• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.405-409
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• 1991

The electrochemical behaviors of copper-1-(2-thiazolylazo)-2-naphthol [Cu(II)-TAN] complex in acetonitrile (AN) solution have been investigated by the use of polarography, controlled potential coulometry and UV-Vis spectroscopy. Cu(II)-TAN complex exhibit three reduction waves at -0.91 V, -1.34 V and -1.65 V vs. S.C.E. in acetonitrile solution containing 5.0 ${\times}\;10^{-3}$M tetraethylammonium perchlorate. Every reduction wave is diffusion controlled. The first reduction wave is considerably reversible and this process is attributed to the formation of anion radical. The second reduction process to the dianion is followed by a chemical reaction producing a complex of hydrazo complex. The third reduction process produce Cu(Hg) amalgam and amine compound.

• Resources Recycling
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• v.31 no.1
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• pp.29-36
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• 2022

The hydrogen reduction behavior of molybdenum oxides was studied using a horizontal-tube reactor. Reduction was carried out in two stages: MoO₃ → MoO₂ and MoO₂ → Mo. In the first stage, a mixed gas composed of 30 vol% H₂ and 70 vol% Ar was selected for the MoO₃ reduction because of its highly exothermic reaction. The temperature ranged from 550 to 600 ℃, and the residence time ranged from 30 to 150 min. In the second step, pure H₂ gas was used for the MoO₂ reduction, and the temperature and residence time ranges were 700-750 ℃ and 30-150 min, respectively. The hydrogen reduction behavior of molybdenum oxides was found to be somewhat different between the two stages. For the first stage, a temperature dependence of the reaction rate was observed, and the best curve fittings were obtained with a surface reaction control mechanism, despite the presence of intermediate oxides under the conditions of this study. Based on this mechanism, the activation energy and pre-exponential were calculated as 85.0 kJ/mol and 9.18 × 10⁷, respectively. In addition, the pore size within a particle increases with the temperature and residence time. In the second stage, a temperature dependence of the reaction rate was also observed; however, the surface reaction control mechanism fit only the early part, which can be ascribed to the degradation of the oxide crystals by a volume change as the MoO₂ → Mo phase transformation proceeded in the later part.

• Journal of the Korean Chemical Society
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• v.37 no.8
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• pp.730-734
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• 1993

The electrochemical reduction behavior or Biliverdin (BV) in N,N-dimethylformamide solvent was studied by DC polarography, cyclic voltammetry and the controlled potential coulometry. The reduced product was indentified by UV-Vis spectroscopy. In DC polarogram, two reduction waves of BV were founded. The half wave potentials of two reduction waves were -0.71 and -0.91 V vs. Ag/Ag$^+$ respectively. The current type of the 1st reduction wave was diffusion-controlled and the 2nd was diffusion current containing a little kinetic current. The 1st electrochemical reduction process was irreversible and BV reduced to Bilirubin.

• Proceedings of the Korean Nuclear Society Conference
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• 1998.05a
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• pp.357-362
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• 1998

PWR 정지시 일차계통 수화학 제어의 주요대상은 계통표면에 침적된 부식생성물의 주성분인 비화학양론적 니켈(코발트)페라이트로서, 산성-환원 단계에서 용존수소에 의해 Ni$^{\circ}$ (또는 Co$^{\circ}$)로 환원되고 산성-산화 단계에서 용존산소에 의해 Ni$^{2+}$ (또는 CO$^{2+}$)로 산화되어 이온교환기에 의해 제거된다 본 연구에서는, 니켈 및 코발트 산화물의 25~300 $^{\circ}C$ 환원 또는 산화반응 시 표준자유에너지의 변화 및 용존수소 또는 용존산소의 요구농도를 계산하여, 원자로 정지시 일차계통수 용존 기체의 제어조건을 고찰하였다. 산성-환원 단계의 냉각재 온도인 300~82$^{\circ}C$ 범위에서 용존수소가 충분할 경우 열역학적으로 $^{58}$ Co(또는 $^{60}$Co)Fe$_2$O$_4$$\longrightarrow$Co의 역반응이 억제되므로서 노심외 계통부위 침적이 감소될 수 있기 때문에, 용존수소를 온도에 따라 요구농도 곡선 위로 약간 높게 유지하는 것보다 25~50 cc/kg-$H_2O$로 유지하는 방식이 바람직한 반면, 용존산소를 제공하는 과산화수소 농도가) 2.7 ppm일 때 NiFe$_2$O$_4$$\longrightarrow$Ni$_2$O$_4$(+$\alpha$-Fe$_2$O$_3$) 반응이 일어날 수 있기 때문에, 산성-산화 단계에서는 과산화수소의 냉각재 농도를 이보다 낮게 유지하는 것이 바람직하다.

• Journal of the Korean Chemical Society
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• v.32 no.3
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• pp.233-242
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• 1988

The uranium(VI) complexes with new unsaturated macrocyclic ligands of cryptand types and the neodymium(III) complexes with cryptand 222 and DBC ligands have been investigated polarographically in dimethylsulfoxide solvent. The reduction states, electron numbers involved in the reduction process, effects of the added acid on the polarograms of complexes, and the mechanisms of the reduction electrode reactions have been examined. The stability constants and mole-ratio of new complexes were also obtained by polarographic method. The reaction of ligands was controlled by the diffusion in the reduction with four electrons at a step, whereas the redox reaction with six electrons at three steps in $UO_2\;^{2+}$ complexes with macrocyclic ligands and the redox reaction with one electron at a step in $Nd^{3+}$ complexes with cryptand 222 and DBC have been observed. The imine ligands formed stable complexes with uranium(VI) above pH 7.0, and the neodymium(III) complexes with cryptand 222 and DBC ligands were stable above pH 4.0.

• Journal of the Korean Chemical Society
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• v.19 no.2
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• pp.104-115
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• 1975

The electrochemical reduction of iodine in non-aqueous media have been studied by polarography, chronopotentiometry, cyclic voltammetry and controlled potential coulometry at dropping mercury electrode and platinum, gold and amalgamated platium electrodes. In amphiprotic solvents such as methanol, ethanol, isopropanol and pyridine, iodine were reduced to iodide ions via one step reduction involving 1 electron and in aprotic solvents such as acetonitrile, dimethylformamide and dimethylsulfoxide via two step reduction involving all 3 electrons. The reductions of iodine give well defined polarograms at dropping mercury electrode and irreversible chronopotentiograms at platinum electrode, but less defined irreversible chronopotentiograms at gold and amalgamated platinum electrodes, those are all diffusion controlled. The diffusion coefficients of iodine in various solvents were estimated from the chronopotentiometric data and Sand equation.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.374-378
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• 1991

The electrochemical reduction behavior of Bilirubin (BR) in phosphate buffer (pH 7.8) solution was studied by DC polarography, differential pulse polarography, cyclic voltammetry and controlled potential coulometry. In DC polarogram, two reduction waves of BR were found. The half wave potentials of two reduction waves were -1.32 and -1.51 volts vs. Ag/AaCl respectively. The current type of 1st reduction wave was diffusion-controlled and the 2$^{nd}$ reduction wave was diffusion current containing a little kinetic current. The electrochemical reduction process of BR at each reduction step was all irreversible. The prewave appeared at lower concentration than 3.4 ${\times}$ 10$^{-4}$M, this prewave was identified as adsorption prewave. And the number of electron transfered in reduction steps, n$_{app}$ was two for the 1st reduction step and one for the 2$^{nd}$ reduction step.

• Journal of the Korean Chemical Society
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• v.32 no.1
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• pp.15-21
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• 1988

The Polarographic behavior of 1-(2-thiazolylazo)-2-naphthol (TAN) in acetonitrile solution was studied. From the DC polarograms of TAN in acetonitrile solution, the type of reduction current and the effect of proton donor such as water have been investigated. In order to explain the reduction mechanism, the number of the electrons for each reduction step was measured by controlled potential coulometric technique and the electrolysis products were identified by UV-Vis spectroscopy and IR spectroscopy. The results were shown that the reduction of TAN in acetonitrile solution occurred with four-one electron steps. In addition, each reduction step was considerably reversible and the reduction current was diffusion controlled.

• Journal of the Korean Magnetics Society
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• v.7 no.1
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• pp.25-30
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• 1997

Physical and magnetic behaviors of reduced Co-Zn-Ti-Sn substituted Ba-ferrite particles with hydrogen are different from those of reduced-pure Ba-ferrite particles. The coercivity of substituted Ba-feffite particles shows a peaking effect with the reduction temperature ranging from 250 to 520 $^{\circ}C$, while the coercivity of pure Ba-ferrite decreases monotonically. The reduction process of substituted Ba-ferrite has been found to be devided into three steps. At the first and second steps, the magneto-plumbite structure maintained. When the reduced-substituted Ba-ferrite particles are reoxidized, the coercivity is reversible at the first step but irreversible at the second step. During the third step of reduction process above 410 $^{\circ}C$. The magneto plumbite structure was collapsed with formation of $\alpha$-Fe and $BaFeO_{3-x}$ phases and consequently the coercivity distribution is broaden and the coercivity irreversible. The coercivity and saturation magnetization decreases and increases up to 130 emu/g respectively. In this study, it is found that the substituted elements prevent the magneto-plumbite structure from collapse during the reduction process and furthermore migrate from the magnetic sites of $2a+4f_{IV}$, 2b, and 12k to $4f_{VI}$ and 12k'. An increase in the coercivity before the collapse of magneto-plumbite structure is attributed to the migration of cations in hexagonal Ba-ferrite structure.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.10a
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• pp.26-26
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• 2011

Fe계 TiC 합금은 미량의 합금원소를 첨가시켜 경화능, 내식성, 내마모성 성질을 개선한 특수 공구용 재료로서 현재 절삭, 내마모성, 광산, 금형재료 등의 분야에 널리 사용되고 있다. 금속과 세라믹의 복합재료인 초경합금은 비열처리용 공구강으로 WC, TiC 등의 4, 5, 6족 금속탄화물에 Co, Ni, Fe등의 철족이 결합금속으로 소결한 복합재료로 WC-Co계 초경합금이 주종을 이루고 있으나, 전략 소재로서 고가인 Co 원료를 대체하기 위한 재료로서 초경재료의 고경도와 공구강의 경제성 및 가공성의 장점을 이용한 Fe-TiC계 초경합금의 연구가 다양하게 진행되고 있다. 본 연구에서는 Fe기지에 서브마이크론 크기의 미세한 TiC 입자가 균일하게 분산된 Fe-TiC 복합분말을 경제적으로 제조하기 위해 순수한 Fe, Ti 원료분말에 비해 단가가 낮고 미세 분쇄가 용이한 FeO, $TiH_2$ 분말을 고에너지 밀링 후 반응 열처리 시키는 유사 기계화학적 공정을 시도하였다. 조성비 Fe-30wt%TiC 복합분말을 제조하기위해 마이크론(micron) 크기의 FeO, $TiH_2$, C 분말을 사용하였고, 1단계로 FeO와 C을 고에너지 밀링으로 혼합 후 반응시켜 환원시키는 공정과 2단계로 이렇게 환원된 분말과 TiH2를 고에너지 밀링으로 다시 혼합, 분쇄한 후 반응열처리 하는 두 단계 공정을 사용하였다. FeO의 환원 단계에서는 $700{\sim}1,000^{\circ}C$ 온도 범위에서 1시간 유지하였고, 고에너지 밀링 시 밀링시간, 회전속도를 변수로 두고 실험하였다. 환원된 분말은 수평관상로를 이용해 아르곤분위기에서 $1,000{\sim}1300^{\circ}C$까지 1시간 유지하여 반응열처리시켜 Fe-TiC 복합분말을 제조하였다. 준비된 복합분말을 XRD와 FE-SEM, EDS, 입도분석기 (LPSA) 등을 이용해 분말의 형태와 특성, 상, 조성, 입도, 분산도 등을 조사하였다. 제조된 Fe-TiC 나노복합분말을 방전플라즈마소결(SPS) 과 상압소결 실험을 진행하였다. Fe-TiC 복합분말 제조공정의 첫 번째 단계인 FeO의 환원반응은 $800^{\circ}C$이상의 온도에서 Fe로 환원이 진행됨을 확인하였다. 두 번째 단계인 반응열처리공정에서는 $1,000^{\circ}C$ 이상에서 TiC가 형성됨을 XRD 상분석을 통해 확인할 수 있었고, $1,100^{\circ}C$ 이상의 온도에서 반응열처리를 했을 때 XRD 분석결과와 산소 조성 분석 결과로부터 반응의 완결성과 순도에서 최적 온도 조건임을 확인하였다. 온도를 $1,300^{\circ}C$로 증가시킬 경우 반응의 완결성에 큰 변화가 없는 반면 분말입자간의 목형성이 일어나 가소결 되는 것을 FE-SEM을 통해 관찰하였다. 또한 최적조건으로 제조된 Fe-TiC 복합분말의 입도분석과 FE-SEM/EDS 관찰/분석을 시행한 결과 평균 입도 0.6 ${\mu}m$의 미세한 Fe-TiC 복합분말 내에 Fe분말 주변과 내부에 나노크기의 TiC입자가 균일하게 분산되어 존재하는 것을 확인하였다.