• Journal of Powder Materials
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• v.31 no.1
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• pp.43-49
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• 2024

In this study, a core-shell powder and sintered specimens using a mechanically alloyed (MAed) Ti-Mo powder fabricated through high-energy ball-milling are prepared. Analysis of sintering, microstructure, and mechanical properties confirms the applicability of the powder as a sputtering target material. To optimize the MAed Ti-Mo powder milling process, phase and elemental analyses of the powders are performed according to milling time. The results reveal that 20 h of milling time is the most suitable for the manufacturing process. Subsequently, the MAed Ti-Mo powder and MoO₃ powder are milled using a 3-D mixer and heat-treated for hydrogen reduction to manufacture the core-shell powder. The reduced core-shell powder is transformed to sintered specimens through molding and sintering at 1300 and 1400℃. The sintering properties are analyzed through X-ray diffraction and scanning electron microscopy for phase and porosity analyses. Moreover, the microstructure of the powder is investigated through optical microscopy and electron probe microstructure analysis. The Ti-Mo core-shell sintered specimen is found to possess high density, uniform microstructure, and excellent hardness properties. These results indicate that the Ti-Mo core-shell sintered specimen has excellent sintering properties and is suitable as a sputtering target material.

• The Journal of Advanced Prosthodontics
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• v.5 no.2
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• pp.161-166
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• 2013

PURPOSE. This study aimed to identify the effects of the sintering conditions of dental zirconia on the grain size and translucency. MATERIALS AND METHODS. Ten specimens of each of two commercial brands of zirconia (Lava and KaVo) were made and sintered under five different conditions. Microwave sintering (MS) and conventional sintering (CS) methods were used to fabricate zirconia specimens. The dwelling time was 20 minutes for MS and 20 minutes, 2, 10, and 40 hours for CS. The density and the grain size of the sintered zirconia blocks were measured. Total transmission measurements were taken using a spectrophotometer. Two-way analysis of variance model was used for the analysis and performed at a type-one error rate of 0.05. RESULTS. There was no significant difference in density between brands and sintering conditions. The mean grain size increased according to sintering conditions as follows: MS-20 min, CS-20 min, CS-2 hr, CS-10 hr, and CS-40 hr for both brands. The mean grain size ranged from 347-1,512 nm for Lava and 373-1,481 nm for KaVo. The mean light transmittance values of Lava and KaVo were 28.39-34.48% and 28.09-30.50%, respectively. CONCLUSION. Different sintering conditions resulted in differences in grain size and light transmittance. To obtain more translucent dental zirconia restorations, shorter sintering times should be considered.

• Journal of Powder Materials
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• v.17 no.1
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• pp.13-22
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• 2010

The unique features of spark plasma sintering process are the possibilities of a very fast heating rate and a short holding time to obtain fully dense materials. $\beta$-SiC powder with 0, 2, 6, 10 wt% of $\alpha$-SiC particles (seeds) and 4 wt% of Al-B-C (sintering aids) were spark plasma sintered at $1700-1850^{\circ}C$ for 10 min. The heating rate, applied pressure and sintering atmosphere were kept at $100^{\circ}C/min$, 40 MPa and a flowing Ar gas (500 CC/min). Microstructural development of SiC as function of seed content and temperature during spark plasma sintering was investigated quantitatively and statistically using image analysis. Quantitative image analyses on the sintered SiC ceramics were conducted on the grain size, aspect ratio and grain size distribution of SiC. The microstructure of SiC sintered up to $1700^{\circ}C$ consisted of equiaxed grains. In contrast, the growth of large elongated SiC grains in small matrix grains was shown in sintered bodies at $1750^{\circ}C$ and the plate-like grains interlocking microstructure had been developed by increasing sintering temperature. The introduction of $\alpha$-SiC seeds into $\beta$-SiC accelerated the grain growth of elongated grains during sintering, resulting in the plate-like grains interlocking microstructure. In the $\alpha$-SiC seeds added in $\beta$-SiC, the rate of grain growth decreased with $\alpha$-SiC seed content, however, bulk density and aspect ratio of grains in sintered body increased.

• Journal of Powder Materials
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• v.15 no.5
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• pp.405-410
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• 2008

SOFC (Solid Oxide Fuel Cell) Ni-YSZ anode was fabricated by the spark plasma sintering (SPS) process and its microstructure and electrical properties were investigated in this study. The spark plasma sintering process was carried out at $800{\sim}1000^{\circ}C$ for holding time of 5 min under 40 MPa. To fabricate Ni-YSZ anode, the SPS processed specimens were reduced at $800^{\circ}C$ under $H_2$ atmosphere. The reduced specimens showed relative density of $48.4{\sim}64.8%$ according to sintering temperature. And also, the electrical conductivity of reduced specimens after sintering at 900 and $1000^{\circ}C$ showed $480{\sim}600$ (S/cm) values at the measuring range of $600{\sim}900^{\circ}C$.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 2000.06a
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• pp.65-86
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• 2000

Rare earth-doped ceria powders with a composition of Ce0.8R0.2O1.9(R=Yb, Y, Gd, Sm, Nd and La) were prepared by heating the oxalate coprecipitate. The green compacts began to shrink at 600$^{\circ}$-700$^{\circ}C$. The relative density after the sintering at 1200$^{\circ}$ and 1400$^{\circ}C$ became higher for the higher green density. The samples were densified above 98% relative density by the sintering ant 1600$^{\circ}C$ for 4 h and the grain sizes (4.7-7.6$\mu\textrm{m}$) showed a tendency to become larger with increasing ionic radius of doped-rare earth element. In the intial stag of sintering at 700$^{\circ}$-800$^{\circ}C$, the dominant mass transport process changed from lattice diffusion to grain boundary diffusion to grain boundary diffusion with heating time. The porosity during the intermediated and final stage of the sintering at 1200$^{\circ}$ and 1400$^{\circ}C$ decreased by the mass transport through lattice diffusion with grain growth.

• Journal of Powder Materials
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• v.21 no.4
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• pp.256-259
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• 2014

A magnetic powder, M-type barium hexaferrite (BaFe12O19), was consolidated with the spark plasma sintering process. Three different holding temperatures, $850^{\circ}C$, $875^{\circ}C$ and $900^{\circ}C$ were applied to the spark plasma sintering process with the same holding times, heating rates and compaction pressure of 30 MPa. The relative density was measured simultaneously with spark plasma sintering and the convergent relative density after cooling was found to be proportional to the holding temperature. The full relative density was obtained at $900^{\circ}C$ and the total sintering time was only 33.3 min, which was much less than the conventional furnace sintering method. The higher holding temperature also led to the higher saturation magnetic moment (${\sigma}_s$) and the higher coercivity ($H_c$) in the vibrating sample magnetometer measurement. The saturation magnetic moment (${\sigma}_s$) and the coercivity ($H_c$) obtained at $900^{\circ}C$ were 56.3 emu/g and 541.5 Oe for each.

• Journal of Powder Materials
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• v.4 no.4
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• pp.298-303
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• 1997

The activated sintering behavior of $MoSi_2$ powder compacts with addition of 0.5 and 1.0 wt.%Ni during the sintering under As atmosphere was studied. The shrinkage was measured and the microstructures were observed by SEM (scanning electron microscopy) and BEI (backscattered electron image) along with the phase analysis by EDS during heating up to 155$0^{\circ}C$ and holding for various time at 155$0^{\circ}C$. The most of shrinkage occurred upon heating and 92% of theoretical density was attained after sintering for 1 hr at 155$0^{\circ}C$. However, little shrinkage ensued even for prolonged sintering over 1 hr at 155$0^{\circ}C$. A liquid film formed at about 135$0^{\circ}C$ along necks and grain boundaries. The polyhedral grain structure composed of $(Mo,Ni)_5Si_3$and $Ni_2Si$ across the $MoSi_2$ grain boundary developed at 155$0^{\circ}C$. It was concluded that the activated sintering of $MoSi_2$ powder by Ni led to the diffusion of Si into Ni decreasing the liquidus temperature and the enhanced diffusion of Mo and Si through such a liquid phase and/or interboundary of $(Mo,Ni)_5Si_3$.

• Journal of Powder Materials
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• v.22 no.3
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• pp.175-180
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• 2015

In this study, ternary compound Max Phase $Ti_2AlC$ material was mixed by 3D ball milling as a function of ball milling time. More than 99.5 wt% pure $Ti_2AlC$ was synthesized by using spark plasma sintering method at 1000, 1100, 1200, and $1300^{\circ}C$ for 60 min. The material characteristics of synthesized samples were examined with relative density, hardness, and electrical conductivity as a function of sintering temperature. The phase composition of bulk was identified by X-ray diffraction. On the basis of FE-SEM result, a terraced structures which consists of several laminated layers were observed. And $Ti_2AlC$ bulk material obtained a vickers hardness of 5.1 GPa at the sintering temperature of $1100^{\circ}C$.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07a
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• pp.127-130
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• 2002

In this study, development of a new LTCC material using a non-glassy system was attempted with respect to reducing the fabrication process steps and cost down. Lowering the sintering temperature can be achieved by liquid phase sintering. For LTCC application, the starting material must have quality factor as high as possible in microwave frequency range. And also, the material should have a low dielectric constant for enhancing the signal propagation speed. Regarding these factors, dielectric constants of various materials were estimated by the Clausius-Mosotti equation. Among them, CaWO$_4$ was tamed out the suitable LTCC material. CaWO$_4$ can be sintered up to 98% of full density at 1200$^{\circ}C$ for 3 hours. It's measured dielectric constant, quality factor, and temperature coefficient of resonant frequency were 10.15, 62880GHz, and -27.8ppm/$^{\circ}C$, respectively. In order to modify the dielectric properties and densification temperature, 0.5∼1.5 wt% LiF were added to CaWO$_4$. LiF addition reduced the sintering temperature/time down to 800$^{\circ}C$/10∼30min due to the reactive liquid phase sintering. Dielectric constant lowered from 10.15 to 9.38 and Q x fo increased up to 92000GHz with increasing LiF content.

• Journal of the Korean Ceramic Society
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• v.50 no.3
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• pp.226-230
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• 2013

We performed high pressure high temperature (HPHT) sintering for the 20 nm MgO powders at the temperatures from $600^{\circ}C$ to $1200^{\circ}C$ for only 5 min under 7 GPa pressure condition. To investigate the microstructure evolution and physical property change of the HPHT sintered MgO samples, we employed a scanning electron microscopy (SEM), density and Vickers hardness measurements. The SEM results showed that the grain size of the sintered MgO increased from 200 nm to $1.9{\mu}m$ as the sintering temperature increased. The density results showed that the sintered MgO achieved a more than 95% of the theoretical density in overall sintering temperature range. Based on Vickers hardness test, we confirmed that hardness increased as temperature increased. Our results implied that we might obtain the dense sintered MgO samples with an extremely short time and low temperature HPHT process compared to conventional electrical furnace sintering process.