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At least 505 records · Page 28

Three-dimensional analysis by serial sectioning of cubic zirconia sinters

Three-dimensional electron backscatter diffraction technique was used for the characterization of grain boundary geometry and pore morphology in cubic zirconia. A set of three samples composed of cubic yttria stabilized zirconia, sintered under different conditions was investigated. Analysis of grain boundaries and pore structure was carried out in a dual-beam scanning electron microscope. For each sample, a volume of 15·10{sup 3} μm{sup 3} was investigated. The results of three-dimensional microstructure analysis were compared to the results derived from regular, two-dimensional maps of the area of 2500 µm{sup 2}. Based on two-dimensional and three-dimensional data the average grain diameter, number of grains, average number of neighbors and porosity were calculated. The average grain diameter varied in the range from 2.39 µm to 2.91 µm and from 3.00 µm to 3.79 µm, while the level of porosity varied in the range from 1.22% to 1.77% and from 1.30% to 5.61% for two-dimensional and three-dimensional data, respectively. The analysis of grain boundary networks revealed a strong dependence between grain boundary density and sample preparation parameters. The parameters of the sintering process affected also the size and distribution of pores. The comparison of the results of 2D and 3D materials characterization revealed significant differences in the values of calculated microstructure parameters.

36 MATERIALS SCIENCE↗

Modeling of flash sintering of ionic ceramics

A fundamental understanding of the influence of defects in ionic ceramics at the atomic, microstructural, and macroscopic levels, before, during, and after the flash sintering event is key to the development of ceramic processing operations that lead to fast, low cost, and environmentally safe fabrication of materials. The observed phenomenology of the flash process encompasses multiple time and length scales and have resulted on a wide variety of what sometimes appears to be contradictory explanations. Here, this article summarizes the latest developments on the modeling and simulation of flash sintering, specifically those related to the understanding of the equilibrium and kinetic properties and the corresponding microstructural evolution of ionic ceramics. Challenges and opportunities in the development of theoretical analyses that include unidentified multiphysical effects are discussed, as they pertain to the processing of technologically relevant ceramic materials for advanced structures and devices.

36 MATERIALS SCIENCE↗

Pressureless Sintering of Pre-Alloyed Nanostructured Bainitic Steel Powders

A recent study shows that powder metallurgy and pressureless sintering are a viable pathway to realize full-density bulk components of nanostructure bainitic steels. A scalable, pressureless supersolidus liquid phase sintering (SLPS) approach to process nanostructured bainitic steel is evaluated. Furthermore, to address the oxidation issues associated with the mechanical alloying of elemental powders, powder atomization is used to produce pre-alloyed nanostructured bainitic steel powders.

mechanical alloying↗

Coupling of Spark Plasma Sintering with Advanced Modeling to Enable Process Scale-Up: LDRD Final Project Poster

Electric-field assisted sintering (EFAS) manufacturing techniques reduce energy usage requirements, fabricate near-net-shape parts, and produce bulk nanostructured materials through rapid heating and cooling rates achievable through Joule heating. Process parameters of pulsed DC voltage and constant pressure are applied through stainless steel rams and graphite tooling to the ceramic yttrium oxide powder to be sintered. Our high-fidelity modeling code application advances manufacturing for extreme environments by enabling process-informed design and improving microstructure consistency through multiphysics multiscale process-structure-property-performance correlation simulations.

36 MATERIALS SCIENCE↗

Time-Resolved Evolution of the 3D Nanoporous Structure of Sintered Ag by X-Ray Nanotomography: Role of the Interface with a Copper Substrate

Here, the evolution of the nanoporous structure of cylindrical sintered silver samples during high temperature aging, ranging from 200 to 350 °C for 350 min, is studied through in situ computed X-ray tomography. Investigations are carried out for two types of specimens: pure sintered silver and specimens containing a silver-copper interface. It is shown that the overall pore evolution is driven by the evolution of very few large ones. The smaller pores, although being more numerous, do not really evolve before being absorbed by the few bigger ones. In pure silver, pore evolution is driven by diffusion (Ostwald ripening) but the presence of an interface promotes faster growth kinetics until the aging time reaches a threshold value, after which a deviation from Ostwald ripening occurs. The transition is a function of the aging temperature. This behavior is associated with the competition between elastic relaxation and surface energy minimization.

42 ENGINEERING↗

On the Origin of Sinter‐Resistance and Catalyst Accessibility in Raspberry‐Colloid‐Templated Catalyst Design

Abstract Nanoparticle (NP) sintering is a major cause of the deactivation of supported catalysts. Raspberry‐colloid‐templated (RCT) catalysts are an emerging class of materials that show an unprecedented level of sinter‐resistance and exhibit high catalytic activity. Here a comprehensive study of the origin of NP stability and accessibility in RCT catalysts using theoretical modeling, 3D electron microscopy, and epitaxial overgrowth is reported. The approach is showcased for silica‐based RCT catalysts containing dilute Pd‐in‐Au NPs previously used in hydrogenation and oxidation catalysis. Modeling of the contact line of the silica precursor infiltrating into the assembled raspberry colloids suggests that a large part of the particles must be embedded into silica, which is confirmed by quantitative visualization of >200 individual NPs by dual‐axis electron tomography. The RCT catalysts have a unique structure in which all NPs reside at the pore wall but have >50% of their surface embedded in the matrix, giving rise to the strongly enhanced thermal and mechanical stability. Importantly, epitaxial overgrowth of Ag on the supported NPs reveals that not only the NP surface exposed to the pore but the embedded interface as well remained chemically accessible. This mechanistic understanding provides valuable guidance in the design of stable catalytic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Spark plasma sintering preparation of reference targets for field spectroscopy on Mars

We propose spark plasma sintering (SPS) as a technique to prepare reference targets for Raman and other spectroscopy instruments involved in future space missions and more generally in–field work. We have tested the effect of SPS on different international standards that are available in the form of minerals and rocks powders. Advantages and potential issues of SPS were considered by analyzing the Raman signal and mechanical properties of the sintered targets. The shape is well controlled; the rupture toughness is enhanced, and the homogeneous distribution of the mineral phases is verified. In conclusion, a suite of calibration targets has thus been implemented for the SuperCam instrument on the National Aeronautics and Space Administration Mars 2020 rover, and SPS may be preferred for future missions as well.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Fusibility and sintering characteristics of ash

The temperature characteristics of ash fusibility are studied for a wide range of bituminous and brown coals, lignites, and shales with ratios R{sub B/A} of their alkaline and acid components between 0.03 and 4. Acritical value of R{sub B/A} is found at which the fusion temperatures are minimal. The sintering properties of the ashes are determined by measuring the force required to fracture a cylindrical sample. It is found that the strength of the samples increases sharply at certain temperatures. The alkali metal content of the ashes has a strong effect on their sintering characteristics.

01 COAL, LIGNITE, AND PEAT↗

Study on Microwave Performance of Low-Temperature Sintered, Ba(CoTi){sub 1.5}Fe{sub 9}O{sub 19} Ferrite for Application at UHF Frequency

M-type barium ferrite, Ba(CoTi){sub 1.5}Fe{sub 9}O{sub 19}, was synthesized via the solid-state reaction method. BBSZ, i.e., B{sub 2}O{sub 3} −Bi{sub 2}O{sub 3} −SiO{sub 2} −ZnO, was added to adjust the sintering temperature to values lower than that of silver (i.e., ∼961 °C). The phase formation characteristics, microstructure, magnetic, and microwave properties were characterized by x-ray diffraction, scanning electron microscope, vibrating sample magnetometer, and impedance analyzer, respectively. The results show that densification of samples were enhanced by increasing the amount of BBSZ with corresponding gains realized in magnetic properties. Such enhanced properties in Ba(CoTi){sub 1.5}Fe{sub 9}O{sub 19} are attributed to the low-melting point experienced as the result of BBSZ glass additives which gave rise to the stabilization of a liquid phase during sintering.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of the Fe/Ba Ratio and Sintering Temperature on Microstructure and Magnetic Properties of Barium Ferrites Prepared by Hydrothermal Method

Magnetoplumbite-type (M-type) hexagonal barium ferrite particles were synthesized by a hydrothermal method. The structure and magnetic properties of barium ferrites were investigated systematically, which indicated that the ratio of Fe/Ba (R{sub F/B}) and sintering temperature have an important effect on structure and performance. Phase composition, micro-morphology, and magnetic properties of the particles were investigated by X-ray powder diffraction (XRD) analysis, scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). When the ratio of Fe/Ba (R{sub F/B}) is even low or high, inferior images of XRD could be attained with certain impurities. When R{sub F/B} = 8, the single phase could be obtained without impurities. Micro-morphology of the particles exhibits the uniform plane hexagonal structures of nano-sized M-type ferrites when sintered at 800 °C. Saturation magnetization (M{sub s}) reaches the maximum value at R{sub F/B} = 7 (M{sub s} = 45.07 emu/g). The value of coercivity (H{sub c}) increases with the growth of R{sub F/B}, and H{sub c} is up to 6207 Oe when R{sub F/B} = 7. The effect of R{sub F/B} and temperature on magnetization (M{sub s}) and coercivity (H{sub c}) was studied in this paper.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Comparison of residual stresses in Inconel 718 simple parts made by electron beam melting and direct laser metal sintering

Residual stress profiles were mapped using neutron diffraction in two simple prism builds of Inconel 718: one fabricated with electron beam melting and the other with direct laser sintering. Spatially indexed stress-free cubes were obtained by EDM sectioning equivalent prisms of similar shape. The (311) interplanar spacing examined for the EDM sectioned sample was compared to the interplanar spacings calculated to fulfill force and moment balance. We have shown that Applying force and moment balance is a necessary supplement to the measurements for the stress-free cubes with respect to accurate stress calculations in additively manufactured components. Furthermore, our work has shown that residual stresses in electron beam melting parts are much smaller than that of direct laser metal sintering parts.

36 MATERIALS SCIENCE↗

Processing and Characterization of Fe-Mn-Cu-Sn-C Alloys Prepared by Ball Milling and Spark Plasma Sintering

In this work, Fe-Mn-Cu-Sn-C alloys were prepared by means of powder metallurgy (PM). Powder mixtures were ball-milled for 8, 30 and 120 h and densified to < 1% porosity using spark plasma sintering (SPS) at 900 °C and 35 MPa. After consolidation, all samples of the Fe alloys were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), hardness and flexural strength tests. Resistance to abrasive wear was evaluated in both three-body abrasion and two-body abrasion tests. The SEM observations revealed an evident dependence of grain size and microstructural homogeneity on milling time. The XRD analysis showed a marked increase in austenite content in the as-sintered specimens with milling time. Although the proportion of deformation-induced martensite was small, the strengthening effect of abrasion on the subsurface layer of the investigated alloys was clearly indicated by Knoop hardness measurements.

36 MATERIALS SCIENCE↗

Study on Microstructures and Mechanical Properties of Foam Titanium Carbide Ceramics Fabricated by Reaction Sintering Process

Foam titanium carbide (TiC) ceramics with a three-dimensional network structure were fabricated by the reaction sintering process, in which polyurethane foam was taken as the template, and TiO{sub 2} and phenolic resin were used as the reactants. Phase, microstructures and fracture morphologies of foam TiC ceramics were characterized by x-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results show that when the mass ratios of phenolic resin and TiO{sub 2} (F/T) are (0.8-1.2): 1, foam TiC ceramics with pure TiC phase can be formed. As the F/T ratios increase, crystal lattice parameters of fabricated foam TiC ceramics become bigger. When the value of F/T decreases from 1.2 to 0.8, grain size of TiC grows larger and microstructures get denser; meanwhile, the compressive strength increases from 0.10 to 1.05 MPa. Additionally, either raising the sintering temperatures or extending holding time can facilitate the completion of the reaction process and increase the compressive strength.

36 MATERIALS SCIENCE↗

Phase Evolution and Mechanical Properties of AlCoCrFeNiSi{sub x} High-Entropy Alloys Synthesized by Mechanical Alloying and Spark Plasma Sintering

In the current investigation, AlCoCrFeNiSi{sub x} (x = 0, 0.3, 0.6 and 0.9 in atomic ratio) high-entropy alloy systems are prepared by mechanical alloying and subsequently consolidated by spark plasma sintering. The microstructural and mechanical properties were analyzed to understand the effect of Si addition in AlCoCrFeNi alloy. The x-ray diffraction analysis reveals the supersaturated solid solution of the body-centered cubic structure after 20 h of ball milling. However, the consolidation promotes the transformation of body-centered phases partially into the face-centered cubic structure and sigma phases. A recently proposed geometric model based on the atomic stress theory has been extended for the first time to classify single phase and multi-phases on the high-entropy alloys prepared by mechanical alloying and spark plasma sintering process. Improved microhardness and better wear resistance were achieved as the Si content increased from 0 to 0.9 in the present high-entropy alloy.

36 MATERIALS SCIENCE↗

Sliding Wear of Spark Plasma Sintered CrFeCoNiCu High-Entropy Alloy Coatings: Effect of Aluminum Addition

High-entropy alloys (HEAs) are considered as attractive coating materials due to their high hardness, good wear and corrosion resistance. Al{sub x}CrFeCoNiCu (x = 0, 1, 2, 3) high-entropy alloy coatings were fabricated on carbon steel substrate using spark plasma sintering. The microstructure evolved from FCC to FCC–BCC mixed structure. Al{sub 3}CrFeCoNiCu coating possesses an average hardness of approximately 682 HV{sub 0.2}, which is the highest hardness in all of the HEA coatings. The dry sliding wear behavior of the HEA coatings was investigated using a ball-on-disk sliding tribo-meter with a silicon nitride ball. In all of the HEA coatings, Al{sub 3}CrFeCoNiCu presents the lowest wear rate 8.81 × 10{sup −5} mm{sup 3} m{sup −1} and Al{sub 2}CrFeCoNiCu has the lowest coefficient of friction 0.195 during 1000 m sliding distance at 0.1 m s{sup −1} sliding velocity under 20 N normal load. Comparing with AISI 52100 steel, spark plasma sintered Al{sub 2}CrFeCoNiCu and Al{sub 3}CrFeCoNiCu HEA coatings exhibit outstanding sliding wear resistance and extremely low friction coefficient. The wear resistance of Al{sub 3}CrFeCoNiCu HEA coating is approximately four times better than the bearing steel, showing a promising application as a wear-resistant material.

36 MATERIALS SCIENCE↗

Effect of Strain Rate on the Plastic Deformation and Fracture of 90W-7Ni-3Fe Alloy Prepared by Liquid-Phase Sintering

In this study, the effect of the strain rates on the plastic deformation behavior and fracture mechanism of 90W-7Ni-3Fe heavy alloy prepared by liquid-phase sintering was investigated. Stress–strain tests were carried out in tensile and compression under quasi-static condition with the strain rate ranging from 10{sup −3} to 1 s{sup −1}. Dynamic test was examined using a compression split Hopkinson bar at strain rates ranging from 1000 to 1700 s{sup −1} in order to evaluate the effects of high strain rate on dynamic plastic deformation behavior. Quasi-static tests results show that the strength and hardness of this alloy increase with increasing strain rate. Results indicate that the as-sintered 90W-7Ni-3Fe heavy alloy has obvious strain-hardening characteristic under tensile or compression deformation under quasi-static condition. At this time, strain hardening is the main factor. Nevertheless, strain-hardening and strain-softening behaviors of the specimens occur simultaneously under dynamic compression condition. The effect of compressive stress on the work hardening is more obvious. A strong relevance of work-hardening effect on strain rate is also found. And the fracture mode of quasi-static and dynamic compression samples is also different.

36 MATERIALS SCIENCE↗

Large-scale production of (GeTe) x (AgSbTe 2 ) 100$-$x (x=75, 80, 85, 90) with enhanced thermoelectric properties via gas-atomization and spark plasma sintering

(GeTe) x (AgSbTe 2 ) 100$-$x : TAGS thermoelectrics are an attractive class of materials due to their combination of non-toxicity and good conversion efficiency at mid-temperature ranges. Here in the present work, we have utilized energy and time efficient high-pressure gas atomization and spark-plasma sintering techniques for large-scale preparation of samples with varying composition (i.e., (GeTe) x (AgSbTe 2 ) 100$-$x where x = 75, 80, 85, and 90). High-temperature x-ray diffraction was used to understand the phase transformation mechanism of the as-atomized powders. Detailed high-resolution transmission electron microscopy of the sintered samples revealed the presence of nanoscale precipitates, antiphase, and twin boundaries. The nanoscale twins and antiphase boundaries serve as phonon scattering centers, leading to the reduction of total thermal conductivity in TAGS-80 and 90 samples. The maximum ZT obtained was 1.56 at 623 K for TAGS-90, which was ~94% improvement compared to values previously reported. The presence of the twin boundaries also resulted in a high fracture toughness (K IC ) of the TAGS-90 sample due to inhibition of dislocation movement at the twin boundary.

36 MATERIALS SCIENCE↗

Sintering inhibition enables hierarchical porosity with extreme resistance to degradation during redox cycling of Fe-Mo foams

High-temperature (800 ºC) steam-hydrogen redox cycling, relevant to grid-scale energy storage, is studied for iron-based freeze-cast lamellar foams. In contrast to previously studied Fe, Fe-Ni, and Fe-Co foams that rapidly degrade, Fe-25Mo foams feature a much-enhanced structural damage resistance. Utilizing in-situ x-ray diffraction, microscopy, and x-ray tomography, strong sintering inhibition is observed in Fe-Mo foams, creating a hierarchically porous lamellar structure. This leads to (i) wide channels between lamellae, enabling high macroscopic porosity (~78%) which can accommodate gas flow as well as volumetric expansion without lamellar contact, and (ii) microporosity within lamellae, providing additional free volume to accommodate expansion during oxidation, limiting both swelling of the lamellae and the formation of Kirkendall pores. Finally, these combined effects enable a near-complete reversibility of the microstructure during cycling, preventing damage produced via internal lamellar buckling, cracking, contacting and sintering, with a remarkably high porosity (65%) remaining after 50 consecutive redox cycles.

36 MATERIALS SCIENCE↗