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At least 73 records · Page 4

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗

Synthesis and Photonic Sintering of Proton Conducting Lanthanide Nickelates

Lanthanide nickelate perovskites are known proton conductors at intermediate temperatures (350-600°C). They are attractive targets for proton conducting fuel cells and electrolyzers due to their operational temperature range and their stability in the presence of CO 2 . These materials have the formula LNiO 3 , with the lanthanide L = La, Ce, Pr, Nd, or Sm. Sintering is challenging due to phase transformations that occur at lower temperatures than those required for sintering. In this project, a series of lanthanide nickelate perovskites was synthesized via both a precursor solid solution method and the glycine nitrate process. Powders derived from the precursor solid solution method for LaNiO 3 and NdNiO 3 were sintered at Utility Global Inc. at various temperatures utilizing fast photonic sintering. LaNiO 3 was successfully sintered while maintaining the perovskite phase. NdNiO 3 underwent a phase transformation at all the conditions tested. The stability of the perovskite phase decreases moving right across the lanthanides in the periodic table, while the expected proton conductivity increases. These results will inform further investigations into lanthanide nickelate perovskites toward the goal of producing a free-standing, sintered, proton-conducting membrane.

36 MATERIALS SCIENCE↗

Pressureless sintering of lithium hydride

Lithium Hydride is a material of growing importance for addressing technological challenges related to nuclear fusion, long-term human space travel, and thermal energy storage. Pressureless sintering provides a straightforward, scalable approach to produce dense LiH parts of all sizes and shapes. Pressed LiH green compacts were sintered at heating rates from 2.5 to 20 °C/min to 650 °C, yielding densities up to 96 ± 1.4 %, with densification initiating at 500 °C. Here, a validated master sintering curve was constructed with a sintering apparent activation energy of 135 kJ/mol. X-ray diffraction and simultaneous thermal analysis revealed Li 2 O formation from 300 – 550 °C and decomposition of LiH into Li metal at 550 °C, each reflected as deviations in the master sintering curve. Computed tomography after thermal treatment to 550 °C showed the formation of corrosion products, and after thermal treatment to 650 °C LiH reduction to Li most significantly at exposed surfaces.

36 MATERIALS SCIENCE↗

Does plasma jet sintering follow an Arrhenius-type expression?

Atmospheric pressure, ambient temperature plasma jets have become a promising candidate for material processing in parallel with developments in additive manufacturing. Recent work has shown that plasma jets can be used to sinter printed nanoparticles at temperatures much lower than typically required for conventional thermal sintering. In this report we conduct a mechanistic study on plasma jet sintering that correlates specific energy input with the electrical conductivity of printed silver films after sintering. Increasing the specific energy input accelerated the sintering process following an Arrhenius-like exponential trend across a large range of conditions, including both helium and argon plasma jets. Although an exponential relationship is also found with the plasma heated substrate temperature, independent studies indicate that heating is not the primary mechanism. These results suggest there is a general behavior that couples the plasma jet with the surface.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Predicting Sintering Window of Binder Jet Additively Manufactured Parts Using a Coupled Data Analytics and CALPHAD Approach

Batch-to-batch variation in powder compositions for binder jet additive manufacturing (BJAM) can significantly deter defining an “ideal” sintering window for a given alloy. One way to overcome the problem is by running sintering experiments at various temperatures for each batch of the powder. However, such an approach increases the time required to achieve large-scale production of parts. The predictive capabilities of computational thermodynamic tools like CALPHAD can be leveraged to overcome the challenge, especially for binder jet additive manufacturing, since the process occurs under near-equilibrium conditions. However, calculating the sintering window using CALPHAD can be computationally expensive, considering many possible feedstock compositions within “specification”. Here, we generate high throughput CALPHAD data for nickel-based superalloys to develop machine learning models to predict the sintering window rapidly. The predictive capability of the models has been validated using published results on BJAM of Inconel 718 and 625. Further, validated models are lightweight and can be deployed in an industrial setting to get sintering window in an accelerated manner.

36 MATERIALS SCIENCE↗

Grand potential sintering simulations of doped UO 2 accident-tolerant fuel concepts

Chromium-doped UO is a widely-studied near-term deployable accident-tolerant fuel concept because it results in a dense, large-grain structure that increases the fuel resistance to densification, swelling, and fission gas release. A new charged-interstitial mechanism was recently proposed to describe the behavior of dopants like chromium in sintered UO 2 . Based on that mechanism, manganese was suggested as an even stronger dopant than chromium. In the current work we use mesoscale sintering simulations in an effort to validate the new mechanism. We compare the relative behavior of Cr-doped and undoped UO 2 against experimental data in the literature. We also make predictions of the relative behavior of Mn-doped UO 2 . Simulations are done using the phase field-based grand potential sintering model. Dopants have two effects on sintered UO 2 . They marginally increase the densification rate and greatly increase the average grain size. Both of these effects are individually tested in small-scale simulations. Then large 3D sintering simulations are used to test the combined behavior of both effects. The results for the densification rate simulations are consistent with experiments for Cr-doped fuels. However, we note the grain growth rates are lower than what is found in the literature for Cr-doped fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Thermomechanical Degradation of Sintered Copper Under High-Temperature Thermal Shock

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronics modules, especially in operating temperatures greater than 150 degrees C. In this paper, we investigate the thermomechanical performance of sintered copper (Cu) as a large-area attachment, bonded between Cu baseplates and active-metal-bonded substrates, under accelerated thermal shock (-40 degrees C to 200 degrees C) conditions. In the fabrication phase of the samples, we used different stencil patterns and found that the grid and stripe patterns resulted in a better outgassing of the residual organics during the sintering process, thereby ensuring a substantially improved bond quality compared to a full-area print. The paste consisted of Cu microflakes, and we performed sintering using a Budatec SP300 sintering press at 275 degrees C with 15 MPa of bonding pressure for 5 minutes in a nitrogen atmosphere. Under accelerated experiments, we monitored the degradation of the sintered Cu bond in the samples through C-mode scanning acoustic microscope (C-SAM) images. To quantify the defect percentage in C-SAM images, we investigated image denoising techniques to exclude the pattern prints. Finally, we cross-sectioned a sample and obtained scanning electron microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS,INORGANIC, ORGANIC, PH↗

Sintering-based Metal Additive Manufacturing Methods for Magnetic Materials

In this chapter, we review the relationship between solid-state sintering and additive manufacturing (AM) methods for fabricating soft and hard magnetic materials. Heat treatment as a post-processing method has been done in conjunction with AM as a method to improve density and/or mechanical properties. In binder jetting (BJT) of metal powders, sintering is a crucial post-processing step and is necessary for obtaining the final product. This is because the parts are only in the “green” state when they leave the BJT printer, with poor mechanical properties and high porosity. Sintering densifies and strengthens the green part into the final product. A potential industrial application for sintering-based AM is the fabrication of magnetic materials. The motivation for doing so, the process and properties of the AM magnets, and the potential applications of post-sintered AM magnets are explored.

Wang, Haobo↗

An Aerosol Jet Printed Resistance Temperature Detector‐Micro Hotplate with Temperature Coefficient of Resistance Stabilized by Electrical Sintering

Abstract Aerosol jet printing (AJP) is an emerging direct write tool enabling rapid prototyping and fabrication of electronics components. AJP provides faster and less expensive production of devices with feature sizes of >10 microns compared to traditional MEMS processes. Herein, the fabrication of a resistance temperature detector‐micro hotplate (RTD‐µHP) is reported using AJP printed silver. AJP eliminates sophisticated MEMS processes such as masking, alignment, and etching. The compatibility of the AJP process with a broad range of materials is demonstrated by printing highly resolved lines on rigid and flexible substrates. Optimal thermal sintering conditions of AJP printed silver (Ag) lines are found by in situ resistance measurements. To stabilize the temperature coefficient of resistance (TCR) of the RTD‐µHP at high operating current levels, electrical sintering is performed on the RTD‐µHPs. Electrical sintering improves the conductivity of fully thermally sintered Ag RTD‐µHPs by 32% and provides a burn‐in mechanism for stabilizing the TCR. The TCR of the RTD‐µHPs after electrical sintering is 3.80 × 10 −3 at 22 °C, close to the value for bulk Ag. The performance of the RTD‐µHPs is tested using a reference thermocouple. The RTD‐µHPs show reliable and repeatable heating and temperature sensing up to 70 °C in air.

Sui, Yongkun↗

Nanoscale stacking fault–assisted room temperature plasticity in flash-sintered TiO 2

Ceramic materials have been widely used for structural applications. However, most ceramics have rather limited plasticity at low temperatures and fracture well before the onset of plastic yielding. The brittle nature of ceramics arises from the lack of dislocation activity and the need for high stress to nucleate dislocations. Here, we have investigated the deformability of TiO 2 prepared by a flash-sintering technique. Our in situ studies show that the flash-sintered TiO 2 can be compressed to ~10% strain under room temperature without noticeable crack formation. The room temperature plasticity in flash-sintered TiO 2 is attributed to the formation of nanoscale stacking faults and nanotwins, which may be assisted by the high-density preexisting defects and oxygen vacancies introduced by the flash-sintering process. Distinct deformation behaviors have been observed in flash-sintered TiO 2 deformed at different testing temperatures, ranging from room temperature to 600°C. Potential mechanisms that may render ductile ceramic materials are discussed.

36 MATERIALS SCIENCE↗

Optimization of Lithium Content and Sintering Additives in Tape Cast Lithium Garnet Electrolyte Sheets

The lithium garnet (LLZO) remains one of the most promising electrolyte materials for producing solid state batteries. Tape casting is one method for producing the thin ceramic electrolyte layer required for a high-performance solid state battery. Processing of LLZO is complicated by several factors including lithium volatilization, abnormal grain growth and phase instability. Many of these issues are exacerbated in tape cast sheets by the sheets' higher surface area to volume ratio, when compared to pellet processing methods. Here, we report on an environmentally friendly aqueous tape casting process for LLZO using methylcellulose as a binder and compare final sheet properties to other, solvent-based, options. Solids loading, binder content, dispersant composition, and wetting agent type are varied to improve ease of casting and enhance properties of the as-cast tape. Lithium content in sintered LLZO sheets is controlled by the inclusion of excess Li 2 CO 3 as lithium source in the ceramic tape itself and by a novel method of producing a lithium-saturated furnace atmosphere. Sintering time and temperature are optimized, and rapid thermal processing is investigated as a method of reducing lithium loss. Al 2 O 3 and MgO are examined for use as sintering additives. Characterization of LLZO sheets is performed with XRD, EIS and SEM. Li 2 CO 3 and sintering additive levels are optimized for ionic conductivity and density. The optimization effort improved the conductivity and density of 100µm thick sintered sheets to greater than 3x10 -4 S/cm conductivity and 90% density.

36 MATERIALS SCIENCE↗

Fundamentals of Spark-Plasma Sintering (Final Report)

This project was focused on the development of the general theory of spark-plasma sintering (SPS) taking into account the role of both thermal and non-thermal factors in the acceleration of SPS mass transport. SPS is a particular kind of field-assisted sintering, which provides potentially revolutionary capabilities to the processing of materials into configurations previously unattainable. This approach significantly improves the processing time- and quality-wise. It carries the potential of maintaining the nano and sub-micron structure in nano-powder-based materials after consolidation. SPS gains particular prominence in connection with its exceptional potential of rapid and ultra-rapid processing of very hard-to-deform materials, which would typically require lengthy consolidation times at significantly elevated temperatures under conditions of conventional powder pressing or sintering. The achievement of the ultimate goal of the formulation of the general theory of spark plasma sintering required the identification of the contributions of all the thermal and non-thermal factors in the enhancement of mass transport under SPS processing conditions. As our research indicated, this enhancement is mostly reduced to the creation of the conditions of controlled non-equilibrium, which is especially important in ultra-rapid field-assisted sintering techniques. Thus, the main project objective was the analysis of the SPS physical basis at multiple scales specifically exploring the role of electric current in the acceleration of mass transport and with an emphasis on the conditions of controlled non-equilibrium.

36 MATERIALS SCIENCE↗

Mechanically Robust High Magnetic Performance Sm-Co Sintered Magnets (Final Report)

Samarium-cobalt based permanent magnets (SmCo 5 and Sm 2 Co 17 ) have excellent magnetic properties, good corrosion resistance, and long-term thermal stability. Sm-Co sintered magnets have been widely used in electric machines, telecommunication, biomedical devices, and magnetic sensors. They are the most preferred magnets for high-temperature applications (200 - 550 °C). However, Sm-Co sintered magnets are brittle. They cannot be used for applications subjected to high stress, vibration, or mechanical shock. Sm-Co sintered magnets are prone to chipping, and fracture in the course of block magnet manufacturing, part machining, assembly, and operation. The brittleness leads to a magnet production loss of up to 20-30% in volume and imposes limitations on part size and shape. Developing mechanically robust high-performance Sm-Co sintered magnets is of great scientific and technical significance. This project is in response to the current market need for mechanically robust high magnetic performance Sm-Co sintered magnets and their novel manufacturing processes. The project will focus on scaling-up, validation, and technology maturation study of the mechanically tough high magnetic performance Sm-Co magnets developed by Ames Laboratory at a lab-scale with the collaboration of the industry partner Electron Energy Corporation (EEC).

36 MATERIALS SCIENCE↗

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↗

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↗

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↗

Spark plasma sintering (SPS) densified U 3 Si 2 pellets: Microstructure control and enhanced mechanical and oxidation properties

Dense U 3 Si 2 pellets with controlled grain structure and enhanced thermal-mechanical and oxidation properties are synthesized with spark plasma sintering (SPS). Microstructure and phase composition of the SPS densified pellets are characterized systematically using SEM, EDS, and XRD. Thermal-mechanical properties and oxidation behavior of the sintered silicide fuel pellets are analyzed by laser flash, indentation, and dynamic thermogravimetric analysis. Dense U 3 Si 2 pellets are consolidated by combining high energy ball milling and rapid sintering by SPS, and the microstructure structures are controlled from micron-sized (~5.7 μm grain size) for conventional silicide to a nanocrystalline matrix with an average grain size of ~280 nm. A dominant phase of distorted U 3 Si 2 was identified with lattice expansion due to residual thermal stress upon SPS consolidation and rapid cooling processes. Both micron-sized and nano-sized pellets show exceptional thermal transport properties, consistent with monolithic silicides reported in literature. The SPS-densified pellets possess simultaneously high hardness and fracture toughness. The SPS-densified silicide pellets also demonstrate exceptional oxidation performance with extended onset oxidation temperature above 500 °C and reduced oxidation kinetics, particularly for nano-sized pellets. A strong strain effect was proposed in which compressive stress in nano-sized pellets enhances the oxidation resistance of silicide fuels, as evidenced by the degradation of oxidation performance upon strain relaxation by isothermal annealing. The correlation among the sintering process – microstructure control – physical properties and fuel behavior is established. A new concept of strain engineering is proposed further properties optimization, enabling the development of potential oxidation and corrosion-resistant silicides with extended performance, the key technological challenge of U 3 Si 2 as the leading concept of accident tolerant fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗