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Electrically conductive sintered, substantially round and spherical particles and methods for producing such electrically conductive sintered, substantially round and spherical particles from an alumina-containing raw material. Methods for using such electrically conductive sintered, substantially round and spherical particles in hydraulic fracturing operations.
A method of forming a water resistant boundary on a fissile material for use in a water cooled nuclear reactor is described. The method comprises mixing a powdered fissile material selected from the group consisting of UN and U 3 Si 2 with an additive selected from oxidation resistant materials having a melting or softening point lower than the sintering temperature of the fissile material, pressing the mixed fissile and additive materials into a pellet, sintering the pellet to a temperature greater than the melting point of the additive. Alternatively, if the melting point of the oxidation resistant particles is greater than the sintering temperature of UN or U 3 Si 2 , then the oxidation resistant particles can have a particle size distribution less than that of the UN or U 3 Si 2 .
A method of forming a water resistant boundary on a fissile material for use in a water cooled nuclear reactor is described. The method comprises mixing a powdered fissile material selected from the group consisting of UN and U3Si2 with an additive selected from oxidation resistant materials having a melting or softening point lower than the sintering temperature of the fissile material, pressing the mixed fissile and additive materials into a pellet, sintering the pellet to a temperature greater than the melting point of the additive. Alternatively, if the melting point of the oxidation resistant particles is greater than the sintering temperature of UN or U3Si2, then the oxidation resistant particles can have a particle size distribution less than that of the UN or U3Si2.
As Electric Field Assisted Sintering (EFAS) gains more industrial acceptance and use, it becomes more important to develop more efficient means to implement this technology. To this aim, 3D printed continuous carbon fiber reinforced carbon (CCC) was manufactured and fabricated into tooling for EFAS systems as an alternative to traditional graphite tooling. The impact of fiber orientation on the thermal and electrical properties of the CCC was characterized. Sample material was sintered in Tokai G535 graphite tooling, under common processing conditions and compared with CCC tooling. There was nearly 50 % energy savings compared to graphite while maintaining equivalent sample density and microstructure plus keeping ram temperatures 39 % cooler. This is due to spatial control of generated heat and thermal diffusivity within the molds, by means of fiber orientation anisotropy. Finite element modeling of the tooling design supported the experimental results as well as displays the effect of optimization of this 3D printed CCC material.
Here, this work studies the microstructural evolution of nanocrystalline (<1 µm) barium titanate (BaTiO 3 ), and presents high pressure in field-assisted sintering (FAST) as a robust methodology to obtain >100 nm BaTiO 3 compacts. Using FAST, two commercial ~50 nm powders were consolidated into compacts of varying densities and grain sizes. Microstructural inhomogeneities were investigated for each case, and an interpretation is developed using a modified Monte Carlo Potts (MCP) simulation. Two recurrent microstructural inhomogeneities are highlighted, heterogeneous grain growth and low-density regions, both ubiqutously present in all samples to varying degrees. In the worst cases, HGG presents an area coverage of 52%. Because HGG is sporadic but homogenous throughout a sample, the catalyst (e.g., the local segregation of species) must be, correspondingly, distributed in a homogenous manner. MCP demonstrates that in such a case, a large distance between nucleating abnormal grains is required—otherwise abnormal grains prematurely impinge on each other, and their size is not distinguishable from that of normal grains. Compacts sintered with a pressure of 300 MPa and temperatures of 900 °C, were 99.5% dense and had a grain size of 90±24 nm. These are unprecedented results for commercial BaTiO 3 powders or any starting powder of 50 nm particle size—other authors have used 16 nm lab-produced powder to obtain similar results.
The assembly and morphology of pores determine thermodynamic, flow and reactive properties of confined fluids. Yet, there is a limited understanding of how pore architectures dynamically develop in engineered and natural materials. To develop a calibrated understanding of fluid properties in confinement, the synthesis of architected materials has been proposed. The design of geo-architected materials has to be informed by the dynamic evolution of the morphology in response to thermal or chemical events. Here, we probe thermally induced morphological evolution of spherical silica nanoparticles 220 ± 30 nm in diameter using in-operando Ultra-Small and Small Angle X-Ray Scattering measurements. The calcination experiments demonstrated that at temperatures up to 600 °C the pore radii remained in the range of 2.15 nm–2.35 nm and the particle diameters in the range of 220 ± 30 nm. Sintering these calcined silica nanoparticles to temperatures up to 1050 °C reduced the pore size from 2.2 ± 0.1 nm to ~1.8–0.2 nm. These changes corresponded to the formation of siloxane (Si-O-Si) bridges resulting from dehydroxylation. The characteristic pore radius of sintered particles was also confirmed by N 2 adsorption measurements. These studies represent the use of non-invasive dynamic characterization methods such as X-ray scattering to elucidate thermally induced morphological evolution in architected siliceous materials.
Epsilon metal (ε-metal), an alloy of Mo, Pd, Rh, Ru, and Tc, is being developed as a waste form to treat and immobilize the undissolved solids and dissolved noble metals from aqueous reprocessing of commercial used nuclear fuel. Epsilon metal is an attractive waste form for several reasons: increased durability relative to borosilicate glass, it can be fabricated without additives (100% waste loading), and in addition it also benefits borosilicate glass waste loading by eliminating noble metals from the glass and thus the processing problems related there insolubility in glass. This work focused on the processing aspects of the epsilon metal waste form development. Epsilon metal is comprised of refractory metals resulting in high reaction temperatures to form the alloy, expected to be 1500 - 2000°C making it a non-trivial phase to fabricate by traditional methods. Three commercially available advanced technologies were identified: spark-plasma sintering, microwave sintering, and hot isostatic pressing, and investigated as potential methods to fabricate this waste form. Results of these investigations are reported and compared in terms of bulk density, phase assemblage (X-ray diffraction and elemental analysis), and microstructure (scanning electron microscopy).
Progress is reviewed on development of an improved near-final bulk magnet fabrication process for alnico 8, as a non-rare earth permanent magnet with promise for sufficient energy density and coercivity for electric drive motors. This study showed that alnico bulk magnets in near-final shape can be made by simple compression molding from spherical high purity gas atomized pre-alloyed powder. Dwell time at peak sintering temperature (1250 °C) greatly affected grain size of the resulting magnet alloys. This microstructure transformation was demonstrated to be useful for gaining partially aligned magnetic properties and boosting energy product. While a route to increased coercivity was not identified by these experiments, manufacturability of bulk alnico magnet alloys in near-final shapes was demonstrated, permitting further processing and alloy modification experiments that can target higher coercivity and better control of grain anisotropy during grain growth.
Laser powder-bed fusion (LPBF) is an additive manufacturing (AM) technology that uses high-power sintering lasers to precisely construct metal designs. Material is accumulated by selectively sintering regions of a metal powder layer to a growing structure underneath forming a 3D geometry. Certain conditions make fusion in this process to operate in "keyhole-mode," characterized by targeted materials evaporating as plasma. While keyhole-mode operations can produce deeper molten pools than that observed in "conduction-mode", this mode of operation is often undesirable, as its molten regions can collapse on themselves, encapsulating metal vapors and forming cavities. The formation of such cavities negatively affects strength and consistency of the fused materials. To identify and avoid these detrimental effects of keyhole-mode operation, considerable data collection and analysis regarding this mode of operation is needed. Therefore, under the support of the "Open Data Initiative," Lawrence Livermore National Lab is releasing a dataset for analysis of this keyhole effect, and the conditions which transition operation from conduction-mode to keyhole-mode melting. This dataset consists of 600+ micrographs from laser powder-bed single track runs, with differing cross-section angles and input parameters, operating under both normal and keyhole mode operations. This journal documents the collection, organization, and usage of this dataset.
Solid tritium breeder materials must first and foremost have sufficiently high concentrations of lithium to enable a plant-scale tritium breeding ratio greater than 1:1. However, in addition to lithium content, such breeder materials must also meet other performance metrics including high tritium release rates, thermal conductivities, and irradiation damage tolerance. Perhaps most importantly, tritium breeders must maintain their mechanical integrity during reactor operation so as to avoid degradation which can jeopardize the functionality of the tritium breeder blanket module, which in most designs takes the form of a pebble bed geometry. Unfortunately, the mechanical robustness of most lithium-bearing ceramics under investigation for fusion applications is often inversely related to the lithium atom density. For example, a material such as lithium oxide (Li2O), which has one of the highest lithium atom densities, has a much lower mechanical splitting strength than lithium metatitanate (Li2TiO3), though Li2TiO3 has less than half the lithium atom density of Li2O. This work seeks to provide an alternative to monolithic ceramic tritium breeders, in the form of metal-reinforced composite tritium breeders. Specifically, composite tritium breeders have been synthesized combining Li2O with various ferrous metal reinforcements via electric field assisted sintering (EFAS), also known as spark plasma sintering (SPS). As the metal reinforcement content is increased, metallic networks are observed, via electron microscopy and X-ray computed tomography, to form throughout the composite material. Through destructive mechanical testing, even dilute metal reinforcement loading enables drastic mechanical strength improvements over pure Li2O while higher loadings give rise to quasi-ductile behavior and higher ultimate strengths than Li2TiO3 – while still maintaining a higher density of lithium atoms than Li2TiO3 and many other breeder candidates. In addition to microstructural characterization and mechanical testing, thermal property measurements and hydrogen permeability testing are underway to further assess the suitability of such composites for fusion reactor applications.
Deploying energy storage and carbon capture at scale is hindered by the substantial endothermic penalty of decomposing CaCO 3 to CaO and CO 2 , and the rapid loss of CO 2 absorption capacity by CaO sorbent particles due to sintering at the high requisite decomposition temperatures. The decomposition reaction mechanism underlying sorbent deactivation remains unclear at the atomic level and nanoscale due to past reliance on postmortem characterization methods with insufficient spatial and temporal resolution. Thus, elucidating the important CaCO 3 decomposition reaction pathway requires direct observation by time-resolved (sub-)nanoscale methods. Here, chemical and structural dynamics during the decomposition of CaCO 3 nanoparticles to nanoporous CaO particles comprising high-surface-area CaO nanocrystallites are examined. Comparing in situ transmission electron microscopy (TEM) and synchrotron X-ray diffraction experiments gives key insights into the dynamics of nanoparticle calcination, involving anisotropic CaCO 3 thermal distortion before conversion to thermally dilated energetically stable CaO crystallites. Time-resolved TEM uncovered a novel CaO formation mechanism involving heterogeneous nucleation at extended CaCO 3 defects followed by sweeping reaction front motion across the initial CaCO 3 particle. These observations clarify longstanding, yet incomplete, reaction mechanisms and kinetic models lacking accurate information about (sub-)nanoscale dynamics, while also demonstrating calcination of CaCO 3 without sintering through rapid heating and precise temperature control.
Abstract The use of a low‐temperature plasma for the synthesis of amorphous silicon carbonitride (SiCN) nanoparticles enables the realization of sintered bulk samples with high thermal stability. Amorphous SiCN nanoparticles are produced from a mixture of silane, methane, and ammonia utilizing a mid‐pressure, radio‐frequency, continuous flow reactor. Particle characterization shows that the nanoparticles are largely amorphous with some crystalline silicon and silicon carbide domains <10 nm in size. Compositional tuning, controlled by varying the precursor flow rates, coupled with the uniform mixing of elements at the nanoscale, results in samples that resist crystallization even when sintered at temperatures as high as 2000°C. This study suggests that the low‐temperature plasma synthesis of nanoparticles has great potential to produce bulk structural materials for application in harsh environments.
Studies are presented of helium porosity in EP-450 oxide-dispersion-hardened yttrium steel, obtained by electopulse sintering, as a function of the Y{sub 2}O{sub 3} content in comparison with EP-450 matrix steel and dispersion-hardened steel fabricated by hot extrusion. It is found that multiple zones with different types of helium porosity and different zone distribution develop in steel with 1 wt.% Y{sub 2}O{sub 3}; in steel with 0.3 wt.% Y{sub 2}O{sub 3}, there are fewer such zones than in matrix steel and steel obtained by hot extrusion. It is proposed that the extremely nonuniform distribution of porosity over volume and size in steel fabricated by electropulse sintering is associated with the initially strongly defective structure, including residual porosity, as well as with the chromium redistribution between ferrite grains and tempered-martensite grains during the sample preparation process.
Perovskite cobaltates are widely recognized as potential candidates for their applications in magnetic and magnetoresistive applications. In this report, pseudo-magnetic CaFe{sub 0.5}Co{sub 0.5}O{sub 3−δ} was synthesized at ambient pressure. Various calcinations, heating times, and sintering temperatures were applied in order to achieve the optimized conditions. The optimal sintering temperature with excellent phase and microstructure was found at ∼1050 °C using CaCO{sub 3} as precursor. Rietveld analysis was carried out to solve and refine the XRD pattern of the final specimens. The sample with excellent refined values was solved in orthorhombic phase and pbcm space group. From the SEM and EDS analysis, the excellent grain growth with high densification and ABO{sub 3} structure was confirmed respectively.
Thin monofilamentary Fe/MgB{sub 2} superconducting wires without barriers are investigated by means of electrical transport measurements and surface and structural analysis methods. Small diameter wires are fabricated by pellet-in-tube method (PeIT) to obtain a high uniform initial filling density and heat treated as a function of various sintering temperatures and times. The results are discussed in terms of the grain connectivity, Fe{sub 2}B phase formation, and the relation between wire diameter and sintering conditions. We suggest that PeIT has a crucial importance to achieve homogeneous initial filling density, which leads to the fabrication of uniform long-length MgB{sub 2} wires.
The sintering temperature for the production of Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub 18} (Y-358) preform powders synthesized in sol-gel spontaneous combustion technique was optimized. A large single-grain bulk Y-358 crystal was fabricated employing a top-seeded melt-growth technique utilizing the optimally sintered preform powders (i.e., at 900 {sup ∘}C for 12 h). Structural, microstructural, elemental, and magnetic properties were investigated by means of X-ray diffraction, scanning electron microscopy, and SQUID, respectively. The structural characterization indicated that the sample is highly textured in (00l) direction. The Y-358 phase fractions were estimated in both preform powders and bulk sample using Rietveld refinement. The onset of superconducting transition is observed at 92.5 K, and the curve is very sharp indicative of the high quality of the produced bulk sample. The field dependence of critical current density (J{sub c}) was determined at 77 K, and the self-field J{sub c} was found to be ∼26 kA/cm{sup 2}. A magnetic field of 0.27 T was trapped by the sample at 77 K.
YBa{sub 2}Cu{sub 3}O{sub 7 − δ} (YBCO) superconducting twisted yarns from electrospun aligned nanofibers are produced with a critical transition temperature of T{sub c} = 92 K. A solution of PVA and Y–Ba–Cu acetates are used as a precursor in the electrospinning to prepare aligned nanofibers and twisted yarns. The aligned nanofibers and twisted yarns are then pyrolysed to remove PVA and sintered to obtain a superconducting phase. Finally, before and after sintering, the aligned nanofibers and twisted yarns are studied by SEM, XRD, and AC magnetic susceptibility techniques. Results are presented in this paper.
The magnetostrictive alloys with composition Tb{sub 0.4}Nd{sub 0.6}(Fe{sub 0.8}Co{sub 0.2}){sub x} (1.50 ≤ × ≤ 1.90) are synthesized using the solid-state mechanical alloying (MA) method followed by sintering. The phase component, structure, thermal stability, and magnetoelastic properties are investigated as functions of composition, milling process, and annealing temperature. An amorphous phase companied by free alpha-iron is formed by MA in a high-energy ball mill, which crystallizes into MgCu{sub 2}-type and PuNi{sub 3}-type structures with different annealing temperatures. A single Laves phase for the high Nd-content Tb{sub 0.4}Nd{sub 0.6}(Fe{sub 0.8}Co{sub 0.2}){sub 1.60} is formed at optimal conditions for heat treating at 700 °C for 30 min. A large linear anisotropic magnetostriction λ{sub a} (=λ{sub ||}–λ{sub ⊥}) as high as 560 ppm at 12 kOe is obtained for the sintered alloy, which may make it a promising magnetostrictive material. Meanwhile, this work may help to open up a new way to search for Laves phase magnetostrictive materials containing Nd.