• Journal of Powder Materials
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• v.23 no.5
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• pp.353-357
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• 2016

In this study, $TiO_2$ powders are synthesized from ammonium hexafluoride titanate (AHFT, $(NH_4)_2TiF_6$) as a precursor by heat treatment. First, we evaluate the physical properties of AHFT using X-ray diffraction (XRD), particle size analysis (PSA), thermogravimetric analysis (TGA), and field-emission scanning electron microscopy (FE-SEM). Then, to prepare the $TiO_2$ powders, is heat-treated at $300-1300^{\circ}C$ for 1 h. The ratio of anatase to rutile phase in $TiO_2$ is estimated by XRD. The anatase phase forms at $500^{\circ}C$ and phase transformation to the rutile phase occurs at $1200^{\circ}C$. Increase in the particle size is observed upon increasing the reaction temperature, and the phase ratio of the rutile phase is determined from a comparison with the calculated XRD data. Thus, we show that anatase and rutile $TiO_2$ powders could be synthesized using AHFT as a raw material, and the obtained data are utilized for developing a new process for producing high-quality $TiO_2$ powder.

• Journal of the Korean Ceramic Society
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• v.37 no.4
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• pp.308-313
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• 2000

Hydrous titanium oxide particles with anatase phase were prepared from 0.05 mol TiCl4 solution using NH4HCO3 as precipitant by the droopping precipitant method. The sequential change of pH is completed by a sudden and steep increase in a pH value of the range of 6~7 to which the concentration of adsorbed OH- and H+ ions on TiO2 surface is equal. Rutile phase started precipitating with anatase phase as an increase of reaction temperature above 6$0^{\circ}C$ in aqueous 0.05mol TiCl4 solution and its specific surface area was found to decrease from 452 $m^2$/g($25^{\circ}C$) to 164$m^2$/g(8$0^{\circ}C$). Specific surface area decreased rapidly when anatase powders precipitated at 4$0^{\circ}C$ were heat-treated at temperature higher 40$0^{\circ}C$. FT-IR result confirmed that it was due to the decrease of OH species within hydrous titanium oxides. The loss of ethanol after illumination of the powder heated at $600^{\circ}C$ and $700^{\circ}C$ for 4 h was 66 and 68.8%, respectively.

• Journal of the Korean Ceramic Society
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• v.41 no.6
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• pp.471-475
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• 2004

TiO$_2$, SiO$_2$, and PBA(Pseudo Boehemite Alumina) sol were prepared by sol-gel process. The particle sizes of these sol exhibited uniform 10∼30 nm. As the amount of SiO$_2$ sol increased, the temperature of phase transition (from anatase phase to rutile phase) was raised temperature than $600^{\circ}C$, which attributed to the enhanced photocatalyst properties. Also, the anatase phase was obtained with very small amount of the rutile phase from the addition of SiO$_2$ (10∼30 wt%) at annealing temperature of 120$0^{\circ}C$. The specimen with 20 wt% SiO$_2$ sol exhibited the maximum photocatalyst properties. But, the specimen with PBA sol did not affect photocatalytic activity due to the presence of rutile phase.

• Journal of the Mineralogical Society of Korea
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• v.25 no.2
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• pp.77-84
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• 2012

Anatase, one of the $TiO_2$ polymorphs, is known to show different phase transition paths depending on its crystalline and shape. Particle size of 15~25 nm anatase has been subjected to high-pressure Raman spectroscopy and X-ray diffraction studies using a diamond anvil cell. We observe that the starting sample transforms to an amorphous phase above approx. 20 GPa, which is retained upon pressure release to ambient condition. This is in contrast to previously established transition to baddeleyite phase and we suspect difference in the particle distribution state trigger phase instability of nanoparticles and hence amorphization.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.11a
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• pp.32-32
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• 2003

최근 환경오염에 대한 문제가 심각해지면서 인체에 유해한 유기물질의 분해에 대한 관심이 높아지고 있으며 따라서 뛰어난 광촉매 특성을 보이는 타이태니아(TiO$_2$)에 대한 많은 연구가 수행되고있다. 타이태니아가 보이는 결정상 중에는 brookite, anatse, rutile이 있는데 이 중에서 anatse 상이 가장 우수한 광촉매 특성을 나타내는 것으로 알려져 있다. 그러나 anatse 상을 얻기 위해서는 $600^{\circ}C$ 이상의 온도로 열처리를 해야 한다는 문제점이 있으며 광촉매 특성을 향상시키기 위해서는 anantase 나노결정을 제조하여 표면적을 극대화시 키는 것이 요구되고 있다. 본 연구에서는 이러 한 두 가지 문제점을 해결하기 위하여 Polyethylen oxide(PEO)-TiO$_2$ 나노하이브리드를 Sol-Gel공정을 이용하여 합성하였으며 이들에 대한 hot-water treatment를 통하여 10$0^{\circ}C$ 이하의 저온에서 anatase 나노결정상의 분말을 합성하는데 성공하였다. 이는 SiO$_2$-TiO$_2$계 하이브리드에서만 hot-water treatment를 통하여 anatase로 결정화가 가능하다는 기존의 연구결과와 상반되는 결과로서 무기질 성분으로서 TiO$_2$만 존재하는 하이브리드에 대한 hoi-water treatment를 통하여 anatase결정상이 형성될 수 있었다.

• Korean Journal of Materials Research
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• v.6 no.8
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• pp.852-857
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• 1996

Crystallization characteristics of titanium oxide thin film during post-annealing of reactive sputter deposition were studied. Amorphous phases of as-deposited films were crystallized into rutile after annealing at $900^{\circ}C$ and anatase at $500^{\circ}C$, respectively when $O_2$ concentration during sputtering was more than 15%. However, rutile was the only phase obtainable after annealing if %$O_2$ was less than 10%. For these films, Magneli phase($Ti_nO_{2n-1}$) were crystallized below $500^{\circ}C$ at first place due to slow oxidation of nonstoichiometric films but $500^{\circ}{\sim}600^{\circ}C$ anatase with nonstoichiometry was crystallized for a short period. It was, therefore, concluded that crystal growth can proceed without phase transition if stoichiometric phase is formed at the first stage of crystallization, and that rutile, the most stable phase, was resulted from any oxygen deficient nonstoichiometric films.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.08a
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• pp.353-353
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• 2011

Titanium dioxide is a suitable material for industrial use at present and in the future because titanium dioxide has efficient photoactivity, good stability and low cost [1]. Among the three phases (anatase, rutile, brookite) of titanium dioxide, the anatase form is particularly photocatalytically active under ultraviolet (UV) light. In fabrication of photocatalytic devices based on catalytic nanodiodes [2], it is challenging to obtain a photocatalytically active TiO2 thin film that can be prepared at low temperature (< 200$^{\circ}C$). Here, we present the synthesis of a titanium dioxide film using TiO2 nanoparticles and sol-gel methods. Titanium tetra-isopropoxide was used as the precursor and alcohol as the solvent. Titanium dioxide thin films were made using spin coating. The change of atomic structure was monitored after heating the thin film at 200$^{\circ}C$ and at 350$^{\circ}C$. The prepared samples have been characterized by X-ray diffraction (XRD), scanning electron microcopy, X-ray photoelectron spectroscopy, transmission electron microscopy, ultraviolet-visible spectroscopy (UV-vis), and ellipsometry. XRD spectra show an anatase phase at low temperature, 200$^{\circ}C$. UV-vis confirms the anatase phase band gap energy (3.2 eV) when using the photocatalyst. TEM images reveal crystallization of the titanium dioxide at 200$^{\circ}C$. We will discuss the switching behavior of the Pt /sol-gel TiO2 /Pt layers that can be a new type of resistive random-access memory.

• Solar Energy
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• v.12 no.3
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• pp.10-20
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• 1992

In this experiment, photochemical reaction has been applied to destroy TCE in water phase. The main target of this work is to investigate the technical feasibility of large scale of solar detoxification reactor for water treatment. The results have revealed that solar detoxification utilizing photon energy from the sun is the most attractive process to decompose organic toxins in water phase at room temperature. The detailed results from this work are as follows; (1) The highest conversion ratio of TCE was obtained by using $TiO_2$, annatase as a photocatalyst among $TiO_2$ anatase, $TiO_2$ rutile and $V_2O_5$ under the same experimental condition. The anatase crystal structure was confirmed with XRD analysis, and its surface area was 7.748 $m^2/g$ from the BET-$N_2$ measurement (2) 0.1 wt% of $TiO_2$ anatase has been adopted as optimal quantity for batch slurry reactor at this experimental conditions. (3) The effect of hydrogen peroxide on the conversion of TCE was investigated. Its optimal quantity was 0.06 vol. % under this experimental conditions. (4) The effect of oxygen on the conversion of TCE also was studied by controlling the head space in photoreactor. Results indicated that sufficient amount of oxygen should be supplied to accomplish the highest conversion rate of TCE in water phase.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2012.05a
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• pp.257-257
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• 2012

Cerium doped anatase titania powders were prepared by sol-gel process, with ammonium (IV) nitrate and Titanium (IV) butoxide as the raw materials. The characteristics of anatase $TiO_2$ and cerium doped $TiO_2$ were investigated by XRD, DTA, FE-SEM and UV/Vis spectroscopy. Research results indicated that XRD data characteristic diffraction peaks of anatase phase and also showed that cerium phase was not observed. Moreover XRD and DTA results imply that the addition of cerium to titania modifies the mechanism of formation of the titania phases.

• Korean Journal of Materials Research
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• v.8 no.3
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• pp.224-228
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• 1998

Phase transition kinetics of nonstoichiometric amorphous titanium oxide thin films deposited by reactive sputtering was investigated after cooling down with various rate followed by l0min.-3hrs. annealing at $500^{\circ}C$~$600^{\circ}C$ After short duration and fast cooling. Magneli was the only crystalline phase because the oxidation rates of $TiO_{2-x}$, could be relatively slower than that of crystallization. When the films were cooled slowly between $500^{\circ}C$~$300{\circ}C$, Magneli was transformed into an anatase and stabilized, but directly into a rutile under fast cooling. Because the rutile also prevailed after cooling from $600^{\circ}C$, it was concluded that the rutile phase could be formed directly from Magneli as well as converted from the anatase. Changes in volume and surface morphology were observed related to crystallization and oxidation processduring heat treatment.