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At least 289 records · Page 16

Compaction and Sintering of Mo Powders

To support the development of Mo-99 production by NorthStar Medical Technologies, LLC, Mo metal powders were evaluated for compaction and sintering characteristics as they relate to Mo-100 accelerator target disk fabrication. Powders having a natural isotope distribution and enriched Mo-100 powder were examined. Various powder characteristics are shown to have an effect on both the compaction and sintering behavior. Natural Mo powders could be cold pressed directly to >90% density. All of the powders, including the Mo-100 samples, could be sintered after cold pressing to >90% density. As an example, a compacted Mo-100 disk reached 89.7% density (9.52 g/cm3) after sintering at 1000 C for 1 hr. in flowing Ar/4%H2. Higher sintering temperatures were required for other powder samples. The relationships between processing conditions and the resulting densities of consolidated Mo disks will be presented.

Nunn, Stephen D↗

Low sintering temperature glass waste forms for sequestering radioactive iodine

Materials and methods of making low-sintering-temperature glass waste forms that sequester radioactive iodine in a strong and durable structure. First, the iodine is captured by an adsorbant, which forms an iodine-loaded material, e.g., AgI, AgI-zeolite, AgI-mordenite, Ag-silica aerogel, ZnI.sub.2, CuI, or Bi.sub.5O.sub.7I. Next, particles of the iodine-loaded material are mixed with powdered frits of low-sintering-temperature glasses (comprising various oxides of Si, B, Bi, Pb, and Zn), and then sintered at a relatively low temperature, ranging from 425.degree. C. to 550.degree. C. The sintering converts the mixed powders into a solid block of a glassy waste form, having low iodine leaching rates. The vitrified glassy waste form can contain as much as 60 wt % AgI. A preferred glass, having a sintering temperature of 500.degree. C. (below the silver iodide sublimation temperature of 500.degree. C.) was identified that contains oxides of boron, bismuth, and zinc, while containing essentially no lead or silicon.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Sintered silver joints via controlled topography of electronic packaging subcomponents

Disclosed are sintered silver bonded electronic package subcomponents and methods for making the same. Embodiments of the sintered silver bonded EPSs include topography modification of one or more metal surfaces of semiconductor devices bonded together by the sintered silver joint. The sintered silver bonded EPSs include a first semiconductor device having a first metal surface, the first metal surface having a modified topography that has been chemically etched, grit blasted, uniaxial ground and/or grid sliced connected to a second semiconductor device which may also include a first metal surface with a modified topography, a silver plating layer on the first metal surface of the first semiconductor device and a silver plating layer on the first metal surface of the second semiconductor device and a sintered silver joint between the silver plating layers of the first and second semiconductor devices which bonds the first semiconductor device to the second semiconductor device.

36 MATERIALS SCIENCE↗

Toward Interpreting Failure in Sintered-Silver Interconnection Systems

The mechanical strength and subsequent reliability of a sintered-silver interconnection system is a function of numerous independent parameters. That system is still undergoing process development. Most of those parameters (e.g., choice of plating) are arguably and unfortunately taken for granted and are independent of the silver s cohesive strength. To explore such effects, shear strength testing and failure analyses were completed on a simple, mock sintered-silver interconnection system consisting of bonding two DBC ceramic substrates. Silver and gold platings were part of the test matrix, as was pre-drying strategies, and the consideration of stencil-printing vs. screen-printing. Shear strength of sintered-silver interconnect systems was found to be was insensitive to the choice of plating, drying practice, and printing method provided careful and consistent processing of the sintered-silver are practiced. But if the service stress in sintered silver interconnect systems is anticipated to exceed ~ 60 MPa, then the system will likely fail.

Wereszczak, Andrew A↗

Microstructure studies of U3Si2 fuel pellets sintered in argon vs. vacuum environment

A comparison study on the effects of sintering U3Si2 pellets under vacuum (~1x10-6 Torr) vs in argon has been carried out as part of a pellet fabrication process for potential light water reactor fuel application. A cross section of pellets sintered in each environment was examined using scanning electron microscopy (SEM) equipped with Energy dispersive spectroscopy (EDS). The average density of pellets sintered under vacuum and argon was 11.90 g/cm3 (97.5% theoretical density (TD)) and 11.37 g/cm3 (93.2% TD), respectively. SEM micrographs and EDS revealed the grain structure of pellets sintered under vacuum (vacuum samples) to be angular with a Si rich phase, U5Si4, along the grain boundaries, while grain structure of pellets sintered in argon (argon samples) reveals smaller average grain size and higher porosity with two separate Si rich phase inclusions: U5Si4 and USi. EDS confirmed the main phase in each pellet to be U3Si2 with an O rich phase inclusion. The estimated area percent of U3Si2 and the O rich phase in the samples from SEM image analysis was: argon samples 83.9% and 5.9% and vacuum samples 81.8% and 4.6%, respectively.

fuel fabrication↗

Failure stress comparison of different pairings of Ag-plating and reflow-oven-processed pressureless-sintered-Ag interconnects

Here, sintered-silver is a candidate material to supplant solders for interconnects in power electronic packaging for many reasons including its desirably high electrical and thermal conductivities and compliance to Restriction of Hazardous Substances (RoHS) guidelines. The shear failure stress of interconnects though is limited by whatever constituent is the weakest, and that includes any employed plating. In the present study, silver-platings were processed electrolytically, electrolessly, and through sputter deposition and their influence on the entire “interconnect system” shear strength was examined. Test sets employing gold plating and no plating were included for comparison and to aid interpretation. Ambient-air, reflow-oven-processed, pressureless-sintered-silver interconnects were identically fabricated with all plating test sets. It was found that all considered silver-plating methods produced consistently strong (characteristic failure stresses > 55 MPa) sintered-silver interconnects. Because failures tended to be adhesive in all six sets, differences in failure stress among the silver-plated sets and the gold-plated or unplated sets were likely due to differences in the adhesive strength of the sintered silver with silver-plating, gold-plating, or direct bonding with copper.

36 MATERIALS SCIENCE↗

Lanthana-bearing nanostructured ferritic steels via spark plasma sintering

Here, a lanthana-containing nanostructured ferritic steel (NFS) was processed via mechanical alloying (MA) of Fe-14Cr-1Ti-0.3Mo-0.5La 2 O 3 (wt.%) and consolidated via spark plasma sintering (SPS). In order to study the consolidation behavior via SPS, sintering temperature and dwell time were correlated with microstructure, density, microhardness and shear yield strength of the sintered specimens. A bimodal grain size distribution including both micron-sized and nano-sized grains was observed in the microstructure of specimens sintered at 850, 950 and1050 °C for 45 min. Significant densification occurred at temperatures greater than 950 °C with a relative density higher than 98%. A variety of nanoparticles, some enriched in Fe and Cr oxides and copious nanoparticles smaller than 10 nm with faceted morphology and enriched in La and Ti oxides were observed. After SPS at 950 °C, the number density of Cr–Ti–La–O-enriched nanoclusters with an average radius of 1.5 nm was estimated to be 1.2 × 10 24 m –3 . The La + Ti:O ratio was close to 1 after SPS at 950 and 1050 °C; however, the number density of nanoclusters decreased at 1050 °C. With SPS above 950 °C, the density improved but the microhardness and shear yield strength decreased due to partial coarsening of the grains and nanoparticles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Onset conditions for flash sintering of UO 2

In this paper, flash sintering was demonstrated on stoichiometric and non-stoichiometric uranium dioxide pellets at temperatures ranging from room temperature (26°C) up to 600°C. The onset conditions for flash sintering were determined for three stoichiometries (UO 2.00 , UO 2.08 , and UO 2.16 ) and analyzed against an established thermal runaway model. The presence of excess oxygen was found to enhance the flash sintering onset behavior of uranium dioxide, lowering the field required to flash and shortening the time required for a flash to occur. Finally, the results from this study highlight the effect of stoichiometry on the flash sintering behavior of uranium dioxide and will serve as the foundation for future studies on this material.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A Double-side Cooled SiC MOSFET Power Module with Sintered-silver Interposers: I. Design, Simulation, Fabrication, and Performance Characterization

Planar, double-side cooled power modules are emerging in electric-drive inverters because of their low profile, better heat extraction, and lower package parasitic inductances. However, there is still concern about their reliability due to the rigid interconnection between the device chips and two substrates of the power module. In this paper, a porous interposer made of low-temperature sintered silver is introduced to reduce the thermo-mechanical stresses in the module. A double-side cooled half-bridge module consisting of two 1200 V, 149 A SiC MOSFETs was designed, fabricated, and characterized. By using the sintered-Ag instead of solid copper interposers, our simulation results showed that at a total power loss of 200 W, the thermo-mechanical stress at the most vulnerable interfaces (interposer-attach layer) was reduced by 42 % and in the SiC MOSFET by 50 % with a trade-off of only 3.6 % increase in junction temperature. The sintered-Ag interposers were readily fabricated into desired dimensions without post-machining and did not require any surface finishing for die-bonding and substrate interconnection by silver sintering. Here, the porous interposers were also deformable under a low force or pressure, which helped to accommodate chip thickness and/or substrate-to-substrate gap variations in the planar module structure, thus simplifying module fabrication. Experimental results on the electrical performance of the fabricated SiC modules validated the success of using the porous silver interposers for fabricating planar, double-side cooled power modules.

42 ENGINEERING↗

Structural, Magnetic, and Dielectric Properties of Conventional- and Microwave-Sintered Ni{sub 0.6}Zn{sub 0.4−x}Cu{sub x}Fe{sub 2}O{sub 4}

In the present work, structural, magnetic, and dielectric properties of conventional- and microwave-sintered Ni{sub 0.6}Zn{sub 0.4-x}Cu{sub x}Fe{sub 2}O{sub 4} (x = 0.0 to 0.4 in steps of 0.1) are studied. X-ray diffraction measurements confirm the formation of a single spinel phase. Crystallite size estimated from Scherrer’s method found between 30–41 nm and 36–28.5 nm in conventional- and microwave-sintered samples respectively. The lattice constant decreases with Cu substitution, suggesting the incorporation of Cu into the spinel lattice. SEM images reveal that microwave sintering results in larger grains with intragranular pores. Saturation magnetization was found to decrease with Cu content. Cation distribution estimated from the magnetization data supports the observed changes in magnetic parameters. A significant influence on microstructure and cation redistribution on dielectric properties are observed for microwave-sintered samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Preparation of Nb{sub 3}Al Superconducting Tapes by a Powder-in-Tube Method Combined with Hot-Pressed Sintering

The precursors of Nb-Al tape were fabricated by a powder-in-tube (PIT) technique. Supersaturated solid solutions of Nb-Al powder were obtained by high-energy ball milling, followed by a powder-in-tube process to prepare series of Nb{sub 3}Al precursor tapes. Compared with sintering under normal pressure, the hot-pressing sintering greatly increased the critical current density of the tapes. The results showed that the Nb{sub 3}Al tapes prepared via the powder-in-tube method and hot-pressed sintering could significantly improve the J{sub c} performance, and the value of J{sub c} (8 K, 0 T) was higher than 6 × 10{sup 5} A/cm{sup 2}. The Nb{sub 3}Al tapes after pressing under the pressure of 20 MPa and sintering at 950 {sup ∘}C for 3 h had the best magnetic flux pinning performance, and the sample reached the maximum flux pinning force (F{sub p,max}) of 3.28109 N/m{sup 3} in the magnetic field of 2.2 T.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Central Band Structures: New Insights into the Coupling Effects Between the Pores and Minerals of Sinter

It is important to elucidate the coupling effects that exist between the pores and minerals of sinter to establish the relationships that exist among the technological parameters, microstructures, and performance of the sinter. Based on the formation mechanism of the pores within sinter, four types of central band structures (CBSs) were defined to represent the microstructures of the sinter. During reduction, the cracking behavior of each CBS was studied through a series of experiments conducted at a temperature of 873 K.

36 MATERIALS SCIENCE↗

Neutron Diffraction and Neutron Radiography Investigation into Powder Sintering of Ti/Al and TiH{sub 2}/Al Compacts

Sintering behaviors of two types of powder compact, i.e., Ti/Al and TiH{sub 2}/Al, under vacuum were studied using in situ neutron diffraction, in situ thermal dilatometric measurement, and ex situ neutron radiography. Their densification, microstructure, hydrogen concentration, and phase transformation features were compared. The results indicate that the predominant phase identified in the samples sintered from both compacts is γ-TiAl phase with minor Ti{sub 3}Al phase. Dehydrogenation of TiH{sub 2} plays a decisive role in the sintering behavior and the resultant microstructure. In comparison with the Ti/Al compact, dehydrogenation occurring in the TiH{sub 2}/Al compact leads to a higher level of densification and faster sintering kinetics.

36 MATERIALS SCIENCE↗

Effect of SiO{sub 2} on the Formation of Acicular Calcium Ferrite in Sinter

SiO{sub 2} greatly influences the formation of acicular calcium ferrite (ACF), which is the main binder phase in sinter, but the mechanism of its influence is not yet clear. Experiments were carried out under air at 1200 °C with different amounts of SiO{sub 2} mixed with Fe{sub 2}O{sub 3} and Ca(OH){sub 2}. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and three-dimensional (3D) reconstruction were used to characterize the phase and morphological changes of the sintered samples. The results show that SiO{sub 2} can form silicon-ferrite of calcium (SFC), which is beneficial to the formation of ACF in sinter. The SFC content first increased and then decreased with the increasing SiO{sub 2} content. The sintered sample contained the highest contents of SFC and ACF when w(SiO{sub 2}) was 3 to 4 pct. The morphological changes in calcium ferrite observed with the increasing SiO{sub 2} content followed a sequence of massive → platy → acicular; both platy calcium ferrite and ACF were the longest in one direction in their 3D morphology. The inclusion of Si{sup 4+} in calcium ferrite crystals changes the crystal growth habit from having no obvious orientation to having a preferential orientation along the (040) or (320) surfaces, as determined by the first-principles calculations and XRD analysis of block samples. Viscosity was the main environmental factor influencing the size of ACF in samples with sufficient liquid phase.

36 MATERIALS SCIENCE↗

Influence of Particle Size on Apparent Diffusivity During Spark Plasma Sintering of Crystalline Powders

Abstract:: A theoretical framework is presented to determine an apparent diffusivity D during powder sintering and further elucidate the underlying interrelation between D and shrinkage behaviors of powders. Furthermore, to eliminate the influence of crystalline defects that are typically present in raw powders, complete crystallization of metallic glass powders is performed to allow the investigation of the influence of particle size solely on powder densification. Furthermore, to validate the framework developed, Ti{sub 40.6}Zr{sub 9.4}Cu{sub 37.5}Ni{sub 9.4}Sn{sub 3.1} crystalline alloy powders constituting particles with different sizes are examined to establish a correlation between D and the sintering behaviors of the powders. The findings show that the value of the apparent diffusivity D increases with the increasing particle size, which accelerates powder densification during spark plasma sintering. Furthermore, the results quantitatively support the argument that particle size can affect atomic diffusion during powder sintering.

36 MATERIALS SCIENCE↗

Effect of Gold on the Microstructural Evolution and Integrity of a Sintered Silver Joint

There is a need for next-generation, high-performance power electronic packages and systems employing wide band gap devices to operate at high temperatures in automotive and electric grid applications. Sintered silver joints are currently being evaluated as an alternative to Pb-free solder joints. Of particular interest is the development of joints based on silver paste consisting of nanoscale or micron scale particles that can be processed without the application of an external pressure. Microstructural evolution at the interface of a pressureless sintered silver joint formed between a SiC die with a Ti/Ni/Au metallization and an Active Metal Brazed substrate with Ag metallization at 250 °C was evaluated using Scanning Electron Microscopy, X-ray microanalysis, and X-ray Photo Electron Spectroscopy. Results from Focused Ion Beam cross-sections show that during sintering, the pores in the sintered region close to the Au layer tend to be smaller and are oriented predominantly with their longer dimension oriented parallel to the interface. With further densification, this results in the alignment of small pores parallel to the interface, creating a path for easy crack propagation. Lastly, X-ray microchemical analyses results confirm interdiffusion between Au and Ag and that a region with poor mechanical strength is formed at the edge of this region of interdiffusion.

36 MATERIALS SCIENCE↗

Effects of Sintering Temperature on the Porosity and Mechanical Behavior of Porous Titanium Scaffolds Prepared by Freeze-Casting

The purpose of this study was to investigate the effects of sintering temperature on the microstructure, and associated mechanical properties of porous titanium scaffolds prepared by freeze-casting. Sintering temperature significantly influenced the porosity and the mechanical properties of the titanium scaffolds. The porosity decreased from 60 to 20% as the sintering temperatures increased from 800 to 1100 °C. The scaffolds were of an open pore structure with pore sizes ranging from 2 to 20 μm. The average wall thickness of the porous titanium was measured, using a micro-computed tomography, to be in the range from 9.2 to 26.2 μm. Elastic modulus was between 2 to 7 GPa, depending on vacuum annealing conditions. The compression strength of the scaffolds may exceed 1000 MPa as the sintering temperature higher than 1000 °C. The increase in titanium strength and stuffiness could be mainly attributed to the decrease in porosity as well as the increase in wall thickness.

36 MATERIALS SCIENCE↗

Functionally Graded W-Cu Materials Prepared from Cu-Coated W Powders by Microwave Sintering

Three-layered W-Cu (W-10Cu/W-20Cu/W-30Cu, weight percentage) functionally graded materials were fabricated by laminate pressing of Cu-coated W composite powders with different Cu contents (10-30 wt.% Cu) and W particle sizes in the powders and microwave sintering of the powder compacts. The microstructure and the physical and mechanical properties of the graded materials were investigated. The experimental results show that the relative density of the graded W-Cu samples sintered at 1250 °C for 20 min is above 97%. Cu has a gradient layer distribution in the thickness direction, and there is good combination between the layers in the graded samples. Furthermore, the graded W-Cu materials exhibit good physical and mechanical properties. The sintered samples have thermal conductivities above 210 W m K{sup −1}, and the maximum bending strength and hardness reach 1004 MPa and 346 HV, respectively. The present results show that functionally graded W-Cu materials with high density, gradient Cu and W distribution, and good properties can be successfully prepared by laminate pressing and microwave sintering.

36 MATERIALS SCIENCE↗