• 한국전기전자재료학회논문지
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• 제14권11호
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• pp.904-911
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• 2001

High-density lead zirconate titanate(Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$, PZT) ceramics were fabricated by a new milling-precipitation(MP) process improved from the conventional solid state process. This process was progressed by a milling impregnation through mixing ZrO$_2$ and TiO$_2$ powders with lead nitrate(Pb(NO$_3$)$_2$) water solution in zirconia ball media, and then milling precipitation was induced from precipitation of PbC$_2$O$_4$ by adding ammonium of oxalate monohydrate((NH$_4$)$_2$C$_2$O$_4$$.$H$_2$O) as a precipitant. As a result of this process, single-phase perovskite structure was formed at the calcination temperature of 750$\^{C}$ for Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$ powders. In addition, the highest density at the sintering temperature of 1100$\^{C}$ was obtained, because of the highly sinterable PZT Powders ground through the re-milling process. Piezoelectric and dielectric properties of sintered sample were improved by MP process.

• 한국세라믹학회지
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• 제47권2호
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• pp.183-188
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• 2010

$Ce_{0.8}Gd_{0.2}O_{1.9}$(GDC20) powder was synthesized by milling of $CeO_2$ slurry and Gd oxalate precipitation. The mixture of $CeO_2$ powder and Gd precipitates calcined at $600^{\circ}C$ for 2 h showed the particle size distribution similar to that of $CeO_2$ powder, which had been milled during the synthesis process. Attrition milling of the calcined powder with an average particle size of $0.36\;{\mu}m$ for 2 h resulted in a decrease in the particle size to $0.24\;{\mu}m$. Although the milled powder consisted of small particles(<$1\;{\mu}m$), a small amount of fine platy $Gd_2O_3$ particles, which had been survived in the milling process, was observed. Sintering of the powder compacts for 4 h showed relative densities of 80.7% at $1300^{\circ}C$ and 97% at $1400^{\circ}C$, respectively. Densification was found to almost complete at $1500^{\circ}C$, resulting in a dense and homogeneous microstructure with a relative density of 99.5%.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2001년도 춘계학술발표강연 및 논문개요집
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• pp.151-151
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• 2001

• 한국세라믹학회지
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• 제43권10호
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• pp.666-672
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• 2006

GDC20($Ce_{0.8}Gd_{0.2}O_{1.9}$) powder was synthesized by oxalate co-precipitation and milling and its thermal decomposition, phase formation, and sinterability were investigated. As-prepared precipitates were non-crystalline due to the milling process and completely decomposed at 400$^{\circ}C$ The powder calcined at 800$^{\circ}C$ for 2 h contained fine p]sty particles with an average size of 0.69 $\mu$m. Attrition milling of the calcined powder for 2 h had a little milling effect, resulting in a slight decrease in the particle size to 0.45 $\mu$m. The milled powder consisted of small spherical primary particles and some large particles, which had been agglomerated during calcination. Due to the excellent sinterability of the powder, sintering of the powder compacts for 4 h showed relative densities of 78.7% at 1000$^{\circ}C$ and 97.8% at 1300$^{\circ}C$, respectively. Densification was found to almost complete at temperature above 1200$^{\circ}C$ and a dense and homogeneous microstructure was obtained. A rapid grain growth occurred between 1200$^{\circ}C$ and 1300$^{\circ}C$. Grains in 0.1$\sim$0.5 $\mu$m sizes at 1200$^{\circ}C$ grew to 0.2$\sim$2 $\mu$m and their size distribution became broader at 1300$^{\circ}C$.

• 한국세라믹학회:학술대회논문집
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• 한국세라믹학회 2003년도 추계총회 및 연구발표회 초록집
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• pp.73.1-73
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• 2003

• 한국세라믹학회지
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• 제40권11호
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• pp.1120-1126
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• 2003

알루미나 분말을 분쇄하면서 Y 수화물을 동시에 침전시켜 YAG 분말을 합성하였다. 하소 분말 (l20$0^{\circ}C$, 4 h)에는 YAG 외에 소량의 YAM이 남아 있었다. 그러나 평균 입경 0.57 $\mu$m으로 분쇄한 분말 성형체에서는 산화물 혼합법에서 YAG 단일상이 얻어지는 온도 (l500∼1$600^{\circ}C$) 보다 훨씬 낮은 130$0^{\circ}C$ 에서 YAG 단일상이 이미 형성되었다. 분말의 소결성은 우수하여 소결조제 SiO$_2$(350 ppm Si) 의 첨가에 관계없이 치밀화가 잘 일어났다. SiO$_2$를 첨가하지 않은 경우, 1$600^{\circ}C$에서 98%의 손결밀도를 얻었다. SiO$_2$를 첨가한 경우에는 150$0^{\circ}C$에서 치밀화가 더 잘 일어나 97.7%의 소결밀도가 얻어졌으며, 1$600^{\circ}C$에서는 SiO$_2$의 소결촉진 효과가 나타나지 않아 밀도는 SiO$_2$를 첨가하지 않은 시편과 비슷하였다.

• 한국세라믹학회지
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• 제39권4호
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• pp.336-340
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• 2002

Pure and nano-sized $TiO_2$ and $CaTiO_3$ powders were fabricated by a polymeric steric entrapment route and planetary milling process. An ethylene glycol was used as a polymeric carrier for the preparation of organic-inorganic precursors. Titanium isopropoxide and calcium nitrate were dissolved in liquid-type ethylene glycol without any precipitation. At the optimum amount of the polymer, the metal cations were dispersed in solution and a homogeneous polymeric network was formed. The dried precursor ceramic gels were turned to porous powders through calcination process. The porous powders were crystallized at low temperatures and the crystalline powders were planetary milled to nano size.

• 한국세라믹학회:학술대회논문집
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• 한국세라믹학회 2000년도 춘계총회,특별강연,심포지움,연구발표회
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• pp.65.1-65.1
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• 2000

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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• pp.386-386
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• 2012

For white light emitting diode (LED) applications, it has been reported that Y3Al5O12:Ce3+ (YAG:Ce) in nano-sized phosphor performs better than it does in micro-sized particles. This is because nano-sized YAG:Ce can reduce internal light scattering when coated onto a blue LED surface. Recently, there have been many reports on the synthesis of nano-sized YAG particles using bottom-up method, such as co-precipitation method, sol-gel process, hydrothermal method, solvothermal method, and glycothermal method. However, there has been no report using top-down method. Top-down method has advantages than bottom-up method, such as large scale production and easy control of doping concentration and particle size. Therefore, in this study, nano-sized YAG:Ce phosphors were synthesized by a high energy beads milling process with varying beads size, milling time and milling steps. The beads milling process was performed by Laboratory Mill MINICER with ZrO2 beads. The phase identity and morphology of nano-sized YAG:Ce were characterized by X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FESEM), respectively. By controlling beads size, milling time and milling steps, we synthesized a size-tunable and uniform nano-sized YAG:Ce phosphors which average diameters were 100, 85 and 40 nm, respectively. After milling, there was no impurity and all of the peaks were in good agreement with YAG (JCPDS No. 33-0040). Luminescence and quantum efficiency (QE) of nano-sized YAG:Ce phosphors were measured by fluorescence spectrometer and QE measuring instrument, respectively. The synthesized YAG:Ce absorbed light efficiently in the visible region of 400-500 nm, and showed single broadband emission peaked at 550 nm with 50% of QE. As a result, by considering above results, high energy beads milling process could be a facile and reproducible synthesis method for nano-sized YAG:Ce phosphors.

• 한국재료학회지
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• 제23권10호
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• pp.543-549
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• 2013

The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried $Zr(OH)_4$ was milled using a HEM machine with distilled water. The particle size of the $Zr(OH)_4$ powder exposed to HEM reduced to 100~150 nm, whereas that of fresh $Zr(OH)_4$ powder without a pre-milling process had a large and irregular size of 100 nm~1.5 ${\mu}m$. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.