• Journal of the Korean Chemical Society
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• v.59 no.3
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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.

• Journal of the Korean Ceramic Society
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• v.36 no.9
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• pp.901-908
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• 1999

Effects of LPMOCVD process parameters on the properties of TiO2 thin film were investigated. Depositions were made in the range of temperature 300-67$0^{\circ}C$ with various TTIP(Titanium Tetraisopropoxide) concentrations by contrlling bubbler temperature(40-8$0^{\circ}C$) and/or flow rate(30-90 sccm). Post annealing treatments were carried out at 500-80$0^{\circ}C$ range in the air. Films deposited at 40$0^{\circ}C$ have denser morphology than those of films deposited at 50$0^{\circ}C$ and $600^{\circ}C$ due to slower deposition rate. Bubbler temperature can affect on the deposition rate in mass transfer controlled regime such as 50$0^{\circ}C$ or higher but not below 50$0^{\circ}C$ where surface reaction rate becomes important. On the contrary for films deposited above 50$0^{\circ}C$ flow rate can raise deposition rate but eventually saturate it at the 50 sccm and above due to retarded adhesion of decomposed species. But for films deposited at 40$0^{\circ}C$ deposition rate increases stadily with flow rate. As the film becomes more porous A(200) texture can not be developed and AnataselongrightarrowRutile transition kinetics increases.

• Proceedings of the Korean Nuclear Society Conference
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• 1996.11a
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• pp.145-150
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• 1996

약 30$0^{\circ}C$, 160 kg/$cm^2$의 원자로냉각재계통에서 사용이 가능한 $^{60}$Co 제거용 고온흡착제를 얻기 위하여, ZrO$_2$를 zirconyl nitrate를 출발물질로 하여 졸-겔법으로, aluminum isopropoxide를 출발 물질로 하여 A1$_2$O$_3$를, aluminum isopropoxide와 titanium tetraisopropoxide를 출발물질로하여 TiO$_2$-A1$_2$O$_3$를, aluminum isopropoxide와 zirconium propoxide를 출발물질로 하여 ZrO$_2$-A1$_2$O$_3$를 금속알콕사이드 가수분해법으로 제조하였다. 제조한 흡착제는 600~140$0^{\circ}C$의 온도로 하소 하였으며, 결정전이, 열적특성, 비표면적 등의 물성변화를 알아보기 위하여 X선회절, 적외선분광분석, 열분석, 전자현미경 관찰, BET 비표면적 등을 측정하였다. 또한, 고온수에서 이들 흡착제의 Co$^{2＋}$ 흡착특성을 autoclave를 이용한 회분식 흡착실험으로 알아보았다. 이들 흡착제 제조시 하소온도에 따른 Co$^{2＋}$ 흡착량, $Al_2$O$_3$ 흡착제 제조시 pH 변화에 따른 Co$^{2＋}$ 흡착량과 TiO$_2$-A1$_2$O$_3$ 흡착제 제조시 TiO$_2$ 함량에 따른 Co$^{2＋}$ 흡착량과 25$0^{\circ}C$의 고온에서 ZrO$_2$와 $Al_2$O$_3$의 표면에 생성된 코발트 화합물을 XPS와 EPMA로 부터 확인하였다.

• Transactions of the Korean Society of Mechanical Engineers B
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• v.28 no.5
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• pp.501-509
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• 2004

Unipolar diffusion charging of non-spherical particles was investigated for various particle shapes. We researched with TiO$_2$agglomerates produced by the thermal decomposition of titanium tetraisopropoxide (TTIP) vapor. TTIP was converted into TiO$_2$, in the furnace reactor and was subsequently introduced into the sintering furnace. Increasing the temperature in the sintering furnace, aggregates were restructured into higher fractal dimensions. The aggregates were classified according to their mobility using a differential mobility analyzer. The projection area and the mass fractal dimension of particles were measured with an image processing technique performed by using transmission electron microscope (TEM) photograph. The selected aggregates were charged by the indirect photoelectric-charger and the average number of charges per particle was measured by an aerosol electrometer and a condensation particle counter. For the particles of same mobility diameter, our results showed that the particle charge quantity decreases as the sintering temperature increases. This result is understandable because particles with lower fractal dimension have larger capacitance and geometric surface area.

• Journal of Korean Society for Atmospheric Environment
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• v.20 no.3
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• pp.411-419
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• 2004

Titania particles are widely used as a photocatalyst to treat various contaminants in air and water. Titania particles were formed by vapor-phase oxidation of titanium tetraisopropoxide (TTIP) in a tube furnace between 773 and 1,273 K. The effect of process variables such as furnace temperature, flow rate of carrier air, and flow rate of sheath air on powder size and phase characteristics was investigated using a scanning mobility particle sizer (SMPS), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The size distribution of synthesized titania particles was characterized with mode diameter and peak concentration. The mode diameter ranging from 20 to 80 nm decreased with increasing flow rates of sheath air and carrier air, and increased with increasing furnace temperature. The peak concentration increased with increasing flow rates of sheath air and carrier air The best synthetic condition for high production rate can be derived from the experimental data set represented by mode diameter and peak concentration. The crystal structure of synthesized titania particles was found to be anatase phase, ensuring high photocatalytic potential.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.05b
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• pp.144-148
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• 2003

알루미나볼 위에 Titanium tetraisopropoxide(TTIP)를 원료로, 화학기상증착법으로 제조된 $TiO_{2}/Al_{2}O_{3}$ 볼을 이용하여 벤젠의 기상 광 분해 실험을 실시하였다. 기상분해 과정의 연속적 측정을 위하여 순환식의 반응장치를 자체 제작하였으며, PID(Photo Ionization Detector)방식의 VOCs meter를 이용하여 광조사에 의한 벤젠의 분해율을 실시간으로 측정하였다. 기상의 벤젠과 $TiO_2/Al_{2}O_{3}$ 볼의 원활한 흡착을 위해 30분간 암반응 시킨 후 광분해율을 측정한 결과 광조사에 의한 분말표면에 흡착된 VOCs의 탈착에 의한 초기 농도증가 현상이 공통적으로 측정되었으며, 흡착 면적이 작을수록 농도 증가 또한 낮게 측정되었다. 또한 최적조건을 기준으로 실시한 분해 실험 결과 60ppm이상의 고농도 영역에서는 VOCs의 분해가 비교적 느리게 진행되었지만, 60ppm이하의 저농도 영역에서는 급속한 VOCs의 분해가 측정되었다. 마찬가지로 반응 표면적이 넓을수록, 광원이 많을수록 그리고 광분해에 사용된 자외선 램프의 강도가 클수록 광반응에 의한 벤젠의 분해율이 증가하였다.

• Journal of Environmental Science International
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• v.19 no.5
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• pp.577-584
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• 2010

The generation of $TiO_2$ nanoparticles by a thermal decomposition of titanium tetraisopropoxide (TTIP) was carried out experimentally using a tubular electric furnace at various synthesis temperatures (700, 900, 1100 and $1300^{\circ}C$) and precursor heating temperatures (80, 95 and $110^{\circ}C$). Effects of degree of crystallinity, surface area and anatase mass fraction of those $TiO_2$ nanoparticles on photocatalytic properties such as decomposition of methylene blue was investigated. Results show that the primary particle diameter obtained from thermal decomposition of TTIP was considerably smaller than the commercial photocatalyst (Degussa, P25). Also, those specific surface areas were more than 134.4 $m^2$/g. Resultant $TiO_2$ nanoparticles showed improved photocatalytic activity compared with Deggusa P25. This is contributed to the higher degree of crystallinity, surface area and anatase mass fraction of $TiO_2$ nanoparticles compared with P25.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.100-100
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• 2010

Hydrophilic $TiO_2$ films were deposited on slide glasses using titanium tetraisopropoxide (TTIP) as a precursor by metal-organic chemical vapor deposition (MOCVD). The temperature of substrate was $400^{\circ}C$ and the temperatures of precursor were kept at $75^{\circ}C$ (sample A) and $60^{\circ}C$ (sample B) during the $TiO_2$ film growth. The deposited $TiO_2$ films were characterized by contact angle measurement and uv/vis spectroscopy. The result show that sample B has very low contact angle of almost zero due to superhydrophilic $TiO_2$ surface and transmittance is $76.85%{\pm}1.47%$ at the range of 400 - 700 nm. So, this condition is very optimal for hydrophilic $TiO_2$ film deposition. However, when the temperature of precursor is lower is lower than $50^{\circ}C$ or higher than $75^{\circ}C$, $TiO_2$ could not be deposited on the substrate and cloudy $TiO_2$ film was formed due to low precursor temperature and the increase of surface roughness, respectively.

• Transactions of the Korean Society of Mechanical Engineers B
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• v.25 no.9
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• pp.1175-1182
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• 2001

Chemical compositions of polydisperse SiO$_2$/TiO$_2$multicomponent aggregates were measured for different heights from the burner surface and different mobility diameters of aggregates. SiO$_2$/TiO$_2$multicomponent particles were generated in a hydrogen/oxygen coflow diffusion flame from two sets of precursors: TTIP(titanium tetraisopropoxide), TEOS(tetraethylorthosilicate). To maintain 1:1 mole ratio of TTIP:TEOS vapor, flow rate of carrier gas $N_2$was fixed at 0.6lpm for TTIP, at 0.1lpm for TEOS. In-situ sampling probe was used to supply particles into DMA(differential mobility analyzer) which was calibrated with using commercial DMA(TSI, model 3071A) and classifying monodisperse multicomponent particles. Classified monodisperse particles were collected with electrophoretic collector. The distributions of composition from particles to particle were determined using EDS(energy dispersive spectrometry) coupled with TEM(transmission electron microscope). The chemical(atomic) compositions of classified monodisperse particle were obtained for different heights; z=40mm, 60mm, 80mm. The results suggested that the chemical(atomic) composition of SiO$_2$decreased with the height from burner surface and the composition of SiO$_2$and TiO$_2$approached to the value of 1 to 1 fat downstream. It is also found that the composition of SiO$_2$decreases as the mobility diameter of aggregate increases.

• Proceedings of the KSME Conference
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• 2000.04b
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• pp.441-446
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• 2000

Chemical compositions of monodisperse $SiO_2/TiO_2$ multicomponent aggregates were measured for different heights from the burner surface and different mobility diameters of aggregates. $SiO_2/TiO_2$ multicomponent particles were generated in a hydrogen/oxygen coflow diffusion flame from two sets of precursors: TTIP (titanium tetraisopropoxide), TEOS(tetraethylorthosilicate). To maintain 1:1 mole ratio of TTIP:TEOS vapor theoretically, flow rate of carrier gas $N_2$ was fixed at 0.61pm for TTIP, at 0.11pm for TEOS. In situ sampling probe was used to supply particles into differential mobility analyzer(DMA) which was calibrated with using commercial DMA(TSI 3071A) and classifying monodisperse multicomponent particles. Classified particles were collected with electrophoretic collector. The distributions of composition from particle to particle were determined using EDS (energy dispersive spectrometry) coupled with TEM (transmission electron microscope). The chemical (atomic) compositions of classified monodisperse particle were obtained for different heights; z=40mm, 60mm, 80mm. The results suggested that the atomic composition of $SiO_2$ decreased with the height from burner surface and the composition of $SiO_2$ and $TiO_2$ approached to the value of 1 to 1 in far downstream. It is also found that the composition of $SiO_2$ decreases as the mobility diameter of aggregate increases.