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At least 379 records · Page 21

Methods of flash sintering

This disclosure provides methods of flash sintering and compositions created by these methods. Methods for sintering multilayered bodies are provided in which a sintered body is produced in less than one minute. In one aspect, each layer is of a different composition, and may be constituted wholly from a ceramic or from a combination of ceramic and metallic particles. When the body includes a layer of an anode composition, a layer of an electrolyte composition and a layer of a cathode composition, the sintered body can be used to produce a solid oxide fuel cell.

30 DIRECT ENERGY CONVERSION↗

Spark plasma sintering of fuel meats for U 3 O 8 based dispersion fuels

Research and test reactors often use dispersion-type fuel due to its increased thermal conductivity and burn-up capabilities compared to conventional fuel. Al-U 3 O 8 (aluminumtriuranium octaoxide) dispersion fuels have several advantages over their competitors, such as higher service temperature and better stability of oxygen stoichiometry. However, the two-step fabrication of dispersion fuel causes undesirable porosity in cold-pressed fuel meats that is preserved in co-extruded fuel plates. To combat this, spark plasma sintering (SPS) was used for the fabrication of Al-15, 20, and 30 vol% U 3 O 8 and 8 and 12 vol% Mo-U 3 O 8 fuel meats for the Al-U 3 O 8 time. The in situ SPS data was used to construct and validate Master Sintering Curves (MSCs) with accuracies in Al fuels at 0.02 g/cm 3 , and Mo fuels at 0.07 and 0.17 g/cm 3 . The as-sintered fuel meats were characterised using x-ray diffraction (XRD) and scanning electron microscopy (SEM) to understand chemical and physical changes following the SPS process. The pellets exhibited very high relative densities, the U 3 O 8 was observed to undergo reduction to UO 2 .

Aluminium↗

Induction ultrafast sintering

This study proposes and demonstrates induction ultrafast sintering (IUS), which enables rapid densification of refractory and other materials via two contactless modalities: direct IUS (d-IUS), where heating occurs through electromagnetic coupling with the sample, and susceptor IUS (s-IUS), where heating is achieved indirectly via an induction-heated metal case. Ultrahigh heating rates of ∼75 to >450 °C/s and temperatures exceeding 2500 °C are readily achieved. Both d-IUS and s-IUS densify molybdenum to high densities within 120 s, with only ∼1–3 % porosity observed by image analysis. Similarly, 3 mol % yttria-stabilized zirconia (3YSZ) reaches ∼97 % relative density in 30 s via s-IUS. This study further demonstrates ultrafast reactive sintering of two difficult-to-sinter materials: a refractory compositionally complex alloy–carbide (RCCA–CCC) composite, NbMoTaW–(Nb 0.37 Mo 0.11 Ta 0.39 W 0.13 ) 2 C, using d-IUS, and a compositionally complex silicide (CCS), (Mo 1/3 Nb 1/3 Zr 1/3 )Si 2 , using s-IUS. This IUS platform offers a versatile route for high-throughput materials discovery and energy-efficient fabrication of bulk refractory materials.

36 MATERIALS SCIENCE↗

Demonstration of the Reproducibility Challenges in the Sintering Behavior of Lithium‐Stuffed Garnets in Scaling up Synthesis

Lithium-stuffed garnets, such as Li 7 La 3 Zr 2 O 12 (LLZO), are promising candidates for next-generation solid-state batteries because of their high room-temperature ionic conductivity and chemical stability against lithium metal anodes, which are crucial for achieving higher energy density. However, realizing LLZO's potential in practical devices requires synthesis methods that can be scaled reliably to large batch sizes for manufacturing. Herein, we investigate the sintering reproducibility of LLZO synthesized at larger scales using ultrasonic spray pyrolysis, a cost-effective and scalable synthesis route. Two 100 g batches of Al-doped LLZO are prepared and their sintering behavior is examined in detail. Both Al-LLZO batches contain over 90 wt.% cubic-phase LLZO, and both batches exhibit room temperature conductivities greater than 1 × 10 −4 S cm −1 at a relative density above 0.8. However, variations in secondary phases and subtle differences in Al content lead to significant differences in densification and microstructure. These results demonstrate that LLZO's sintering behavior is highly sensitive to small changes in secondary phases and Al content, creating reproducibility challenges when moving from laboratory- to manufacturing-scale synthesis.

36 MATERIALS SCIENCE↗

Microwave-Hydrothermal Synthesis of Y{sub 3}Fe{sub 5}O{sub 12} Nanoparticles: Sintering Temperature Effect on Structural, Magnetic and Dielectric Properties

Herein, we report a facile microwave-assisted hydrothermal method for the preparation of yttrium iron garnet (YIG, Y{sub 3}Fe{sub 5}O{sub 12})nanocrystals and realized the synergy between its structural and magnetic properties. The as-prepared powder thermal stability was characterized in detail by using thermogravimetric-differential thermal analysis (TG-DTA). The synthesized powder was microwave sintered at six different temperatures ranging from 973 to 1373 K for 60 min and characterized using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Magnetic properties were investigated by vibrating-sample magnetometer (VSM) and ferromagnetic resonance (FMR) studies. The frequency variation of dielectric and magnetic properties was measured in the frequency range of 100 kHz–1.8 GHz. The observed magnetic and dielectric parameters such as saturation magnetization, coercivity, permeability, linewidth, dielectric constant and magnetodielectric losses are strongly affected by sintering temperature. The saturation magnetization and coercivity of YIG were found in the range 14.4–28.0 emu/g and 35–87 Oe, respectively. Furthermore, the FMR linewidth decreases from 844 to 204 Oe. This analysis undoubtedly demonstrates that the synthesis method and sintering temperature have the prominent effect on the electrical and magnetic properties of YIG and would be very useful for the garnet-based microwave device applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Comparative Study of Magnetocaloric Effect in La{sub 0.67}Ca{sub 0.20}Sr{sub 0.13}MnO{sub 3} Manganite Prepared by Sol-Gel Method and Spark Plasma Sintering

The La{sub 0.67}Ca{sub 0.20}Sr{sub 0.13}MnO{sub 3} nanoparticles and bulks were prepared by using sol-gel method (SGM) and spark plasma sintering (SPS), respectively. The X-ray diffraction analysis indicates each sample crystal in a single rhombohedral perovskite structure (space group R 3-bar c). The Curie temperature is slightly improved and the phase transition is sharpened after processing with SPS. The enhancement of magnetocaloric effect (MCE) is also observed in the samples prepared by SPS. For a field change of 3 T, the maximum isothermal entropy change is improved by 32 and 117% when different sintering temperatures and sintering pressures are applied. The magnetic phase transition and MCE can be well described by the Landau theory. The present studies suggest that the perovskite bulks prepared by SPS could be useful for the application of magnetic refrigeration.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Structure and Properties of VT6 Alloy Obtained by Layered Selective Sintering of a Powder

This paper is focused on a clarification and analysis of the regularities of formation of the structure and properties of samples of the titanium-based alloy VT6, obtained by methods of conventional metallurgy and formed by layered selective electron-beam sintering in vacuum (using the Arcam A2X (3D printer) system (Arcam, Sweden)) of VT6 titanium powder with particle size 40–100 μm. Additional modification of the samples was realized by irradiating the surface with an intense pulsed electron beam (15 keV, 45 J/cm{sup 2}, 200 μs, 10 pulses, 0.3 s{sup –1}, 3.5·10{sup –2} Pa). It is shown that the action of a pulsed electron beam on the surface of samples formed by layered selective electron-beam sintering leads to a significant reduction in the porosity of the surface layer of the material and formation in the surface layer of a polycrystalline structure (grain size 15–60 μm) with a substructure in the form of crystallization cells (cell size 0.5–1.2 μm). Electron-beam processing of samples prepared by methods of conventional metallurgy for the indicated electron-beam parameters leads to the formation in the surface layer of a polycrystalline structure (grain size 50–800 μm) with a laminar intragrain substructure. Mechanical tests, performed by stretching flat samples, showed that the highest combination of mechanical strength and plasticity is possessed by samples obtained by layered selective electron-beam sintering with subsequent irradiation by an intense pulsed electron beam.

36 MATERIALS SCIENCE↗

Tensile Properties and Fracture Characteristics of Nanostructured Copper and Cu-SiC Nanocomposite Produced by Mechanical Milling and Spark Plasma Sintering Process

The presence of large grains within nanometric and ultrafine grain matrix is an effective method in order to enhance strength while keeping the high ductility of metals. For this purpose, in this research, spark plasma sintering (SPS) was used to consolidate milled Cu and Cu-SiC powders. In SPS process, local sparks with high temperature between particles take place and locally lead to intense grain growth, and therefore, this method has the ability to produce bimodal grain structures in copper and copper-based composites. Microstructural and mechanical studies showed ≈ 185 and ≈ 437 nm matrix grain sizes, high tensile yield strength values of ≈ 188.4 and ≈ 296.9 MPa, and fracture strain values of 15.1 and 6.7% for sintered Cu and Cu-4 vol.% SiC nanocomposite materials, respectively. The presence of nanoparticles promoted the occurrence of static recrystallization and decreased the fraction of coarse grains in microstructure. The high tensile properties of the produced materials are attributed to fine grain size, homogenous dispersion of nanoparticles and retarded grain boundary migration during sintering.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Thermophysical Properties of High-Frequency Induction Heat Sintered Graphene Nanoplatelets/Alumina Ceramic Functional Nanocomposites

This paper concerns the thermophysical properties of high-frequency induction heat (HFIH) sintered alumina ceramic nanocomposites containing various graphene nanoplatelets (GNP) concentrations. The GNP/alumina nanocomposites demonstrated high densities, fine-grained microstructures, highest fracture toughness and hardness values of 5.7 MPa m{sup 1/2} and 18.4 GPa, which found 72 and 8%, superior to the benchmarked monolithic alumina, respectively. We determine the role of GNP in tuning the microstructure and inducing toughening mechanisms in the nanocomposites. The sintered monolithic alumina exhibited thermal conductivity value of 24.8 W/mK; however, steady drops of 2, 15 and 19% were recorded after adding respective GNP contents of 0.25, 0.5 and 1.0 wt.% in the nanocomposites. In addition, a dwindling trend in thermal conductions with increasing temperatures was recorded for all sintered samples. Simulation of experimental results with proven theoretical thermal models showed the dominant role of GNP dispersions, microstructural porosity, elastic modulus and grain size in controlling the thermal transport properties of the GNP/alumina nanocomposites. Thermogravimetric analysis showed that the nanocomposite with up to 0.5 mass% of GNP is thermally stable at the temperatures greater than 875 °C. The GNP/alumina nanocomposites owning a distinctive combination of mechanical and thermal properties are promising contenders for the specific components of the aerospace engine and electronic devices having contact with elevated temperatures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Tailoring Microstructure and Properties of a Superelastic Ti–Ta Alloy by Incorporating Spark Plasma Sintering with Thermomechanical Processing

A powder metallurgy Ti–35 at.% Ta alloy was produced using a spark plasma sintering process. The sintered alloy exhibited Ta-rich regions at a sintering temperature of 1100 °C. Complete diffusion of elemental powders was achieved via homogenization heat treatment at 1500 °C for 12 h, but the ductility declined drastically. The brittle behavior of the homogenized sample was due to the high-oxygen content, continuous grain boundary α-phase and high-angle grain boundaries. Excellent mechanical properties were achieved when hot forging was used along with preheating the homogenized specimen at 1100 °C. The mechanisms underlying this phenomenon were suppression of the solid grain boundary α-phase, high fraction of low-angle grain boundaries and dynamic recrystallization. Tensile strength improved to the maximum value of 868 MPa. The strain recovery ratio increased to 90% in the first cycle during a cyclic loading–unloading test. Incomplete strain recovery of the first cycle was due to the presence of the martensite phase (α″).

36 MATERIALS SCIENCE↗

Microstructure and Mechanical Properties of B{sub 4}C-Blended M3:2 High-Speed Steel Powders Consolidated by Sintering and Heat Treatment

Water-atomized powders of M3:2 high-speed steel (HSS) were blended with B{sub 4}C and consolidated by cold press sintering. With the addition of B{sub 4}C (~ 0.2 vol.%), satisfactory mechanical properties were achieved for HSS by sintering at a temperature as low as 1190 °C [e.g., 53.2 ± 0.2 in the Rockwell hardness (HRC) and 3074 ± 56 MPa in bending strength]. High relative density (98.5%) and good strength were attributed to the mechanism described as follows: First, the atoms of boron and carbon escaped after the reaction between B{sub 4}C and iron matrix. Then, the sintered HSS was strengthened by boron atoms while they were distributed in M{sub 6}C or MC carbides and iron matrix. Second, a plenty of M{sub 6}C carbides were formed due to the release of carbon atoms. As a result, the value of solidus temperature was reduced. In addition, mechanical properties were greatly improved by heat treatment (quenching and tempering) (e.g., 61.2 ± 0.3 in HRC, 4356 ± 64 MPa in bending strength, and 42.3 ± 0.5 MPa m{sup 1/2} in fracture toughness, respectively).

36 MATERIALS SCIENCE↗

In situ probing of interfacial roughness and transient phases during ceramic cold sintering process

The ceramic cold sintering process (CSP) offers an eco-friendly approach to producing fully dense ceramics at low temperatures. However, an incomplete mechanistic understanding hinders its optimization and widespread adoption. In this study, we analyze the microstructural and structural changes in ZnO, a model CSP system, using in situ synchrotron-based high-energy small-angle X-ray scattering and X-ray diffraction techniques. Our results reveal the time evolution of ZnO particles' surface area and roughness, reflecting the dissolution and re precipitation processes that enable densification. The in situ measurements supply valuable kinetic data for these stages of CSP. Alongside microstructural changes and densification, we observed the evolution of secondary phases representing reaction products between ZnO and acetic acid, the solvent used. The initial ZnO/solvent mixture's dominant secondary phase is attributed to zinc acetate, which is gradually replaced by a zinc soap-type structure during CSP. This structure has a large (≈ 21 Å) lattice parameter and is assumed to have a layered nature. The formation of this soap phase, which is retained in the sintered product as an intergranular component, appears to be a signature of successful cold sintering as it facilitates mass transport, leading to densification. Here, our study underscores the potential of in situ synchrotron characterization for revealing microstructural and phase-evolution details during CSP. These findings, which would be challenging to obtain through ex situ measurements, provide crucial data to guide and validate theoretical models, ultimately enhancing CSP's effectiveness and adoption.

36 MATERIALS SCIENCE↗

Electrochemical grand potential-based phase-field simulation of electric field-assisted sintering

Here, an electrochemical grand potential functional was proposed to describe the sintering of an ionic ceramic green body. The resultant phase-field description enables simulation of the consolidation of an arbitrary number of granular particles and their interactions with the surrounding void phase. The model includes the effects of charged vacancies and the associated interactions between internal and applied electric fields. Defect segregation to grain boundaries is also accounted for, as well as enhanced interfacial defect mobilities. The model was parameterized for Y 2 O 3 . Simulations of two-particle systems showed that the applied electric field had an increasingly important impact on neck growth as particle size increased. A sudden rapid increase in temperature occurred for larger field strengths, which has been reported to be correlated to the onset of a flash event in flash sintering. Simulations of many particles showed that internal heat generation by Joule heating was localized at particle–particle contacts (grain boundaries), even though their conductivities were lower than nearby internal particle-void interfaces. A percolative path for ionic charge across the green body and the ceramic sintered solid was thus defined, accelerating the Joule heating process as the porosity of the green body is removed.

36 MATERIALS SCIENCE↗

Densification of W–Ni–Fe powders using laser sintering

In this paper, Laser Sintering (LS) of 90%W–7%Ni–3%Fe (wt.%) powders have been investigated, with the goal to understand the influence of final density by laser power, scanning speed, laser trace width, and the number of scanning passes. The results suggest that the laser power and scanning speed are the most important factors influencing density; the influence of trace width and number of scanning passes are not significant. With the increase of laser power and decrease of scanning speed, higher density can be achieved. Additionally, the microstructure analysis indicated that the porosity changed from open porosity to closed porosity with higher laser energy input. Energy-Dispersive X-ray Spectroscopy (EDX) analysis shows that during the sintering process, W was not melted but dissolved into the Ni–Fe matrix. Contact flattening and grain accommodation of W grains have been observed. It suggests that both rearrangement and solution-reprecipitation mechanisms are responsible for the densification. The sintered density with respect to laser power and scanning speed was modeled by continuum modeling theory and compared with experimental results.

42 ENGINEERING↗

Mechanically strengthened heterogeneous Sm-Co sintered magnets

Samarium-cobalt sintered magnets offer excellent magnetic properties, thermal stability, and corrosion resistance. They are used in a variety of defense and civilian applications, especially when elevated operation temperatures (e.g., 200 ºC to 550 ºC) are required. However, the utilization of these materials is restricted by their brittleness. Improving their mechanical resilience would make them more cost-effective, efficient, and robust in decarbonization and other function-related applications while reducing the pressure on critical material supply chains. In this paper, we engineer a series of novel heterogeneous microstructures, such as laminated coarse grain (CG)/fine grain (FG) and core/shell CG/FG microstructures, to produce unprecedented combinations of superior mechanical and magnetic properties without altering the chemical compositions of the magnets or common heat treatment procedures. Further, a 60% flexural strength enhancement is obtained using heterogeneous Sm 2 (CoFeCuZr) 17 sintered magnets with little impact on their magnetic properties. The mechanically robust heterogeneous Sm-Co sintered magnets have a minor (e.g., less than 4.6%) reduction in the energy product (BH) max due to a slightly reduced squareness of the demagnetization curve, with no decrease in either the remanence (B r ) or the intrinsic coercivity (H ci ). The flexural strengths of these heterogeneous Sm-Co magnets depend on the volume ratios and mean grain sizes of the FG/CG regions, as well as their microstructural architectures. The fine-grained regions act as mechanical strengthening sites, which can be strategically used when designing the magnet for different applications. This technology is highly compatible with existing magnet manufacturing processes and thus can be adopted readily by the magnet industry.

36 MATERIALS SCIENCE↗

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↗

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↗

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↗