• 한국세라믹학회지
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• 제41권6호
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• pp.471-475
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• 2004

졸겔 공정으로 안정한 TiO$_2$, SiO$_2$, PBA(Pseudo Boehemite Alumina) 졸을 제조하였다. 제조한 졸 용액은 비교적 균일한 10∼30nm의 입자크기를 나타내었다. TiO$_2$졸에 SiO$_2$졸의 첨가량이 증가함에 따라, anatase상에서 rutile 상으로 전이되는 상전이 온도를 $600^{\circ}C$ 이상으로 증가시켜 광분해 특성을 향상시켰다. 또한, TiO$_2$ 졸 용액에 SiO$_2$ 졸을 10∼30wt% 첨가하여 120$0^{\circ}C$ 이상의 고온 소성 후에도 anatase가 주된 상으로 소량의 rutile 상이 관찰되었다 또한 SiO$_2$20wt% 첨가 시, 최대의 광분해 특성을 나타내었다. 그러나, PBA 졸의 첨가는 첨가량에 관계없이 광분해 특성에 영향을 주지 않았다.

• 대한화학회지
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• 제59권3호
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• pp.238-245
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• 2015

The crystallization and morphology change of amorphous titanias by hydrothermal treatment have been investigated. The amorphous titanias were prepared by pure water hydrolysis of two different precursors, titanium tetraisopropoxide (TTIP) and TTIP modified with acetic acid (HOAc) and characterized prior to hydrothermal treatment. In order to avoid complicate situation, the hydrothermal treatment was performed in a single solvent water with and without strong acids at various temperatures. The effects of strong acid, temperature and time were systematically investigated on the transformation of amorphous titania to crystalline TiO₂ under simple hydrothermal condition. Without strong acid the titanias were transformed into only anatase phase nanoparticle regardless of precursor type, temperature and time herein used (up to 250 ℃ and 48 hours). The treatment temperature and time effected only on the crystalline size, not on the crystal phase et al. However, it was clearly revealed that the strong acids such as HNO₃ and HCl catalyzed the formation of rutile phase depending on temperature. HCl was slightly better than HNO₃ in this catalytic activity. The morphology of rutile TiO₂ formed was also a little affected by the type of acid. The precursor modifier, HOAc slightly reduced the catalytic activity of the strong acids in rutile phase formation.

• 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.

• 대한전기학회논문지:전기물성ㆍ응용부문C
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• 제55권7호
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• pp.349-353
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• 2006

[ $TiO_2-Nb_2O_5$ ] sol was prepared using sol-gel method. Crystalline properties of gel powder changed from rutile phase to anatase phase with increasing $Nb_2O_5$ additives at $800^{\circ}C$, while they retained rutile phase regardless of $Nb_2O_5$ additives at $900^{\circ}C,\;1,000^{\circ}C$. They retained amorphous phase from $50^{\circ}C\;to\;400^{\circ}C$, retained anatase phase from $500^{\circ}C\;to\;600^{\circ}C$ and had rutile phase over $700^{\circ}C$ at 1mole% $Nb_2O_5$ additive. After $TiO_2-Nb_2O_5$ sol retained low viscosity with normal chain structure for a long time, its viscosity increased fast with network structure. DTA properties of gel powder had endothermic reaction due to evaporation of propanol and water about $78^{\circ}C$, had exothermic reaction due to propanol combustion about $290^{\circ}C$ and had exothermic reaction due to changing of $TiO_2$ phase about $640^{\circ}C$.

• International Journal of Oral Biology
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• 제46권3호
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• pp.105-110
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• 2021

The physicochemical properties of crystalline titanium dioxide nanoparticles (TiO₂ NPs) were investigated by comparing amorphous (amTiO₂), anatase (aTiO₂), metaphase of anatase-rutile (arTiO₂), and rutile (rTiO₂) NPs, which were prepared at various calcination temperatures (100℃, 400℃, 600℃, and 900℃). X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses confirmed that the phase-transformed TiO₂ had the characteristic features of crystallinity and average size. The surface chemical properties of the crystalline phases were different in the spectral analysis. As anatase transformed to the rutile phase, the band of the hydroxyl group at 3,600-3,100 cm^-1 decreased gradually, as assessed using Fourier transform infrared spectroscopy (FT-IR). For ultraviolet-visible (UV-Vis) spectra, the maximum absorbance of anatase TiO₂ NPs at 309 nm was blue-shifted to 290 nm at the rutile phase with reduced absorbance. Under the electric field of capillary electrophoresis (CE), TiO₂ NPs in anatase migrated and detected as a broaden peak, whereas the rutile NPs did not. In addition, anatase showed the highest photocatalytic activity in an UV-irradiated dye degradation assay in the following order: aTiO₂ > arTiO₂ > rTiO₂. Overall, the phases of TiO₂ NPs showed characteristic physicochemical properties regarding size, surface chemical properties, UV absorbance, CE migration, and photocatalytic activity.

• 한국재료학회지
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• 제12권10호
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• pp.809-813
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• 2002

Commercial nano crystalline $TiO_2$ powders were used to characterize photocatalyst, using thermal spray coating technique. The microstructure of coating layers were examined by SEM, FE-SEM and TEM. Also the cross sectional areas of TiO$_2$ coating layers were observed by SEM. The phases were analyzed by X-ray diffraction methed. Surface roughness and hardness were measured. It was found that phase transformation from anatase to rutile occurred, and the melted splats are all rutile, and unmeted nano particles were anatase. These unmelted anatase phase may enhance te play a role of photocatalyst.

• 한국세라믹학회지
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• 제48권2호
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• pp.178-182
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• 2011

The Rutile - type brown pigments doped with chromium were synthesized. Samples of $Ti_{1-x}Cr_xO_2$ ($0.02{\leq}X{\leq}0.08$) were synthesized by the solid state method. Solid solution limit of Cr contents to the rutile structure and its coloration were studied. Optimum composition was investigated accordingly. The characteristics of synthesized pigments were analyzed by XRD, SEM, Raman spectroscopy and UV. As a result, single phase of Rutile was observed from $1000^{\circ}C$ by XRD. The maximum limit of solid solution was 0.06 mole $Cr_2O_3$. The glazed sample showed brown color, and the value of CIE $L^*a^*b^*$ was $L^*$ 33.27, $a^*$ 10.64, $b^*$ 20.84.

• 연구논문집
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• 통권33호
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• pp.123-135
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• 2003

Using the residence time calculated by computer simulation for temperature and gas velocity distribution in CVC reactor, the kinetics on the formation of $TiO_2$ nano powder was analyzed for coagulation process, After abrupt increase of particle size at initial growth stage (< 0.2 $\mus$ ), the particle grew in proportion of cubic root to time. The numerically calculated particle sizes well agreed with the experimental results. However, the coarse rutile $TiO_2$ powders having the particle size of over 40 nm were formed on the surface of quratz rod in the reactor. it is thought that the fine anatase particles condensed on quratz rod were sintered in a heated CVC reactor to grow and transform to coarse rutile phase, and the critical size for phase transformation anstase-to-rutile was around 25 nm tn this study.

• Korean Chemical Engineering Research
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• 제56권2호
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• pp.261-268
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• 2018

본 연구에서는 수열합성법과 주형합성법을 이용하여 메조포어를 지닌 $TiO_2$를 합성하였다. 수열합성법을 이용해서 anatase 구조의 메조포러스 $TiO_2$를 합성했다. Rutile 구조의 메조포러스 $TiO_2$를 제조하기 위해서 수열합성법으로 제조된 메조포러스 $TiO_2$를 $300^{\circ}C$부터 $700^{\circ}C$까지 소성시켰더니 $600^{\circ}C$부터 anatase에서 rutile 결정구조로 상전이가 일어났다. 하지만, 메조포어가 붕괴되었다. 메조포어을 지닌 $TiO_2$를 합성하기 위해서 메조포러스 실리카 KIT-6을 주형으로 사용하는 주형합성법을 사용하였다. 먼저 메조포어 내부에 $TiO_2$를 형성시키고 소성온도를 800, $900^{\circ}C$로 높여서 anatase에서 rutile로의 상전이 거동을 조사하였다. 수열합성을 통해 제조된 자유로운 상태의 메조포러스 $TiO_2$의 경우 $600^{\circ}C$에서 anatase에서 rutile로의 상전이가 일어났지만 제한된 공간인 메조포러스 기공 내부에 형성된 $TiO_2$의 경우 $800^{\circ}C$까지 가열하더라도 rutile구조로 상전이가 일어나지 않았고, $900^{\circ}C$로 소성시키자 일부의 anatase가 rutile로의 상전이가 일어나기 시작하였다. 이러한 상전이는 산소 빈자리의 형성에 의해서 일어나야 한다고 알려져 있지만 실리카 기공 내부에 형성된 $TiO_2$는 실리카 기공 표면이 산소 빈자리 형성을 방해해서 상전이가 억제되는 것으로 판단된다. $900^{\circ}C$의 높은 소성온도로 인해서 anatase와 rutile 구조가 섞여있으며 실리카 기공 내부에 형성된 $TiO_2$는 NaOH 수용액을 이용해서 주형인 KIT-6과 분리해서 메조포어를 지닌 $TiO_2$를 제조하였다.

• 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.