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At least 55 records · Page 3

All sources NASA NTRS DOE OSTI

DOE OSTI2022

CO 2 Laser Sintering of Garnet-Type Solid-State Electrolytes

We report the processing of garnet-type solid-state electrolytes remains challenging as densification conventionally requires high sintering temperatures and long processing times, which can result in severe Li loss, the formation of secondary phases, and thus high porosity and low ionic conductivity. Here, we report an ultrafast sintering method based on CO 2 laser scanning with the assistance of a heating stage. We demonstrate the rapid densification of low-packing-density Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO) films, which are difficult to densify by conventional furnace sintering methods. This unique approach has three fingerprint characteristics: (1) mitigation of Li loss through ultrafast sintering (dwelling time $\ll$1 s); (2) a unique anisotropic shrinkage behavior that greatly reduces film thickness; (3) wave-like surface topology from point scanning strategy that enables 3D interfacial contacts with electrode materials. Herein, highly dense (95.68%) and highly conductive (0.26 mS·cm –1 at 25 °C) LLZTO films are obtained through CO2 laser sintering. This work provides a unique, scalable, and widely applicable ultrarapid laser sintering technique to overcome the difficulties associated with classic methods for the integration of SSEs for practical all-solid-state Li-metal battery applications.

36 MATERIALS SCIENCE↗

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 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 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 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 OSTI2023

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↗

DOE OSTI2024

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↗

DOE OSTI2024

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↗

DOE OSTI2023

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↗

DOE OSTI2022

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↗

DOE OSTI2022

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↗