• Korean Journal of Materials Research
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• v.28 no.5
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• pp.261-267
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• 2018

Hydrothermal synthesis of highly crystalline $TiO_2$ nanorods is a well-developed technique and the nanorods have been widely used as the template for growth of various core-shell nanorod structures. Magneli/CdS core-shell nanorod structures are fabricated for the photoelectrochemical cell (PEC) electrode to achieve enhanced carrier transport along the metallic magneli phase nanorod template. However, the long and thin $TiO_2$ nanorods may form a high resistance path to the electrons transferred from the CdS layer. $TiO_2$ nanorods synthesized are reduced to magneli phases, $TixO_{2x-1}$, by heat treatment in a hydrogen environment. Two types of magneli phase nanorods of $Ti_4O_7$ and $Ti_3O_5$ are synthesized. Structural morphology and X-ray diffraction analyses are carried out. CdS nano-films are deposited on the magneli nanorods for the main light absorption layer to form a photoanode, and the PEC performance is measured under simulated sunlight irradiation and compared with the conventional $TiO_2/CdS$ core-shell nanorod electrode. A higher photocurrent is observed from the stand-alone $Ti_3O_5/CdS$ core-shell nanorod structure in which the nanorods are grown on both sides of the seed layer.

• Journal of the Korean institute of surface engineering
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• v.25 no.6
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• pp.293-298
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• 1992

Various vanadium-oxide thin films were deposited by e-beam and thermal evaporation of V2O5, V2O3, and VO2 powders. Films with thickness of $2000\AA$ were subjected to annealing at $300^{\circ}C$~$450^{\circ}C$ in N2 atmosphere for the crystallization and desification purposes. For the films deposited from V2O5 and VO2 sources, sources, Magneli (VnO2n-1$ 4\leq$ $n\leq$ 8) and VO2 phase appeared at $300^{\circ}C$, respectively, but VO2 phase also transformed into Magneli phase at $450^{\circ}C$ by severe reduction. On the contrary, VO2/VO mixed phases resulted from congruent evaporation of V2O3 unchanged after the same annealing treatment due to the balanced reduction and oxidation of VO2 and VO whcih have different equilibrium O2 pressures. It is suggested that the annealing in the controlled oxidation atmosphere or the deposition using mixed oxide sources are necessary to get the film containing VO2 phase.

• 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.

• 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 Magnestics Society Conference
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• 2003.12a
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• pp.330-330
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• 2003

• Korean Journal of Materials Research
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• v.9 no.1
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• pp.57-64
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• 1999

The electrical conductivity of TiO$_2$ doped with 0.05~1.5mol% WO$_3$ was measured in the oxygen partial pressure range of 10\ulcorner~10\ulcorner atm and temperature range of 1100~130$0^{\circ}C$ to investigate the defect types and the electrical properties. The grain size and density were increased as the liquid phase was formed by the doped WO$_3$. The secondary phase and WO$_3$peaks at the sample doped up to 4.0 mol% were not detected from the XRD results. The data(log$\sigma$/logPo$_2$) over 110$0^{\circ}C$ were divided into the four regions. From these experimental results, we proposed the following defect regions. 1) Magneli phase(extended defect), 2) Reduced rutile region which is similar to the behavior of undoped rutile, 3) Nearly stoichiometric Ti\ulcornerW\ulcornerO$_2$region in which extra charge of W\ulcorner cation is expected to be compensated by an electron, 4) Overstoichiometric Ti\ulcornerW\ulcornerO\ulcorner region which is a metal deficiency not to be observed in pure TiO$_2$. The electrical conductivity of w-doped TiO$_2$ was influenced by the measuring temperature, oxygen partial pressure, and the dopig content.

• Proceedings of the Korea Society for Energy Engineering kosee Conference
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• 1994.05a
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• pp.121-125
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• 1994

전극물질 및 전극촉매로서의 세라믹물질의 중요성은 상당히 크다. magneli phase를 갖는 $Ti_4O_{7}$과 rock salt구조를 갖는 TiO등의 티타늄 아산화물들은 전도성 세라믹으로서 전기전도도는 탄소보다도 좋으며, 높은 산화전위에서도 산화되지 않을 뿐만아니라, 강산용액에서도 내식성이 강하여 $SO_2$나 $O_2$의 산화전극 물질로 사용할 수 있다. $SO_2$나 $O_2$의 산화에 뛰어난 활동도를 보이는 촉매인 Pt나 Ru를 전기화학적으로 $Ti_4O_{7}$이나 TiO에 입혀서 그 전기화학적인 특성을 조사하였다.

• Journal of the Korean Ceramic Society
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• v.36 no.12
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• pp.1335-1341
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• 1999

The electrical conductivity ($\sigma$) of TiO2 doped with 0.05-4.0mol% Nb2O5 was measured in the oxygen partial pressure range of 10-17 to 100 atm and temperature range of 1100 to 130$0^{\circ}C$ to investigate the electrical properties and defect types. The oxygen partial pressure dependence of the electrical conductivity (log$\sigma$/logPo2) above 110$0^{\circ}C$ was divided into the four regions. From these experimental results the following defect regions were proposed ; 1) Magneli phase(extended defect) 2) reduced rutile region where intrinsic defect predominates 3) nearly stoichiometric region which is independent on the oxygen partical pressure and 4) overstoichiometric region which is not observed in pure TiO2 The electrical conductivity of Nb-doped TiO2 depended on the doping content the oxygen partial pressure and the measuring tem-perature.

• Journal of Powder Materials
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• v.11 no.1
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• pp.28-33
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• 2004

In the present study, the focus is on the analysis of carbothermal reduction of the titanium-cobalt-oxygen based oxide powder by solid carbon for the optimizing synthesis process of ultra fined TiC/Co composite powder. The titanium-cobalt-oxygen based oxide powder was prepared by the combination of the spray drying and desalting processes using the titanium dioxide powder and cobalt nitrate as the raw materials. The titanium-cobalt-oxygen based oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under a flowing argon atmosphere. The changes in the phase structure and thermal gravity of the mixture during carbothermal reduction were analysed using XRD and TGA. The synthesized titanium-cobalt-oxygen based oxide powder has a mixture of $TiO_2$ and $CoTiO_3$. This oxide powder was transformed to a mixed state of titanium car-bide and cobalt by solid carbon through four steps of carbothermal reduction steps with increasing temperature; reduction of $CoTiO_3$ to $TiO_2$ and Co, reduction of $TiO_2$, to the magneli phase($Ti_nO_{2n-1}$, n>3), reduction of the mag-neli phase($Ti_nO_{2n-1}$, n>3) to the $Ti_nO_{2n-1}$(2$\leq$n$\leq$3) phases, and reduction and carburization of the $Ti_nO_{2n-1}$(2$\leq$n$\leq$3) phases to titanium carbide.

• Journal of the Korean Ceramic Society
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• v.36 no.2
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• pp.167-171
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• 1999

Titanium dioxide bodies sintered at 130$0^{\circ}C$ for 10 h under the oxygen flowing were reduced with hydrogen in 1200, 1250 and 130$0^{\circ}C$ for 4~20 h. Reduction kinetics were evaluated by measuring a weight loss between before and after reduction, and the thickness of reduced layer, respectively. The reduction followed the parabolic rate law, indicating that the rate-determining process is diffusion. From the Arrhenius plots, the apparent activation energies for the reduction were obtained as 210$\pm$10 kJ/mol.