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 500oC, 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 300oC 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℃ 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.
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 900oC. 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℃. 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 1,300oC via liquid phase sintering of MCAS additive, and complete densification could be achieved after sintering at 1,600oC, which is a reduction in sintering temperature by 200oC compared to conventional AlN-Y2O3 systems. The MCAS glass phase is satisfactorily distributed between AlN particles after sintering at 1,600oC, existing as an amorphous secondary phase. The AlN specimen attained a thermal conductivity of 82.6 W/m·K at 1,600oC.
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℃ and 800℃. Instead of LBO, the compound Li2+xC1-xBxO3 (LCBO) is unexpectedly synthesized after a heat-treatment of 700℃. 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℃, 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℃, while the pure LLZ specimen had a densify of 2.98 g/cm3 and Li-ion conductivity of 5.98 × 10−6 Scm-1.
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℃, 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℃ to 1400℃, 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 700oC. 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.
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 currentcapability at high operation temperature. Salts such as a LiCl-KCl were added as a binder for improving electrical per-formance and formability of FeS2 cathode powder. In this study, the effects of the addition of Li2O in LiCl-KCl binderon the formability of FeS2 powder compact were investigated. With the increasing amount of Li2O addition to LiCl-KClbinder salts, the strength of the pressed compacts increased considerably when the powder mixture were pre-heat-treatedabove 350oC. The heat-treatment resulted in promoting the coating coverage of FeS2 particles by the salts as Li2O wasadded. The observed coating as Li2O addition might be attributed to the enhanced wettability of the salt rather than itsreduced melting temperature. The high strength of compacts by the Li2O addition and pre-heat-treatment could improvethe formability of FeS2 raw materials.
Ultra-fine zirconium carbide (ZrC) powder with nano-sized primary particles was synthesized by the carbothermal reduction method by using nano-sized and nano-sized graphite powders mixture. The synthesized ZrC powder was well dispersed after simple milling process. After heat-treatment at for 2 h under vacuum, ultra-fine ZrC powder agglomerates (average size, ) were facilely obtained with rounded particle shape and particle size of ~200 nm. Ultra-fine ZrC powder with an average particle size of 316 nm was obtained after ball milling process in a planetary mill for 30 minutes from the agglomerated ZrC powder.
Nanocrystalline powder could be synthesized by solid-state reaction using the mixture which was prepared by a high energy milling process in a bead mill for and nanocrystalline powders mixture. Effect of the milling time on the powder characteristic of the synthesized powder was investigated. Nanocrystalline with a particle size of 50 nm was obtained at . High tetragonal powder with a tetragonality(=c/a) of 1.009 and a specific surface area of was acquired after heat-treatment at for 2 h. High energy ball milling was effective in decreasing the reaction temperature and increasing the tetragonality.