large thermal gradient test conditions. Since an increased radiation contribution is observed at these very high surface test temperatures, by varying the laser heat-flux and coating average test temperature, the complex relation between the lattice and radiation conductivity as a function of surface and interface test temperature may be derived.
Zhu, Dongming↗
Development of Low Conductivity and Ultra High Temperature Ceramic Coatings Using A High-Heat-Flux Testing Approach
The development of low conductivity, robust thermal and environmental barrier coatings requires advanced testing techniques that can accurately and effectively evaluate coating thermal conductivity and cyclic resistance at very high surface temperatures (up to 17OOOC) under large thermal gradients. In this study, a laser high-heat-flux test approach is established for evaluating advanced low conductivity, ultra-high temperature ceramic thermal and environmental barrier coatings under the NASA Ultra Efficient Engine Technology (UEET) program. The test approach emphasizes the real-time monitoring and assessment of the coating thermal conductivity: the initial conductivity rise under a steady-state high temperature thermal gradient test due to coating sintering, and the later coating conductivity reduction under a subsequent cyclic thermal gradient test due to coating cracking/delamination. The coating system is then evaluated based on the damage accumulations and failure after the combined steady-state and cyclic thermal gradient tests. The lattice and radiation thermal conductivity of advanced ceramic coatings can also be evaluated using laser heat-flux techniques. The coating external radiation resistance is assessed based on the measured specimen temperature response under a laser heated intense radiation flux source. The coating internal radiation contribution is investigated based on the measured apparent coating conductivity increases with the coating surface test temperature under large thermal gradient test conditions. Since an increased radiation contribution is observed at these very high surface test temperatures, by varying the laser heat-flux and coating average test temperature, the complex relation between the lattice and radiation conductivity as a function of surface and interface test temperature is derived.
Zhu, Dongming↗
Low-Temperature Catalyst Redispersion: A Route to Enhanced Stability of Supported Metal Catalysts?
Sintering poses a significant challenge to achieving the long-term stability of supported metal catalysts under reaction conditions. Here, in this study, we report a low-temperature catalyst redispersion mechanism, in which platinum single atoms, which aggregate into nanoparticles under Reverse Water Gas Shift (RWGS) conditions at elevated temperatures, fragment into atomically dispersed species upon cooling. Using multimodal operando characterization combined with first-principles theoretical modeling, we track the structural evolution of Pt single atoms supported on ceria nanodomes, deposited either on ceria or ceria–titania mixed oxides. We find that fragmentation is more pronounced when cooling occurs under RWGS conditions compared to CO alone, owing to a synergistic interplay of the effects of H 2 , CO 2 , and CO. The support architecture has a strong influence on the extent of redispersion: while CO alone induces fragmentation on ceria, interfacial confinement and vacancy pinning at the ceria–titania interface suppress restructuring. In contrast, RWGS conditions overcome these barriers, enabling redispersion across both supports. These findings point toward a pathway for catalyst stabilization via reaction-induced redispersion under mild conditions.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Kinetics of Sintering Chromium Carbide
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MATERIALS - TEMPERATURES, HIGH↗
Dielectric Performance of a High Purity HTCC Alumina at High Temperatures - a Comparison Study with Other Polycrystalline Alumina
A very high purity (99.99+%) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this alumina material for co-firing processing. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96% polycrystalline alumina (96% Al2O3), where 96% alumina was used as the benchmark. A prototype packaging system based on regular 96% alumina with Au thickfilm metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500 C. In order to evaluate this new high purity HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96% alumina and a previously tested LTCC alumina from room temperature to 550 C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96% alumina and a selected LTCC alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.
Electronic packaging↗
Crystallization Mechanism in Spark Plasma Sintered Bulk Metallic Glass Analyzed using Small Angle Neutron Scattering
Understanding the thermal stability of metallic glasses is critical to determining their safe temperatures of service. In this paper, the crystallization mechanism in spark plasma sintered Fe 48 Cr 15 Mo 14 Y 2 C15B6 metallic glass is established by analyzing the crystal size distribution using x-ray diffraction, transmission electron microscopy and in-situ small angle neutron scattering. Isothermal annealing at 700 °C and 725 °C for 100 min resulted in the formation of (Fe,Cr) 23 C 6 crystals, measured from transmission electron micrographs, to be from 10 to 30 nm. The small angle neutron scattering intensity measured in-situ, over a Q-range of 0.02 to 0.3 Å -1 , during isothermal annealing of the sintered samples, confirmed the presence of (Fe,Cr) 23 C 6 crystals. The measured scattering intensity, fitted by the maximum entropy model, over the Q-range of 0.02 to 0.06 Å -1 , revealed that the crystals had radii ranging from 3 to 18 nm. The total volume fraction of crystals were estimated to be 0.13 and 0.22 upon isothermal annealing at 700 °C and 725 °C for 100 min respectively. The mechanism of crystallization in this spark plasma sintered iron based metallic glass was established to be from pre-existing nuclei as confirmed by Avrami exponents of 0.25 ± 0.01 and 0.39 ± 0.01 at the aforesaid temperatures.
42 ENGINEERING↗