• 한국세라믹학회지
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• 제35권11호
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• pp.1212-1221
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• 1998

• 한국세라믹학회지
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• 제24권4호
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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.

• 한국세라믹학회지
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• 제37권5호
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• pp.473-478
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• 2000

The TiO2 powder with the values of the large specific surface area more than 150$m^2$/g has been prepared with the homogeneous precipitation process below 5$0^{\circ}C$ and its formation mechanism was investigated using the SEM, TEM and Raman Spectroscopy. With the spontaneous hydrolysis of aqueous TiOCl2 solutions, all the precipitates were fully and homogeneously crystallized with the rutile TiO2 phase simply by heating, which as transformed to the anatase TiO2 phase as increasing the addition of SO42- ions to the aqueous TiOCl2 solution. The precipitates were formed with spherical secondary particles which consisted of acicular, spherical and mixed primary particles corresponding to the rutile, anatase and mixed phases, respectively. It can be thought that the formation and phase determination of crystalline TiO2 powders even at ambient temperature would be related with the existence of the capillary force. This force might be varied depending on the shape change of the primary particles.

• 한국재료학회지
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• 제12권12호
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• pp.947-954
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• 2002

HCl concentration and reaction time are the decisive factors in determining the structure of precipitates in the process of synthesis of $TiO_2$ particles from aqueous $TiOCl_2$ solution by precipitation and the volumetric proportion of brookite phase in $TiO_2$ particles can be controlled by these two factors. As reaction rate increases with increase of reaction temperature, the reaction time, at which maximum volumetric proportion of brookite phase in $TiO_2$ particles was obtained, was reduced. The brookite was transformed directly to rutile phase with only increase of reaction time. And precipitation was delayed with increase of HCl concentration because the amount of $H_2$O, which is necessary source of oxygen for conversion of $Ti^{+4}$ to $TiO_2$, was relatively reduced with increase of that. Brookite in the mixture phase powder was finally transformed to rutile phase via anatase through heat-treatment.

• 대한화학회지
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• 제4권1호
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• pp.15-17
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• 1957

1. Preparation of Titanium tetrachloride; The following precesses were strictly followed as the preliminary step to obtain pure $TiOCl_2$, titanyl chloride; First, pure Titanium Oxide mixed with carbon is rolled into pills. After drying up perfectly, these pills are heated at 900∼1000${\circ}C$. And then the pills are subjected to the flow of $Cl_2$ gas in a quartz tube heated to 900-1000${\circ}C$. Thus Titanium tetrachloride is obtained. 2. Preparation of $TiOCl_2$ ; Yellowish trobrown solution is made by pouring 80 g of conc. HCl (sp.gr. 1.19) to 45 gr of Titanium tetrachloride (approx. 2 times of theoretical amount). Then this solution is kept settled for 5-days in a desiccator filled with phosphorous pentoxide at room temperature. As the colorless amorphous solid thus obtained is washed with aceton, 36.5 g of the pure salt are obtained. 3. Determination of composition. The analysis of the sample taken from the deposit desiccated gives the following data; (A) Qualitative analysis; a) $Ti(OH)_4$ is precipitated by adding NaOH in water solution of the salt. b) Adding $AgNO_3$ solution, the water solution of the salt gives white precipitate of AgCl. c) When acid and $H_2O_2$ are added, the solution turns its color to redish brown (This proves that $TiO^{++}$ was converted into $TiO^{++}$ by oxidation of $H_2O_2$. (B) Quantitative analysis; a) $Ti(OH)_4$ precipitated by $10{\%}$ NaOH isalitatsubjected consecutively to the filtration and ignition in porcelain crucible at approx. 1000${\circ}C$. , then $TiO_2$ thus formed is weighed and calculated into Ti content. b) Chlorine involved in water solution of the salt is determined by Vorhardt method. Result: The values obtained from previous analysis, devied by their atomic weight gives the following composition: Ti : Cl = 1 : 2 Therefore $TiOCl_2$ should be given as its molecular formula. 4. Summary. When $TiCl_4$ is additated into conc. HCl, $TiO^{++}$ formed exists as a stable form, and forms $TiOCl_2$. However $TiOCl_2$ is unstable to heating. When the temperature is raised to $65{\circ}C$the decomposition of the solution is accelerated, and gives $TiO_2$ aq. $TiOCl_2$ in addition is highly hygroscopic.

• 공업화학
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• 제16권6호
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• pp.785-789
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• 2005

$TiCl_4$와 염산수용액을 사용하여 균일침전반응으로 브루카이트상과 루틸상의 혼합상 $TiO_2$ 분말을 제조하여 분말특성을 조사하였다. 분석결과로부터 순수한 루틸상과 혼합상이 합성되기 위한 침전용액의 ${Cl^-}_{total}:Ti^{+4}$의 몰 비율이 제시되었다. 또한, 혼합상이 얻어지는 조건에서는 염산의 농도가 증가할수록 브루카이트상의 부피분율이 증가하였으며, 이 분말을 열처리한 결과 브루카이트상은 루틸상으로 직접 상변화하지 않고 $800^{\circ}{\sim}850^{\circ}C$에서 아나타제상으로 상전이한 후 $1000^{\circ}C$에서 최종적으로 안정한 루틸상으로 상변화되었다.

• 청정기술
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• 제27권2호
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• pp.152-159
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• 2021

다양한 환경문제를 일으키는 휘발성 유기 화합물(volatile organic compounds, VOCs)은 산업 지대 및 도심의 실내외에서 다양하게 발생한다. 악취성 VOCs는 심미적 불쾌함과 더불어 인체에 심각한 영향을 미칠 수도 있다. 기존에 악취성 VOCs를 저감하는 방식에 비하여, 전기 분해를 통해 생산된 산화제를 이용한 수세정 방식은 오염 물질 저감과 동시에 산화제의 재생이 가능하다는 장점이 있다. 본 연구에서는 염소계 산화제인 OCl^-을 생산하기 위한 최적 조건을 연구하였다. 산화 및 환원 전극의 종류와 전해질의 종류, 전해질의 농도 및 전류 밀도를 변화시켰다. 산화 전극은 Ti/IrO₂, 환원 전극은 Ti을 사용하였을 때 OCl^- 생산이 가장 우수하고 안정적이었다. 전해질의 OCl^- 생산 능력은 KCl과 NaCl이 유사하게 나타났으나, 경제적이고 쉽게 구할 수 있는 NaCl이 최적이라고 판단하였다. OCl^- 생산 속도가 우수하고 농도가 가장 높게 생산된 NaCl 농도 및 전류 밀도 조건은 0.75 M NaCl, 0.03 A cm^-2이었다. 하지만 전력 비용을 고려했을 때 본 실험에서는 1.00 M NaCl, 0.01 A cm^-2의 조건의 OCl^- 생산이 가장 효율적이었다. 실제 현장 적용시 오염물질의 농도 및 특성에 따라서 전류밀도를 조절하여 OCl^-을 생산하는 것이 바람직할 것이다.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2006년도 춘계학술발표대회 및 제10회 신소재 심포지엄 논문개요집
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• pp.33.2-33.2
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• 2006

• 한국세라믹학회지
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• 제35권4호
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• pp.325-332
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• 1998

Crystalline TiO2 ultrafine powders were prepared simply by heating and stirring aqueous TiOCl2 solution with {{{{ {Ti }^{4+ } }} concentration of 0.5 M from room temperature to 10$0^{\circ}C$ under 1 atmoshpere. The crystallinity and the particle shape of TiO2 ultrafine powders obtained by simple precipitation method were analyzed us-ing XRD(X-ray diffractometer). SEM(scanning electron microscopy) and TEM(transmission electron mi-croscopy) TiO2 crystalline precipitate with rutile phases is fully formed at the temperatures of up to $65^{\circ}C$ and then TiO2 crystalline precipitate with anatase phase starts to be formed above temperatures $65^{\circ}C$ showing its full formation at 10$0^{\circ}C$ These behaviors of TiO2 crystalline precipitate directly from an aqueous TiOCl2 solution would be caused due to the existence of {{{{ OMICRON ^2+ }} ions from distilled water which oxydize TiOCl2 to TiO2 not hydrolyzing it to Ti(OH)4 Here thermodynamically stable TiO2 rutile phase generally formed at higher temperature is practically precipitated at lower temperatures in this study This may be due to the precipitation by very slow reaction enough to make TiO2 particles allocated into stable rutile structure.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2003년도 춘계학술발표강연 및 논문개요집
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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.