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At least 37 records · Page 2

Improved cladding nano-structured materials with self-repairing capabilities

When designing nuclear reactors or the materials that go into them, one of the key challenges is finding materials that can withstand an outrageously extreme environment. In addition to constant bombardment by radiation, reactor materials may be subjected to extremes in temperature, physical stress, and corrosive conditions. A limitation in fuel burnup is and usage of the nuclear fuel material is related to the structural material radiation damage, that makes the fuel be removed with low-burnup and immobilized in the waste storage pools. The advanced burnup brings cladding material embitterment due to radiation damage effects corroborated with corrosion effects makes the fuel pellet life shorter. The novel nano-clustered structured sintered material may mitigate simultaneously the radiation damage and corrosion effects driving to more robust structural materials that may make the nuclear reactor safer and more reliable. The development of nano-clustered sinter alloys provides new avenues for further examination of the role of grain boundaries and engineered material interfaces in self-healing of radiation-induced defects driving to the design of highly radiation-tolerant materials for the next generation of nuclear energy applications. (authors)

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Effect of Annealing on the Impact Resistance and Fracture Mechanism of PNC-60 Sinters After Cold Plastic Deformation

Compaction of sintered metal powders by free upsetting at room temperature dangerously reduces their plastic properties, particularly the fracture toughness. The reason for the occurrence of two unfavorable phenomena accompanying this deformation route is sought. The first phenomenon depends on the initial porosity of the preform and the amount of cold work resulting in the destruction of bonds and violation of continuity between sintered powder particles. The second phenomenon is the deformation of the metal matrix, which reduces the plasticity of the sintered product. To correctly assess the effect of changes occurring in the matrix as a result of deformation, it is necessary to use the properly defined sintered matrix hardening parameter discussed in this study. The adverse effects of cold forming can be eliminated by annealing the deformed sinters at a temperature below the sintering point and above the recrystallization temperature. The annealing temperature causes favorable changes in the structure and increases the impact resistance of the deformed sinters depending on the degree of deformation of the sintered matrix and the initial porosity of the preform. Annealing at a properly selected temperature restores the ductility of the metal matrix and improves the integrity of the sintered material impaired by the effect of deformation. Annealing also causes favorable changes in the porosity morphology, removing defects in the form of gaps and resulting in the spheroidization of voids. With an appropriately selected initial porosity and degree of deformation, subsequent annealing of sinters compacted by free cold upsetting provides products with strength properties comparable to sinters with the same density and subjected to single compaction and sintering but with considerably higher fracture toughness.

36 MATERIALS SCIENCE↗

Rapid microwave synthesis of indium filled skutterudites: An energy efficient route to high performance thermoelectric materials

Graphical abstract: Filled skutterudites are promising thermoelectric materials. We report the microwave assisted synthesis of CoSb{sub 3} and In{sub 0.2}Co{sub 4}Sb{sub 12}. This method reduces the calcination time for skutterudite phase formation from 2 days to 2 min, thereby significantly reducing the time and energy needed to produce materials suitable for property and device testing. Highlights: Black-Right-Pointing-Pointer The microwave assisted solid state synthesis of CoSb{sub 3} and In{sub 0.2}Co{sub 4}Sb{sub 12} is reported. Black-Right-Pointing-Pointer This method allows the calcination time to be reduced from 2 days to 2 min. Black-Right-Pointing-Pointer Physical properties of microwave samples match those prepared conventionally. -- Abstract: Filled skutterudites are promising thermoelectric materials due to reduced thermal conductivity upon inserting a guest atom or 'rattler' into the CoSb{sub 3} structure. By using an indium rattler dimensionless Figure of Merit (ZT) values >1 at 650 K have been reported. The conventional synthesis of these compounds typically takes several days ({approx}3 days) to obtain the final well-sintered material for property measurements. We report here a microwave-assisted synthesis method that reduces the initial calcination time from 2 days to 2 min. This route significantly reduces the time needed to produce materials suitable for property and device testing.

36 MATERIALS SCIENCE↗

Power Electronics Thermal Control (Presentation)

Thermal management plays an important part in the cost of electric drives in terms of power electronics packaging. Very promising results have been obtained by using microporous coatings and skived surfaces in conjunction with single-phase and two-phase flows. Sintered materials and thermoplastics with embedded fibers show significant promise as thermal interface materials, or TIMs. Appropriatecooling technologies depend on the power electronics package application and reliability.

33 ADVANCED PROPULSION SYSTEMS↗

Ultra‐Uniform Nanocrystalline Materials via Two‐Step Sintering

Abstract Nanocrystalline materials with superior properties are of great interest. Much is discussed about obtaining nanograins, but little is known about maintaining grain‐size uniformity that is critical for reliability. An especially intriguing question is whether it is possible to achieve a size distribution narrower than what Hillert theoretically predicted for normal grain growth, a possibility suggested—for growth with a higher growth exponent—by the generalized mean‐field theory of Lifshitz, Slyozov, Wagner (LSW), and Hillert but never realized in practice. Following a rationally designed two‐step sintering route, it has been made possible in bulk materials by taking advantage of the large growth exponent in the intermediate sintering stage to form a uniform microstructure despite residual porosity, and freezing the grain growth thereafter while continuing densification to reach full density. The bulk dense Al 2 O 3 ceramic thus obtained has an average grain size of 34 nm and a size distribution much narrower than Hillert's prediction. Bulk Al 2 O 3 with a grain‐size distribution narrower than the particle‐size distribution of starting powders is also demonstrated, as are highly uniform bulk engineering metals (refractory Mo and W‐Re alloy) and complex functional ceramics (BaTiO 3 ‐based alloys with superior dielectric strength and energy capacity).

Dong, Yanhao↗

Synthesis of ZrO{sub 2} nanoparticles by hydrothermal treatment

Zirconium oxide (zirconia, ZrO{sub 2}) is the most common material used for electrolyte of solid oxide fuel cells (SOFCs). Zirconia has attracted attention for applications in optical coatings, buffer layers for growing superconductors, thermal-shield, corrosion resistant coatings, ionic conductors, and oxygen sensors, and for potential applications including transparent optical devices and electrochemical capacitor electrodes, fuel cells, catalysts, and advanced ceramics. In this work, zirconia particles were synthesized from ZrCl{sub 4} precursor with hydrothermal treatment in a batch reactor. Hydrothermal treatment may allow obtaining nanoparticles and sintered materials with controlled chemical and structural characteristics. Hydrothermal treatment was carried out at temperatures of 150 – 200°C with precursor concentration of 0.1 – 0.5 M. Zirconia particles obtained from this treatment were analyzed by using SEM, PSD and XRD to characterize the morphology, particle size distribution, and crystallinity, respectively. Based on the analysis, the size of zirconia particles were around 200 nm and it became smaller with decreasing precursor concentration. The increasing temperature caused the particles formed having uniform size. Zirconia particles formed by hydrothermal treatment were monoclinic, tetragonal and cubic crystal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Chromium segregation at phase boundaries in Cr-doped WC-Co cemented carbides

Highlights: • Experimental evidence of a mixed (W,Cr) carbide layer on WC grain surfaces • Evidence of Cr segregation in the Co-rich binder phase in front of WC grain surfaces • Temperature dependent equilibrium segregation of Cr estimated from atom probe data • Experimental observations supported by predictions from thermodynamic modelling - Abstract: Atom probe tomography has shown (Cr,W)C to be present as a thin WC grain surface layer in an as-sintered Cr-doped WC-Co cemented carbide microstructure slowly cooled from the sintering temperature. The Co-rich binder phase contained a segregation of Cr in front of this surface layer. The mixed carbide layer was not observed when the as-sintered material had been heat treated at 1000 °C for 3000 s and then quickly cooled. A reduced amount of segregated Cr was, however, still present in the binder phase in front of the WC grain surface. These observations are supported by predictions from thermodynamic modelling; (Cr,W)C becomes stable at temperatures below 940 °C in the absence of other secondary carbides. The equilibrium segregation of Cr in the binder phase was estimated to 0.8 and 0.4 monolayer in the as-sintered and heat treated materials, respectively. The energy of segregation was calculated to 0.22 eV/Cr atom from the atom probe data. This value would result in a Cr segregation of 0.3 monolayer at the sintering temperature 1410 °C, provided that the energy of segregation in the Co-rich liquid phase sintering medium is the same as in the Co-rich binder phase. This Cr segregation may explain the WC grain growth inhibiting effect of Cr additions to WC-Co cemented carbide materials.

36 MATERIALS SCIENCE↗

DEVELOPMENT OF CERAMIC WASTE FORMS FOR AN ADVANCED NUCLEAR FUEL CYCLE

A series of ceramic waste forms were developed and characterized for the immobilization of a Cesium/Lanthanide (CS/LN) waste stream anticipated to result from nuclear fuel reprocessing. Simple raw materials, including Al{sub 2}O{sub 3} and TiO{sub 2} were combined with simulated waste components to produce multiphase ceramics containing hollandite-type phases, perovskites (particularly BaTiO{sub 3}), pyrochlores and other minor metal titanate phases. Three fabrication methodologies were used, including melting and crystallizing, pressing and sintering, and Spark Plasma Sintering (SPS), with the intent of studying phase evolution under various sintering conditions. X-Ray Diffraction (XRD) and Scanning Electron Microscopy coupled with Energy Dispersive Spectroscopy (SEM/EDS) results showed that the partitioning of the waste elements in the sintered materials was very similar, despite varying stoichiometry of the phases formed. Identification of excess Al{sub 2}O{sub 3} via XRD and SEM/EDS in the first series of compositions led to a Phase II study, with significantly reduced Al{sub 2}O{sub 3} concentrations and increased waste loadings. The Phase II compositions generally contained a reduced amount of unreacted Al{sub 2}O{sub 3} as identified by XRD. Chemical composition measurements showed no significant issues with meeting the target compositions. However, volatilization of Cs and Mo was identified, particularly during melting, since sintering of the pressed pellets and SPS were performed at lower temperatures. Partitioning of some of the waste components was difficult to determine via XRD. SEM/EDS mapping showed that those elements, which were generally present in small concentrations, were well distributed throughout the waste forms.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB{sub 2}

Steel-8TiB{sub 2} composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB{sub 2} particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB{sub 2} composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB{sub 2} composites. •New phases of different size and morphology were identified.

36 MATERIALS SCIENCE↗

PRELIMINARY STUDY OF CERAMICS FOR IMMOBILIZATION OF ADVANCED FUEL CYCLE REPROCESSING WASTES

The Savannah River National Laboratory (SRNL) developed a series of ceramic waste forms for the immobilization of Cesium/Lanthanide (CS/LN) and Cesium/Lanthanide/Transition Metal (CS/LN/TM) waste streams anticipated to result from nuclear fuel reprocessing. Simple raw materials, including Al{sub 2}O{sub 3}, CaO, and TiO{sub 2} were combined with simulated waste components to produce multiphase ceramics containing hollandite-type phases, perovskites (particularly BaTiO{sub 3}), pyrochlores, zirconolite, and other minor metal titanate phases. Identification of excess Al{sub 2}O{sub 3} via X-ray Diffraction (XRD) and Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM/EDS) in the first series of compositions led to a Phase II study, with significantly reduced Al{sub 2}O{sub 3} concentrations and increased waste loadings. Three fabrication methodologies were used, including melting and crystallizing, pressing and sintering, and Spark Plasma Sintering (SPS), with the intent of studying phase evolution under various sintering conditions. XRD and SEM/EDS results showed that the partitioning of the waste elements in the sintered materials was very similar, despite varying stoichiometry of the phases formed. The Phase II compositions generally contained a reduced amount of unreacted Al{sub 2}O{sub 3} as identified by XRD, and had phase assemblages that were closer to the initial targets. Chemical composition measurements showed no significant issues with meeting the target compositions. However, volatilization of Cs and Mo was identified, particularly during melting, since sintering of the pressed pellets and SPS were performed at lower temperatures. Partitioning of some of the waste components was difficult to determine via XRD. SEM/EDS mapping showed that those elements, which were generally present in small concentrations, were well distributed throughout the waste forms. Initial studies of radiation damage tolerance using ion beam irradiation at Los Alamos National Laboratory (LANL) showed little if any modification of the material after irradiation. Additional study in this area is needed. Chemical durability was briefly studied using the Product Consistency Test (PCT). Most of the elements measured were retained by the ceramic waste forms, indicating good chemical durability. Cs, Mo, and Rb were released at somewhat higher rates as compared to the matrix components, although benchmark compositions and additional characterization are needed in order to qualify the PCT results.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Integrating fiber optic sensors into metallic components for sensing in harsh environments

The integration of fiber optic sensors into high-temperature materials is critical for real-time monitoring and autonomous operation of engineering systems. This study demonstrated a spark plasma sintering (SPS)-assisted embedding process for integrating sapphire fiber optic sensors into stainless steel components during part fabrication. Optical fibers were encapsulated in stainless steel 316L powders which were sintered at different fabrication conditions using SPS to investigate the effects of sintering parameters on the embedment. Measurements of optical transmittance, combined with microstructural analysis (X-ray computed tomography and scanning electron microscopy) and mechanical testing (tensile and microhardness), were conducted to examine the fiber functionality, fiber–matrix bonding quality, and properties of the sintered materials. Here, the results show that under suitable fabrication conditions, intact optical fibers can be encapsulated in highly-densified (>98 % relative density) stainless steel components. These conditions also led to a good bond at the fiber–matrix interface with micron-sized material interdiffusion across the interface. The sintering parameters were observed to affect fiber optical attenuation, where high temperature, pressure, and hold time during SPS enhanced fiber–matrix bonding and adversely affected optical transmission. Tensile testing confirmed the superior tensile strength and ductility of the matrix fabricated by SPS. Furthermore, the materials exhibited limited strength reduction (~70 MPa) upon the integration of fibers. This study demonstrates the effectiveness of SPS for fiber-material integration for high-temperature applications.

36 MATERIALS SCIENCE↗

Strength and microstructure of Si3N4 sintered with ZrO2 additions

Densities greater than 99 percent of theoretical were obtained with stabilized ZrO2 additions to Si3N4. Material sintered at 2140 C under 2.5 MPa nitrogen overpressure with 3.8, 9.9, and 13.4 wt pct ZrO2 had a predominantaly equiaxed grain size ranging from 0.2 to 7.0 microns. At 1370 C, the latter composition exhibited a flexural strength of about 487 MPa, equal to that of a finer-grain-size, hot-pressed Si3N4 + ZrO2 material having excellent high-temperature static fatigue properties. Transmission electron microscopy of the sintered Si3N4 revealed a glassy grain-boundary phase at all three ZrO2 levels and partially crystalline triple points for the 9.9 and 13.4 wt pct ZrO2-containing materials. Slow crack growth was observed for 1370 C flexure tests and correlated with nonlinear load deflection traces for stresses greater than 503 MPa. The crystallization of the grain-boundary glass is insterpreted as beneficial to the attainment of high (1370 C) flexural strength.

Sanders, W. A.↗

High-temperature nanoindentation creep studies on castable and sintered nanostructured low-activation ferritic-martensitic alloys

In this article, we present the creep characteristics of two reduced activation ferritic-martensitic steels of identical starting compositions formed by different fabrication routes: a nanostructured ferritic alloy commonly referred to as a castable nanostructured alloy (CNA) and a sintered nanostructured alloy (SNA) variant. Through a series of nanoindentation experiments spanning a temperature range of 25 °C to 650 °C, with a maximum load of 100 mN, we find creep behaviors in the cast and sintered materials to be remarkably similar. The creep stress exponent (n) for CNA and SNA were found to be in the range of 8–35 and the activation volume was ∼14–42b 3 , underscoring a dominance of dislocation-mediated mechanisms in both alloys. Notably, we observed a decline in the creep stress exponent with increasing temperature, attributable to the heightened influence of thermally activated dislocations. This phenomenon suggests a potential transition in the deformation mechanism towards a thermally activated dislocation climb process, significantly impacting the observed creep behavior.

36 MATERIALS SCIENCE↗

Sintering behavior of Lanthana-bearing nanostructured ferritic steel consolidated via spark plasma sintering

Elemental powder mixture of Fe–14Cr–1Ti–0.3Mo–0.5La 2 O 3 (wt%) composition is mechanically alloyed for different milling durations (5, 10 and 20 h) and subsequently consolidated via spark plasma sintering under vacuum at 950 °C for 7 min. The effects of milling time on the densification behavior and density/microhardness are studied. The sintering activation energy is found to be close to that of grain boundary diffusion. The bimodal grain structure created in the milled and sintered material is found to be a result of milling and not of sintering alone. The oxide particle diameter varies between 2 and 70 nm. As a result, faceted precipitates smaller than 10 nm in diameter are found to be mostly La–Ti–Cr-enriched complex oxides that restrict further recrystallization and related phenomena.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Friction and wear of sintered fibermetal abradable seal materials

Three abradable gas-path seal-material systems based on a sintered NiCrAlY fiber metal structure were evaluated under a range of wear conditions representative of those likely to be encountered in various knife-edge seal (labyrinth or shrouded turbine) applications. Conditions leading to undesirable wear of the rotating knife were identified, and a model proposed based on thermal effects arising under different rub conditions. It was found, and predicted by the model, that low incursion (plunge) rates tended to promote smearing of the low-density sintered material with consequent wear to the knife edge. Tradeoff benefits between baseline 19 percent dense material, a similar material of increased density, and a self-lubricating coating applied to the 19 percent dense material were identified on the basis of relative rub tolerance and erosion resistance.

Bill, R. C.↗

Flash sintering of stoichiometric and hyper-stoichiometric urania

Flash sintering (FS), a novel fabrication technique belonging to the family of field assisted sintering (FAS) techniques, has been utilized in this study to fabricate uranium dioxide (UO 2 ) pellets. Stoichiometric (UO 2.00 ) and hyper-stoichiometric (UO 2.16 ) pellets were flash sintered at 600 °C within a few (2–3) minutes. This is in sharp contrast to conventional sintering where temperatures hundreds of degrees higher are necessary and the sintering time extends to hours. Relating this in terms of the homologous temperature ratio (T H ) for both conditions shows that in the case of flash sintering at 600 °C, T H = 0.3 versus T H = 0.6 for conventional sintering at 1600 °C. The highest density achieved for a UO 2.00 pellet was 81% theoretical density (TD) when flash sintered at 600 °C for 184 s at a field of 188 V/cm and a current density of 442 mA/mm 2 . For the UO 2.16 pellet, the highest achieved density was 92% TD when flash sintered at 600 °C for 140 s at a field of 188 V/cm and a current density of 632 mA/mm 2 . X-ray diffraction (XRD) characterization of the sintered pellets showed the final sintered material to be single cubic fluorite phase. Scanning electron microscopy (SEM) of longitudinal sections revealed non-uniform microstructures with regions of high density where the grain size ranged from 1 to 15 μm. Comparisons between conventionally and flash sintered pellets that achieved equivalent shrinkage strains were also conducted. Lastly, in all cases, the flash sintered pellets achieved similar densification to the conventionally sintered pellets at much lower furnace temperatures and shorter times.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The feasibility of solar reflector production from lunar materials for solar power in space

Science Applications International Corporation (SAIC) investigated the feasibility of producing solar reflectors from indigenous lunar materials for solar power production on the moon. First, lunar construction materials and production processes were reviewed, and candidate materials for reflector production were identified. At the same time, lunar environmental conditions were reviewed for their effect on production of concentrators. Next, conceptual designs and fabrication methods were proposed and studied for production of dish concentrators and heliostats. Finally, fabrication testing was performed on small-scale models using earth analogs of lunar materials. Findings from this initial investigation indicate that production of concentrators from lunar materials may be an attractive approach for solar energy production on the moon. Further design and testing are required to determine the best techniques and approaches to optimize this concept. Four materials were identified as having high potential for solar reflector manufacture. These baseline materials were foamed glass, concrete with glass-fiber reinforcement, a glass-fiber/glass-melt composite, and an iron-glass sintered material.

Source record↗

Measuring Elastic Modulus of Sintered Metal

Technique minimizes effect of substrate on thin sintered coating. Uniaxial tension test yields approximate value for elastic modulus of sintered material on thin substrate. Electrode composed of central perforated nickel plated steel sheet about 4 mils (0.1mm) thick, coated on each face by porous sintered nickel about 8 mils (0.2mm) thick.

Fedors, R. F.↗