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

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

• Korean Chemical Engineering Research
• /
• v.56 no.2
• /
• pp.261-268
• /
• 2018

To prepare mesoporous $TiO_2$ ($meso-TiO_2$) with anatase and rutile crystal structures, hydrothermal and template synthesis were used. $Meso-TiO_2$ with anatase structure was obtained by hydrothermal synthesis. The crystal structure of $meso-TiO_2$ by hydrothermal synthesis converted from anatase to rutile by simple heating at $600^{\circ}C$ and above. However, their mesopore structure collapsed due to phase transition. To prepare $meso-TiO_2$ with rutile structure, template synthesis method was applied using mesoporous silica KIT-6 as a template. Once we incorporated anatase $TiO_2$ inside mesopores of silica, the phase transition temperature of $TiO_2$ confined inside KIT-6 was much higher ($900^{\circ}C$) than that of free-standing $TiO_2$ ($600^{\circ}C$). The suppression of $TiO_2$ phase transition inside mesopores of KIT-6 is closely related with the interaction between $TiO_2$ surface and silica walls in KIT-6 because oxygen vacancy in $TiO_2$ is regarded as the starting point for phase transition. After removal of silica template by NaOH solution washing, $meso-TiO_2$ with mixed phase between anatase and rutile was obtained.

• Journal of the Korean Ceramic Society
• /
• v.41 no.6
• /
• pp.471-475
• /
• 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 Korean Ceramic Society
• /
• v.37 no.5
• /
• pp.473-478
• /
• 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.

• Journal of the Korean Chemical Society
• /
• v.59 no.3
• /
• pp.238-245
• /
• 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 Powder Materials
• /
• v.26 no.6
• /
• pp.487-492
• /
• 2019

Titanium dioxide (TiO₂) is a typical inorganic material that has an excellent photocatalytic property and a high refractive index. It is used in water/air purifiers, solar cells, white pigments, refractory materials, semiconductors, etc.; its demand is continuously increasing. In this study, anatase and rutile phase titanium dioxide is prepared using hydroxyl and carboxyl; the titanium complex and its mechanism are investigated. As a result of analyzing the phase transition characteristics by a heat treatment temperature using a titanium complex having a hydroxyl group and a carboxyl group, it is confirmed that the material properties were different from each other and that the anatase and rutile phase contents can be controlled. The titanium complexes prepared in this study show different characteristics from the titania-formation temperatures of the known anatase and rutile phases. It is inferred that this is due to the change of electrostatic adsorption behavior due to the complexing function of the oxygen sharing point, which crystals of the TiO₆ structure share.

• Journal of the Korean Society for Heat Treatment
• /
• v.6 no.4
• /
• pp.204-212
• /
• 1993

The preparation of $TiO_2$ fine particles from $TiCl_4$ and oxygen by the vapor-phasereaction was investigated at $850^{\circ}C$ with an emphasis on the effect of its experimental conditions on the crystal type of the products. Anatase $TiO_2$ particles prepared by experiment were used to study anatase-rutile transition by calcination temperature, the additives and gas atmosphere. The results were as follows. The kinetics of anatase-rutile transition was well agreed with A vrami equation, and the activation energy of transition was 35kcal/mol. The addition of CuO in anatase $TiO_2$ particles accelerated the anatase-rutile transition, and its transition was retarded in vaccum.

• The Transactions of the Korean Institute of Electrical Engineers C
• /
• v.55 no.7
• /
• pp.349-353
• /
• 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 $640^{\circ}C$.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.2
• /
• pp.402-404
• /
• 2009

The band structures and the densities of states at the Fermi energy for rutile, anatase and brookite phases are investigated along with the structure-photocatlaytic relationship by using DFT method. Bands are less dispersive in anatase phase than in rutile phase, and they are almost flat in brookite phase. As a result, the DOS value near the Fermi energy for brookite is highest among three types of $TiO_{2}$, which means that the numbers of electrons near the Fermi energy are largest in brookite. The calculation shows that brookite phase may exhibit highest photocatalytic efficiency among three types of $TiO_{2}$.