• Korean Journal of Materials Research
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• v.3 no.6
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• pp.565-574
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• 1993

The Ar/Ar- $H_{2}$ plasma method Lvas applied to reduce and refine high purity Nb metal. Inaddition, the reaction between molten Nb metal and hydrogen were also analyzed in the Ar-(20%)$H_{2}$plasma. The metallic Nb of 99.5wt% was obtained at the ratio of $C/Nb_{2}O_{5}$=5.00 in the Ar plasma reductionand the $O_2$ loss from the thermal decomposition of niobium oxides did not take place. In the Ar-(20%)Hi plasma the metallic Nb of 99.8wt% was produced at the ratio of $C/Nb_{2}O_{5}$=4.80. It was observedthat a major reaction of the deoxidation was the reaction with H, Hi, and a deoxidation by the evaporationof $NbO_x$ did not occur but a mass loss of Nb did by a "splash" effect. The deoxidation reaction rateobeyed the 1st order reaction kinetics and the reaction rate constant(k') of deoxidation was $7.8 \times 10_{-7}$(m/sec).The solubility of hydrogen in Nb metal was 60ppm and it was larger than the solubility of molecularstate hydrogen by 40ppm in the Ar-(20%)$H_{2}$ plasma method. A saturation was within 60sec anda hydrogen content was reduced below lOppm by a Ar plasma re-treatment.by a Ar plasma re-treatment.

• Proceedings of the Korean Vacuum Society Conference
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• 2015.08a
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• pp.198-198
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• 2015

전기변색재료는 전압을 인가하였을 때 전계방향에 따라 가역적으로 색이 변화하는 재료를 말한다. 스마트윈도우용 전기 변색재료는 지속적으로 전기를 가해줄 필요 없이 한번 변색되면 색이 지속되는 특징을 가지므로 에너지 효율적으로 우수하여 태양열 차단 창호나 디스플레이 분야에 응용될 것으로 기대된다. 이러한 전기 변색재료에는 산화형 전기 변색 재료, 환원형 전기 변색 재료가 있는데 이중 가장 널리 연구되고 있는 재료는 환원형 전기변색재료이다. 대표적인 재료로 $WO_3$가 쓰이는 데 이는 전기 변색적 특성이 우수하고 또한 내구성이 다른 재료에 비해 우수하다는 장점 때문이다. 그러나, 상용화를 위해서는 내구성의 개선이 요구되고 있다. 한편, $TiO_2$는 안정성이 매우 뛰어나지만 전기변색적 특성이 $WO_3$에 비해 낮은 점이 지적되고 있다. 이러한 $WO_3$ 및 $TiO_2$ 박막은 스퍼터링 또는 sol-gel법 등으로 제작되고 있는데, 일반적으로 스퍼터링의 경우 치밀한 박막이 형성되기 때문에 Porous 한 박막을 얻기 힘들다. 따라서 본 연구에서는 기판에 입사하는 스퍼터 입자들의 각도를 조절하여 shadowing 효과로 인해 박막의 구조가 porous해지는 Glancing angle deposition을 도입하였다. 이러한 증착법을 이용하여 $WO_3$와 $TiO_2$를 각도를 조절하여 증착하고 $TiO_2$와 $WO_3$ 박막의 특성을 비교하여 본다. 두께 300 nm를 가지는 $WO_3$ 및 $TiO_2$ 박막은 GLAD RF 마그네트론 스퍼터링법을 이용하여 Corning glass(corning E-2000)기판 위에 증착하였다. 기판 입사 각도는 $0^{\circ}$, $30^{\circ}$, $45^{\circ}$, $60^{\circ}$로 증착하였고 직경 3 in의 $TiO_2$, $WO_3$ 타겟을 사용하였다. 또한 스퍼터링 파워는 400 W, 작업압력 1.0 Pa, 그리고 스퍼터링 가스는 O2/Ar+O2 유량 10%에서 30%로 증착을 상온에서 진행하였다. 전기화학적 특성을 평가하기 위하여 $TiO_2$ 및 $WO_3$ 박막을 100 nm 두께의 ITO/glass 위에서 증착하였다. 박막의 미세구조는 XRD와 SEM을 통해 확인하였고, 전기화학적 특성은 Ar 분위기의 Glove box안에서 parstat 2273을 통해 측정하였다. 전해질은 1 M $LiPF_6/PC$로 진행하였고, 대향 전극는 Pt전극을, 참고 전극은 칼로멜 전극을 사용하였다. Potential 범위는 2 V에서 4 V로 진행하였고, scan rate는 50 mV/s로 측정하였다. 투과도는 UV/VIS spectrometer로 측정하였다. 전기변색 특성의 상관관계 및 에 대해서는 학회 당일 발표할 예정이다.

• Korean Chemical Engineering Research
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• v.60 no.3
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• pp.446-451
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• 2022

In this study, to improve capacity and cycle stability, the pitch coated nano silicon sheets/CNT composites were prepared through electrostatic bonding of nano silicon sheets and CNT. Silica sheets were synthesized by hydrolyzing TEOS on the crystal planes of NaCl, and then nano silicon sheets were prepared by using magnesiothermic reduction method. To fabricate the nano silicon sheets/CNT composites, the negatively charged CNT after the acid treatment was used to assemble the positively charged nano silicon sheets modified with APTES. THF as a solvent was used in the coating process of PFO pitch. The physical properties of the prepared anode composites were analysed by FE-SEM, XRD and EDS. The electrochemical performances of the synthesized anode composites were performed by current charge/discharge, rate performances, differential capacity and EIS tests in the electrolyte LiPF₆ dissolve solvent (EC:DMC:EMC = 1:1:1 vol%). It was found that the anode material with high capacity and stability could be synthesized when high composition of silicon and conductivity of CNT were used. The pitch coated nano silicon sheets/CNT anode composites showed initial discharge capacity of 2344.9 mAh/g and the capacity retention ratio of 81% after 50 cycles. The electrochemical property of pitch coated anode material was more improved than that of the nano silicon sheets/CNT composites.

• Journal of the Korean Ceramic Society
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• v.41 no.4
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• pp.297-301
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• 2004

Nano-sized mullite (3Al$_2$O$_3$$.$2SiO$_2$) colloids were prepared by use of the spray combustion method. For combustion reaction, Al(NO$_3$)$_3$$.$9$H_2O$, and CH$_{6}$N$_4$O were used as an oxidizer and a fuel respectively, and then colloidal silica was also added as 2SiO$_2$source for mullite. The temperature of the reaction chamber was kept at 80$0^{\circ}C$ to initiate the ignition of droplets of the mixed precursors. For preventing droplet coagulation, the droplet number concentration was reduced using the metal screen filter, and the residence time of aerosol was kept at 2.5 seconds for laminar flow. The synthesized colloidal particles had an uniform spherical shape with 130 nanometer size and the crystalline phase showed the mullite with stoichiometry in the observations of XRD and TEM.

• Journal of the Korean Chemical Society
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• v.35 no.2
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• pp.151-157
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• 1991

A sensitive stripping voltammetric study of the complex of indium with 8-hydroxyquinoline at a hanging mercury drop electrode was investigated in 0.1M acetate buffer solution. The effects of various analytical conditions on the reduction peak current of the adsorbed complex were discussed. Optimal analytical conditions were found to be the ligand concentration of $2 {\times}10^{-5}$M, solution pH 4.75, scan rate of 10 mV/s, deposition potential of -0.450V, a deposition time of 90 second. Interferences by other trace metals and Triton X-100 were also discussed. Detection limit was 0.2 ppb of indium after 90 sec. Deposition time, and the relative standard deviation(n = 10) at 4 ppb was 3.2%.

• Applied Chemistry for Engineering
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• v.18 no.4
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• pp.320-325
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• 2007

Nickel powders were prepared from an aqueous nickel acetate solution and hydrazine hydrate using diethanolamine as the nonaqueous organic solvent in the conventional and microwave synthetic method. It was investigated that microwave non-thermal effect and synthetic condition affect the preparation of nickel powders by means of X-ray diffractometry, scanning electron microscopy, thermal gravymetry analysis, and X-ray photoelectron spectroscopy analysis. Compared with the conventional synthetic method, less of aggregation, smaller particle size, and more uniform distribution of particle size were obtained in the microwave synthetic method due to the non-thermal effect of microwaves.

• Korean Chemical Engineering Research
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• v.61 no.1
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• pp.32-38
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• 2023

In this study, the electrochemical properties of dopamine coated silicon/silicon carbide/carbon(Si/SiC/C) composite materials were investigated to improve cycle stability and rate performance of silicon-based anode active material for lithium-ion batteries. After synthesizing CTAB/SiO₂ using the Stöber method, the Si/SiC composites were prepared through the magnesium thermal reduction method with NaCl as heat absorbent. Then, carbon coated Si/SiC anode materials were synthesized through polymerization of dopamine. The physical properties of the prepared Si/SiC/C anode materials were analyzed by SEM, TEM, XRD and BET. Also the electrochemical performance were investigated by cycle stability, rate performance, cyclic voltammetry and EIS test of lithium-ion batteries in 1 M LiPF₆ (EC: DEC = 1:1 vol%) electrolyte. The prepared 1-Si/SiC showed a discharge capacity of 633 mAh/g and 1-Si/SiC/C had a discharge capacity of 877 mAh/g at 0.1 C after 100 cycles. Therefore, it was confirmed that cycle stability was improved through dopamine coating. In addition, the anode materials were obtain a high capacity of 576 mAh/g at 5 C and a capacity recovery of 99.9% at 0.1 C/0.1 C.

• Korean Journal of Crystallography
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• v.9 no.1
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• pp.21-29
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• 1998

The rare-earth orthoborate family, RM3(BO3)4 is known to be the most promising material for the microlaser host. To grow LaSc3(BO3)4 single crystal, the phase relation of the system LaBO3-ScBO3 was investigated by DTA method. LaSc(BO3)4 was the unique intermediate compound in the binary system the peritectic reaction point of which was 1495 ±2℃. Owing to the peritectic behavior of the compound, the crystal growth of the rare-earth Sc-borate was carried out by pulling from the melt-soultion of La1+xSc3-x(BO3)4. The optimal conditions for the growth of LaSc3(BO3)4 were determined by traditional CZ method : pulling speed 0.7mm/hr, rotation speed 7-10 rpm under reduction condition. Pt and Ir crucibles could be used for about 8-10 times of growth. The effect of thermal configurations on the temperature distribution was investigated. A special two-coordinate manipulator was made for the precise movement of thermocouples from the melt to the top of the furnace for several thermal configurations. The radial gradient on the melt surface depends strongly on the construction of the afterheater. On the other hand, the axial gradient was mainly propotional to both the opening degree of baffle plate and the mutual positions of crucible and heater.

• Korean Chemical Engineering Research
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• v.57 no.1
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• pp.118-123
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• 2019

In this study, the electrochemical characteristics of Graphite/Silicon/Pitch anode composites were analyzed to improve the low theoretical capacity of graphite as a lithium ion battery. The Graphite/Silica composites were synthesized by bonding silica onto polyvinylpyrrolidone coated graphite. The surface of used silica was treated with (3-Aminopropyl)triethoxysilane(APTES). Graphite/Silicon/Pitch composites were prepared by carbonization of petroleum pitch, the fabrication processes including the magnesiothermic reduction of nano silica to obtain silicon and varying the mass ratio of silica. The Graphite/Silicon/Pitch composites were analysed by XRD, SEM and XRD. Also the electrochemical performances of Graphite/Silicon/Pitch composite as the anode of lithium ion battery were investigated by constant current charge/discharge, rate performance, cyclic voltammetry and electrochemical impedance tests in the electrolyte of $LiPF_6$ dissolved in organic solvents (EC:DMC:EMC=1:1:1 vol%). The Graphite/Silicon/Pitch anode composite (silica 28.5 in weight) has better capacity (537 mAh/g). The cycle performance has an excellent capacity retention to 30th cycle of 95% and the retention rate capability of 98% in 0.1 C/0.2 C.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.2
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• pp.45-49
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• 2019

Relatively fine silicon carbide (SiC) crystalline aggregates have been synthesized with the carbonized rice husks, paper sludge, coffee grounds as the carbon sources and the silica powder. The main reaction source to obtain silicon carbide (SiC) aggregates from the mixture of carbon sources and silica was inferred as the gaseous silicon monoxide (SiO) phase, being created from this mixture through the carbothermal reduction reaction. The silicon carbide (SiC) crystalline aggregates, fabricated from the carbonized rice husks and paper sludge, coffee grounds and silica ($SiO_2$) powder, were investigated by XRD patterns, FE-SEM and FE-TEM images. In these specimens, obtained from the carbonized rice husks, paper sludge and silica, XRD patterns showed rather high strong peak of (111) plane near $35^{\circ}$. The FE-TEM images and patterns of specimens, synthesized from carbonized rice husks, paper sludge, coffee grounds and silica under Ar atmosphere, showed relatively fine particles under $1{\mu}m$ and crystalline peak (110) of silicon carbide (SiC) diffraction pattern.