• Title/Summary/Keyword: 수소환원법

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Plasma pretreatment of the titanium nitride substrate fur metal organic chemical vapor deposition of copper (Cu-MOCVD를 위한 TiN기판의 플라즈마 전처리)

  • Lee, Chong-Mu;Lim, Jong-Min;Park, Woong
    • Korean Journal of Materials Research
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    • v.11 no.5
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    • pp.361-366
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    • 2001
  • It is difficult to obtain high Cu nucleation density and continuous Cu films in Cu-MOCVD without cleaning the TiN substrate prior to Cu deposition. In this study effects of plasma precleaning on the Cu nucleation density were investigated using SEM, XPS, AES, AFM analyses. Direct plasma pretreatment is much more effective than remote plasma pretreatment in enhancing Cu nucleation. Cleaning effects are enhanced with increasing the rf-power and the plasma exposure time in hydrogen plasma pretreatment. The mechanism through which Cu nucleation is enhanced by plasma pretreatment is as follows: Hydrogen ion\ulcorner in the hydrogen plasma react with TiN to form Ti and $NH_3$ Cu nucleation is easier on the Ti substrate than TiN substrate.

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Synthesis of SiC Whiskers from Rice Hulls (생왕겨를 이용한 실리콘 카바이드 합성)

  • 길경선;김종학;고인용
    • Resources Recycling
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    • v.2 no.4
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    • pp.17-22
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    • 1993
  • SiC whiskers were synthesized from rice hulls and activated carbon by carbothermal reduction method. The effects of gases and various additives were studied. Carbothermal reduction to produce SiC whiskers was conducted at $1450^{\circ}C$ and the synthesized SiC whiskers were examined using SEM and XRD. The length of whiskers is increased with the increases of $H_2$concentration and total gas flows. The most favorable form of SiC whiskers couble be obtained in the following experimental conditins : Ar : $H_2$=300:45(ml/min), $SiO_2$(inrice hulls): $CaF_2$=1:0.5:0.5(mole ratio) and the addition of Ni flakes ($1{\times}1$mm).

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Fabrication and properties of Calcium-aluminate electride thin films using by sol-gel process (Sol-Gel 법을 이용한 칼슘-알루미네이트계 전자화물 박막의 제조와 특성)

  • Kim, K.H.;Park, J.S.;Chae, J.H.;Seo, W.S.;So, S.M.;Kim, T.K.;Kim, H.S.;Lee, B.H.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.6
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    • pp.262-266
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    • 2010
  • The Calcium-aluminate electride thin films on the quartz substrates was coated by sol-gel process. The crystallization of the C12A7 thin film was observed at $800^{\circ}C$ and high density C12A7 thin film was achieved on heat treatment at $1,200^{\circ}C$ for 1 hour. The reduction heat treatment of C12A7 thin film could be converted from insulator to conductor and the electrical conductivity was 120 S/cm in the C12A7 thin film heat treated at $1,200^{\circ}C$ with $H_2$ gas for 48 hours.

Determination of brightener concentrations in Watt-type Ni Electroplating bath using dilution titration-cyclic voltammetry stripping (DT-CVS) (희석 적정-순환전류전압법을 이용한 와트욕 내부 광택제 농도 모니터링)

  • Choe, Seung-Hoe;Gwon, Yeong-Hwan;Lee, Ju-Yeol;Kim, Man;Park, Yeong-Bae;Lee, Gyu-Hwan
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.30-30
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    • 2018
  • 스마트 도금공장을 구축하기 위해서는 도금액 내부의 화학 물질 농도 변화를 측정할 수 있는 화학 센서 기술이 필수적으로 요구된다. 와트욕은 대표적인 고속 니켈 도금액 중 하나로 기본적으로 황산니켈, 염화니켈, 보릭산의 염과 함께 케리어(type-1 광택제), 광택제(type 2-광택제), 응력 제어제 등의 유기 첨가제로 구성되어 있다. 이러한 유기 첨가제는 전차된 니켈층의 두께 균일도, 조도, 미세 구조, 내부 응력 등 다양한 특성을 제어하며, 정밀한 농도 관리가 필수적으로 요구되나, 분석 기술의 부재로 인하여 지금까지도 대부분의 액관리는 할셀법이나 작업자의 경험에 의존하고 있다. Cyclic voltammetry stripping(CVS) 방법은 전기화학 분석 과정에서 나타나는 첨가제의 가속, 감속 특성 등과 여기에 수반되는 stripping peak의 변화를 이용하여 개별 첨가제의 농도를 측정하는 방법이며, 지금까지 인쇄회로기판의 비아필 공정, 전해 동박 제조, 반도체 배선 등 구리도금 산업 전반에 걸쳐 첨가제 관리에 효과적으로 적용되고 있다. 그러나 수소 발생으로 인한 stripping 효율 문제로 인하여 니켈, 주석, 아연 등 표준 환원 전위가 높은 금속 도금액 내부 첨가제 농도 측정은 아직 어려운 상황이다. 본 연구에서는 이 문제를 극복하기 위해 염소를 과량 첨가한 구리 도금액을 CVS 분석의 base 용액으로 이용하여 니켈 도금액 내부 여러 광택제 (polyetylene glycol(PEG) 계열, thiourea 계열, 2-butyne-1,4-diol 등) 농도를 측정하는 법을 제시하였다. 제시된 방법은 CVS 분석 과정에서 구리-염소 사이의 상호 작용으로 인해 생성되는 3가지 stripping peak의 상대적인 크기 변화가 첨가제 농도에 따라 영향을 받는다는 사실에 기반하였다. 본 연구에서는 여기에 관한 원인에 대해 고찰하였으며, 제시된 방법을 통해 광택제 계열 첨가제 농도 측정을 선택적으로 할 수 있다는 것을 증명하였다.

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Separation and Recovery of Tin and Indium from Spent ITO Sludge (폐 ITO 슬러지로부터 주석과 인듐의 분리·회수)

  • Lee, Ki-Woong;Kim, Hong-In;Son, Hyun-Tae;Ahn, Jae-Woo;Kim, Yong-Hwan
    • Resources Recycling
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    • v.23 no.2
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    • pp.53-60
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    • 2014
  • In order to separate Indium and Tin from spent indium tin oxide (ITO) sludge, direct hydrochloric acid leaching and thermal reduction followed by HCl leaching were applied. In case of direct leaching of spent ITO, leaching rate of In and Sn was 18.5% and 19.95%, respectively. Whereas, in case of thermal hydrogen treatment of ITO sludge at different temperatures such as $700^{\circ}C$, $800^{\circ}C$, $900^{\circ}C$ and $1100^{\circ}C$, followed by HCl leaching, we obtained the result of more than 97% leaching rate of Sn. Specially, thermal treatment at $800^{\circ}C$ showed the highest leaching rate of 98.2% of Sn. Precipitation method was used for separation and recovery of Sn from leached mixed solution. If the solution pH were adjusted 2.0, 99.69% of Sn precipitated and 10.3% of In was precipitated. This confirmed the possibility of separation of Sn and In from leached solution by precipitation method.

Growing Behaviors in Colloidal Solution of Pt Crystal for PEMFC Cathode (콜로이드 용액 내의 수소연료전지 공기극 촉매용 백금 입자 성장 속도 관찰)

  • Ham, Kahyun;Chung, Sunki;Choi, Mihwa;Yang, Seugran;Lee, Jaeyoung
    • Applied Chemistry for Engineering
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    • v.30 no.4
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    • pp.493-498
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    • 2019
  • In polymer exchange membrane fuel cells, it is crucial to fabricate a highly active and thin Pt catalyst layer for the smooth mass transport of dissolved oxygen and water. Although a highly loaded platinum (Pt) catalyst based on the hydrothermal synthesis has been reported in several studies, its growing behaviors and kinetics were yet to be understood. In this study, we investigated the growth of Pt crystal in suspension after the reduction step depending on a stirring time and evaluated the electrochemical activity. For only a couple of hours in the early stage, Pt colloids were adsorbed on the Pt-carbon catalyst and the Pt crystal was grown. After that, the small Pt colloid was formed by another nucleation step, which did not involve the growth of Pt crystal. We reveal that the Pt-Carbon catalyst with stirring for 6 h showed a high activity toward the oxygen reduction reaction.

Removal of Nitrogen Oxides Using Hydrocarbon Selective Catalytic Reduction Coupled with Plasma (플라즈마가 결합된 탄화수소 선택적 촉매환원 공정에서 질소산화물(NOx)의 저감)

  • Ihm, Tae Heon;Jo, Jin Oh;Hyun, Young Jin;Mok, Young Sun
    • Applied Chemistry for Engineering
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    • v.27 no.1
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    • pp.92-100
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    • 2016
  • Low-temperature conversion of nitrogen oxides using plasma-assisted hydrocarbon selective catalytic reduction of (HC-SCR) was investigated. Plasma was created in the catalyst-packed bed so that it could directly interact with the catalyst. The effect of the reaction temperature, the shape of catalyst, the concentration of n-heptane as a reducing agent, the oxygen content, the water vapor content and the energy density on $NO_x$ removal was examined. $NO_x$ conversion efficiencies achieved with the plasma-catalytic hybrid process at a temperature of $250^{\circ}C$ and an specific energy input (SIE) of $42J\;L^{-1}$ were 83% and 69% for one-dimensional Ag catalyst ($Ag\;(nanowire)/{\gamma}-Al_2O_3$) and spherical Ag catalyst ($Ag\;(sphere)/{\gamma}-Al_2O_3$), respectively, whereas that obtained with the catalyst-alone was considerably lower (about 30%) even with $Ag\;(nanowire)/{\gamma}-Al_2O_3$ under the same condition. The enhanced catalytic activity towards $NO_x$ conversion in the presence of plasma can be explained by the formation of more reactive $NO_2$ species and partially oxidized hydrocarbon intermediates from the oxidation of NO and n-heptane under plasma discharge. Increasing the SIE tended to improve $NO_x$ conversion efficiency, and so did the increase in the n-heptane concentration; however, a further increase in the n-heptane concentration beyond $C_1/NO_x$ ratio of 5 did not improve the $NO_x$ conversion efficiency any more. The increase in the humidity affected negatively the $NO_x$ conversion efficiency, resulting in lowering the $NO_x$ conversion efficiency at the higher water vapor content, because water molecules competed with $NO_x$ species for the same active site. The $NO_x$ conversion efficiency increased with increasing the oxygen content from 3 to 15%, in particular at low SIE values, because the formation of $NO_2$ and partially oxidized hydrocarbon intermediates was facilitated.

Characterisitics of Redox Reaction of the Magnetite Powder Prepared by Hydrothermal Synthesis (수열합성법으로 합성된 마그네타이트 분말에 대한 산화.환원 특성)

  • Park, Sung Youl;Kang, Min Pil;Rhee, Young Woo;Nam, Sung Chan
    • Korean Chemical Engineering Research
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    • v.43 no.6
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    • pp.751-755
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    • 2005
  • Carbon dioxide, included in the flue gas from the combustion of fossil fuel, was known as a representative green house gas and various removal and utilization technologies of it has been studied for the prevention of global warming. This study was performed as an effort to find out a method to reuse carbon dioxide separated from flue gas by magnetite powder. Magnetite powder was synthesized using various oxidizers and alkalinity controlled aqueous solutions of $FeSO_4{\cdot}7H_2O$ and NaOH at 50, 80, 90, $100^{\circ}C$ and analyzed by XRD and SEM. The analysis results showed that magnetite powder synthesized at higher alkalinity and temperature had crystalline spinel and cubic structure. The reduction by hydrogen and the oxidation by carbon dioxide of synthesized powder were studied by TGA. The results showed that magnetite powder synthesized at low alkalinity and temperature was non-cubical amorphous but crystalline and cubical at high alkalinity and temperature. Comparing magnetite powders synthesized using oxidants(air and oxygen) and nitrogen, magnetite powder using more oxygen containing oxidant synthesized more crystalline magnetite powder. The experimental results of redox reaction of the synthesized magnetite powder showed that the reduction by hydrogen and the oxidation by carbon dioxide were seldom observed below $400^{\circ}C$ and observed well at $500^{\circ}C$. Magnetite powder synthesized at $100^{\circ}C$ and alkalinity(molal concentration ratio of $FeSO_4{\cdot}7H_2O$ to NaOH) of 2.0 using $O_2$ showed the highest reduction of 27.15 wt% and oxidation of 26.73 wt%, especially at reaction temperature of $500^{\circ}C$.

Determination of cimetidine injection by square wave voltammetry (네모파 전압전류법에 의한 Cimetidine 주사액의 정량분석)

  • Lee, Soo-Jung;Hahn, Young-Hee
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.68-73
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    • 2010
  • In order to develop the square wave voltammetric method determining cimetidine in an ampoule for injection, $5.00{\times}10^{-4}\;M$ cimetidine HCl solutions prepared with phosphate buffers of various pH values (3.01~8.97) were investigated by SWV. The well defined single peak due to the electrochemical reduction of -C=N-C$\equiv$N- in the structure of cimetidine moved towards the cathodic direction by -0.051V/pH as the pH values were increased indicating the involvement of hydrogen in its reduction. The calibration curves of cimetidine HCl in the concentration range between $1.00{\times}10^{-5}\;M$ and $5.00{\times}10^{-3}\;M$ prepared using three phosphate buffers yielded the slopes of 127,407nA/M (pH 3.01), 115,125nA/M (pH 5.00) and 111,287nA/M(pH 7.00) with excellent linearities of $R^2{\geqq}0.9997$. When one ampoule of Tagma Inj.$^{(R)}$ was analyzed by standard addition method by SWV, the within-day precision study (n=4) on the day of sample preparation resulted in the contents of cimetidine as $203{\pm}3.8\;mg$ (102% of the specified contents, RSD of 1.9%) and the inter-day precision (n=4) through 5 days was reasonable as 1.3% of RSD.

Reaction Gas Composition Dependence on the Properties of SnO2 Films on PET Substrate by ECR-MOCVD (반응가스조성이 PET기판위에 ECR 화학증착법에 의해 제조된 SnO2 박막특성에 미치는 영향)

  • Kim, Yun-Seok;Lee, Joong-Kee
    • Journal of the Korean Electrochemical Society
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    • v.8 no.3
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    • pp.139-145
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    • 2005
  • [ $SnO_x$ ] films on the flexible substrate of PET film were prepared at ambient temperature under a $(CH_3)_4Sn(TMT: tetra-methyl tin)-H_2-O_2$ atmosphere in order to obtain transparent conductive polymer by using ECR-MOCVD(Electro Cyclotron Resonance Metal Organic Chemical Yfpor Deposition) system. The prepared $SnO_x$ thin films show generally over $90\%$ of optical transmittance at wavelength range of 380-780nm and about $1\times10^{-2\~3}ohm{\cdot}cm$ of electrical resistivity. In the present study, effects of $O_2/TMT\;and\;H_2/TMT$ mole ratio on the properties of $SnO_x$ films are investigated and the other process parameters such as microwave power, magnetic current power, substrate distance and working pressure are fixed. Based on our experimental results, the $SnO_x$ film composition ratio of Sn and O directly influences on the electrical and optical properties of the films prepared. The $SnO_x$ film with low electric resistivity and high transmittance could be obtained by controlling the process parameters such as $O_2/TMT\;and\;H_2/TMT$ mole ratio, which play an important role to change the composition ratio between Sn and O. An increase of $O_2/TMT$ mole ratio brought on the increases 0 content in the $SnO_x$ film. On the other hand, an increase of $H_2/TMT$ mole ratio lead to decreases the oxygen content in the film. The optimized composition ratio of oxygen : tin Is determined as 2.4: 1 at $O_2/TMT$ of 80 and $H_2/TMT$ of 40 mole ratio, respectively.