• 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.

• Proceedings of the Korea Water Resources Association Conference
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• 2019.05a
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• pp.197-197
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• 2019

총인처리시설에서는 응집제를 주입하여 인이나 오염물질을 침전시켜 처리하고 있으며 PAC(poly aluminum chloride)나 $FeCl_3$, $Al_2(SO_4)_3$, 등 다양한 종류의 응집제가 사용되어지고 있다. 하지만 기존에 사용되어 지고 있는 알루미늄계열의 응집제는 처리수에 잔류이온이 존재하게 되어 인체에 축적돼 알츠하이머 병 등 신체질환을 유발할 수 있는 단점이 있다. 따라서 이러한 단점을 사전에 예방하기 위해 $TiCl_4$와 같은 티타늄계열 응집제에 대한 연구가 진행되고 있다. $TiCl_4$ 응집제는 인 제거에 효과적으로 적용할 수 있으며 수중에 잔류이온을 유발하지 않으며 Ti이온은 치과임플란트나 의료장비로 사용될 만큼 인체에 무해하다고 알려져 있다. 응집제 사용에 따라 생성된 응집슬러지의 처리방안에 있어서 기존 응집제의 경우 생성된 슬러지의 대부분은 하수슬러지 위탁처리업체를 통해 소각 및 매립, 재활용 되고 있으나, $TiCl_4$를 응집제로 사용할 경우 생성된 슬러지를 인발하여 건조 및 소성을 통해 이산화티타늄으로 재활용할 수 있어 슬러지를 친환경적으로 처리가 가능해 기존 슬러지 처리방안의 경제적, 환경적 부담을 줄일 수 있는 장점이 있다. 따라서 본 연구에서는 $TiCl_4$를 하수처리장 방류수에 주입하여 수중의 총인(T-P)을 처리한 후 생성된 슬러지를 인발하여 건조와 소성과정을 거쳐 이산화티타늄을 제조하였다. 방류수를 취수해 2.5mg/L의 초기 총인 농도를 가진 원수를 제조하였으며 제조된 원수에 $TiCl_4$를 0.6mL 주입하였을 때 99.93%의 총인제거효율을 얻을 수 있었다. 응집 실험 후 생성된 슬러지를 인발하여 건조 후 $300{\sim}1000^{\circ}C$의 각각 다른 온도조건에서 소성하여 이산화티타늄을 제조하였으며, SEM과 XRD를 통해 제조된 이산화티타늄의 표면특성과 결정성 분석을 실시하였다. 제조된 이산화티타늄은 $500{\sim}800^{\circ}C$에서는 아나타제, $900{\sim}1000^{\circ}C$에서는 루타일 결정구조가 나타났다. 또한, $TiCl_4$ 주입량에 따른 이산화티타늄의 최종 생산량과 제조 시 사용되는 건조로 및 소성로의 경제적 비용 등을 고려하여 이산화티타늄 1Ton을 제조하기 위해 필요한 단가를 산출하였다. 본 연구에서 제조된 이산화티타늄 1kg의 생산단가는 약 5,400원으로 나타났으며, 가장 많이 사용되는 P-25 광촉매 보다 저렴한 가격으로 제조 및 판매를 기대할 수 있다. 따라서 하수처리장에 적용 시 기존 응집제 보다 비싼 $TiCl_4$ 비용을 보완하고 친환경적인 슬러지 처리로 제조된 이산화티타늄의 유통 및 현장적용을 통해 경제적, 환경적으로 우수하다고 판단된다.

• 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 $1000^{\circ}C$.

• Journal of the Korean Chemical Society
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• v.4 no.1
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• pp.58-61
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• 1957

The organic titanium compounds, $Ti(OR)_4\;and\;Cl_2Ti(OR)_2$ were prepared by adding theoretical amounts of $TiCl_4$ to ROH in the medium of $CCl_4$. Among the compounds of the above two types, the former $Ti(OR)_4$was polymerized by refluxing them with R·OH and water at ordinary temperature and the latter, $Cl_2Ti(OR)_2$, by adding water to them.

• Journal of the Semiconductor & Display Technology
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• v.10 no.1
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• pp.95-99
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• 2011

$(1-x)BaTiO_3+(x)Cd_5(PO_4)_3Cl$ ceramics were prepared by the conventional ceramic technique, i.e., solid state reaction at high temperature. The concentration of $Cd_5(PO_4)_3C$ was varied from 0.01 to 0.15 mole fraction. In order to study the phase transitions of our ceramics, the Raman scattering spectra were measured as functions of concentration x and temperature. It was found that the soluble limit of $Cd_5(PO_4)_3Cl$ in $BaTiO_3$ was the x=0.05 composition and $BaTiO_3$ phase disappeared above x=0.10. A new phase identified as $Ba_4Ti_3P_2O_{15}$ was detected in all samples of our compositions. The Curie temperature shifts up to $130^{\circ}C$ as the concentration x increases from zero to 0.05 and shift down to $95^{\circ}C$ as further increases to 0.08. For the increase of the Curie temperature, it is suggested that it can result from the inhibition of displacement of $Ti^{4+}$ in the distorted octahedron due to well dispersed $Ba_4Ti_3P_2O_{15}$ and $Cd_5(PO_4)_3Cl$ phase.

• 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.

• Journal of the Korean Ceramic Society
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• v.29 no.7
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• pp.525-532
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• 1992

TiO2 fine powder was synthesized in the gas phase by chemical vapor deposition using hydrolysis of TiCl4. Content of rutile phase in the powder was investigated. Powder characteristics such as size, crystallinity and morphology were also studied by means of TEM, SEM and XRD. Rutile phase in TiO2 powder started to be formed from 100$0^{\circ}C$ and the content increased with the reaction temperature and TiCl4 concentration. As the temperature increased from 80$0^{\circ}C$ to 140$0^{\circ}C$, the primary particle size increased while secondary particle size decreased. Spherical secondary particle with fine primary crystals agglomerated was produced at low temperature of 80$0^{\circ}C$ whereas the grown primary particle being final particle size was produced at higher temperature of 140$0^{\circ}C$. Other effects of TiCl4 and H2O partial pressures on particle size were also reported in this study.

• Journal of the Korean Institute of Telematics and Electronics D
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• v.36D no.4
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• pp.56-62
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• 1999

In this study, (Ba, Sr)$TiO_3$ thin films were etched with $Cl_2$/Ar gas mixing ratio in an inductively coupled plasma (ICP) by varying the etching parameter such as rf power, dc bias voltage, and chamber pressure. The etch rate was 56 nm/min under $Cl_2$/($Cl_2$+Ar) gas mixing ratio of 0.2, rf power of 600 W, dc bias voltage of 250 V, and chamber pressure of 5 mTorr. At this time, the selectivity of BST to Pt, $SiO_2$ was respectively 0.52, 0.43. The surface reaction of the etched (Ba, Sr)$TiO_3$ thin films was investigated with X-ray photoelectron spectroscopy (XPS). Ba is removed by chemical reaction between Sr and Cl to remove Sr. Ti is removed by chemical reaction such as $TiCl_4$ with ease. The results of secondary ion mass spectrometer (SIMS) analysis compared with the results of XPS analysis and the results were the same.

• Korean Journal of Materials Research
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• v.12 no.5
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• pp.391-397
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• 2002

Synthesis and process development of nano-size Ti powder by SFE(Sodium/halide Flame Encapsulation) method were investigated. Four concentric coflow burner was used and its flame configuration was $TiCl_4/Ar/Na/Ar$ in order from the center. Flame has been controlled by the various processing parameters such as temperature of burner and flow rates of both $TiCl_4$(g) precursor and Na(g). It was found that yellow-colored flame was shown in the flow rates of 70cc/min of $TiCl_4$(g) precursor and 2 $\ell$ /min of Na(g) which were regarded as optimum flame condition. The powders encapsuled by NaCl were produced having the average powder size of 250nm. The results of X-ray diffraction showed that powders from the optimized condition consisted of pure Ti and NaCl. TEM analysis confirmed that the several Ti powders of 20-100nm were encapsulated with NaCl. After removing sodium chloride by heat treatment, the spherical Ti powders with the size range of 80 to 150nm were obtained.

• Korean Journal of Materials Research
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• v.25 no.1
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• pp.43-47
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• 2015

$Zn(BH_4)_2$ was prepared by milling $ZnCl_2$ and $NaBH_4$ in a planetary ball mill in an Ar atmosphere, and XRD analysis, SEM observation, FT-IR analysis, DTA, and TGA were performed for synthesized $Zn(BH_4)_2$ samples. 90 wt% $MgH_2$+1.67 wt% $Zn(BH_4)_2(+NaCl)$+5 wt% Ni+1.67 wt% Ti+1.67 wt% Fe (named $90MgH_2+1.67Zn(BH_4)_2(+NaCl)$+5Ni+1.67Ti+1.67Fe) samples were also prepared by milling in a planetary ball mill in an $H_2$ atmosphere. The gas absorption and release properties of the $Zn(BH_4)_2(+NaCl)$ and $90MgH_2+1.67Zn(BH_4)_2(+NaCl)_2(+NaCl)$+5Ni+1.67Ti+1.67Fe samples were investigated. An FT-IR analysis showed that $Zn(BH_4)_2$ formed in the $Zn(BH_4)_2(+NaCl)$ samples prepared by milling $ZnCl_2$ and $NaBH_4$. At the first cycle at $320^{\circ}C$, $90MgH_2+1.67Zn(BH_4)_2(+NaCl)$+5Ni+1.67Ti+1.67Fe absorbed 2.95 wt% H for 2.5 min and 4.93 wt% H for 60 min under 12 bar $H_2$, and released 1.46 wt% H for 10 min and 4.57 wt% H for 60 min under 1.0 bar $H_2$.