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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Mechanically robust high magnetic-performance Sm-Co sintered magnets through microstructure engineering

Samarium-cobalt (Sm-Co) sintered magnets have high magnetic energy densities, great resistance to demagnetization and corrosion, and excellent thermal stability in a wide temperature range (–50–550 °C). However, the utilization of these magnets is restricted by their brittleness. Based on micromechanical and the Zener pinning model, Sm-Co sintered magnets with improved mechanical properties have been designed and fabricated via microstructure engineering. A small amount of fine Sm 2 O 3 particulates (0–3 wt%) has been incorporated into Sm 2 (CoFeCuZr) 17 sintered magnets to refine the grain size by up to approximately 50% (from 45 to 22 µm) and narrow the grain size distribution. Doping with 3 wt% Sm 2 O 3 increased the flexural strength by 62% while maintaining magnetic performance. Both grain-refined unimodal microstructure and heterogeneous laminated coarse/fine grain microstructure were formed by strategically designed assemblies of Sm 2 O 3 -added Sm-Co powder feedstock mixtures. The technology is compatible with existing magnet manufacturing processes. Numerical micromechanics simulation indicates that the fracture is dominated by intragranular mode. The mechanical strength is mainly enhanced by the additive-induced grain refinement, while the small amount of Sm 2 O 3 addition has a small direct positive contribution. Finally, these magnets will be more cost-effective, efficient, and robust for various functional applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Densification of non-radioactive porous siliceous particles loaded with cesium potassium copper hexacyanoferrate by spark plasma sintering

In the development of a conditioning process for cesium-bearing sorbents from the decontamination of aqueous waste streams, the treatment of a granular material composed of (Cs,K) 2 CuFe(CN) 6 loaded onto mesoporous silica particles has been investigated in an additive-free two-step conditioning process involving (i) calcination at 1000 °C to remove volatile species and (ii) densification by spark plasma sintering. A 92.0 % dense pellet was obtained after 10 min sintering at 850 °C under 100 MPa. Density and microstructural measurements indicate that densification is first driven by the viscous flow of a vitreous phase containing Cs, formed during calcination. Additionally, the density of the sample then increases further during sintering by grain boundary diffusion. However, a limited but non negligible part of cesium is lost during densification.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Synthesis, sintering, and grain growth kinetics of Hf 6 Ta 2 O 17

Here Aasystematic study of the solid-state synthesis, pressureless sintering, and grain growth kinetics of Hf 6 Ta 2 O 17 is presented. The ideal conditions for solids-state synthesis of Hf 6 Ta 2 O 17 powder with minimal particle necking was 1250 °C for 2 h in air. The resultant powder has an average particle size of 210 ± 70 nm. The combined synthesis and ball-milling procedure produces highly sinterable Hf 6 Ta 2 O 17 powder, achieving > 97 % of theoretical density after pressureless sintering at 1600 °C for 2 h in air. The grain growth mechanism was sensitive to processing conditions, appearing to be primarily driven by surface diffusion below 1600 °C and grain boundary diffusion above 1650 °C. The respective activation energies for grain growth were found to be Q S = 659 ± 79 kJ mol -1 and Q GB = 478 ± 63 kJ mol -1 .

36 MATERIALS SCIENCE↗
DOE OSTI2023

Internal defect detection and characterization of samarium-cobalt sintered magnets by ultrasonic testing technique

Excessive quantities of samarium-cobalt (Sm-Co) magnet material are being scrapped needlessly due to a lack of understanding of inhomogeneity distribution and unacceptable internal defects. If there is a way to identify, locate, characterize and when needed separate the defective portions of magnet material, utilization can be increased and product quality improved. Further, the magnets’ magnetic and mechanical performance can be improved by reducing the occurrence of internal defects. This paper reports on a cost-effective and efficient nondestructive evaluation method based on an ultrasonic testing (UT) technique applied for detecting and characterizing internal defects in Sm-Co sintered magnets. Applying the UT technique will allow users to comprehensively analyze internal defects, such as inclusions, porosity, microcracks, and other structural irregularities, check for homogeneity and anomalous regions and give the locations of these internal anomalies and defects within the Sm-Co sintered magnets. The UT technique can also be applied to other rare-earth permanent magnets, such as sintered or die-upset neodymium-iron-boron (Nd-Fe-B) magnets. The UT technique can effectively guide quality control and acceptable product selection, in addition to optimizing the magnet alloy design and production processes. Therefore, it can facilitate the improvement of magnet manufacturing efficiency and machinability, reduce scrap, prolong service life, increase the use of what would be post-production waste, and enhance product reuse and recycling at end-of-life disposition.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The effect of Si on the microstructure and mechanical properties of spark plasma sintered boron carbide

Highlights: • Si addition leads to a dense final product at a low sintering temperature. • The added Si preferentially formed SiC and borosilicate glass instead of replacing the chain atoms in boron carbide. • The hardness of our Si-containing boron carbide is 30–35% greater than currently in-use commercial boron carbide plates. - Abstract: Fully dense boron carbide discs were achieved by spark plasma sintering boron carbide powders with 10 wt% silicon. The silicon did not diffuse into boron carbide grains to produce a solid solution of Si-doped boron carbide; instead the silicon reacted with impurities in the starting powder to form β-SiC and borosilicate glass. The resultant new phases facilitated densification of the multiphase ceramic through liquid phase-assisted sintering. The resultant material exhibits improved hardness (34.3 GPa Vikers hardness under 1 kg load) with toughness comparable to both Si-free and commercially available boron carbide.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Phase evolution during spark plasma sintering of novel Si3N4-doped TiB2–SiC composite

Highlights: • The effect of Si{sub 3}N{sub 4} addition on microstructure of TiB{sub 2}–SiC composite was studied. • Fully dense TiB{sub 2}-based composite was obtained by addition of SiC and Si{sub 3}N{sub 4}. • TiC, B{sub 4}C and SiO{sub 2} were formed in Si{sub 3}N{sub 4}-free and Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC ceramics. • TiN and BN were in-situ formed only in Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC sample. - Abstract: Spark plasma sintering process was employed to fabricate TiB{sub 2}–SiC and novel Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC ceramic composites at 1900 °C for 7 min under 40 MPa. The microstructural development of TiB{sub 2}-based composites was significantly influenced by the addition of SiC as a reinforcement phase and Si{sub 3}N{sub 4} as a sintering aid. Thermodynamic assessment, X-ray diffractometry, scanning electron microscopy and energy dispersive spectroscopy disclosed the in-situ formation of TiC, B{sub 4}C and SiO{sub 2} in both samples as well as TiN and BN in the Si{sub 3}N{sub 4}-doped TiB{sub 2}–SiC sample through the chemical reactions of SiC and Si{sub 3}N{sub 4} additives with the surface oxide impurities of TiB{sub 2} particles (TiO{sub 2} and B{sub 2}O{sub 3}). The elimination of harmful oxide layers and the in-situ formation various secondary phases had remarkable influences on the sinterability and final microstructure of TiB{sub 2}.

36 MATERIALS SCIENCE↗
DOE OSTI2021

On the Arrhenius-like behavior of conductivity during flash sintering of 3 mol% yttria stabilized zirconia ceramics

Here, we discuss the Arrhenius behavior of electrical conductivity σ during flash sintering of 3 mol% yttria stabilized zirconia (3YSZ). In situ x-ray diffraction is used to determine sample temperature. Sintering contribution to σ is excluded by investigating the flash event on a dense ceramic. We show that total conductivity follows an Arrhenius-like equation in both dense and green samples, even during Stage II of flash. The non-linearity often verified during flash sintering of 3YSZ is therefore related to the furnace temperature instead of the sample temperature when building the ln(σ) vs. 1/T plots. Furthermore, we verified a change in the activation energy for conduction prior to the ignition of the flash event and discussed the possible mechanisms. For instance, the decrease in activation energy from Stage I to II in the dense sample is attributed to a contribution from electronic carriers.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Ultrafast Reactive Laser Sintering of Highly Conductive Garnet-Type LLZTO Solid Electrolytes

Rapid and scalable fabrication of garnet-type solid electrolytes remains a major challenge for the practical deployment of lithium metal batteries. Here, we report reactive laser sintering (RLS) as an ultrafast and potentially scalable strategy for fabricating garnet-type Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO) solid electrolytes. RLS of LLZTO enables simultaneous reaction and densification, achieving ∼95% relative density while minimizing lithium loss and suppressing secondary phase formation. Compared to conventional furnace sintering, RLS promotes enhanced grain growth and improved densification, leading to improved ionic conductivity (0.36 ± 0.08 mS cm −1 ) while maintaining comparable activation energies for Li + transport. Structural characterization by X-ray diffraction (XRD), Raman spectroscopy, and solid-state 6 Li/ 7 Li NMR confirms the formation of cubic garnet LLZTO with homogeneous microscale elemental distribution. In addition, nanoindentation measurements demonstrate that RLS preserves the mechanical properties of the garnet framework despite ultrafast localized thermal processing. By integrating simultaneous reaction and densification with tunable microstructural control, reactive laser sintering provides a promising manufacturing pathway for high-performance garnet solid electrolytes toward next-generation solid-state batteries.

CO2 laser↗
DOE OSTI2024

Surface Self-Diffusion Induced Sintering of Nanoparticles

Despite the critical role of sintering phenomena in constraining the long-term durability of nanosized particles, a clear understanding of nanoparticle sintering has remained elusive due to the challenges in atomically tracking the neck initiation and discerning different mechanisms. Through the integration of in situ transmission electron microscopy and atomistic modeling, this study uncovers the atomic dynamics governing the neck initiation of Pt–Fe nanoparticles via a surface self-diffusion process, allowing for coalescence without significant particle movement. Real-time imaging reveals that thermally activated surface morphology changes in individual nanoparticles induce significant surface self-diffusion. Further, the kinetic entrapment of self-diffusing atoms in the gaps between closely spaced nanoparticles leads to the nucleation and growth of atomic layers for neck formation. This surface self-diffusion-driven sintering process is activated at a relatively lower temperature compared to the classic Ostwald ripening and particle migration and coalescence processes. The fundamental insights have practical implications for manipulating the morphology, size distribution, and stability of nanostructures by leveraging surface self-diffusion processes.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Sintering time effect on crystal structure and magnetic properties of Bi{sub 0.8}La{sub 0.2}FeO{sub 3} multiferroics

Effect of sintering time over the structure and magnetic properties has been studied in Bi{sub 0.8}La{sub 0.2}FeO{sub 3} multiferroic ceramics prepared by solid state reaction technique. The structure changes with the advent mixed phase rhombohedral and orthorhombic symmetry to immaculate orthorhombic structure with sintering time from 2 to 3 hour, as revealed by means of the simulation of XRD patterns via Rietveld analysis through FullProf software. The M – H plots depict decent enhancement in magnetization with values of remnant magnetization (Mr) from 0.01868emu/g to 0.09357emu/g while the sintering time is varied from 2 to 3 hour. The metamagnetic transition may be attributed to the crumpling of the modulated spin cycloid existing inherently in the pristine compound. The presented study may have considerable impact in commercial as well as advanced electronic applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Effect of sintering treatment on structural and magnetic properties of Ni{sub 0.5}Co{sub 0.5}Fe{sub 2}O{sub 4} ferrites

Two sets of Ni{sub 0.5}Co{sub 0.5}Fe{sub 2}O{sub 4} ferrites were synthesized using sol-gel method. Both the samples were heat treated at different temperatures. The effect of sintering treatment analyzed on structural and magnetic properties. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used for structural analysis. Alternating gradient magnetometer (AGM) is used for magnetic measurements. In structural analysis, grains size is calculated using Debye - Scherrer’s formula and Williamson-Hall (W-H) plot. From both the techniques, grain size is found nearly same and increased in size with increase sintering temperature. Increased particle size is confirmed from SEM micrographs. Strain value is calculated from intercept of W-H plot. In both the samples, compressive strain in nature is found. Magnetic properties were also varying under different heat treatment. The change in magnetic properties with change in structural change at different sintering treatment is discussed in this report.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

The effects of composition and sintering temperature on the silica foam fabricated by slurry method

Reticulated ceramic or open pore ceramic foam is a well-known material which exhibits extremely high porosities, with a significant degree of interconnectivity that makes them desirable in a wide range of applications. There were broad types of ceramic foam fabrication method such as polymeric sponge method, direct foaming, and starch consolidation. In this study, the slurry method has been chosen to fabricate Silica (SiO{sub 2}) foam. In this process, Polyurethane (PU) foam template was dipped into ceramic slurry and followed by drying and sintering to obtain foam which contains porosity in the range of 50% to 70%. The compositions of SiO{sub 2} were varied starting from 55 wt.%, 60 wt.%, 65 wt.% and 70 wt.%. The samples of SiO{sub 2} that have been dipped and dried were sintered at 900°C, 1000°C, 1100°C, and 1250°C. The sintered SiO{sub 2} ceramic foam samples were characterized to observe their morphology, and physical properties. Thus, the microstructure of the SiO{sub 2} ceramic foams samples was examined by Scanning Electron Microscopy (SEM), and Electron Dispersive Spectroscopy (EDS). Meanwhile, the physical properties of the SiO{sub 2} ceramic foam samples such as the total porosity (%) and bulk density were determined using Archimedes method. It was found that the density of ceramic foam produced was in the range of 0.25 g/cm{sup 3} up to 0.75 g/cm{sup 3}, whereas the level of porosity percentage was in the range of 61.81% to 82.18% with the size of open pore or window cells were in between 141 µm up to 626 µm.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Reliability Analysis of Large-Area, Low Pressure-Assisted Silver Sintering for Medium-Voltage Power Modules

Multi-layer insulating ceramic substrates can enable medium-voltage (MV) power modules with reduced peak electric field. This benefit is particularly important for MV silicon carbide (SiC) MOSFETs due to their higher operating voltages. Large-area, low-pressure assisted silver sintering is a potential solution for bonding substrates to create a multi-layer structure. The voiding content and defect density of the bond used to create the multi-layer substrate stack-up is critical to the reliability of the power module and the thermal performance, as this bond is in the primary path for heat dissipation in the power module structure. Here, samples of two-layer direct bonded aluminum (DBA) stacks have been fabricated and subjected to thermal cycling to analyze their reliability. Passive thermal cycling from -40 degrees C to 200 degrees C was performed. Cross-sections were cut at pre-determined intervals and imaged with Scanning Electron Microscopy (SEM). After 1000 thermal cycles, adhesive failures are observed between the sintered silver and the DBA surface. Cross-sections were cut and imaged via optical microscope and SEM. Thermal analyzer measurements are recorded on a 10-kV SiC power module utilizing the sintered DBA substrate stacks.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2023

Pressureless sintering of dual-phase, high-entropy boride–carbide ceramics

Here, dual-phase, high-entropy boride–carbide ceramics were densified by pressureless sintering. Relative densities up to approximately 96% were obtained for ceramics containing about 30 vol% high-entropy boride and 70 vol% high-entropy carbide. Isostatic pressing at 200 MPa resulted in higher relative densities of both the green bodies and final ceramics compared to uniaxial pressing. The highest relative density of 96.3% was achieved for a ceramic that was isostatically pressed at 200 MPa and sintered at 2300°C for 2 h. Grain sizes of the resulting ceramics were approximately 2 µm. This is the first report of pressureless sintering of dual-phase, high-entropy boride–carbide ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of the Sintering Temperature on the Formation of Ferroelectric Properties of a Lead Zirconate–Titanate Ceramic

Effect of the sintering temperature on the formation of the microstructure, the domain structure, and the ferroelectric properties of a lead zirconate–titanate Pb(Ti{sub x}Zr{sub 1–} {sub x})O{sub 3} piezoelectric ceramics has been studied. It is shown that the ferroelectric phase forms at a sintering temperature of 860°C. At higher sintering temperatures, the main effect on the properties is due to a unit cell deformation and free charge carriers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Spark Plasma Sintering of SmS-Based Ceramic Targets for the Magnetron Sputtering

The results of studying the electric-spark plasma sintering of samarium monosulfide ceramics are presented. The dependence of the microstructure and phase composition of ceramics on the temperature of spark plasma sintering is studied on the basis of the data of scanning electron microscopy, energy dispersion X-ray microanalysis, and powder X-ray diffraction of synthesized samples. It is shown that a dense, nonporous ceramics, the phase composition of which is close to the composition of the initial powder, is formed at a sintering temperature of 1200°C.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

"Sintering" Models and In-Situ Experiments: Data Assimilation for Microstructure Prediction in SLS Additive Manufacturing of Nylon Components

Selective laser sintering methods are workhorses for additively manufacturing polymer-based components. The ease of rapid prototyping also means it is easy to produce illicit components. It is necessary to have a data-calibrated in-situ physical model of the build process in order to predict expected and defective microstructure characteristics that inform component provenance. Toward this end, sintering models are calibrated and characteristics such as component defects are explored. This is accomplished by assimilating multiple data streams, imaging analysis, and computational model predictions in an adaptive Bayesian parameter estimation algorithm. From these data sources, along with a phase-field model, bulk porosity distributions are inferred. Model parameters are constrained to physically-relevant search directions by sensitivity analysis, and then matched to predictions using adaptive sampling. Using this feedback loop, data-constrained estimates of sintering model parameters along with uncertainty bounds are obtained.

3D printing, Additive Manufacturing, polymer, sint↗
DOE OSTI2016

Microstructure and microchemistry of flash sintered K 0.5 Na 0.5 NbO 3

In this paper, flash sintering experiments were performed, for the first time, on sodium potassium niobate (KNN) ceramics. A theoretical density of 94% was achieved in 30 s under 250 V/cm electric-field at 990°C. These conditions are ~100°C lower and faster than the conventional sintering conditions. Grains tended to grow after 30 s. flash sintering duration under constant electric-field. Detailed microstructural and chemical investigations of the sample showed that there was inhomogenous Na, K distribution and it resembles a core–shell structure where K is more in the shell and Na is more in the core region. The inhomogenous distribution of Na and K was correlated with the doubling of the unit cell within the grain along 002 direction. Compositional equilibrium is achieved after a heat treatment at 1000°C for 4 h. Finally, the compositional variations appeared to have been linked to grain boundary melting during flash and consequent recrystallization as the sample cooled.

36 MATERIALS SCIENCE↗