• Applied Chemistry for Engineering
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• v.24 no.4
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• pp.438-442
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• 2013

In the present work, electroless plating was used for coating thin films consisting mainly of Ni and P on carbon fiber. Structural changes appeared upon the post-annealing at various temperatures of the Ni-P film on carbon fiber was studied using various analysis methods. Scanning, a flat surface structure of Ni-P film on carbon fiber was found after electroless plating of Ni-P film on carbon fiber without post-annealing, whereas annealing at $350^{\circ}C$ resulted the formation of porous structures. With increasing the annealing temperature to $650^{\circ}C$ with an interval of $50^{\circ}C$, the pore size increased, but the density decreased. X-ray diffraction (XRD) showed the existence of metallic Ni, and Ni-P compounds before post-annealing, whereas the post-annealing resulted in the appearance of NiO peaks, and the decrease in the intensity of the peak of metallic Ni. Using X-ray photoelectron spectroscopy (XPS), phosphorous oxides were detected on the surface upon annealing at $650^{\circ}C$, and $700^{\circ}C$, which can be attributed to the phosphorous compounds originally existing in the deeper layers of the Ni films, which undergo sublimation and escape from the film upon annealing. Escape of phosphorous species from the bulk of Ni-P film upon annealing could leave a porous structure in the Ni films. Porous materials can be of potential applications in diverse fields due to their interesting physical properties such as high surface area, and methods for fabricating porous Ni films introduced here could be easily applied to a large-scale production, and therefore applicable in diverse fields such as environmental filters.

• Korean Chemical Engineering Research
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• v.43 no.2
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• pp.215-221
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• 2005

A Fe-containing mesoporous silica (Fe-MCM-41) in which part of Si in the framework was replaced by Fe(Si-O-Fe) has been successfully prepared using $Fe^{3+}$ salt by a direct synthesis route. Physical properties of the material were characterized by XRD, $N_2$ adsorption, SEM/TEM, UV-vis and FT-IR spectroscopies. Fe-MCM-41 exhibited high catalytic activity in phenol hydroxylation using $H_2O_2$ as oxidant, giving phenol conversion of ca. 60% at $50^{\circ}C$ [phenol : $H_2O_2$ = 1:1, water solvent]. Fe-MCM-41 was also applied to the growth of CNTs, utilizing a thermal-CVD reactor using acetylene gas, which demonstrated that multi-wall CNTs could be prepared efficiently using the Fe-MCM-41 catalyst.

• Korean Chemical Engineering Research
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• v.46 no.5
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• pp.863-867
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• 2008

Pitch based activated carbon fiber(ACF) was prepared from reformed naphtha cracking bottom oil(NCB oil) by melt spinning. The fibers obtained were stabilized, carbonized, and then steam activated. The ACF was sensitized with Pd-Sn catalytic nuclei via a single-step activation approach. This sensitized ACF was used as precursors for obtaining copper plated ACFs via electroless plating. ACFs uniformly decorated with metal particles were obtained with reduced copper plating in the reaction solution. Effects of the amount of copper on characteristics of ACF/Cu catalysts were investigated through BET surface area, X-ray diffraction, scanning emission microscopy, and ICP. The amount of copper increased with plating time, but the surface area as well as the pore volume decreased. NO conversion increased with reaction temperature. NO conversion decreased with increasing the amount of copper, which is seemed to be due to the reduction of surface area as well as the dispersion of copper.

• Journal of Korean Society of Environmental Engineers
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• v.38 no.11
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• pp.603-610
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• 2016

This work studies the synthesis of birnessite (${\delta}-MnO_2$), a catalyst of oxidative-coupling reactions, from the powder of spent alkaline manganese batteries (SABP, <8 mesh) and evaluate its reactivity for 1-naphthol (1-NP) removals. Manganese oxides using commercial reagents ($MnSO_4$, $MnCl_2$) and the acid birnessite (A-Bir) by McKenzie method were also synthesized, and their crystallinity and reactivity for 1-NP were compared with one another. 96% Mn and 98% Zn were extracted from SABP by acid leaching at the condition of solid/liquid (S/L) ratio 1:10 in $1.0M\;H_2SO_4+10.5%\;H_2O_2$ at $60^{\circ}C$. From the acid leaching solution, 69% (at pH 8) and 94.3% (pH>13) of Mn were separated by hydroxide precipitation. Optimal OH/Mn mixing ratio (mol/mol) for the manganese oxide (MO) synthesis by alkaline (NaOH) hydrothermal techniques was 6.0. Under this condition, the best 1-NP removal efficiency was observed and XRD analysis confirmed that the MOs are corresponding to birnessite. Kinetic constants (k, at pH 6) for the 1-NP removals of the birnessites obtained from Mn recovered at pH 8 (${Mn^{2+}}_{(aq)}$) and pH>13 ($Mn(OH)_{2(s)}$) are 0.112 and $0.106min^{-1}$, respectively, which are similar to that from $MnSO_4$ reagent ($0.117min^{-1}$). The results indicated that the birnessite prepared from the SABP as a raw material could be used as an oxidative-coupling catalyst for removals of trace phenolic compounds in soil and water, and propose the recycle scheme of SAB for the birnessite synthesis.

• Journal of the Korean Chemical Society
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• v.36 no.2
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• pp.261-272
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• 1992

Tetradentate Schiff base Cobalt(II)(3MeOSED)$(H_2O)_2$ complexe was synthesized and allowed to react with dry oxygen to form oxygen adducts of Cobalt(III) complexes such as ${\mu}$-peroxo type [Co(III)(3MeOSED)(DMF)]$_2O_2$ and [Co(III)(3MeOSED)(DMSO)]$_2O_2$in DMF and DMSO or superoxo type [Co(III)(3MeOSED)(Py)]$O_2$ in pyridine. The oxygen adducted complex was investigated by cyclic voltammetry and DPP method with glassy carbon electrode in 0.1M TEAP-DMF (-DMSO,-Py) as supporting electrolyte solution. As a result the reduction reaction process occurred to four steps including prewave Of $O_2^-$in 1 : 1 oxygen adducted superoxo type [Co(III)(3MeOSED)(Py)]$O_2$complex and three steps not including prewave of $O_2^-$ in 1 : 2 oxygen adducted ${\mu}$-peroxo type [Co(III)-(3MeOSED)(DMF)]$_2O_2$ and [Co(III)(3MeOSED)(DMSO)]$_2O_2$. A superoxo type [Co(III)(3MeOSED)(L)]$O_2\;(L: CH_3OH)$ was generated with oxygen in methanol. Selectively oxidized hydrazobenzene $(H_2AB)$ to trans-azobenzene(t-AB) and the rate constant k for oxidation reaction of the following equation is $(2.96 {\pm} 0.2)$${\times}$ $10^{-1}$M/sec. $H_2AB$ + Co (II)(3MeOSED)$(L_2)+O_2\;{\rightleftarrow^K}$ [Co(III)(3MeOSED)(L)]$O_2{\cdot}H_2AB{\longrightarrow^K}$ Co(II(3MeOSED)$(L)_2$+t-AB+$H_2O_2 $.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.386.2-386.2
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• 2014

본 연구에서는 바이오 센서 응용을 위해 그래핀을 전극으로 제작하여 그래핀 표면 결함준위에 따른 센서의 민감도를 전기화학 실험을 통해 관찰하였다. 그래핀은 니켈/구리촉매를 이용한 저 진공 화학 기상 증착 장비(Low-Pressure Chemical Vapor Deposition; LP-CVD)와 Photo-lithography로 제작한 것과 탄소 산화물을 환원시켜 만든 환원-그래핀, 두 가지를 사용하였다. 전기화학 실험에서 그래핀 전극 및 Silver/Silver chloride (Ag/AgCl), Fluorine doped Tin Oxide (FTO)은 작업 전극 및 기준 전극, 상대 전극으로 각각 사용하였고, 반응용액은 potassium hexacyanoferrate (III)를 농도를 다르게 하여 사용하였다. 그래핀의 표면 상태, 층수, 결함 정도 등 구조적인 특성은 원자력현미경(Atomic Force Microscopy; AFM), 주사 전자 현미경(Secondary Electron Microscopy; SEM)과 Raman spectroscopy를 각각 이용하여 확인하였고, 그래핀의 결함준위에 따른 반응면적 및 센서 감도 의존성을 전류모드-원자력현미경(Current-Atomic Force Microscopy; I-AFM)과 전기화학 임피던스 분광법(Electrochemical Impedance Spectroscopy; EIS)를 통해 그래핀 전극의 성능을 분석하고, 그래핀 결함 준위에 따른 센서 감도 의존성은 순환전위 분광법 (Cyclic Voltammetry; CV)를 이용하여 관찰하였다. 또한 농도가 다른 반응용액은 센서의 민감도를 관찰하는데 사용하였다. 결과적으로 LP-CVD로 성장한 그래핀과 환원-그래핀의 결함준위에 따른 센서의 성능을 비교 분석한 결과와 반응용액 농도에 따른 센서의 민감도 결과는 그래핀 바이오센서에 대한 응용 및 상용화를 앞당기는데 기여할 것으로 예상한다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.96-96
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• 2016

나노섬유(nanofiber), 나노선(nanowire), 그리고 나노튜브(nanotube)와 같은 1차원 구조의(one-dimensional structure) 나노재료는 벌크(bulk) 및 박막(film) 재료와는 다르게 물리적, 화학적으로 특이한 성질을 가지고 있으며, 이러한 성질은 나노재료의 구조, 형상, 크기 등에 큰 영향을 받는다. 첫 째, 전기방사(electrospinning) 공정을 이용한 나노섬유의 합성; 용액의 특성, 전기장 세기, 방사시간 등의 변수를 조절하게 되면 방출되는 재료의 형상을 입자 혹은 섬유상의 형태로 얻을 수 있으며, 전기방사를 통해 합성된 나노재료의 소결 온도 및 시간을 달리함으로써 나노입자의 크기를 조절할 수 있다. 또한, 템플레이트 합성법(template synthesis) 및 이중노즐(coaxial nozzle)을 이용해 속이 빈 형태인 중공(hollow) 구조의 나노섬유를 얻을 수 있으며, 전기방사에 사용되는 전구물질에 원하는 금속 및 산화물을 첨가함으로써 복합체(composite) 나노섬유를 얻을 수 있다. 둘 째, VLS(Vapor-Liquid-Solid) 공정을 이용한 나노선의 성장; 온도, 압력, 전구물질의 양, 그리고 시간 등의 변수를 조절하게 되면 원하는 직경 및 길이를 갖는 나노선을 성장시킬 수 있다. 그리고 ALD(Atomic Layer Deposition)를 이용해 나노선에 추가적인 층을 형성함으로써 코어-셀 구조를 형성할 수 있으며, 감마선, UV와 같은 공정을 이용해 귀금속 촉매를 나노선에 기능화 시킬 수도 있다. 코어-셀 구조를 갖는 나노선/나노섬유는 코어 혹은 셀 층의 전자나 홀의 이동을 유발하여 전자공핍층(electron depletion layer) 또는 정공축적층(hole accumulation layer)을 확대 및 축소시켜 센서의 초기저항을 증가시키거나 감소시키는 역할로써 이용되고 있으며, 특히, 셀 층의 두께가 셀 층 재료의 Debye length와 유사한 크기를 갖게 되면, 셀 층은 완전공핍층(fully depleted layer)을 형성해 최대의 감도를 나타낼 수 있다. 본 연구에서는 다양한 제조 공정을 통해 제작될 수 있는 1차원 나노-구조물을 가스센서에 적용하는 사례들을 소개하고, 이러한 가스센서의 감응성능을 향상시키기 위한 방법의 한 가지로 원자층증착법으로 나노선/나노섬유의 표면에 셀층을 형성하여 감응성 향상 메커니즘 및 관련 주요 변수들을 조사하고자 한다.

• Polymer(Korea)
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• v.25 no.6
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• pp.782-788
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• 2001

The $[Ru(v-bpy)_3]^{2+}$ and vinylbenzoic acid (vba) were electrochemically copolymerized to afford electrodes modified with dopamine to study their properties such as electropolymerization rate, redox process, and electron transfer. The optimum mole ratio of the monomers was 5:2, which gave $1.84{ imes}10^{-2}s^{-1}$ of rate constant for first order reaction, while the ratio of the substances on the copolymeric film produced was 5:1.68. The formal potential produced from the hydroquinone=quinone+$2H^+2e^-$reaction at the electrode of GC/p- $[Ru(v-bpy)_3]^{2+}$/vba-dopamine was 0.17 V in phosphate buffer (pH=7.10). The electrocatalytic rate was $2.58{ imes}10^5cms^{-1}$;2.41 times faster than that of non-modified one. The mass change measured by EQCM was $3.28{ imes}10^3$$gmol^{-1}$ which is larger than that of non-modified one.

• Korean Chemical Engineering Research
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• v.50 no.6
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• pp.1082-1085
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• 2012

CdTe nanoribbons feature their unique optical properties compared with CdTe nanoparticles. Slow oxidation of tellurium ions on CdTe nanoparticles resulted in the organization of individual nanoparticle into nanoribbons. The light-controlled self-assembly of CdTe nanoparticles led to twisted ribbons. It was found that irradiation improved the oxidation of tellurium ions. Transmission electron microscopy (TEM) were performed to characterize the synthesized nanostructures and showed nanowires were twisted after self-assembly. The photoluminescence was slightly blue-shifted from 550 to 544 nm. This synthetic procedure could potentially provide a key step toward the fabrication of nanowires.

• Applied Chemistry for Engineering
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• v.17 no.3
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• pp.274-279
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• 2006

To synthesize ZnO colloidal solution by a sol-gel process, zinc acetate ($C_{4}H_{6}O_{4}Zn{\cdot}2H_{2}O{\cdot}0.2\;mol$) and lithium hydroxide ($LiOH{\cdot}H_{2}O{\cdot}0.14\;mol$) in the ethanol were added to the solution containing a dispersing agent, hydroxypropyl cellulose (HPC). The nanosize and physical shape of the synthesized ZnO particles were determined by HPC acting as the dispersing agent. Nanosized ZnO particles were also obtained by a precipitation method based on zinc-2-ethylhexagonate. The precipitates were characterized by DLS, XRD, FE-SEM, and UV-vis. As the results, the ZnO colloids tend to self-assemble into a well-ordered hexagonal close-packed structure. The ZnO nanoparticles have an average diameter of nearly 40 nm with a narrow size distribution.