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Deposition of ZrO$_2$ and TiO$_2$ Thin Films Using RF Magnet ron Sputtering Method and Study on Their Structural Characteristics

  • Shin, Y.S.;Jeong, S.H.;Heo, C.H.;Bae, I.S.;Kwak, H.T.;Lee, S.B.;Boo, J.H.
    • Journal of the Korean institute of surface engineering
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    • v.36 no.1
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    • pp.14-21
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    • 2003
  • Thin films of ZrO$_2$ and TiO$_2$ were deposited on Si(100) substrates using RF magnetron sputtering technique. To study an influence of the sputtering parameters, systematic experiments were carried out in this work. XRD data show that the $ZrO_2$ films were mainly grown in the [111] orientation at the annealing temperature between 800 and $1000^{\circ}C$ while the crystal growth direction was changed to be [012] at above $1000^{\circ}C$. FT-IR spectra show that the oxygen stretching peaks become strong due to $SiO_2$ layer formation between film layers and silicon surface after annealing, and proved that a diffusion caused by either oxygen atoms of $ZrO_2$ layers or air into the interface during annealing. Different crystal growth directions were observed with the various deposition parameters such as annealing temperature, RF power magnitude, and added $O_2$ amounts. The growth rate of $TiO_2$ thin films was increased with RF power magnitude up to 150 watt, and was then decreased due to a sputtering effect. The maximum growth rate observed at 150 watt was 1500 nm/hr. Highly oriented, crack-free, stoichiometric polycrystalline $TiO_2$<110> thin film with Rutile phase was obtained after annealing at $1000^{\circ}C$ for 1 hour.

Degradation Characteristics of Wood Cellulose by Ruminal Cellulolytic Anaerobic Bacterium Ruminococcus albus F-40 (혐기성 세균 Ruminococcus albus F-40에 의한 목재 cellulose의 분해특성)

  • Kim, Yoon-Soo;Wi, Seung-Gon;Myung, Kyu-Ho
    • Journal of the Korean Wood Science and Technology
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    • v.25 no.3
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    • pp.83-95
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    • 1997
  • The degradation mode of lignocellulose by anaerobic ruminal cellulolytic bacterium Ruminococcus albus F-40 was investigated. Birchwood holocellulose and filter paper were incubated as the sole carbohydrate sources with using the Hungate techniques. After 2 or 4 days of incubation, samples were employed for chemical and electron microscopic evaluations. The degradation rate of cellulosic substrates and the adhesion rate of bacteria to the substrates increased proportionally with the decrease of relative crystallinity of cellulose, indicating the preferential breakdown of amorphous cellulose, by this bacterium. X-ray diffraction analyses and polarized light microscopy showed, however, that crystalline cellulose was also degraded by R. albus. FT-IR spectra indicated that not only cellulose but hemicellulose was also degraded by this bacterium. Electron microscopic investigations showed the protuberant structures on the surface of R. albus. These structures were much more significant when bacterial cells were grown in the media containing insoluble substrates, such as cellulose, indicating clearly that bacterial protuberant structures were induced by the substrates. Protuberant structures extended from the bacterial cells adhered tightly to the substrates and numerous vesicles covered the surface of cellulosic substrates affected. Cellulosome-like structures were distributed on the cellulose matrix. Electron microscopic works showed that diverse surface organells of R. albus were involved in the degradation of cellulosic materials. SEM examinations showed the breakdown of cellulose by R. albus was proceeded by severeal routes : short fiber formation, defibrillation and destrafication of cellulose microfibril.

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Kinetics and Mechanism of the Oxidation of Alcohols by C9H7NHCrO3Cl (C9H7NHCrO3Cl에 의한 알코올류의 산화반응에서 속도론과 메카니즘)

  • Park, Young-Cho;Kim, Young-Sik;Kim, Soo-Jong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.8
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    • pp.378-384
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    • 2018
  • $C_9H_7NHCrO_3Cl$ was synthesized by reacting $C_9H_7NH$ with chromium (VI) trioxide. The structure of the product was characterized by FT-IR (Fourier transform infrared) spectroscopy and elemental analysis. The oxidation of benzyl alcohol by $C_9H_7NHCrO_3Cl$ in various solvents showed that the reactivity increased with increasing dielectric constant(${\varepsilon}$) in the following order: DMF (N,N'-dimethylformamide) > acetone > chloroform > cyclohexane. The oxidation of alcohols was examined by $C_9H_7NHCrO_3Cl$ in DMF. As a result, $C_9H_7NHCrO_3Cl$ was found to be an efficient oxidizing agent that converts benzyl alcohol, allyl alcohol, primary alcohols, and secondary alcohols to the corresponding aldehydes or ketones (75%-95%). The selective oxidation of alcohols was also examined by $C_9H_7NHCrO_3Cl$ in DMF. $C_9H_7NHCrO_3Cl$ was the selective oxidizing agent of benzyl, allyl and primary alcohol in the presence of secondary ones. In the presence of DMF with an acidic catalyst, such as $H_2SO_4$, $C_9H_7NHCrO_3Cl$ oxidized benzyl alcohol (H) and its derivatives ($p-OCH_3$, $m-CH_3$, $m-OCH_3$, m-Cl, and $m-NO_2$). Electron donating substituents accelerated the reaction rate, whereas electron acceptor groups retarded the reaction rate. The Hammett reaction constant (${\rho}$) was -0.69 (308K). The observed experimental data were used to rationalize hydride ion transfer in the rate-determining step.

A Study on the Characteristics of CO Oxidation by NO Poisoning in Pt/TiO2 Catalyst (Pt/TiO2 촉매에서의 NO 피독에 의한 CO 산화반응특성 연구)

  • Kim, Min Su;Kim, Se Won;Hong, Sung Chang
    • Clean Technology
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    • v.25 no.4
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    • pp.296-301
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    • 2019
  • This study was conducted to investigate the characteristics of CO oxidation by NO poisoning in Pt/TiO2 catalyst prepared by wet impregnation method and calcined at 400 ℃. In order to confirm the NO poisoning effect of the Pt/TiO2 catalyst, the change of reaction activity was observed when NO was injected during the CO+O2 reaction where it was ascertained that the CO conversion rate rapidly decreased below 200 ℃. Also, CO conversion was not observed below 125 ℃. Recovery of initial CO conversion was not verified even if NO injection was blocked at 125 ℃. Accordingly, various analyses were performed according to NO injection. First, as a result of the TPD analysis, it was confirmed that NO pre-adsorption in catalyst inhibited CO adsorption and conversion desorption from adsorbed CO to CO2. When NO was pre-adsorbed, it was confirmed through H2-TPR analysis that the oxygen mobility of the catalyst was reduced. In addition, it was validated through FT-IR analysis that the redox cycle (Pt2+→Pt0→Pt2+) of the catalyst was inhibited. Therefore, the presence of NO in the Pt/TiO2 catalyst was considered to be a poisoning factor in the CO oxidation reaction, and it was determined that the oxygen mobility of the catalyst is required to prevent NO poisoning.

Chromium(VI) Removal from Aqueous Solution using Acrylic Ion Exchange Fiber (아크릴계 이온교환섬유를 이용한 수중 크롬(VI) 제거)

  • Nam, Aram;Park, Jeong-Ann;Do, Taegu;Choi, Jae-Woo;Choi, Ungsu;Kim, Kyung Nam;Yun, Seong-Taek;Lee, Sanghyup
    • Journal of Korean Society of Environmental Engineers
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    • v.39 no.3
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    • pp.112-117
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    • 2017
  • Ion exchange fiber, PADD was synthesized by the reaction between PAN based acrylic fiber and DETA with $AlCl_3{\cdot}6H_2O$, and was analyzed by FT-IR and SEM to investigate its characteristics. The experimental results of Cr(VI) removal by PADD were better fitted with Langmuir adsorption isotherm, and the maximum uptake value ($Q_{max}$) was calculated to be 6.93 mmol/g. The kinetic data can be well described by Lagergen pseudo-second order rate model. The Cr(VI) adsorption capacity of PADD was 4.11 mmol/g at pH 2, which shows the effect of pH changes on the removal of Cr(VI). The adsorption selectivity of Cr(VI) was higher than phosphate and As(V). Total ion exchange capacity of PADD was 4.70 mmol/g, which was measured by acid-base back titration.

Study on the hydrophobic modification of zirconia surface for organic-inorganic hybrid coatings (유-무기 하이브리드 코팅액 제조를 위한 지르코니아 표면의 소수화 개질 연구)

  • Lee, Soo;Moon, Sung Jin;Park, Jung Ju
    • Journal of the Korean Applied Science and Technology
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    • v.34 no.2
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    • pp.260-270
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    • 2017
  • Zirconia has white color and physical, chemical stability, also using in high temperature materials and various industrial structural ceramics such as heat insulating materials and refractories due to their low thermal conductivity, excellent strength, toughness, and corrosion resistance. If hydrophobically modified zirconia is introduced into a hydrophobic acrylate coating solution, the hardness, chemical, electrical, and optical properties will be improved due to the better dispersibility of inorganic particle in organic coating media. Thus, we introduced $-CH_3$ group through silylation reaction using either trimethylchlorosilane(TMCS) or hexamethyldisilazane(HMDZ) on zirconia surface. The $Si-CH_3$ peaks derived from TMCS and HMDZ on hydrophobically modified zirconia surface was confirmed by FT-IR ATR spectroscopy, and introduction of silicon was confirmed by FE-SEM/EDS and ICP-AES. In addition, the sedimentation rate result in acrylate monomer of the modified zirconia showed the improved dispersibility. Comparison of the sizes of a pristine and the modified zirconia particles, which were clearly measured not by the normal microscope but by particle size analysis, provided a pulverizing was occurred by physical force during the silylation process. From the BET analysis data, the specific surface area of zirconia was approximately $18m^2/g$ and did not significantly change during modification process.

Studies on the Micelle Formation of Surfactant Solution(2) - Self-Diffusion by Phase Transition in Ternary System of Surfactant/Hydrocarbon/Water - (계면활성제 수용액에서 미셀형성(제2보) - 계면활성제/탄화수소/물의 상 변화에 따른 자기확산 -)

  • Choi, Seung Ok;Lee, Jin Hee;Kim, Sang Chun;Nam, Ki Dae
    • Applied Chemistry for Engineering
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    • v.10 no.1
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    • pp.112-117
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    • 1999
  • The pulsed field gradient NMR method has been used to determine self-diffusion coefficients in ternary N-alkyl-N, N-dimethylamine oxide/hydrocarbon/$D_2O$ system. For n = 12, 14, 16 and n' = 8, 10, 12, 14, 16, in the micellar phase, diffusion is chiefly governed by the hydrodynamic transport of micelles, supplemented by an exchange of solubilized hydrocarbon upon micellar collisions. This investgation is performed by variations in both the surfactant alkyl chain length and in the size of the hydrocarbon molecules. In cubic phases, the solvent still exhibits values of the diffusion coefficients which are typical for motion in a continuous water phase, with the microemulsion droplets acting as obstacle. Mobilities of the surfactant in the gel state were low and have been determined only for the surfactant($C_{12}DMAO$) with the shortest alkyl chain length. Exchange of hydrocarbon between micellar entities in the gel was found to be occured by a hopping process, the associated rate decreased with alkyl chain length of the surfactant.

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Effect of $N_2$-back-flushing Time and TMP in Lake Water Treatment Using Multichannel Ceramic Microfiltration Membranes (다채널 세라믹 정밀여과막으로 호소수 처리시 질소 역세척 시간 및 막간 압력차의 영향)

  • Park, Jin-Yong;Park, Bo-Reum
    • Membrane Journal
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    • v.17 no.2
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    • pp.124-133
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    • 2007
  • In this study, we treated lake water by 2 kinds of multichannel ceramic micro filtration membranes. We could investigate effects of $N_2-back-flushing$ time (BT) and transmembrane pressure (TMP), and find optimal operating conditions. The BT were changed in $10{\sim}60$ sec, TMP in $0.6{\sim}2.0$ bar at fixed filtration time (FT) 8 min, flow rate 2.0 L/min and back-flushing pressure 2.0 bar. Also, the optimal conditions were discussed in the viewpoints of resistance of membrane fouling $(R_f)$, dimensionless permeate flux $(J/J_o)$, permeate flux (J) and total permeate volume $(V_T)$. As result, optimal back-flushing conditions for HC04 ($0.4{\mu}m$ pore size) and HC10 membrane $(1.0{\mu}m)$ were BT=10 sec and BT=20 sec, respectively. Then, higher TMP should increase the driving force, and could produce more VT. Average rejection rates of pollutants were higher than 95.4% for turbidity, $12.7{\sim}20.1%\;for\;COD_{Mn},\;0.0{\sim}6.4%\;for\;NH_3-N,\;1.9{\sim}4.6%$ for T-N and $34.9{\sim}88.4%$ for T-P.

APPLICATION STUDY OF CHEMOINFOMETRICAL NEAR-INFRARED SPECTROSCOPY IN PHARMACEUTICAL INDUSTRY

  • Otsuka, Makoto;Kato, Fumie;Matsuda, Yoshihisa
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.2111-2111
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    • 2001
  • A chemoinfometrical method for evaluating the quantitative determination of crystallinity one polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the and compared with the conventional powder X-ray diffraction method was performed. [Method] The pPure a and g forms of indomethacin (IMC) were prepared by reportedusing published methods. Six kinds of standard samples obtained by physically mixing of a and g forms. After the powder X-ray diffraction profiles of samples have been measured, the intensity values were normalized to against the intensity of silicon powder as the as an external standard. The calibration curves for quantification of crystal content were based upon the total relative intensity of four diffraction peaks from of the form g crystal. FT-NIR spectra of six calibration sample sets were recorded 5 times with the NIR spectrometer (BRAN+LUEBBE). Chemoinfometric analysis was performed on the NIR spectral data sets by applying the principal component regression (PCR). [Results] The relation between the actual and predicted polymorphic contents of form g IMC measured using by the X-ray diffraction method shows a good straight linen linear relation., and it has slope of 0.023, an intercept of 0.131 and a correlation coefficient of 0.986. PCR analyses wereis was performed based on normalized NIR spectra sets offer standard samples of known content of IMC g form. IMC. A calibration equation was determined to minimize the root mean square error of the predictionthe prediction. Figure 1 shows a plot of the calibration data obtained by NIR method between the actual and predicted contents of form g IMC. The predicted values were reproducible and had a smaller standard deviation. Figure 2 shows that the plot for the predicted transformation rate (%) of form a IMC to form g as measured by X-ray diffractomeoy against to those as measured by NIR method. The plot has a slope of 1.296, an intercept of 1,109, and a correlation coefficient of 0.992. The line represents a satisfactory correlation between the two predicted values of form g IMC content. Thus NIR spectroscopy is an effective method for the evaluation to the pharmaceutical products of quantitative of polymorph.

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Effect of Immobilization Method in the Biosorption and Desorption of Lead by Algae, Chlorella pyrenoidosa (Chlorella pyrenoidosa에 의한 납 흡.탈착시 고정화 방법의 영향)

  • Shin, Taek-Soo;Lim, Byung-Seo;Lee, Sang-Woo;Rhu, Kwon-Gul;Jeong, Seon-Ki;Kim, Kwang-Yul
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.8
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    • pp.663-672
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    • 2009
  • In this studies, the adsorption test using Chlorella pyrenoidosa was conducted to examine the effect of Pb adsorption according to various immobilized methods such as Ca-alginate, K-carrageenan, and Polyacrylamide. From the results, the duration to need to reach adsorption equilibrium was delayed according to the immobilization. And, the higher adsorption capacity of immobilized Chlorella pyrenoidosa was represented in the higher concentration of Pb, the smaller amount of immobilizing agent, and the higher pH of solution. The maximum adsorption capacity of Pb was shown in the adsorption test using Chlorella pyrenoidosa immobilized with Ca-alginate even though it was sensitive pH. The adsorption results properly represented with Freundlich isotherm equations. And, pseudo second-order chemisorption kinetic rate equation was applicable to all the biosorption data over the entire time range. The FT-IR analysis showed that the mechanism involved in biosorption of Pb by Chlorella pyrenoidosa was mainly attributed to Pb binding of carbo-acid and amide group. Adsorbed Pb on immobilized Chlorella prenoidosa was easily desorbed in the higher concentration of desorbents(NTA, HCl, EDTA, $H_2SO_4,\;Na_2CO_3$). Among the several desorbents, NTA showed the maximum desoption capacities of Pb from Chlorella pyrenoidosa immobilized with Ca-alginate and K-carrageenan and EDTA was the most effective in Chlorella pyrenoidosa immobilized with polyacrylamide. The desoprtion efficiency in the optimum condition was 90.0, 83.0, and 80.0%, respectively.