• Journal of the Korean Ceramic Society
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• v.53 no.3
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• pp.325-331
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• 2016

Anatase particles of titanium dioxide were prepared from $TiCl_4$ aqueous solution by using an electro-dialysis [ED] process. For the preparation of an aqueous solution of $TiCl_4$ precipitates, $TiCl_4$ liquid frozen in ice was transferred to a neck flask and then hydrolyzed using deionized [DI] $H_2O$. During the hydrolysis of the $TiCl_4$ solution at $0^{\circ}C$, a slurry solution of $TiOCl_2$ was obtained and the color changed from red to orange. The ED process was applied for the removal of chlorine content in the slurry solution. Two kinds of hydrolyzed slurry solution with lower [$Ti^{4+}$] and higher [$Ti^{4+}$] were sampled and the ED process was applied for the samples according to the removal time of [$Cl^-$]. With de-chlorination, the solution status changed from sol to gel and the color quickly changed to blue. Finally, white crystalline powders were formed and the phase was confirmed by XRD to be anatase crystallites. The morphology of the hydrous titania particles in the solution was observed by FE-SEM. The hydrous titania particles were nano-crystalline, and easily coagulated with drying.

• Journal of the Korean Ceramic Society
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• v.23 no.1
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• pp.27-32
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• 1986

This study is aimed at synthsizing high dielectric material (Ba, Sr)$TiO_3$ through direct wet process. Pure and ultra fine particle of (Ba, Sr)$TiO_3$ Powder was synthesized from $BaCl_2$ $SrCl_2$ and TiCl4 aqeous solution at KOH Solution in the $N_2$ gas atmosphere. $BaCl_2$ $SrCl_2$ and TiCl4 were Mixed with the mole ratio of 1:9, 3:7:10, 5:5:10, 7:3:10, 9:1:10 and sythesized at 4$0^{\circ}C$~9$0^{\circ}C$ for 10min~15hrs. The particle size particle shape crystallinity and synthesis condition of (Ba, Sr)$TiO_3$ powder with the variation of temperature and reaction time in the aqueous solution studied by the exprimental instruments of DTA. TGA, X-ray diffratometer SEM.

• 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 $1000^{\circ}C$.

• Applied Chemistry for Engineering
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• v.18 no.6
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• pp.545-551
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• 2007

HCl concentration, reaction temperature, and $Ti^{4+}$ concentration are the decisive factors in determining the structure of precipitates in the process of synthesis of $TiO_2$ particles from aqueous $TiCl_4$ solution by precipitation and the volumetric proportion of brookite phase in $TiO_2$ particles can be controlled by these factors. Pure brookite-type $TiO_2$ nanoparticles were synthesized by heating the aqueous $TiCl_4$ solution with no more than 1.0 M of $Ti^{4+}$, in which the concentration of HCl was kept in the range of about 2.53~6.41 M during reaction, at the temperature below $70^{\circ}C$ for 20 h. Also, Pure brookite was finally transformed to a rutile phase via an anatase phase through heat-treatment.

• Journal of Powder Materials
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• v.16 no.1
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• pp.43-49
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• 2009

Titanium carbides are widely used for cutting tools and grinding wheels, because of their superior physical properties such as high melting temperature, high hardness, high wear resistance, good thermal conductivity and excellent thermal shock resistance. The common synthesizing method for the titanium carbide powders is carbo-thermal reduction from the mixtures of titanium oxide($TiO_2$) and carbon black. The purpose of the present research is to fabricate nano TiC powders using titanium salt and titanium hydride by the mechanochemical process(MCP). The initial elements used in this experiment are liquid $TiCl_4$(99.9%), $TiH_2$(99.9%) and active carbon(<$32{\mu}m$, 99.9%). Mg powders were added to the $TiCl_4$ solution in order to induce the reaction with Cl-. The weight ratios of the carbon and Mg powders were theoretically calculated. The TiC and $MgCl_2$ powders were milled in the planetary milling jar for 10 hours. The 40 nm TiC powders were fabricated by wet milling for 4 hours from the $TiCl_4$+C+Mg solution, and 300 nm TiC particles were obtained by using titanium hydride.

• Journal of the Korean Ceramic Society
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• v.30 no.9
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• pp.740-746
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• 1993

TiO2-SnO2 fine powders prepared by coprecipitation from TiCl4-SnCl4 aqueous solution, and their crystal structures were studied. All the TiO2-SnO2 fine powders calcined at 180~$700^{\circ}C$ showed the complete solid solution between TiO2(rutile structure) and SnO2(rutile structure). This crystal structure of TiO2-SnO2 powders is thought to be originated mainly from the heterogeneous nucleation of Ti-hydroxde on the Sn-hydroxide with coherent structure.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.2
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• pp.342-342
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• 1998

The effect of pH on the dehydration reaction of TiCl₄solution. KOH and HCl were used as a accelerater and retarder in dehydration. Results are follow. Neutralization point is pH 7.4 in the system of $TiCl_4-KOH$ and the production which is produced at acidic side is Ti-gel of poly metatitanic acid. The production which is produced at alkalic side is aligomer and crystalline potasium titanate is not detected.

• Proceedings of the Korean Ceranic Society Conference
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• 2003.04a
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• pp.156.1-156
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• 2003

• 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.

• Journal of Powder Materials
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• v.19 no.5
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• pp.356-361
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• 2012

The ultra-fine and less agglomerated titanium carbonitride particles were successfully synthesized by magnesiothermic reduction with low feeding rate of $TiCl_4+1/4C_2Cl_4$ solution. The sub-stoichiometric titanium carbide ($TiC_{0.5{\sim}0.6}$) particles were produced by reduction of chlorine component by liquid magnesium at $800^{\circ}C$ of gaseous $TiCl_4+1/4C_2Cl_4$ and the heat treatments in vacuum were performed for 5 hours to remove the residual magnesium and magnesium chloride mixed with produced $TiC_{{\sim}0.5}$. The final $TiC_{{\sim}0.5}N_{0{\sim}0.5}$ particle with near 100 nm in mean size and high specific surface area of $65m^2/g$ was obtained by nitrification under nitrogen gas at $1,150^{\circ}C$ for 2 hrs.