• Journal of the Korean Ceramic Society
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• v.35 no.11
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• pp.1212-1221
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• 1998

• 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.37 no.5
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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.

• Korean Journal of Materials Research
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• v.12 no.12
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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.

• Journal of the Korean Chemical Society
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• v.4 no.1
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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.

• Applied Chemistry for Engineering
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• v.16 no.6
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• pp.785-789
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• 2005

$TiO_2$ powders with rutile and brookite phases were synthesized through homogeneous precipitation of the aqueous $TiOCl_2$ solution, prepared from $TiCl_4$ and HCl solution, and their properties were characterized. Based on the analytical results appropriate molar ratios of ${Cl^-}_{total}:Ti^{+4}$ in precipitating solution for synthesis of pure rutile phase and a mixture of rutile and brookite phases were proposed. The volumetric proportion of brookite increased with increasing HCl concentration under a typical condition obtaining mixed phase of rutile and brookite. The brookite phase in the mixture was transformed to anatase phase by heat treatment at about $800^{\circ}C{\sim}850^{\circ}C$, and finally converted to rutile phase at $1000^{\circ}C$.

• Clean Technology
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• v.27 no.2
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• pp.152-159
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• 2021

Volatile organic compounds (VOCs) occur in indoor and outdoor industrial and urban areas and cause environmental problems. Malodorous VOCs, along with aesthetic discomfort, can have a serious effect on the human body. Compared with the existing method of reducing malodorous VOCs, a wet scrubbing method using an electrolytic oxidant has the advantage of reducing pollutants and regenerating oxidants. This study investigated the optimal conditions for producing OCl^-, a chlorine-oxidant. Experiments were conducted by changing the type of anode and cathode electrode, the type of electrolyte, the concentration of electrolytes, and the current density. With Ti/IrO₂ as the anode electrode and Ti as the cathode electrode, OClproduction was highest and most stable. Although OCl^- production was similar with the use of KCl or NaCl, NaCl is preferable because it is cheap and easy to obtain. The effect of NaCl concentration and current density was examined, and the OCl^- production rate and concentration were highest at 0.75 M NaCl and 0.03 A cm^-2. However, considering the cost of electric power, OCl^- production under the conditions of 1.00 M NaCl and 0.01 A cm^-2 was most effective among the conditions examined. It is desirable to produce OCl^- by adjusting the current density in accordance with the concentration and characteristics of pollutants.

• Proceedings of the Materials Research Society of Korea Conference
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• 2006.05a
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• pp.33.2-33.2
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• 2006

• Journal of the Korean Ceramic Society
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• v.35 no.4
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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.

• 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.