• Journal of the Korean Ceramic Society
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• v.24 no.4
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• pp.397-403
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• 1987

Pb(Zr0.52Ti0.48)O3 powders were prepared by hydrothermal synthesis. Using soluble salts such as Pb(NO3)2, TiCl4 and ZrOCl2$.$8H2O and oxide such as PbO and TiO2 as starting materials, PZT powder was hydrothermally synthesized at the temperature range between 150$^{\circ}C$ and 200$^{\circ}C$. The result showed that reactivity by alkali was decreased in the sequence of Pb(NO3)2, TiCl4, ZrOCl2, PbO, TiO2 and ZrO2. Using the first three soluble salts, PZT powder was synthesiged at 150$^{\circ}C$ for 1hr. In PbO-TiCl4-ZrOCl2 system, PZT powder was synthesized at 150$^{\circ}C$ for 8rs. In Pb(NO3)2-TiO2-ZrOCl2 system, PZT powder was synthesized at 150$^{\circ}C$ for 16hrs, in PbO-TiO2-ZrOCl2 system, the powder was synthesized at 200$^{\circ}C$ for 8hrs.

• Journal of the Korean Ceramic Society
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• v.24 no.2
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• pp.186-192
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• 1987

ZrO2 powders having high purity were prepared from domestic zircon sand using the caustic fusion method and the soda ash sintering process. In the caustic fusion method, ZrO2 recovery was reached to 96% when 100/140 mesh zircon was reacted with NaOH at the NaOH/Zircon mole ratio 6 and at 650$^{\circ}C$ for 2 hours. And in the soda ash sintering process, ZrO2 was recovered to 88.5% when -325 mesh zircon was reacted with Na2CO3 at the Na2CO3/Zircon mole ratio 1.1 and 1050$^{\circ}C$ for 2 hours. In both cases, Zr component was extracted to ZrOCl2, subsequently crystallized to ZrOCl2$.$8H2O to increase the purity, and converted to ZrO2 by precipitation. And to increase the sinter ability of powder, Cl- ion was removed and strong agglomeration was avoided by methanol distribution of Zr(OH)4 precipitates.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.12 no.3
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• pp.126-132
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• 2002

The nanocrystalline zirconia powder with anisotropic shapes was synthesized by hydrothermal treatment of the tetragonal zirconia prepared by aging the zirconium hydroxide precipitate, which was obtained from the reaction between $ZrOCl_2{\cdot}8H_2O$ and KOH solutions under the fixed pH of 13.5, at $100^{\circ}C$ for 24 h. With increasing the hydrothermal reaction temperature and time, the fraction of tetragonal phase with spherical zirconia decreased, whereas, relatively the fraction of monoclinic phase with spindle-like and rod shape zirconia increased. As increased concentration of the NaOH solution it promoted the particle size to become larger and the crystalline phase to transform tetragonal to monoclinic. However, the specific surface area at the early stage of the reaction increased and subsequently decreased because of grain growth in powder with longer reaction time.

• 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.

• Korean Journal of Materials Research
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• v.17 no.1
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• pp.18-24
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• 2007

Mullite-PSZ composite was prepared by sol-gel method using $Al(sec-OC_4H_9)_3,\;Si(OC_2H_5)_4,\;ZrOCl_2\;8H_2O\;and\;Y_2O_3$. The sinterability ana mechanical properties of powder compacts sintered at $1,650^{\circ}C$ for 4 hrs were investigated for various PSZ contents. In result Al-Si spinel formed at $980^{\circ}C$ from amorphous dried gel, and zirconia as well as mullite crystal formed above $1,200^{\circ}C$. The sintered body was densified to $97{\sim}98%$ except the specimen containing 25vol% PSZ which showed the relative density of about 95% obtained by sintering at $1,650^{\circ}C$ for 4 h. The flexural strength of the sintered body was a maximum value of 290 MPa in 20 vol% PSZ, which was also considerably larger than the value of 200 MPa without PSZ. The value of the fracture toughness increased linearly with increase of PSZ content and showed a maximum value of $4.3MPam^{1/2}$ in 25 vol% PSZ, Namely this value was remarkably larger than the $value(2.6MPam^{1/2})$ of pure mullite without PSZ.