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The Effect of the Crystalline Phase of Zirconia for the Dehydration of Iso-propanol (이소프로판올의 탈수반응에서 지르코니아 촉매의 결정상에 따른 영향)

  • Sim, Hye-In;Park, Jung-Hyun;Cho, Jun Hee;Ahn, Ji-Hye;Choi, Min-Seok;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.208-213
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    • 2013
  • Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

Preparation of ZnO/SiO2 Nano-Composition and Photocatalysts and Antibacterial Activity (ZnO/SiO2 나노 입자의 화학적 합성과 광촉매 및 항균성 특성에 관한 연구)

  • Kim, Jae-Uk;Yuk, Young-Sam;Kim, Jong-Gyu
    • Journal of the Korean Chemical Society
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    • v.61 no.4
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    • pp.179-184
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    • 2017
  • In this paper, a $ZnO/SiO_2$ nano-composite was prepared by a simple chemical method at room temperature. For the synthesis of ZnO nanoparticles (NPs), a sonochemical method was used, and $SiO_2$ NPs were prepared by precipitation method. The formation of $ZnO/SiO_2$ NCs was characterized by X-ray diffractometer (XRD) and confirmed by field-emission scanning electron microscopy (FE-SEM) and Fourier transform infra-red spectroscopy(FT-IR). The photocatalytic properties of $ZnO/SiO_2$ NCs formed at different concentrations of $SiO_2$ were evaluated by rhodamine-B dye. It was confirmed that increasing $SiO_2$ concentration resulted in an increase in the photocatalytic property. In addition, the antibacterial activity of $ZnO/SiO_2$ NCs was conducted against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). As a result, the antibacterial activities of E.coli and S. aureus were increased in the presence of thick SiO NPs layer.

A Study on the Low Temperature Epitaxial Growth of $CoSi_2$ Layer by Multitarget Bias cosputter Deposition and Phase Sequence (Multitarget Bias Cosputter증착에 의한 $CoSi_2$층의 저온정합성장 및 상전이에 관한 연구)

  • Park, Sang-Uk;Choe, Jeong-Dong;Gwak, Jun-Seop;Ji, Eung-Jun;Baek, Hong-Gu
    • Korean Journal of Materials Research
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    • v.4 no.1
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    • pp.9-23
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    • 1994
  • Epitaxial $CoSi_2$ layer has been grown on NaCl(100) substrate at low deposition temperature($200^{\circ}C$) by multitarget bias cosputter deposition(MBCD). The phase sequence and crystallinity of deposited silicide as a function of deposition temperature and substrate bias voltage were studied by X-ray diffraction(XRD) and transmission electron microscopy(TEM) analysis. Crystalline Si was grown at $200^{\circ}C$ by metal induced crystallization(M1C) and self bias effect. In addition to, the MIC was analyzed both theoretically and experimentally. The observed phase sequence was $Co_2Si \to CoSi \to Cosi_2$ and was in good agreement with that predicted by effective heat of formation rule. The phase sequence, the CoSi(l11) preferred orientation, and the crystallinity had stronger dependence on the substrate bias voltage than the deposition temperature due to the collisional cascade mixing, the in-situ cleaning, and the increase in the number of nucleation sites by ion bombardment of growing surface. Grain growth induced by ion bombardment was observed with increasing substrate bias voltage at $200^{\circ}C$ and was interpreted with ion bombardment dissociation model. The parameters of $E_{Ar}\;and \alpha(V_s)$ were chosen to properly quantify the ion bombardment effect on the variation in crystallinty at $200^{\circ}C$ with increasing substrate bias voltage using Langmuir probe.

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Synthesis and Properties of Polyurethane/Clay Nanocomposites Containing Siloxane Segment (실록산 세그먼트를 가진 폴리우레탄/점토 나노복합체의 제조 및 물성에 관한 연구)

  • Lee Jung Eun;Kim Hyung Joong
    • Polymer(Korea)
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    • v.29 no.2
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    • pp.177-182
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    • 2005
  • Montmorillonite (MMT) modified with siloxane diamine was reacted with a reactant obtained from 4,4'-diphenyl methane diisocyanate (MDI) and polyester type polyol, $Nippollan4010(\bar{M}_n2000)$. Finally, polyurethane (PU)/MMT composites were prepared by using 1,4-butane diol as a chain extender in $25\;wt\%$ solution of N,N-dimethyl acetamide (DMAc). It was expected that these nanocomposites had superior exfoliation property to that of MMT dispersed polyurethanes produced by simple mixing due to insertion of siloxane main chain to the silicate interlayer of MMT. Extent of reaction and formation of final products were analysed by using FT-IR spectroscopy. Dispersion into the PU and intercalation of MMT were identified by applying X-ray diffraction (XRD) and transmission electron microscopy (TEM). Tensile data were acquired by universal test machine (UTM). Thermal stability and variation of surface energy were characterized by thermal gravimetric analysis (TGA) method and measurement of contact angle on the synthesized composites, respectively. As the results the organo-MMT modified with siloxane diamine in the PU composites has an intercalated structure relatively well-expanded rather than a completely exfoliated structure. The tensile strengths and the moduli for the PU/organo-MMT composites were drastically enhanced in comparison to those of $PU/Na^+-MMT$ composites.

The Electrical, Optical and Structural Characteristics of ITO Films Formed by RF Reactive Magnetron Sputtering (저온 스퍼터링법으로 증착된 ITO박막의 온도 변화에 따른 구조, 표면 및 전기적 특성)

  • Lee, Seok-Ryoul;Choi, Jae-Ha;Kim, Ji-Soo;Jung, Jae-Hak;Lee, Lim-Soo;Kim, Jae-Yeal
    • Journal of the Korean Vacuum Society
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    • v.20 no.1
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    • pp.30-34
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    • 2011
  • We investigated the structural, electrical and optical characteristics of thin films with ITO deposited by a low temperature RF reactive magnetron sputtering. The deposited thin films were annealed for 2 hours at various temperatures of $50^{\circ}C$, $100^{\circ}C$, $150^{\circ}C$, $200^{\circ}C$ and $250^{\circ}C$ and were analyzed by using X-ray diffractometer, scanning electron microscopy and 4 point probe. The films annealed at temperatures higher than $150^{\circ}C$ were found to be crystallized and their electrical resistance were decreased from $40{\Omega}cm$to $18{\Omega}cm$. The optical transmittance of the film annealed at $150^{\circ}C$ was increased by over 87% in the 450 nm ~ 900 nm wavelength range. Our results indicate that the films with ITO deposited at even a low temperature can show better optical and electrical properties through a proper heat treatment.

Synthesis and Crystal Structure of Amorphous Calcium Carbonate by Gas-Liquid Reaction of System CaO-$C_2 H_5 OH$-$CO_2$ (CaO-$C_2 H_5 OH$-$CO_2$계의 기.액반응에 의한 비정질 탄산칼슘의 합성 및 결정구조)

  • Im, Jae-Seok;Im, Goeng
    • The Journal of Engineering Research
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    • v.6 no.1
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    • pp.97-109
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    • 2004
  • The synthesis and crystal structure of amorphous calcium carbonate obtained from gas-liquid reaction of CaO-$C_2 H_5 OH$-$CO_2$ system according to change of added amount of calcium oxide by blowing $CO_2$ gas and reaction time using ethanol and ethylene glycol were investigated by electric conductivity, X-ray diffraction, and scanning electron microscope. The powdery or gelatinous phases were prepared by passing $CO_2$ gas at a flow rate of 1$\ell$/min into the suspensions containing 10~40g of CaO in mixing solutions 900ml of $C_2 H_5 OH$- and 100ml of ethylene glycol. By rapid filtration and drying the both phases at $60^{\circ}C$ under reduced pressure, the phases converted to the spherical vaterite and amorphous phase. The stable phase of amorphous calcium carbonate(ACC) was formed in the region pH 7-9 but the formation regions of amorphous phase were remarkably affected by pH in the mother liquor. It seems that a part of ACC changed into chain calcite as an intermediate products. The initial reactants prior to the formation of precipitated calcium carbonate is ACC. And ACC is unstable in the aqueous solution and crystallizes finally to calcite by the through-solution reaction. Especially ACC was produced or gelatinous phase which precipitated from the reaction of CaO-$C_2 H_5 OH$-$CO_2$ system.

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Preparation of epitaxial bismuth titanate thin films by the sol-gel process (졸-겔법을 이용한 Epitaxial Bismuth Titanate 박막의 제조)

  • 김상복;이영환;윤연흠;황규석;오정선;김병훈
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.2
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    • pp.56-62
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    • 2003
  • Epitaxial $Bi_4Ti_3O_{12}$ films on $SrTiO_3$(100), L$aA1O_3$(100) and MgO(100) were prepared by sol-gel process using metal naphthenate as a starting material. As-deposited films were pyrolyzed at $500^{\circ}C$ for 10 min In air and annealed at $750^{\circ}C$ for 30 min in air. Crystallinity and in-plane alignment of the film were investigated by X-ray diffraction $\theta$-2$\theta$ scan and P scanning. A field emission-scanning electron microscope and an atomic force microscope were used for characterizing the surface morphology and the surface roughness of the film. The film prepared on MgO(100) showed the most poor crystallinity and in-plane alignment, compared to those on the other substrates. While the films on $LaA1O_3$(100) and $SrTiO_3$(100) having high crystallinity and in-plane alignment showed the form of columnar grain growth, the film on MgO(100) which had poor crystallinity showed the form of acicula grain growth.

A Study on the Preparation of Electrolytic Manganese Dioxide (전해 이산화망간 제조에 관한 연구)

  • Lee Mook Lee;Jae Won Kim;Ung Up Chi;Jong Ju Shin
    • Journal of the Korean Chemical Society
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    • v.17 no.4
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    • pp.306-313
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    • 1973
  • With the intention of obtaining technical data for the industrial production of ${\gamma}-MnO_2$ for dry cell depolarizer by electrolytic oxidation of acidic manganese sulfate solution made from domestic rhodochrosite, optimum conditions of ore leaching, purification of leached solution and electrolytic oxidation of divalent manganes to tetravalent were investigated using simulated micro pilot plant having a production capacity of 4 kg of $MnSO_4$ per day. The nature and quality of the products were investigated by means of chemical analysis, DTA, X-ray diffraction and electron microscopy. The cell activity of $MnO_2$were examined by cell discharging character measurements. The optimum electrolysis conditions were as follow: Temperature of the electrolyte, above $90^{\circ}C$; current density, 0.7${\sim}A/dm^2$; anode materials, graphite or lead ; concentration of electrolyte, $MnSO_4 50{\sim}150g/l $ g/l and $H_2SO_4/MnSO_4 = 0.15{\sim}0.25$. Under the best condition the current efficiency was 99% and the products were almost pure ${\gamma}-MnO_2$. The cell discharging character were good and almost the same as that of regular grade commercial electrolytic manganese dioxide.

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Mineralogical Properties and Paragenesis of H-smectite (H-스멕타이트의 광물학적 특성과 생성관계)

  • Noh, Jin-Hwan;Hong, Jin-Sung
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.4
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    • pp.377-393
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    • 2010
  • Pumiceous tuffs occurring in the Beomgockri Group are examined applied-mineralogical characteristics and their controling factors to evaluate their potentials as the adsorption-functional mineral resources. The pumiceous tuffs are diagenetically altered to low-grade zeolitcs and bentonites in the Janggi area. Compositional specialty due to the presence of pumice fragments induces the altered tuffs to exhibit the characteristic adsorption property combined with cation exchange capacity, specific surface area, and acidic pH. Unusual lower pH in the adsorption-functional mineral substances is turned out to be originated from the presence of H-smectite having $H^+$ in the interlayer site of the sheet structure. On account of disordered crystallinity resulting from the exchanged $H^+$ in the interlayer site, the smectite commonly forms crenulated edges in the planar crystal form and exhibits characteristic X-ray diffraction patterns showing comparatively lower intensities of basal spacings including (001) peak than conventional Ca-smectite. Based on the interpretation of paragenetic relations and precursor of the H-smectite, a genetic model of the peculiar clay mineral was proposed. The smectite formation may be facilitated resulting from the precipitation of opal-CT at decreasing pH condition caused by the release of H+ during diagenetic alteration of pumice fragments. Because of the acidic smectite, the low-grade mineral resources from the Beomgockri Group may be applicable to the adsorption industry as the raw materials of acid clays and bed-soil.

Crystallinity and Chemical Reactivity of Bimessite(δ-MnO2) Influenced by Iron (철에 의한 버네사이트의 결정도 및 화학적 활성의 변화)

  • Kim, Jae-Gon
    • Korean Journal of Soil Science and Fertilizer
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    • v.32 no.4
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    • pp.327-332
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    • 1999
  • Manganese (Mn) oxides in soils have been a research subject since they react with nutrients and contaminants and Mn itself is an essential element for plant growth. Birnessite was synthesized in the presence of iron (Fe) in the precipitating solution. Influence of Fe, one of common elements in soils, on crytallinity, morphology, and chemical reactivity of birnessite was examined using X-ray diffraction (XRD), electron microscope, canon exchange capacity (CEC), and chromium (Cr) oxidation capacity. With increasing Fe concentration in the precipitating solution, crystallinity and crystal size decreased. Hexagonal plates of the birnessites formed at low Fe concentration were dominant and replaced more and more by aggregate of small particles with increasing the Fe concentration. There is no significant change in CEC with changing the Fe concentration. Chromium oxidation capacity of the birnessite increased with increasing the Fe concentration. Iron in the precipitating solution poisoned crystal growth by adsorption on the surface and increased nucleation. Since Fe is a common constituent under pedogenic environment and Fe and Mn oxides often coexist in Mn oxide nodules, the birnessite with small particle, low crystallinity, and high chemical reactivity is the form which is more likely to be formed in soils. The high CEC ($140cmol_ckg^{-1}$) and oxidation capacity of birnessite indicate that birnessite can be used in environment and agriculture.

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