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At least 811 records · Page 45

Suppression of grain growth by additive in nanostructured p-type bismuth antimony tellurides

Grain growth is a major issue in the preparation of nanostructured bismuth-antimony-tellurides during hot pressing the nanopowders into dense bulk samples. To prevent grain agglomeration during ball milling and growth during hot pressing, organic agent (Oleic Acid, OA) as additive was added here into the materials at the beginning of the ball milling process. With different concentrations of OA (0.5, 1.0, 1.5, 2.0, and 2.5 wt%), grains with different sizes are obtained. Structural analysis clearly shows that it is the particle size of the nanopowders that determines the final grain size in the densely compacted bulk samples. A combination of small grains ~200–500 nm and nanopores leads to effective phonon scattering, which results in the decrease of lattice thermal conductivity, and ZT of ~1.3 at 373 K for the sample with 2.0 wt% OA.

36 MATERIALS SCIENCE↗

Cold compaction study of Armstrong Process Ti-6Al-4V powders

This work investigates the cold compaction behavior of Ti-6Al-4V powders produced by Armstrong Process . As-received as well as milled powders were characterized and these powders were uniaxially die-pressed at designated pressures up to 690 MPa to form disk samples with different aspect ratios. Samples with high aspect ratio exhibited non-uniform density along the pressing axis and the density distribution is in consistent with the result predicted by finite element analysis. The linear regression analysis on the experimental density data can be used to predict density of compacts with different aspect ratios. In the studied pressure range, an empirical powder compaction equation represents the green density pressure relationship very well for both the as-received and 1-hr milled Armstrong Ti-6Al-4V powders.

99 GENERAL AND MISCELLANEOUS↗

Rapid Microwave Preparation of Thermoelectric TiNiSn and TiCoSb Half-Heusler Compounds

The 18-electron ternary intermetallic systems TiNiSn and TiCoSb are promising for applications as high-temperature thermoelectrics and comprise earth-abundant, and relatively nontoxic elements. Heusler and half-Heusler compounds are usually prepared by conventional solid state methods involving arc-melting and annealing at high temperatures for an extended period of time. Here, we report an energy-saving preparation route using a domestic microwave oven, reducing the reaction time significantly from more than a week to one minute. A microwave susceptor material rapidly heats the elemental starting materials inside an evacuated quartz tube resulting in near single phase compounds. The initial preparation is followed by a densification step involving hot-pressing, which reduces the amount of secondary phases, as verified by synchrotron X-ray diffraction, leading to the desired half-Heusler compounds, demonstrating that hot-pressing should be treated as part of the preparative process. For TiNiSn, high thermoelectric power factors of 2 mW/mK{sup 2} at temperatures in the 700 to 800 K range, and zT values of around 0.4 are found, with the microwave-prepared sample displaying somewhat superior properties to conventionally prepared half-Heuslers due to lower thermal conductivity. The TiCoSb sample shows a lower thermoelectric figure of merit when prepared using microwave methods because of a metallic second phase.

36 MATERIALS SCIENCE↗

Zn migration during spark plasma sintering of thermoelectric Zn{sub 4}Sb{sub 3}

The phase homogeneity of spark plasma sintered thermoelectric Zn{sub 4}Sb{sub 3} pellets along the pressing direction has been studied by potential Seebeck microprobe scanning and spatially resolved x-ray diffraction. Significant variations in the Seebeck coefficient reflect presence of different crystalline phases. The emergence of the ZnSb phase at the bottom of the pellet and metallic Zn impurity at the top explains the variation in the Seebeck coefficients. Quantitative phase distributions along the pressing axis were determined from the Rietveld refinements of spatially resolved x-ray diffraction patterns. These reveal a migration of highly mobilized Zn atoms under the direct current applied during spark plasma sintering.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Hot deformation induced defects and performance enhancement in FeSb{sub 2} thermoelectric materials

The effect of hot deformation induced defects and texture on thermoelectric properties of FeSb{sub 2} bulk crystals has been investigated. The transport properties of the samples along both parallel and perpendicular direction of pressing were measured from 3 K to 300 K. The results showed that thermal conductivity of the deformed samples was significantly reduced. After twice deformation, the thermal conductivity of the sample along the perpendicular direction of pressing was decreased to 4 W/mK, which was only one third of that before deformation. Transmission electron microscopy observation revealed the presence of high density of lattice defects in the deformed samples. The lattice thermal conductivity was analyzed using the Debye-Callaway approximation, and the results showed that the deformation induced lattice imperfections play an important role in enhancing phonon scattering. In addition, both the electrical resistivity and Seebeck coefficient exhibited a weak anisotropy in the deformed samples. The figure of merit ZT of the bulk FeSb{sub 2} was significantly improved from 0.010 to 0.021 after deformation.

36 MATERIALS SCIENCE↗

Thermoelectric properties of p-type PbTe/Ag{sub 2}Te bulk composites by extrinsic phase mixing

We investigated the thermoelectric properties of PbTe/Ag{sub 2}Te bulk composites, synthesized by hand milling, mixing, and hot press sintering. From x-ray diffraction and energy dispersive x-ray spectroscopy measurements, we observed Ag{sub 2}Te phase separation in the PbTe matrix without Ag atom diffusion. In comparison with previously reported pseudo-binary (PbTe){sub 1−x}(Ag{sub 2}Te){sub x} composites, synthesized by high temperature phase separation, the PbTe/Ag{sub 2}Te bulk composites fabricated with a low temperature phase mixing process give rise to p-type conduction of carriers with significantly decreased electrical conductivity. This indicates that Ag atom diffusion in the PbTe matrix changes the sign of the Seebeck coefficient to n-type and also increases the carrier concentration. Effective p-type doping with low temperature phase separation by mixing and hot press sintering can enhance the thermoelectric performance of PbTe/Ag{sub 2}Te bulk composites, which can be used as a p-type counterpart of n-type (PbTe){sub 1−x}(Ag{sub 2}Te){sub x} bulk composites.

36 MATERIALS SCIENCE↗

Detector-device-independent quantum key distribution: Security analysis and fast implementation

One of the most pressing issues in quantum key distribution (QKD) is the problem of detector side-channel attacks. To overcome this problem, researchers proposed an elegant “time-reversal” QKD protocol called measurement-device-independent QKD (MDI-QKD), which is based on time-reversed entanglement swapping. However, MDI-QKD is more challenging to implement than standard point-to-point QKD. Recently, an intermediary QKD protocol called detector-device-independent QKD (DDI-QKD) has been proposed to overcome the drawbacks of MDI-QKD, with the hope that it would eventually lead to a more efficient detector side-channel-free QKD system. Here, we analyze the security of DDI-QKD and elucidate its security assumptions. We find that DDI-QKD is not equivalent to MDI-QKD, but its security can be demonstrated with reasonable assumptions. On the more practical side, we consider the feasibility of DDI-QKD and present a fast experimental demonstration (clocked at 625 MHz), capable of secret key exchange up to more than 90 km.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Thermal conductivity of (VO 2 ) 1-x Cu x composites across the phase transition temperature

In this paper, the thermal conductivity across the metal-insulator transition (MIT) of hot-pressed polycrystalline vanadium dioxide (VO 2 ) samples is studied. The change in the total thermal conductivity (k) of hot-pressed VO 2 is insignificant across the MIT temperature. By adding copper (Cu) to make (VO 2 ) 1-x Cu x composites with x from 0 to 0.5, we find an increase in the electrical conductivity from 4 × 10 4 S m -1 to 1 × 10 6 S m -1 at 120 °C, resulting in an electronic thermal conductivity increase from 0.38 W m -1 K -1 for x = 0 to 3.8 W m -1 K -1 for x = 0.3, which is a significant increase. However, the total thermal conductivity did not increase due to the decrease in the value of the Lorenz number by an order of magnitude than its standard value using the Wiedemann-Franz relationship. Finally, on the basis of our experimental result, an empirical model is proposed to explain the thermal conductivity behavior of all (VO 2 ) 1-x Cu x samples with different Cu concentrations.

36 MATERIALS SCIENCE↗

New alnico magnets fabricated from pre-alloyed gas-atomized powder through diverse consolidation techniques

Fine Alnico 8 spherical powder produced by gas atomization was consolidated through hot pressing (HP), hot isostatic pressing (HIP), and compression molding and subsequent sintering (CMS) techniques. The effects of different fabrication techniques and processing parameters on microstructure and magnetic properties were analyzed and compared. The HP, HIP, and CMS magnets exhibited different features in microstructures and magnetic properties. Magnetically annealed at 840°C for 10 min and subsequently tempered at 650°C for 5h and 580°C for 15h, the HIP sample achieved the best coercivity (H cj =1845 Oe) due to spinodally decomposed (SD) phases with uniform and well-faceted mosaic morphology. As a result, the CMS sample had a lower Hcj than HIP and HP samples, but a higher remanence and thus the best energy product (6.5 MGOe) due to preferential grain alignment induced by abnormal grain growth.

36 MATERIALS SCIENCE↗

Processing and characteristics of transparent Gd 3 TaO 7 polycrystalline ceramics

Transparent polycrystalline Gd 3 TaO 7 ceramics were successfully developed. A sol-gel process was used to synthesize Gd 3 TaO 7 powder with a uniform composition and an estimated average particle size of 100 nm. Simultaneous thermal gravimetric analysis and differential thermal analysis (TGA/DTA) was used to identify the decomposition sequence as a function of temperature for the as-synthesized sol-gel powders. Crystallization was confirmed by X-ray diffraction (XRD) and a single phase was achieved by calcining at 1000°C. The calcined powders were hot-pressed at 1400°C to achieve >96% theoretical density with closed pore structure followed by a hot isostatic pressing at 1400°C at 207 MPa to achieve a fully dense structure. Microstructural characterization shows a uniform grain size distribution with an average grain size of about 7 μm. In-line transmission measurements revealed high transparency in the red and infrared. Thermal conductivity was measured to be >1.6 W/mK at room temperature, decreasing to ~1.3 W/mK by 500°C. Dielectric properties remain stable with relative permittivity values just above 200 and loss tangents <0.005 up to 350°C.

36 MATERIALS SCIENCE↗

Microstructure and Electrical Transport Properties of Bi{sub 3}TiNbO{sub 9} High-Temperature Piezoceramics

High-density ceramic samples of the Bi{sub 3}TiNbO{sub 9} ferroelectric phase with a layered perovskite-like structure have been produced by tape casting slurry technology and hot pressing processes. The samples have been characterized by X-ray diffraction and dielectric, piezoelectric, and pyroelectric measurements. The results demonstrate that the samples have a well-defined texture due to the preferential orientation of the basal planes of their platelike grains across the pressing axis or along the film casting direction. The Curie temperature of the samples has been determined to be T{sub C} = 1180 K. The samples have anisotropic electrical transport characteristics. Their piezoelectric constants d{sub 33} in directions perpendicular and parallel to the texture plane is 22 and 5 pC/N, respectively. The conclusion has been drawn that the synthesized materials are potentially attractive for producing high-temperature piezoelectric elements.

36 MATERIALS SCIENCE↗

The Influence of Powder Ferritization Technology on the Degree of Magnetic Texture in Plates of BaFe{sub 12}O{sub 19} and SrFe{sub 12}O{sub 19} Hexaferrites

We have studied the influence of a technology used for ferritization of the powders of barium and strontium hexaferrites on the degree of magnetic texture in pressed plates based on these powders. It is established that, in comparison to the traditional ceramic technology, the use of a chemical deposition method allows hexaferrite plates with a 19–22% higher degree of magnetic texture to be obtained by pressing raw blanks at the same values of magnetic field.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Detonation Shock Dynamics (DSD) Calibration for LX-17

The goal of this report is to summarize the results of a Detonation shock dynamics (DSD) calibration for the explosive LX-17. Considering that LX-17 is very similar to PBX 9502 (LX-17 is 92.5% TATB with 7.5% Kel-F 800 binder, while PBX 9502 is 95% TATB with 5% Kel-F 800 binder), we proceed with the analysis assuming many of the DSD constants are the same. We only change the parameters $D_{CJ}, B$ and $\bar{C}_6$ ($\bar{C}_6$ controls the how $D_{CJ}$ changes with pressing density). The parameters $D_{CJ}$ and $\bar{C}_6$ were given by Josh Coe and Sam Shaw's EOS. So, only B was optimized in fitting all the calibration data. This report first discusses some general DSD background, followed by a presentation of the available dataset to perform the calibration, and finally gives the results of the calibration and draws some conclusions. A DSD calibration of LX-17 has been conducted using the existing diameter effect data and shock shape records. The new DSD fit is based off the current PBX 9502 calibration and takes into account the effect of pressing density. Utilizing the PBX 9502 calibration, the effects of initial temperature can also be taken into account.

36 MATERIALS SCIENCE↗

Powder Metallurgy Fabrication of Molybdenum Accelerator Target Disks

Powder metallurgy approaches for the fabrication of accelerator target disks are being examined to support the development of Mo-99 production by NorthStar Medical Technologies, LLC. An advantage of powder metallurgy is that very little material is wasted and, at present, dense, quality parts are routinely produced from molybdenum powder. The proposed targets, however, are thin wafers, 29 mm in diameter with a thickness of 0.5 mm, with very stringent dimensional tolerances. Although tooling can be machined to very high tolerance levels, the operations of powder feed, pressing and sintering involve complicated mechanisms, each of which affects green density and shrinkage, and therefore the dimensions and shape of the final product. Combinations of powder morphology, lubricants and pressing technique have been explored to produce target disks with minimal variations in thickness and little or no distortion. In addition, sintering conditions that produce densities for optimum target dissolvability are being determined.

43 PARTICLE ACCELERATORS↗

Annealing of (DU-10Mo)-Zr Co-Rolled Foils

Producing uranium-10wt% molybdenum (DU-10Mo) foils to clad with Al first requires initial bonding of the DU-10Mo foil to zirconium (Zr) by hot rolling, followed by cold rolling to final thickness. Rolling often produces wavy (DU-10Mo)-Zr foils that should be flattened before further processing, as any distortions could affect the final alignment and bonding of the Al cladding to the Zr co-rolled surface layer; this bonding is achieved by a hot isostatic pressing (HIP) process. Distortions in the (DU-10Mo)-Zr foil may cause the fuel foil to press against the Al cladding and thus create thinner or thicker areas in the Al cladding layer during the HIP cycle. Post machining is difficult and risky at this stage in the process since there is a chance of hitting the DU-10Mo. Therefore, it is very important to establish a process to flatten and remove any waviness. This study was conducted to determine if a simple annealing treatment could flatten wavy foils. Using the same starting material (i.e. DU-10Mo coupons of the same thickness), five different levels of hot rolling and cold rolling, combined with five different annealing treatments, were performed to determine the effect of these processing variables on flatness, bonding of layers, annealing response, microstructure, and hardness. The same final thickness was reached in all cases. Micrographs, textures, and hardness measurements were obtained for the various processing combinations. Based on these results, it was concluded that annealing at 650°C or higher is an effective treatment to appreciably reduce foil waviness.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Creation and Shaping of Three-Dimensional Ultrafine-Grain Materials

On account of their improved physicomechanical characteristics, materials with ultrafine-grain and nanocrystalline structure are of great interest in manufacturing and elsewhere. There has been considerable research on methods of producing such materials. The techniques most commonly used to produce three-dimensional ultrafine-grain materials are equal-channel angular pressing; cumulative rolling; intense rolling; and friction with mixing. However, little information is available regarding the influence of the shaping conditions on the structure and properties of three-dimensional ultrafine-grain materials. Accordingly, there is a pressing need to find effective structuring and shaping methods for the manufacture of parts from ultrafine-grain materials with enhanced performance. Analysis of structuring and shaping methods indicates that the production of high-quality parts from three-dimensional ultrafine-grain and nanocrystalline materials calls for the development of processes, equipment, and tools such that the physicomechanical characteristics and structure of the materials formed by intense plastic deformation are retained.

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↗