YSZ (Y₂O₃-stabilized zirconia)-based ceramics have excellent mechanical properties, such as high strength and wear resistance. In the application, YSZ is utilized in the bead mill, a fine-grinding process. YSZ-based parts, such as the rotor and pin, can be easily damaged by continuous application with high rpm in the bead mill process. In that case, adding WC particles improves the tribological and mechanical properties. YSZ-30 vol.% WC composite ceramics are manufactured via hot pressing under different pressures (10/30/60 MPa). The hot-pressed composite ceramics measure the physical properties, such as porosity and bulk density values. In addition, the phase formation of these composite ceramics is analyzed and discussed with those of physical properties. For the increased applied pressure of hot pressing, the tetragonality of YSZ and the crystallinity of WC are enhanced. The mechanical properties indicate an improved tendency with the increase in the applied pressure of hot pressing.

The 3D printing process provides a higher degree of freedom when designing ceramic parts than the conventional press forming process. However, the generation and growth of the microcracks induced during heat treatment is thought to be due to the occurrence of local tensile stress caused by the thermal decomposition of the binder inside the green body. In this study, an alumina columnar specimen, which is a representative ceramic material, is fabricated using the digital light process (DLP) 3D printing method. DTG analysis is performed to investigate the cause of the occurrence of microcracks by analyzing the debinding process in which microcracks are mainly generated. HDDA of epoxy acrylates, which is the main binder, rapidly debinded in the range of 200 to 500°C, and microcracks are observed because of real-time microscopic image observation. For mitigating the rapid debinding process of HDDA, other types of acrylates PETA, PUA, and MMA are added, and the effect of these additives on the debinding rate is investigated. By analyzing the DTG in the 25 to 300°C region, it is confirmed that the PETA monomer and the PUA monomer can suppress the rapid decomposition rate of HDDA in this temperature range.

In this study, acoustic and viscosity data are collected in real time during the ball milling process and analyzed for correlation. After fast Fourier transformation (FFT) of the acoustic data, changes in the signals are observed as a function of the milling time. To analyze this quantitatively, the frequency band is divided into 1 kHz ranges to obtain an integral value. The integrated values in the 2–3 kHz range of the frequency band decrease linearly, confirming that they have a high correlation with changes in viscosity. The experiment is repeated four times to ensure the reproducibility of the data. The results of this study show that it is possible to estimate changes in slurry properties, such as viscosity and particle size, during the ball milling process using an acoustic signal.

W₂C is synthesized through a reaction-sintering process from an ultrafine-W and WC powder mixture using spark plasma sintering (SPS). The effect of various parameters, such as W:WC molar ratio, sintering temperature, and sintering time, on the synthesis behavior of W₂C is investigated through X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) analysis of the microstructure, and final sintered density. Further, the etching properties of a W₂C specimen are analyzed. A W₂C sintered specimen with a particle size of 2.0 μm and a relative density over 98% could be obtained from a W-WC powder mixture with 55 mol%, after SPS at 1700°C for 20 min under a pressure of 50 MPa. The sample etching rate is similar to that of SiC. Based on X-ray photoelectron spectroscopy (XPS) analysis, it is confirmed that fluorocarbon-based layers such as C-F and C-F2 with lower etch rates are also formed.

In the development of advanced ceramic tools, material improvements and design freedom are critical in improving tool performance. However, in the die press molding method, many factors limit tool design and make it difficult to develop innovative advanced tools. Ceramic 3D printing facilitates the production of prototype samples for advanced tool development and the creation of complex tooling products. Furthermore, it is possible to respond to mass production requirements by reflecting the needs of the tool industry, which can be characterized by small quantities of various products. However, many problems remain in ensuring the reliability of ceramic tools for industrial use. In this study, alumina inserts, a representative ceramic tool, was manufactured using the digital light process (DLP), a 3D printing method. Alumina inserts prepared by 3D printing are pressurelessly sintered under the same conditions as coupon-type specimens prepared by press molding. After sintering, a hot isostatic pressing (HIP) treatment is performed to investigate the effects of relative density and microstructure changes on hardness and fracture toughness. Alumina inserts prepared by 3D printing show lower relative densities than coupon specimens prepared by powder molding but indicate similar hardness and higher fracture toughness values.

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• Vat photopolymerization-based 3D printing of complex-shaped and high-performance Al2O3 ceramic tool with chip-breaking grooves: Cutting performance and wear mechanism
  Haidong Wu, Wei Liu, Yuerui Xu, Lifu Lin, Yehua Li, Shanghua Wu
  Journal of Asian Ceramic Societies.2023; 11(1): 159.     CrossRef

This study demonstrates the effect of addition of Fe particles of different sizes on the critical properties of the superconductor MgB₂. Bulk MgB₂ is synthesized by ball milling Mg and B powders with Fe particles at 900°C. When Fe particles with size less than 10 μm are added in MgB₂, they easily react with B and form the FeB phase, resulting in a reduction in the amount of the MgB₂ phase and deterioration of the crystallinity. Accordingly, both the critical temperature and the critical current density are significantly reduced. On the other hand, when larger Fe particles are added, the Fe₂B phase forms instead of FeB due to the lower reactivity of Fe toward B. Accordingly, negligible loss of B occurs, and the critical properties are found to be similar to those of the intact MgB₂.

In this study, a process is developed for 3D printing with alumina (Al₂O₃). First, a photocurable slurry made from nanoparticle Al₂O₃ powder is mixed with hexanediol diacrylate binder and phenylbis(2,4,6-trimethylbenzoyl) phosphine oxide photoinitiator. The optimum solid content of Al₂O₃ is determined by measuring the rheological properties of the slurry. Then, green bodies of Al₂O₃ with different photoinitiator contents and UV exposure times are fabricated with a digital light processing (DLP) 3D printer. The dimensional accuracy of the printed Al₂O₃ green bodies and the number of defects are evaluated by carefully measuring the samples and imaging them with a scanning electron microscope. The optimum photoinitiator content and exposure time are 0.5 wt% and 0.8 s, respectively. These results show that Al₂O₃ products of various sizes and shapes can be fabricated by DLP 3D printing.

In this study, the effect of the content of MgO-CaO-Al₂O₃-SiO₂ (MCAS) glass additives on the properties of AlN ceramics is investigated. Dilatometric analysis and isothermal sintering for AlN compacts with MCAS contents varying between 5 and 20 wt% are carried out at temperatures ranging up to 1600°C. The results showed that the shrinkage of the AlN specimens increases with increasing MCAS content, and that full densification can be obtained irrespective of the MCAS content. Moreover, properties of the AlN-MCAS specimens such as microhardness, thermal conductivity, dielectric constant, and dielectric loss are analyzed. Microhardness and thermal conductivity decrease with increasing MCAS content. An acceptable candidate for AlN application is obtained: an AlN-MCAS composite with a thermal conductivity over 70 W/m·K and a dielectric loss tangent (tan δ) below 0.6 × 10⁻³, with up to 10 wt% MCAS content.

In this study, MgO–CaO–Al₂O₃–SiO₂ (MCAS) nanocomposite glass powder having a mean particle size of 50 nm and a specific surface area of 40 m²/g is used as a sintering additive for AlN ceramics. Densification behaviors and thermal properties of AlN with 5 wt% MCAS nano-glass additive are investigated. Dilatometric analysis and isothermal sintering of AlN-5wt% MCAS compact demonstrates that the shrinkage of the AlN specimen increases significantly above 1,300°C via liquid phase sintering of MCAS additive, and complete densification could be achieved after sintering at 1,600°C, which is a reduction in sintering temperature by 200°C compared to conventional AlN-Y₂O₃ systems. The MCAS glass phase is satisfactorily distributed between AlN particles after sintering at 1,600°C, existing as an amorphous secondary phase. The AlN specimen attained a thermal conductivity of 82.6 W/m·K at 1,600°C.

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• Effect of MgO-CaO-Al₂O₃-SiO₂ Glass Additive Content on Properties of Aluminum Nitride Ceramics
  Kyung Min Kim, Su-Hyun Baik, Sung-Soo Ryu
  Journal of Korean Powder Metallurgy Institute.2018; 25(6): 494.     CrossRef

In this study, the compound Li₃BO₃ (LBO) is intended to be prepared by a polymeric complex method as a sintering aid for the densification of Li₇La₃Zr₂O₁₂ (LLZ) solid electrolyte. A polymeric precursor containing Li and B is heat-treated in an air atmosphere at a temperature range between 600°C and 800°C. Instead of LBO, the compound Li_2+xC_1-xB_xO₃ (LCBO) is unexpectedly synthesized after a heat-treatment of 700°C. The effect of LCBO addition on sintering behavior and ion conductivity of LLZ is studied. It is found that the LCBO compound could lead to significant improvements in the densification and ionic conductivity of LLZ compared to pure LLZ. After sintering at 1100°C, the density of the LLZ-12wt%LBO composite is 3.72 g/cm³, with a high Li-ion conductivity of 1.18 × 10⁻⁴ Scm^-1 at 28°C, while the pure LLZ specimen had a densify of 2.98 g/cm³ and Li-ion conductivity of 5.98 × 10⁻⁶ Scm^-1.

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• Characterization of Li1.5Al0.5Ge1.5(PO4)3 Solid Electrolyte with an Added Sintering Aid
  Hyun-Joon Lee, Liyu-Liu, Won-Jong Jeong, Seoung-Ki Lee, Bong-Ki Ryu
  Electronic Materials Letters.2023; 19(1): 55.     CrossRef

Aluminum nitride (AlN) powder specimens are treated by high-energy bead milling and then sintered at various temperatures. Depending on the solvent and milling time, the oxygen content in the AlN powder varies significantly. When isopropyl alcohol is used, the oxygen content increases with the milling time. In contrast, hexane is very effective at suppressing the oxygen content increase in the AlN powder, although severe particle sedimentation after the milling process is observed in the AlN slurry. With an increase in the milling time, the primary particle size remains nearly constant, but the particle agglomeration is reduced. After spark plasma sintering at 1400°C, the second crystalline phase changes to compounds containing more Al₂O₃ when the AlN raw material with an increased milling time is used. When the sintering temperature is decreased from 1750°C to 1400°C, the DC resistivity increases by approximately two orders of magnitude, which implies that controlling the sintering temperature is a very effective way to improve the DC resistivity of AlN ceramics.

A Nanosized WO₃ and CuO powder mixture is prepared using novel high-energy ball milling in a bead mill to obtain a W-Cu nanocomposite powder, and the effect of milling time on the structural characteristics of WO₃-CuO powder mixtures is investigated. The results show that the ball-milled WO₃-CuO powder mixture reaches at steady state after 10 h milling, characterized by the uniform and narrow particle size distribution with primary crystalline sizes below 50 nm, a specific surface area of 37 m²/g, and powder mean particle size (D₅₀) of 0.57 μm. The WO₃-CuO powder mixtures milled for 10 h are heat-treated at different temperatures in H₂ atmosphere to produce W-Cu powder. The XRD results shows that both the WO₃ and CuO phases can be reduced to W and Cu phases at temperatures over 700°C. The reduced W-Cu nanocomposite powder exhibits excellent sinterability, and the ultrafine W-Cu composite can be obtained by the Cu liquid phase sintering process.

A thick film of Li₇La₃Zr₂O₁₂ (LLZO) solid-state electrolyte is fabricated using the tape casting process and is compared to a bulk specimen in terms of the density, microstructure, and ion conductivity. The final thickness of LLZO film after sintering is 240 μm which is stacked up with four sheets of LLZO green films including polymeric binders. The relative density of the LLZO film is 83%, which is almost the same as that of the bulk specimen. The ion conductivity of a LLZO thick film is 2.81 × 10⁻⁴ S/cm, which is also similar to that of the bulk specimen, 2.54 × 10⁻⁴ S/ cm. However, the microstructure shows a large difference in the grain size between the thick film and the bulk specimen. Although the grain boundary area is different between the thick film and the bulk specimen, the fact that both the ion conductivities are very similar means that no secondary phase exists at the grain boundary, which is thought to originate from nonstoichiometry or contamination.

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• Powder Aerosol Deposition as a Method to Produce Garnet‐Type Solid Ceramic Electrolytes: A Study on Electrochemical Film Properties and Industrial Applications
  Tobias Nazarenus, Yanyan Sun, Jörg Exner, Jaroslaw Kita, Ralf Moos
  Energy Technology.2021;[Epub]     CrossRef
• Synthesize of Nd₂Fe₁₄B Powders from 1-D Nd₂Fe₁₄B Wires using Electrospinning Process
  Nu Si A Eom, Su Noh, Muhammad Aneeq Haq, Bum Sung Kim
  Journal of Korean Powder Metallurgy Institute.2019; 26(6): 477.     CrossRef

W-10vol.%ZrC composites reinforced by micrometric and nanosized ZrC particles were prepared by hot-pressing of 25 MPa for 2 h at 1900°C. The effect of ZrC particle size on microstructure and mechanical properties at room temperature and elevated temperatures was investigated by X-ray diffraction analysis, scanning electron microscope and transmission electron microscope observations and the flexural strength test of the W-ZrC composite. Microstructural analysis of the W-ZrC composite revealed that nanosized ZrC particles were homogeneously dispersed in the W matrix inhibiting W grain growth compared to W specimen with micrometric ZrC particle. As a result, its flexural strength was significantly improved. The flexural strength at room temperature for W-ZrC composite using nanosized ZrC particle being 740 MPa increased by around 2 times than that of specimen using micrometric ZrC particle which was 377 MPa. The maximum strength of 935 MPa was tested at 1200°C on the W composite specimen containing nanosized ZrC particle.

The effects of particle size of Li-Si alloy and LiCl-KCl addition as a binder phase for raw material of anode were investigated on the formability of the thermal battery anode. The formability was evaluated with respect to filling density, tap density, compaction density, spring-back and compressive strength. With increasing particle size of Li-Si alloy powder, densities increased while spring-back and compressive strength decreased. Since the small spring-back is beneficial to avoiding breakage of pressed compacts, larger particles might be more suitable for anode forming. The increasing amount of LiCl-KCl binder phase contributed to reducing spring-back, improving the formability of anode powder too. The control of particle size also seems to be helpful to get double pressed pellets, which consisted of two layer of anode and electrolyte.

FeS₂ has been widely used for cathode materials in thermal battery because of its high stability and current capability at high operation temperature. Salts such as a LiCl-KCl were added as a binder for improving electrical performance and formability of FeS₂ cathode powder. In this study, the effects of the addition of Li₂O in LiCl-KCl binder on the formability of FeS₂ powder compact were investigated. With the increasing amount of Li₂O addition to LiCl-KCl binder salts, the strength of the pressed compacts increased considerably when the powder mixture were pre-heat-treated above 350°C. The heat-treatment resulted in promoting the coating coverage of FeS₂ particles by the salts as Li₂O was added. The observed coating as Li₂O addition might be attributed to the enhanced wettability of the salt rather than its reduced melting temperature. The high strength of compacts by the Li₂O addition and pre-heat-treatment could improve the formability of FeS₂ raw materials.

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• Effects of Particle Size and Binder Phase Addition on Formability of Li-Si Alloy Powder for Thermal Battery Anode
  Sung-Soo Ryu, Hui-Sik Kim, Seongwon Kim, Hyung-Tae Kim, Hae-Won Cheong, Sung-Min Lee
  Journal of Korean Powder Metallurgy Institute.2014; 21(5): 331.     CrossRef