• Journal of the Korean Ceramic Society
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• v.25 no.4
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• pp.408-414
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• 1988

This thesis is 2nd thesis from "Mechanism of Intercalation Compounds in Graphite with Hydrogen sulfate(J. Korea Cer. Soc. Vol. 22. No.6, 1985). We have oxidized natural Graphite flakes(0.1~0.2mm., Kropfm hl passau in Deutchland. S40) with a solution of CrO3 in H2SO4. Whilst persulfate ions were intercalated, too, below 7$^{\circ}C$, no evidence for intercalation of a peroxo compound was found at 22$^{\circ}C$. The reaction was interrupted after various times by filtering and washing with concentrated H2SO4. X-ray diffraction showed that the 2nd stage compound had already been formed after 2 minutes. We could only follow further oxidation to the blue stage compound which was completed after 35 minutes. We have found six distinct intermediate stage between 2nd stage and 1 stage. Experiments are described on the formation of intermediate stage color and X-ray diffraction analysis.ysis.

• Applied Chemistry for Engineering
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• v.7 no.6
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• pp.1078-1086
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• 1996

The peroxo-polytungstic acid was formed by the direct reaction of tungsten powder with the hydrogen peroxide solution. Peroxo-polytungstic powder were prepared by rotary evaporator using the fabricated on to ITO coated glass as substrate by dip-coating method using $2g/10mL(W-IPA/H_2O)$ sol solution. A substrate was dipped into the sol solution and after a meniscus had settled, the substrate was withdrawn at a constant rate of the 3mm/sec. Thicker layer could be built up by repeated dipping/post-treatment 15 times cycles. The layers dried at the temperature of $65{\sim}70^{\circ}C$ during the withdrawn process, and then tungsten oxides thin film was formed by final heating treatment at the temperature of $230{\sim}240^{\circ}C$ for 30min. A linear rotation between the thickness of thin film and the number of dipping/post-treatment cycles for tungsten oxides thin films made by dip-coating was found. The thickness of thin film had $60{\AA}$ after one dipping. From the patterns of XRD, the structure of tungsten oxides thin film identified as amorphous one and from the photographs of SEM, the defects and the moderate cracks were observed on the tungsten oxides thin film, but the homogeneous surface of thin films were mostly appeared. The electrochemical characteristic of the $ITO/WO_3$ thin film electrode were confirmed by the cyclic voltammetry and the cathodic Tafel polaization method. The coloring bleaching processes were clearly repeated up to several hundreds cycles by multiple cyclic voltammetry, but the dissolved phenomenon of thin film revealed in $H_2SO_4$ solution was observed due to the decrease of the current densities. The diffusion coefficient was calculated from irreversible Randles-Sevick equation from the data obtained by the cyclic voltammetry with various scan rates.

• Journal of Korean Society of Environmental Engineers
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• v.22 no.4
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• pp.765-773
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• 2000

The degradation of humic acid using $TiO_2$ coatings was studied, $TiO_2$ coatings were prepared by dip-coating method. Sol solutions for coating were prepared by mixing the gel, which can be produced by the reaction of $TiOCl_2$ and $NH_4OH$ solution, and hydrogen peroxide solution, and hydrolysis of titanium tetraisopropoxide (TTIP). It was shown from XRD that coatings from sol aged at $100^{\circ}C$ for 18h with titanium peroxo solution were crystallized to anatase in the range of temperatures of $25^{\circ}C$ to $500^{\circ}C$. In contrast, those coated from TTIP were crystallized to anatase at temperature above $400^{\circ}C$. So the sols originated from $TiCl_4$ can be applied for not only on the heat-resistance substrates but on the plastic substrates. Thickness and the quality of the films were dependent on the withdrawing speed, the concentration of sol, and the number of coating. The films showed various interference colors depending on the thickness of them. In the case that the films coated 2 times at withdrawing speed of 2.5cm per minute by 0.2M sol, the films had a transparent light blue color with thickness of around 50nm. It was known from the result of photo-degradation by $TiO_2$ coatings using humic acid that the removal efficiency of $COD_{cr}$ was over 85% after illumination of $UV/H_2O_2$ for 40min. and that of UV/VIS absorbable materials was over 95%.

• Applied Chemistry for Engineering
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• v.21 no.4
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• pp.435-439
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• 2010

Pt-$MoO_3$ electrodes were fabricated on ITO-coated glass by electrodeposition method using 20 mM hydrogen hexachloroplatinate ($H_2PtCl_6$) and 10 mM Mo-peroxo electrolyte. Deposition order was varied, and catalytic activities of synthesized electrodes were compared with that of pure Pt electrode. Scanning Electron Microscopy (SEM) was utilized to examine surface morphology. The crystallinity of synthesized films was analyzed by X-ray Diffraction (XRD), and the oxidation state of both the platinum and molybdenum were determined by X-ray Photoelectron Spectroscopy (XPS) analyses. The catalytic activity and stability for methanol oxidation were measured using cyclic voltammetry (CV) and chronoamperometry (CA) in a mixture of 0.5 M $H_2SO_4$ and 0.5 M $CH_3OH$ aqueous solution. $MoO_3$ electrodeposited on the surface of Pt showed much higher catalytic acitivity and stability than pure Pt electrode due to the good contact between Pt and $MoO_3$.

• Journal of the Korean Ceramic Society
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• v.40 no.6
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• pp.577-582
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• 2003

BaTiO$_3$ fine powders were synthesized by hydrothermal process from peroxo-coprecipitate precursors. The peroxo-coprecipitates were obtained by addition of the BaCl$_2$, TiCl$_4$, and $H_2O$$_2$ aqueous solution to an ammonium solution. Hydrothermal reaction was conducted at various reaction temperatures, times and pH ranges. Unlike the conventional hydrothermal synthesis which needs highly alkaline condition over pH 13 with KOH or NaOH, the present method offered well-developed crystalline (perovskite) BaTiO$_3$ powders synthesized below pH 12 with use of ammonium solution. It was found that the phase-pure fine powders were formed at temperatures as low as 11$0^{\circ}C$ and the properties of the powders synthesized over 13$0^{\circ}C$ were almost same regardless of the reaction time. BET surface area of the prepared powder was as high as 76 $m^2$/g and the calculated particle (particulate) size was below 20 nm. The ultrafine particulates formed weak agglomerates. The microstructure and dielectric properties of BaTiO$_3$ ceramics sintered at the temperature range of 1150~125$0^{\circ}C$ were evaluated.

• Journal of the Korean Chemical Society
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• v.35 no.6
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• pp.689-698
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• 1991

Activated oxidation catalysts are generated by the treatment of pentadentate Schiff base cobalt(Ⅱ) complexes with the oxygen saturated DMF solution. Oxidation of 2,6-di-tert-butylphenol by homogeneous oxidation catalysts of superoxo type pentadentate schiff base cobalt(Ⅲ) complexes yields 2,6-di-tert-butylbenzoquinone(BQ) as a major product. And $O_2$/Co mole ratio of homogeneous oxidative catalysts such as [Co(Ⅲ)(sal-DET)]$O_2$ and [Co(Ⅲ)(sal-DPT)]$O_2$by PVT method of the oxygen absorption in DMSO and pyridine solution was 1:1, 1:1.52 in DMF solution and ${\mu}$-peroxo type cobalt(Ⅲ) complexes formed at solid state. The redox reaction processes of superoxo type cobalt(Ⅲ) complexes as homogeneous oxidation catalysts were investigated by cyclic voltammetry and DPP method at a glassy carbon electrode. As a result of electrochemical measurements the reduction processes of oxygen adducted superoxo type cobalt(Ⅲ) complexes occurred to four steps including prewave of $O_2$-in 0.1M TEAP-DMSO and 0.1 M TEAP-Pyridine as supporting electrolyte solution.

• Journal of the Korean Chemical Society
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• v.34 no.1
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• pp.51-62
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• 1990

Pentadentate Schiff base cobalt(II) complexes; Co(II)(Sal-DET) and Co(II)(Sal-DPT) were synthesized and these complexes were allowed to react with dry to form oxygen adducts of cobalt(II) complexes such as [Co(III)(Sal-DET)]$_2O_2$ and [Co(III)(DPT)]$_2O_2$ in aprotic solvents. These complexes have been identified by IR spectra, TGA, DSC, magnetic susceptibility measurements, and elemental analysis. It has been found that the oxygen adadduct complexes of $\mu$-peroxo type have hexaccordinated octahedral configuration with pentadentate schiff base cobalt(II) and oxygen, but the mole ratio of oxygen to cobalt(III) complexes of first step for oxygen adduct formation reaction of cobalt(II) complexes in aprotic solvents are 1:1. The redox reaction processes of Co(II)(Sal-DET), Co(II)(Sal-DPT), and oxygen adduct of cobalt(II) complexes were investigated by cyclic voltammetry and DPP method with glassy carbon electrode in 0.1M TEAP-DMSO and 0.1M TEAP-pyridine. As a result the reduction reaction processes of Co(III)/Co(II) and Co(II)/Co(I) for cobalt(II) complexes and oxygen adducts of cobalt(II) complexes are two irreversible steps of one eletron process, and reaction processes of oxygen for oxygen adducts complexes were quasireversible and redox range of potential was $E_{pc}$ = -0.97V∼-0.86V and $E_{pa}$ = -0.87V ∼ 0.64V.

• Journal of Korean Society of Environmental Engineers
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• v.22 no.6
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• pp.1073-1081
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• 2000

The photo-oxidation of an aqueous humic acid solution using $TiO_2$ sols. which is transparent in visible range, was studied. The $TiO_2$ sols were prepared by a process wherein hydrogen peroxide was added to a gel of $TiO(OH)_2$ originated from hydrolysis of $TiCl_4$, and the resulting titanium peroxo solution(TPS) was heated. The concentration of $TiO_2$ used for photo-oxidation was about 100ppm, determined by comparing the photoluminescence(PL) intensity measured as a function of $TiO_2$ concentration. $TiO_2$ sols aged at $100^{\circ}C$ for more than 12h were found to exhibit a maximum rate in photocatalytic decomposition of humic acid. and the efficiency was better than that of Degussa P25. In addition, the resulting aqueous humic acid after photocatalytic decomposition with sols had an excellent transmittance of visible light, while that treated with Degussa P25 was still turbid. caused by $TiO_2$ particles.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.03a
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• pp.207-207
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• 2003

최근 광촉매 재료로 각광받고 있는 TiO$_2$는 band gap 에너지가 3.0-3.2eV로 자외선 영역과 일부 가시광선 영역에서 활성을 갖는 것으로 알려져 있다. 따라서 용액 중에 결정화 및 안정화 되어있는 TiO$_2$의 band gap 에너지를 낮춘다면 가시광 영역의 광반응을 얻을 수 있다. 이에 본 연구는 G. Sato등이 제안한 방법으로 TiO$_2$ sol을 제조할 때 band gap 에너지를 낮추고자 천이 금속원소를 첨가하여 복합 및 담지된 TiO$_2$계 복합 sol을 합성하고자 하였다 출발원료는 TiC1$_4$를 가수분해하여 제조한 TiOCl$_2$에 천이금속원소인 V, Cr, Fe, Ni, Nb 등의 chloride 화합물을 첨가하여 중화 및 세척과정을 거친 후, 과산화수소수에 용해하여 전구체 용액인 titania peroxo용액을 제조하였다 제조된 전구체 용액은 온도와 시간을 변수로 각각 열처리하여 TiO$_2$계 복합 sol을 합성하였다. 제조된 시편은 X-선 회절 분석, 투과전자현미경, particle size analyzer, ζ-potential analyzer 및 UV-VIS Spectrometer 통을 이용하여 천이금속 첨가에 따른 TiO$_2$계 복합 sol의 형성과정과 특성변화를 관찰하였다.

• Journal of the Korean Chemical Society
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• v.39 no.12
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• pp.932-939
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• 1995

Rates of the decomposition of hydrogen peroxide by copper(Ⅱ)-Schiff base complexes were measured at various concentrations of hydrogen peroxide. Decomposition rates of hydrogen peroxide increased with increasing pH for CuⅡBSDT and CuⅡBSTP but then decreased with the same variation of the pH for CuⅡBSTT. A possible mechanism in accord with experimental results was proposed. The mechanism involves the deprotonation of copper(Ⅱ)-Schiff base complexes of hydrogen peroxide, followed by the formation of peroxo complexes at the rate-determining step.