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At least 217 records · Page 12

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DOE OSTI2026

Metal hybridization in dilute-alloy catalysts promotes sintering resistance by decreasing surface mobility

Dilute-metal-alloy nanoparticles exhibit enhanced catalytic performance compared with monometallic nanoparticles for many reactions. Anecdotal reports indicate that very dilute alloying can also slow the sintering rates of supported nanoparticles, although this has not been rigorously assessed and cannot be explained using bulk descriptors such as metal melting temperature. Here, in this study, we utilize methanol synthesis reactivity, microscopy and in situ spectroscopy measurements to demonstrate that 1 atom% Pt addition to ~1–2-nm-diameter Cu (Pt 1 Cu 100 ) nanoparticles supported on SiO 2 dramatically decreases their sintering rates. Minimal sintering of Pt 1 Cu 100 nanoparticles is observed during aging in H 2 up to 700 °C versus 500 °C for Cu nanoparticles. Scanning tunnelling microscopy reveals that the addition of 0.01 monolayer of Pt to a Cu(110) surface decreases the detachment rate of undercoordinated atoms, demonstrating that dilute dopants can locally decrease the rate of the first step in nanoparticle sintering. Density functional theory calculations quantify the stabilization and predict other sinter-resistant dilute alloys. We find that the degree of host–dopant d-state hybridization correlates with decreased surface mobility, providing a mechanistic framework for designing sinter-resistant catalysts.

Finzel, Jordan [Univ. of California, Santa Barbara↗

DOE OSTI2020

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↗

DOE OSTI2022

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↗

NASA NTRS1975

Effect of additions of coarse grains and fibers on the densification of a sinterable SiC

This note reports the effects on densification of independent additions of coarse equiaxed SiC grains and fibrous SiC that were mixed with fine beta-SiC to develop a duplex microstructure with improved toughness. The fine-matrix SiC did not contain excess boron and carbon. The equiaxed CVD beta-SiC was introduced in the fine beta-SiC matrix material in amounts of 5 and 10 wt%. Results indicate that the CVD beta-SiC, which is quite coarse, exhibits little indication of sinterability. The effect of these coarse-grained and fibrous additions on the sinterability of fine beta-SiC may result from a geometric type of interaction. This interpretation is reinforced by X-ray diffraction of the powders and sintered pellets via monochromatic CuK-alpha radiation; the diffraction patterns of the sintered composite structures are virtually a combination of those of the components. The addition of nonsinterable SiC to the sinterable material slightly reduces sinterability, the larger particles interacting geometrically with the fine matrix material to prevent complete densification.

Abe, H.↗

NASA NTRS1977

Pressureless sintered beta prime-Si3N4 solid solution: Fabrication, microstructure, and strength

Si3N4, AlN, and Al2O3 were used as basic constituents in a study of the pressureless sintering of beta prime-Si3N4 solid solution as a function of temperature. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 MPa were achieved at moderate temperature (1000 C), but decreased to 228 MPa at 1380 C. This substantial strength loss was attributed to a glassy grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

NASA NTRS1977

Pressureless sintered beta-prime-Si3N4 solid solution - Fabrication, microstructure, and strength

Pressureless sintering of beta-prime-Si3N4 solid solution was studied as a function of temperature using Si3N4, A1N, and Al2O3 as basic constituents. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta-prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 M Pa were achieved at moderate temperature (1000 C), but decreased to 228 M Pa at 1380 C. This substantial strength loss was attributed to a 'glassy' grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

NASA NTRS1984

Sinterability, strength and oxidation of alpha silicon carbide powders

An investigation is made of pressureless sintering of commercially available alpha-SiC powders at temperatures between 1900 and 2150 C for periods of 10 to 240 min under one atmosphere of argon pressure. It is found that alpha-SiC powder containing boron and carbon sintering aids is sinterable at 2150 C for a period of 30 min to a high final density (greater than 96 percent of theoretical). In alpha-SiC powder containing aluminum and carbon sintering aids, the final density achieved is only about 80 percent of theoretical. Determinations are made of room temperature and high temperature (1370 C) flexure strength and oxidation resistance on sintered high density (more than 96 percent of theoretical) alpha-SiC (boron, carbon) material. It is found that both the strength and the resistance to oxidation are equivalent and comparable to those of the sintered alpha-SiC which represents the state of the art.

Dutta, S.↗

NASA NTRS1992

Tribological and mechanical comparison of sintered and hipped PM212: High temperature self-lubricating composites

Selected tribological, mechanical and thermophysical properties of two versions of PM212 (sintered and hot isostatically pressed, HIPped) are compared. PM212, a high temperature self-lubricating composite, contains 70 wt percent metal bonded chromium carbide, 15 wt percent CaF2/BaF2 eutectic and 15 wt percent silver. PM212 in the sintered form is about 80 percent dense and has previously been shown to have good tribological properties from room temperature to 850 C. Tribological results of a fully densified, HIPped version of PM212 are given. They are compared to sintered PM212. In addition, selected mechanical and thermophysical properties of both types of PM212 are discussed and related to the tribological similarities and differences between the two PM212 composites. In general, both composites display similar friction and wear properties. However, the fully dense PM212 HIPped composite exhibits slight lower friction and wear than sintered PM212. This may be attributed to its generally higher strength properties. The sintered version displays stable wear properties over a wide load range indicating its promise for use in a variety of applications. Based upon their properties, both the sintered and HIPped PM212 have potential as bearing and seal materials for advanced high temperature applications.

Dellacorte, Christopher↗

NASA NTRS1992

Sintering time and atmosphere influences on the microstructure and mechanical properties of tungsten heavy alloys

The present paper traces the microstructure and mechanical property variations vs sintering time under conditions where the atmosphere was adjusted to suppress pore generation. Attention is given to tracing the mechanical property links to the grain size under optimized sintering conditions. The optimal cycle is used to sinter two heavy alloy compositions (88 and 95 wt pct W) for times up to 600 minutes at 1480 C. The 88-pct-W samples slumped, but the 95-pct-W samples were fully densified and suitable for tensile testing. At long sintering times, the tungsten grains flattened and the tungsten contiguity decreased, indicating a transition to low-energy configurations for the solid-liquid interfaces. The cube of the mean grain size varied linearly with the isothermal sintering time. This allowed the determination of grain size effects on mechanical properties, showing a decreasing yield strength with increasing time in agreement with the Hall-Petch behavior. The tensile strength and elongation were highest for sintering times from 30 to 90 min, reflecting a minimum in the residual porosity.

German, R. M.↗

NASA NTRS1992

Tribological and mechanical comparison of sintered and HIPped PM212 - High temperature self-lubricating composites

Dellacorte, Christopher↗

DOE OSTI2012

The investigation of die-pressing and sintering behavior of ITP CP-Ti and Ti-6Al-4V powders

This paper investigated the die-pressing and sintering behavior of the low-cost CP-Ti and Ti-6Al- 4V powders made by the Armstrong Process . The Armstrong powders have an irregular coral like, dendritic morphology, with a dendrite size of approximately 2-5 m. As-received as well as milled powders were uniaxially pressed at designated pressures up to 690 MPa to form disk samples with different aspect ratios. In the studied pressure range, an empirical powder compaction equation was applied to linearize the green density pressure relationship, and powder compaction parameters were obtained. The Armstrong Ti-64 powder exhibited a significantly higher sinterability than the CP-Ti powder. This was explained to be due to the higher diffusivity of V at the sintering temperature. The Ti-64 samples with a green density of 71.0% increased to 99.6% after sintering at 1300oC for 1 hour. An ex-situ technique was used to track the powder morphology change before and after sintering.

36 MATERIALS SCIENCE↗

DOE OSTI2024

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↗

DOE OSTI2018

Preliminary design setup and experimental results of laser sintering for use in aerosol jet printing

It is imperative to understand the application of emerging advanced manufacturing techniques to nuclear related capabilities. The Advanced Manufacturing thrust of the In-Pile Instrumentation Initiative seeks to apply techniques such as aerosol jet printing to allow for manufacturing of novel sensor designs. As part of this thrust, a laser sintering system is being developed. The preliminary design allows for benchtop experiments that are controlled with a manual stage. The preliminary results did not appear to achieve sufficient temperatures to sinter the specimen, and temperatures were not accurately measured by the IR camera. A calibration to link silver emissivity with temperature must be performed in order to quantitatively measure temperatures with the IR camera. This calibration will be performed, and a second sintering experiment performed in detail to determine required laser exposure times and temperatures to achieve sintering with the system. Future updates for the system include a higher resolution lens for the IR camera to allow for higher magnification temperature observations, as well as a motorized stage and control framework to link the stage movements to the specimen geometry and desired exposure time during the sintering process.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2016

Cold Sintering Process of Composites: Bridging the Processing Temperature Gap of Ceramic and Polymer Materials

Co-sintering ceramic and thermoplastic polymer composites in a single step with very high volume fractions of ceramics seems unlikely, given the vast differences in the typical sintering temperatures of ceramics versus polymers. These processing limitations are overcome with the introduction of a new sintering approach, namely “cold sintering process” (CSP). CSP utilizes a transient low temperature solvent, such as water or water with dissolved solutes in stoichiometric ratios consistent with the ceramic composition, to control the dissolution and precipitation of ceramics and effect densification between room temperature and ≈200 °C. Under these conditions, thermoplastic polymers and ceramic materials can be jointly formed into dense composites. Three diphasic composite examples are demonstrated to show the overall diversity of composite material design between organic and inorganic oxides, including the microwave dielectric Li 2 MoO 4 –(-C 2 F 4 -) n , electrolyte Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 –(-CH 2 CF 2 -) x [-CF2CF(CF3)-] y, and semiconductor V 2 O 5 –poly(3,4-ethylenedioxythiophene) polystyrene sulfonate composites. Cold sintering is more general and shall have a major impact on the processing of composite materials for many different applications, mechanical, thermal, and electronic, to mention a few possibilities. CSP concepts open up new composite material design and device integration schemes, impacting a wide variety of applications.

36 MATERIALS SCIENCE↗

DOE OSTI2022

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↗

DOE OSTI2019

Mössbauer Study and Curie Temperature Configuration on Sintering Nano-Ni-Zn Ferrite Powder

Variations of Curie temperature and strength of magnetic phases with sintering temperature and Ni concentration is investigated in the present work. The AC susceptibility studies show a decrease in Curie temperature (TC) with an increase in Ni concentration in the samples. Comparison of Curie temperatures with the reported results reveals that samples in the present work show higher TC enabling high thermal stability. The Mössbauer spectra of nano- and sintered Ni-Zn ferrite samples were recorded at room temperature to monitor the local environment around Fe cations through Mössbauer hyperfine parameters as a function of composition and sintering temperatures. The increase in sharpness of the Mössbauer sextet with an increase in Ni concentration and sintering temperature corroborate improvement in homogeneity and ferrimagnetic ordering. The results of hyperfine parameters offer the possibility of having close view on configuring Curie temperature through monitoring hyperfine field by altering sintering temperature and/or Ni concentration. As the temperature dependence of magnetic and magnetoelastic properties is strongly influenced by the Curie temperature, the successful possible configuration of Curie temperature in the present work can be further investigated for desired sensor applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2012

In-Situ X-Ray Diffraction Observations of Low Temperature Ag-Nanoink Sintering and High Temperature Eutectic Reaction with Copper

Nanoinks, which contain nm sized metallic particles suspended in an organic dispersant fluid, are finding numerous microelectronic applications. Nanoinks sinter at much lower temperatures than bulk metals due to their high surface area to volume ratio and small radius of curvature, which reduces their melting points significantly below their bulk values. The unusually low melting and sintering temperatures have unique potential for materials joining since their melting points increase dramatically after initial sintering. In this paper Ag nanoink is studied using in-situ synchrotron based x-ray diffraction to follow the kinetics of the initial sintering step by analysis of diffraction patterns, and to directly observe the high remelt temperature of sintered nanoinks. Ag nanoink is further explored as a possible eutectic bonding medium with copper by tracking phase transformations to high temperatures where melting occurs at the Ag-Cu eutectic temperature, demonstrating nanoinks as a viable eutectic bonding medium.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Sintering Kinetics of Inkjet Printed Conductive Silver Lines on Insulating Plastic Substrate

This paper focuses on sintering kinetics of inkjet printed lines containing silver nanoparticles deposited on a plastic substrate. Upon heat treatment, the change of resistance in the printed lines was measured as a function of time and sintering temperatures from 150 to 200 C. A critical temperature was observed for the sintering process, beyond which there was no further reduction in resistance. Analysis shows the critical temperature correlates to the boiling point of the solvent, which is attributed to a liquid-mediated sintering mechanism. It is demonstrated that the sintering process shuts down after the solvent has completely evaporated.

36 MATERIALS SCIENCE↗