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At least 415 records · Page 23
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Sintering Mechanism of Pt/Al 2 O 3 in Complex Emission Gases Elucidated via In Situ Environmental STEM

Emission control catalysts are crucial for protecting human health by preventing the release of harmful gases and unburnt fuel into the atmosphere. These catalysts often face deactivation through sintering processes in high-temperature, chemically reactive environments containing multiple gas species. Here, we use in situ environmental scanning transmission electron microscopy to monitor the sintering behavior and transient morphologies of Pt/Al 2 O 3 in various relevant gas environments through controlled experiments. Our results reveal the particle migration and atomic ripening behavior of Pt/Al 2 O 3 at the atomic scale in the presence of water vapor and oxygen, which differs from behaviors observed in single gas environments. We identify an atomic ripening mechanism involving the dissociation and migration of Pt adatom chains from Pt nanoparticles, observed only in combinational gases. Finally, these findings provide valuable insights into catalyst degradation behavior in complex gas environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Revealing Sintering Kinetics of MoS 2 -Supported Metal Nanocatalysts in Atmospheric Gas Environments via Operando Transmission Electron Microscopy

The decoration of two-dimensional (2D) substrates with nanoparticles (NPs) serve as heterostructures for various catalysis applications. Deep understanding of catalyst degradation mechanisms during service conditions is crucial to improve the catalyst durability. In this work, we studied the sintering behavior of Pt and bimetallic Au-core Pt-shell (Au@Pt core–shell) NPs on MoS 2 supports at high temperatures under vacuum, nitrogen (N 2 ), hydrogen (H 2 ), and air environments by in situ gas-cell transmission electron microscopy (TEM). The key observations are summarized as effect of environment: while particle migration and coalescence (PMC) was the main mechanism that led to Pt and Au@Pt NPs degradation under vacuum, N 2 , and H 2 environments, the degradation of MoS 2 substrate was prominent under exposure to air at high temperatures. Pt NPs were less stable in H 2 environment when compared with the Pt NPs under vacuum or N 2 , due to Pt–H interactions that weakened the adhesion of Pt on MoS 2 . Effect of NP composition: under H 2 , the stability of Au@Pt NPs was higher in comparison to Pt NPs. This is because H 2 promotes the alloying of Pt–Au, thus reducing the number of Pt at the surface (reducing H 2 interactions) and increasing Pt atoms in contact with MoS 2 . Effect of NP size: The alloying effect promoted by H 2 was more pronounced in small size Au@Pt NPs resulting in their higher sintering resistance in comparison to large size Au@Pt NPs and similar size Pt NPs. The present work provides key insights into the parameters affecting the catalyst degradation mechanisms on 2D supports.

2D materials↗
DOE OSTI2016

Effect of sintering temperature on the structural and electrical properties of Zn{sub 0.95}Cr{sub 0.05}O

In this communication, we report the results of the studies on the sintering temperature dependent structural properties and dielectric behavior of 5% Cr doped Zn{sub 0.95}Cr{sub 0.05}O samples synthesized by cost effective sol-gel technique. Crystallographic orientations, crystallinity and crystallite size (CS) have been understood by performing X-ray diffraction (XRD) measurement at room temperature. Values of CS have been further verified by carrying out Williamson – Hall (W-H) plot analysis and the difference between the CS from XRD and W-H analyses has been discussed. Dielectric behavior has been studied and its dependence on the sintering temperature has been understood in the light of crystallite size, crystal boundary density and oxygen vacancies induced possible conductivity in the samples.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Sintering temperature effect on electric transport properties and magnetoresistance of La{sub 0.67}Ca{sub 0.33}MnO{sub 3}

A compound of La{sub 0.67}Ca{sub 0.33}MnO{sub 3} (LCMO) is known as a famous colossal magnetoresistance material. Many studies have been carried in order to get more information about the electric and magnetic characteristic of the sample. The effect of two different sintering temperatures on manganite material La{sub 0.67}Ca{sub 0.33}MnO{sub 3} (LCMO) which prepared by solid state reaction, has been investigated in order to find the relations between the sintering temperature and the manganite’s electric transport properties. Characterization using X-Ray Diffractometer shows that the two samples have a single phase pattern. However, from the resistivity measurement both samples show a different value, but similar behavior. The resistivity reach maximum value in specific temperature T{sub p}, before it decreases once again to its lowest value in low temperature region.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Uniaxial compressive creep tests by spark plasma sintering of 70% theoretical density α -uranium and U-10Zr

Metallic fuels hold numerous advantages over conventional uranium dioxide fuels and are a key component of several liquid metal-cooled advanced reactor concepts including sodium fast reactors. These fuels undergo rapid swelling during early burnup; consequently, they spend most of their reactor lifetime in a porous state. The presence of this porosity alters many of the mechanical properties of the fuel including creep impacting fuel deformation during axial swelling. This work investigates the creep behavior of the porous fuel using a spark plasma sintering technique. Creep tests were performed for the first time on porous α-phase uranium and uranium with 10 wt. % zirconium (U-10Zr) samples. The samples of α-phase uranium and U-10Zr were fabricated from depleted uranium by spark plasma sintering and subjected to uniaxial compressive creep testing. Calculated stress exponents were found to be 2.6±1.6 and 5.7±1.4 for α-U and U-10Zr, respectively, and calculated activation energies were found to be 61.6±1.1kJ/mol for α-U. The creep data were also used to evaluate existing porosity inclusive in creep models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Packaging of an 8-kV Silicon Carbide Diode Module with Double-Side Cooling and Sintered-Silver Joints

Packaging innovations are needed for medium-voltage wide bandgap power semiconductor modules to enable their adaptation in grid applications. A unique challenge for packaging medium-voltage power modules is managing the trade-off between insulation demand and heat dissipation. The focus of this work was on developing a packaging innovation that improves the module heat dissipation and offers more flexibility to its insulation design. Two strategies were explored for the packaging of an 8-kV SiC diode rectifier module:(1) double-side cooling and (2) sintered-silver bonding. Double-side cooling was realized by using short metal posts rather than long and thin wire bonds for device interconnection, forming a low-profile package with devices sandwiched between two insulated metal substrates. Sintered-silver bonding enabled the devices to function reliably at over 250 °C. Simulations of the packaged module showed a low interconnect inductance of 2.67 nH and a 50% less heat transfer coefficient required to cool the chips. Prototypes of the module were fabricated, and preliminary electrical testing results validated the package design.

27 ARPA - Advanced Research Projects Agency-Energy↗
DOE OSTI2019

Soft Magnetic Multilayered FeSiCrB–Fe$_{x}$N Metallic Glass Composites Fabricated by Spark Plasma Sintering

Novel multilayered FeSiCrB–Fe $_{x}$ N ( x = 2–4) metallic glass composites were fabricated using spark plasma sintering of FeSiCrB amorphous ribbons (Metglas 2605SA3 alloy) and Fe $_{x}$ N ( x = 2–4) powder. Crystalline Fe $_{x}$ N can serve as a high magnetic moment, high electrical resistance binder, and lamination material in the consolidation of amorphous and nanocrystalline ribbons, mitigating eddy currents while boosting magnetic performance and stacking factor in both wound and stacked soft magnetic cores. Stacking factors of nearly 100% can be achieved in an amorphous ribbon/iron nitride composite. FeSiCrB–Fe $_{x}$ N multilayered metallic glass composites prepared by spark plasma sintering have the potential to serve as a next-generation soft magnetic material in power electronics and electrical machines.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Copper Electrode on Flexible Substrate by Intense Pulsed Light Sintering of Microsized Copper Particles

Metal electrodes deposited in a grid pattern onto flexible polymer substrates have been shown to be a viable alternative to replace indium tin oxide (ITO) as the transparent anode for organic photovoltaics. copper may be a better alternative in terms of cost and stability for large area low-cost solar modules, specifically on roll-to-roll platforms. These customized electrode patterns can be fabricated from copper nanoparticles through various printing techniques applicable to solution phase processing. The Intense Pulsed Light (IPL) technique has been used to sinter copper nanoparticles (~100nm) to fabricate conductive copper electrodes on flexible polymer substrates. However, compared to nanosized (~100 nm) copper particles, microsized (~2 um) copper is much cheaper. In this work, microsized (~2 um) copper is used to produce high conductive copper inks. The conductivity of the print can be adjusted through the use of surfactant. IPL sintering was optimized to obtain high conductivity copper films. In conclusion, several microscopic and electrical spectroscopic characterization techniques such as scanning electron microscopy (SEM), x-ray diffraction (XRD), 4-point probe resistivity measurements were employed to characterize the copper electrodes.

14 SOLAR ENERGY↗
DOE OSTI2023

Development of Dy-free Nd-Fe-B-based sintered magnet through grain boundary engineering using Pr-Cu alloys

For this study, Dy-free sintered magnets were fabricated by mixing Nd-Fe-B powder with various amounts of Pr-Cu powder followed by the common procedures for making Nd-Fe-B based sintered magnets. With the Pr-Cu addition increasing from 0 to 10 wt.%, the obtained magnets’ H cj increases from the original 14.5 kOe to 18.6 kOe. The highest (BH) max achieved was 35.0 MGOe with 7.5 wt.% PrCu. The distribution of the Pr and Cu elements was primarily at grain boundary and triple junctions, leading to a reduced coupling among grains, thus an enhanced H cj .

36 MATERIALS SCIENCE↗
DOE OSTI2022

Thermal properties of field-assisted-sintered SiCN–Y 2 O 3 composites

Polymer-derived amorphous SiCN has excellent high-temperature stability and properties. To reduce the shrinkage during pyrolysis and to improve the high-temperature oxidation resistance, Y 2 O 3 was added as a filler. In this study, polymer-derived SiCN–Y 2 O 3 composites were fabricated by mixing a polymeric precursor of SiCN with Y 2 O 3 submicron powders in different ratios. The mixtures were cross-linked and pyrolyzed in argon. SiCN–Y 2 O 3 composites were processed using field-assisted sintering technology at 1350°C for 5 min under vacuum. Dense SiCN–Y 2 O 3 composite pellets were successfully made with relative density higher than 98% and homogeneous microstructure. Due to low temperature and short time of the heat-treatment, the grain growth of Y 2 O 3 was substantially inhibited. The Y 2 O 3 grain size was ~1 μm after sintering. The composites’ heat capacity, thermal diffusivity, and thermal expansion coefficients were characterized as a function of temperature. The thermal conductivity of the composites ceramics decreased as the amount of amorphous SiCN increased and the coefficient of thermal expansion (CTE) of the composites increased with Y 2 O 3 content. However, the thermal conductivity and CTE did not follow the rule of mixture. This is likely due to the partial oxidation of SiCN and the resultant impurity phases such as Y 2 SiO 5 , Y 2 Si 2 O 7 , and Y 4.67 (SiO 4 ) 3 O.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Additive manufacturing of high‐density silicon carbide ceramics through post‐processing spark plasma sintering

This research advances the field of additive manufacturing (AM) of silicon carbide (SiC) ceramics by integrating spark plasma sintering (SPS) to enhance material density, mechanical strength, and thermal properties. Traditional AM techniques struggle to achieve the high‐density SiC required for demanding applications, such as aerospace engineering, where high thermal conductivity and mechanical strength are paramount. Here, our study addresses these challenges by incorporating SPS as a post‐processing step, achieving near‐theoretical maximum densities and significantly reducing porosity, thereby resulting in outstanding thermal conductivity in SiC ceramics. We developed a specialized SiC ink optimized for 3D printing, ensuring structural integrity after deposition through tailored rheological properties. The application of SPS facilitates rapid, uniform sintering, essential for attaining superior density, mechanical properties, and thermal performance. Our experimental results, confirmed through scanning electron microscopy analysis, demonstrate significant microstructural properties, mechanical strength, and thermal conductivity, showcasing the effectiveness of integrating SPS in AM processes. This innovative approach not only expands the capabilities of AM in producing complex, high‐density ceramic structures but also broadens the potential applications of SiC in demanding environments.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Suppressing η-phase development in steel-cemented tungsten carbide: A spark plasma sintering study

We describe the phase stability of a cemented tungsten carbide prepared using a high-vanadium tool steel as the cementing/binder phase and confirm suppression of (Fe, W) 6 C η-phase formation, attributed to the preferential formation of a V 0.78 W 0.22 C 1-x phase that exists as islands within the Fe-rich binder matrix. The samples were prepared using spark plasma sintering (SPS), starting from commercially available WC and A11-LVC tool steel powders. The starting powders were ball milled adding 10, 15, and 20 vol.% steel. An A11-LVC tool steel was chosen as a low-cost hard steel (49 HRC) that does not contain Ni or Co but has a high vanadium (~9 wt.%) and carbon (~1.75 wt.%) content. Our results show that sintering by SPS can produce high-density (>98%) WC-steel specimens in which the matrix wets the WC grain surfaces and formation of the brittle η-phase is avoided. The η phase is often regarded as embrittling and undesirable, and its presence can result in degradation of mechanical properties. Microhardness values for the WC-10 and WC-15 vol.% steel samples were 12.3 ± 1.2 and 13.0 ± 0.9 GPa, respectively, whereas the fracture toughness values were 8.83 ± 0.48 and 8.81 ± 0.61 MPa·m 1/2 , respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Oxidation effects on spark plasma sintering of molybdenum nanopowders

Surface-oxidized molybdenum nanopowders are compacted by spark plasma sintering (SPS). The oxide impurity behavior is analyzed under various sintering temperatures. The densification mechanism of the nanopowders with a melted oxide phase is identified in situ by regression analysis of the experimental data on the temperature-dependent porosity change and on the SPS multistep pressure dilatometry. To increase the density of the compacted pellets, the nanopowders with the oxide phase are consolidated by SPS using the two in situ oxide removal methods: carbothermic reduction and particle surface cleaning by the electric current flow through the powders. Finally, the advantages and disadvantages of these methods in terms of the density, grain size, and mechanical properties of the final products are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

An Experimental Investigation of Sintered Particle Effect on Heat Transfer Performance in an “Annular Flow” Evaporation Tube

Wicking structures have been widely used within passive heat transfer devices with high heat fluxes, such as heat pipes, to enhance their thermal performance. While wicking structures promote capillary pumping of the working fluid and thin film evaporation, they can result in capillary evaporation and further enhance the evaporation heat transfer. In this study, a 0.5 mm thick layer of 105 µm sintered copper particles was added to the inner wall of a copper tube, aiming to form an “annular flow” and enhance the heat transfer characteristics by taking advantage of thin film and capillary evaporation. Acetone was chosen as the working fluid, and the performance of an evaporation tube was tested for power inputs of 10, 30, 50, and 70 W. For each power input, trials were run at inclination angles varying from -90 deg to 90 deg to investigate the capillary effects. The temperature measurements showed that the temperature distribution along the evaporation tube is always downward sloping, meaning the temperature at the fluid inlet is larger than the outlet. In conclusion, results show that an “annular flow” formed by a thin layer of sintered particles can promote thin film and capillary evaporation and, therefore, boost the evaporation heat transfer coefficient.

42 ENGINEERING↗
DOE OSTI2015

Phenomenological model of sintering of oxide nuclear fuel with doping admixtures

It is shown that a change in the linear dimension of compacted UO{sub 2} in the sintering process is associated with its plastic yielding under the action of the forces of residual stress and capillary forces. From the curves of sintering of a fuel with doping admixtures in various gaseous media, its rate of creep is reduced.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Role of Excess Manganese in Formation of the Structure and Transport Properties of Manganite (Nd{sub 0.67}Sr{sub 0.33}){sub 1–x}Mn{sub 1+} {sub x}O{sub 3} (x = 0, 0.2) Sintered at 1273–1473 K

The Nd{sub 0.67}Sr{sub 0.33}MnO{sub 3} manganite is a material promising for application as a cathode for medium-temperature solid oxide fuel elements. A high electrical conductivity of such a cathode is the parameter determining the efficiency of the operation of a fuel element. In this report, the effect of influence of excess manganese on the structure and the conductivity of manganite ceramics with compositions (Nd{sub 0.67}Sr{sub 0.33}){sub 1–x}Mn{sub 1+} {sub x}O{sub 3±Δ} (x = 0, 0.2) sintered at temperatures 1273–1673 K is presented for the first time. The existence of 20% excess manganese in the initial manganite powder after sintering is shown to lead to that the conductivity of the obtained ceramics in the temperature range 823–1073 K is several times higher than the conductivity of the ceramics without excess manganese.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Impact of the Sintering Additive Al{sub 2}O{sub 3} on the Electrical Conductivity of Proton-Conducting Electrolyte CaZr{sub 0.95}Sc{sub 0.05}O{sub 3 – δ}

The impact of sintering additive Al{sub 2}O{sub 3} on the electrical conductivity of calcium zirconate-based polycrystalline proton-conducting electrolyte CaZr{sub 0.95}Sc{sub 0.05}O{sub 3 – δ} (CZS) is studied. With the sintering additive Al{sub 2}O{sub 3}, ceramic samples synthesized by a combustion technique are denser, and relatively low synthesis temperatures can be used (1470°C). Adding 0.1–0.5 wt % Al{sub 2}O{sub 3} leads to an increase in the grain size from 100 nm to 1–2 μm. Increasing the Al{sub 2}O{sub 3} content up to 0.3 wt % favors a growth in the electrolyte conductivity. For samples containing Al{sub 2}O{sub 3}, calcium aluminates are detected at grain boundaries. In samples exposed to humid air, charge transfer both in the grain bulk and at intergrain boundaries is found to be mediated by protons.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Study of the Microstructure of the Aluminum-Based Composite Material with the Addition of Carbon Nanotubes after Spark Plasma Sintering

Electron microscopy is used to study samples of an aluminum matrix composite material with multiwalled carbon nanotubes (MWCNTs). The features of microstructure changes occurring during the preparation of a composite in a spark plasma sintering (SPS) setup are identified. The results of the simulation of the SPS process are presented taking into account the high electro- and heat-conducting properties of MWCNTs, which qualitatively explain the differences in the sintering processes of pure aluminum and composite samples.

77 NANOSCIENCE AND NANOTECHNOLOGY↗