• Journal of the Korean Ceramic Society
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• v.30 no.12
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• pp.1023-1028
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• 1993

To obtain a single phase of Ba2Ti9O20 at lower temperature than previious other researches. We investigated the effect of Zr substitution for predetermined portions of Ti in Ba2Ti9O20. In this study, the four compounds(x=0, 0.028, 0.048, 0.068) of Ba2(Ti1-xZrx)9O20 were prepared by coprecipitation reaction of BaCl2, TiCl4 and ZrOCl2 with (NH4)2CO3 and NH4OH as the coprecipitating agents and pH regulators, in queous solution. Owing to 4.8 mol% addition, the single phase of Ba2Ti9O20 showing high Q was obtained at 115$0^{\circ}C$ which is lower by 25$0^{\circ}C$ than the temperature in case of mechanical mixtures of BaCO3 and TiO2.

• Journal of the Korean Ceramic Society
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• v.31 no.8
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• pp.879-885
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• 1994

Coprecipitation technique was used to synthesize ZrO2+12 mol% CeO2 powders with ZrOCl2.8H2O and Ce(NO3)3.6H2O as starting materials. The powders were dried on different conditions such as distilled water, ethanol, and azeotropic distillation. The powders prepared by azeotropic distillation showed weak aggregation of particles and the average particle size of powders calcined at 85$0^{\circ}C$ for 1 hour was 0.19 ${\mu}{\textrm}{m}$. The optimum sintering temperature and holding time are 130$0^{\circ}C$ and 2.5~10 hours, respectively. Beyond the optimum conditions, a phase transition from tetragonal to monoclinic causes to produce cracks in the sintered bodies and to decrease the density.

• Journal of the Korean Ceramic Society
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• v.25 no.4
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• pp.364-372
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• 1988

The mechanical properties and microstructure of ceramics of the system Al2O3-ZrO2-Y2O3 sintered at 1$650^{\circ}C$ for 2h after powder preparation by the precipitation method from Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were investigated. The Al2O3-ZrO2-Y2O3 ceramics sintered at 1$650^{\circ}C$ for 2h after mixing alpha-Al2O3 and ZrO2-Y2O3 powders, both were separately precipitated and calcined, were found to have the relative density higher than 97.5% so that the strengthening and toughening mechanisms could be explained mainly as the stress-induced phase transformation. On the other hand, the sintered bodies prepared by co-precipitating the three starting materials were measured to have the relative density lower than 85% so that the degradation of strength were observed above 15 vol% ZrO2 contents due to the high porosity by which the effect of stress-induced phase transformation was assumed to be depressed.

• Journal of the Korean Ceramic Society
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• v.27 no.8
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• pp.991-1003
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• 1990

A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent, various types of metal hydroxides were obtained by single precipitation(series A) and co-precipitation(series B) method at the pH condition between 7 and 11. Fine Al2O3-ZrO2 powders were prepared at optimum calcination condition and the effects of ZrO2 on microstructures and mechanical properties of Al2O3 were investigated. The composition of Al2O3/ZrO2 composites wax fixed as Al2O3-15 v/o ZrO2(＋3m/o Y2O3). ZrO2 limited the grain growth of Al2O3 and increased grain size homogeneity of Al2O3 more effectively than MgO.Flexural strength values in Al2O3 and Al2O3/ZrO2 composites were 340-430 MPa and 540-820 MPa, respectively, and the effect of strength improvement showed 20-50% by adding ZrO2 to Al2O3. Fracture toughness of Al2O3/ZrO2 composites was improved by stress-induced phase transformation of tetragonal ZrO2 and toughening effect by microcrack was not observed. Also, ZrO2 particles located at Al2O3 grain junction contributed to toughening, while spherical ZrO2 particles located within Al2O3 grain did not contribute to toughening. Weibull moduli of Al2O3 ceramics and Al2O3/ZrO2 composites of series A and series B were 4.34, 5.17 and 9.06, respectively. Above 0.5 of failure probability, strength values in Al2O3 ceramics and Al2O3/ZrO3 composites of series A and series B were above 400 MPa, 700 MPa and 650 MPa, respectively.

• Journal of the Korean Ceramic Society
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• v.26 no.3
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• pp.423-437
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• 1989

Al2O3/ZrO2 composites were prepared by precipitation method using Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O as starting materials and NH4OH as a precipitation agent. Al2O3/ZrO2 composites(series A) were prepared by mixing Al2O3 powder obtained by single precipitation method with ZrO2(＋3m/o Y2O3) powder obtained by co-predipitation method. Al2O3/ZrO2 composites (series B) were prepared by co-precipitation method using the three starting materials. In all cases, the composition was controlled as Al2O3-15v/o ZrO2(＋3m/o Y2O3). The composites of series A showed higher final relative densities than those of series B and tetagonal ZrO2 in all cases was retained to about 95% at room temperature. ZrO2 particles were coalesced more rapidly in grain boundary of Al2O3 than within Al2O3 grain. ZrO2 particles were located at 3-and 4-grain junction of Al2O3 and limited the grain growth of Al2O3. It was observed that MgO contributed to densification of Al2O3 but limited grain growth of Al2O3 by MgO was not remarkable. In all Al2O3/ZrO2 composites, exaggerated grain growth of Al2O3 was not observed and Al2O3/ZrO2 composites were found to have homogeneous microstructures.

• Journal of the Korean Ceramic Society
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• v.28 no.1
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• pp.11-18
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• 1991

A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics, and the effects of stress-induced phase transformation of ZrO2 on thermal shock behavior of Al2O3-ZrO2 ceramics were investigated. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Metal hydroxides were obtained by single precipitation(process A) and co-precipitation(process B) method at the condition of pH=7, and the composition of Al2O3-ZrO2 composites was fixed as Al2O3-15v/o ZrO2(+3m/o Y2O3). Critical temperature difference showing rapid strength degradation by thermal shock showed higher value in Al2O3/ZrO2 composites(process A : 20$0^{\circ}C$, process B : 215$^{\circ}C$) than in Al2O3(175$^{\circ}C$). The improvement of thermal shock property for Al2O3/ZrO2 composites was mainly due to the increase of strength at room temperature by adding ZrO2. The strength degradation was more severe for the sample with higher strength at room temperature. Crack initiation energies by thermal shock showed higher values in Al2O3/ZrO2 composites than in Al2O3 ceramics due to increase of fracture toughness by ZrO2.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.03a
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• pp.208-208
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• 2003

저온균일침전법(HPPLT)으로 제조된 TiO$_2$나노분말은 10$0^{\circ}C$이하의 온도에서 rutile상을 얻을 수 있다. 또한, rutile에서 anatase로의 상변화는 합성시간, 가열속도, 반응온도 그리고 음이온 첨가에 의해 일어난다고 보고되어졌지만, 금속양이온들에 의한 상변화는 알려진 바가 없다. 따라서, 다양한 양이온을 첨가하여 저온균일침전법에서 TiO$_2$의 상변화가 어떻게 일어나는지를 조사하였다. 출발원료인 TIC1$_4$를 사용하여 가수분해하여 0.67M의 TiOCl$_2$을 얻었다. 얻어진 TiOCl$_2$ 수용액에 각각 0.01M의 금속염화물(ZrOCl$_2$, NiCl$_2$, CuCl$_2$, FeCl$_3$, AlCl$_3$ 그리고 NbCl$_{5}$)을 첨가한 후 반응기에 넣고 10$0^{\circ}C$에서 4시간동안 가열하였다 가열한 후 얻어진 침전물에 NaOH 수용액을 이용하여 PH 7-8로 중화한 후 증류수로 Cl$^{-}$이온이 제거될 때까지 충분히 세척하였다. 세척된 침전물을 105$^{\circ}C$에서 24h동안 건조하여 분말을 얻었고, rutile에서 anatase로의 상변화특성을 관찰하기 위하여 XRD, SEM, TEM, ICP 분석을 실시하였다.

• Journal of the Korean Ceramic Society
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• v.39 no.11
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• pp.1017-1022
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• 2002

$(Ba_{1-x}Ca_x)(Ti_{1-y}Zr_y)O_3(BCTZ)$ powders for the Ni-electrode Multilayer Ceramic Capacitor(MLCC) were synthesized via hydrothermal treatment using mixed aqueous solutions of $BaCl_2{\cdot}2H_2O,\Ca(NO_3)2{\cdot}4H_2O,\ ZrOCl_2{\cdot}8H_2O$ and $TiCl_4$. Two component and three component systems were also extensively studied for basic data. BT, CT and BZ powders were crystalline but CZ was determined to be amorphous under the same synthetic condition. In BTZ system, Zr and Ti were completely soluble and Ca would be substituted for Ba up to ∼6 mol% in BCT. The submicron-sized $(Ba_{0.95}Ca_{0.05})(Ti_{0.80}Zr_{0.20})O_3$ powder of the target composition was successfully synthesized at $150{\circ}$ for 12h.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.11a
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• pp.130-130
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• 2003

현재, 메탈의 내부식성 코팅막 제조에 사용되고 있는 크로메이트 기반 코팅제는 유독성 물질에 대한 환경 규제에 따라 조만간 사용이 금지 될 예정이다. 본 연구에서는 이러한 유독성 금속 내부식성 코팅제를 대체할 새로운 환경 친화적인 코팅 재료로서 A1OOH 나노졸이 분산된 ZrOCl$_2$ㆍ8$H_2O$-GPS(3-Glycidoxypropyltrimethoxysilane)하이브리드 졸을 제조하고 이의 내 부식성 특성에 대하여 조사하였다. AlOOH 졸이 첨가된 유/무기 하이브리드 졸은 염화 알루미늄을 염기로 침전 시킨 수산화 알루미늄 침전물에ZrOCl$_2$ㆍ8$H_2O$를 10 ~ 20 wt% 첨가하고 열처리한 후 여기에 GPS를 AlOOH에 대하여 4 ~ 6몰 배 첨가하여 제조하였다. 제조된 하이브리드 형 졸은 가시관 투광성이 우수하며 시간에 따른 범도 변화가 거의 없었다. 이 코팅 졸을 아연 도금 강판에 딥 코팅법으로 코팅한 후, 상온~20$0^{\circ}C$에서 열처리하여 염수 시험법으로 하이브리드 졸의 조성 및 열처리 조건에 따른 코팅막의 내부식성 특성을 조사하였다. 또한, 코팅막의 두께를 전자 현미경으로 관찰하였고, 코팅막 경도는 연필 경도계로 조사하였다.

• Journal of the Korean Ceramic Society
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• v.39 no.7
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• pp.704-709
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• 2002

To improve the mechanical properties of $Al_2$O$_3$/ZrO$_2$composites, the homogeneous dispersion of ultra low size ZrO$_2$ particles in $Al_2$O$_3$ceramics have been controlled by coprecipitation method. In case of mechanical mixing of ZrO$_2$ powders with $Al_2$O$_3$, homogeneous dispersion and controlling the ZrO$_2$ size were relatively difficult due to high sintering temperature. So nanosized Zr hydroxide was coprecipitated from ZrOCl$_2$/Y(NO$_3$)$_3$ solution with commercial sub-micron sized $\alpha$-alumina (Sumitomo : AES-11(0.4 ${\mu}{\textrm}{m}$)) and high purity ultra low sized $\alpha$-alumina (Taimei Chemical (0.22 ${\mu}{\textrm}{m}$)) for low temperature sintering. By this partial coprecipitation method, relatively low sized ZrO$_2$ dispersion in $Al_2$O$_3$/ZrO$_2$ composites was achieved at 150$0^{\circ}C$-1$600^{\circ}C$ of sintering temperature range and their mechanical properties were measured.