• Title/Summary/Keyword: X-ray Diffractometer

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Titanium oxide-based photocatalysts for highly efficient hydrogen generation ($TiO_2$ 기반 고효율 광촉매의 수소 생산)

  • Choe, Jin-Yeong;Park, Won-Ung;Jeon, Jun-Hong;Mun, Seon-U;Kim, Eun-Gyeom;Im, Sang-Ho;Han, Seung-Hui
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.215-215
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    • 2012
  • 급속한 산업의 발달은 심각한 환경오염 및 에너지 문제를 가져왔다. 이를 해결하기 위한 방안으로 수소에너지에 대한 관심이 증가하고 있으며, 수소에너지를 생산하는 방법 중 하나로 태양에너지를 원천으로 하는 광촉매(photocatalyst)에 대한 연구가 점차적으로 증가하고 있는 추세이다. 현재 광촉매로 가장 많이 사용되는 $TiO_2$의 경우, 뛰어난 광활성과 저렴한 가격, 광 안정성, 화학적 안정성을 가짐에도 불구하고, 3.2 eV라는 넓은 band gap을 가지기 때문에 385 nm 이상의 긴 파장을 갖는 가시광선은 흡수할 수 없다. 또한, 광촉매 반응과정 중 recombination으로 인한 효율의 손실이 크기 때문에 이러한 문제들을 해결하기 위해 많은 연구가 진행되어 왔다. 본 연구에서는 ICP-assisted DC magnetron sputtering 방법을 이용하여 높은 결정성을 갖는 $TiO_2$ 박막을 제조하였다. 제작된 $TiO_2$ 박막은 높은 광촉매 특성을 나타냈으며, 또한 $TiO_2$의 anatase phase와 rutile phase의 bilayer structure를 통하여 recombination을 감소시킴으로써 높은 효율을 갖는 광촉매를 제작하였다. 박막의 chemical state와 crystallinity를 확인하기 위하여 X-ray photoelectron spectroscopy와 X-ray diffractometer를 이용하여 분석을 수행하였으며, 물 분해 장치(water splitting device)를 제작하여 수소와 산소 생성시 흐르는 전류를 측정하여 광촉매 특성을 평가하였다.

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Photocatalytic Degradation of Oxytetracycline Using Co-precipitation Method Prepared Fe2O3/TiO2 Nanocomposite

  • Jia, Yuefa;Liu, Chunli;Li, Rong
    • Journal of Magnetics
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    • v.21 no.1
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    • pp.46-50
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    • 2016
  • $Fe_2O_3/TiO_2$ nanocomposite were successfully synthesized by co-precipitation method using $Fe(NO_3)_3{\cdot}9H_2O$ and $Ti(SO_4)_2$ as raw materials. Structural and textural features of the mixed oxide samples were characterized by X-ray diffractometer, field emission scanning electron microscopy and energy-dispersive X-ray. The effects of initial concentration of oxytetracycline (OTC), different competitive ions and organics on the photocatalytic degradation rate of OTC by the $Fe_2O_3/TiO_2$ nanocomposite were analyzed under UV and visible light irradiation. The results indicate that the optimized initial concentration of OTC was 50 mg/L to achieve the best photocatalytic efficiency. $Cu^{2+}$, $NH_4{^+}$, $C_3H_8O$ and EDTA in the aqueous suspension were found to suppress the degradation rate of OTC, whereas the effect of $NO_3{^-}$ and $H_2C_2O_4$ can be ignored.

The Characteristic of Formation CoSi2/Si Thin Film by the RF-Sputtering Method (RF-Sputtering법에 의한 CoSi2/Si 박막 형성에 관한 특성)

  • Cho, Geum-Bae;Lee, Kang-Yoen;Choi, Youn-Ok;Kim, Nam-Oh;Jeong, Byeong-Ho
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.59 no.7
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    • pp.1255-1258
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    • 2010
  • In this paper, the $CoSi_2$ thin films with thicknesses of about $5{\mu}m$ were deposited on n-type silicon (111) substrates by RF magnetron sputtering method using a $CoSi_2$ target (99.99%). The flow rate of argon of 50 sccm, substrate temperature of $100^{\circ}C$, RF power of 60 watts, deposition time of 30 minutes, and the vacuum of $1\times10^{-6}$ Torr. The annealing treatments of the $CoSi_2$ thin film were performed from 500, 700 and $900^{\circ}C$ for 1h in air ambient by an electric furnace. In order to investigate the $CoSi_2$ thin film X-ray diffraction patterns were measured using the X-ray diffractometer (XRD). The structure of the thin films were investigated by using scanning the electron microscope (SEM) were used for review. The surface morphology of the thin films was measured with a atomic force microscopy (AFM). Temperature dependence of sheet resistivity and property of Hall effect was measured in the $CoSi_2$ thin film.

Determination of crystallinity index of cellulose depending on sample preparation and analysis instruments (시료 조건 및 측정방법에 따른 셀룰로오스의 결정화도 평가)

  • Ahn, Jung-Eon;Youn, Hye-Jung;Joung, Yang-Jin;Kim, Tae-Young
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.44 no.4
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    • pp.43-50
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    • 2012
  • The crystallinity index is an important characteristic of cellulose. The crystallinity value is different depending on the adopted instrument. In this study, we determined a crystallinity index of cotton and wood celluloses using wide-angle X-ray scattering (WAXS), powder X-ray diffractometer (PXRD), and cross polarization/magic angle spinning solid-state $^{13}C$ nuclear magnetic resonance spectroscopy (CP/MAS solid-state $^{13}C$ NMR). The specimen was prepared in forms of powder, sheet and pallet. With the comparison of the obtained crystallinity indices of the cellulose, the effects of the analysis instrument, the sample preparation and analysis method were investigated. Among three instruments, the crystallinity indices by PXRD and NMR had a good relationship and reproducibility, and WAXS gave the crystallinity index with poor reproducibility. In the case of analysis methods of crystallinity indices, the Segal method showed higher value than that of the Ruland-Vonk method. We expect that this study would be applicable to evaluate the crystallinity index of various cellulose materials with accuracy and reproducibility.

Effects of Current Density and Phosphoric Acid Concentration on Anodic Oxide Film of Titanium (전류밀도와 전해액의 인산농도가 Ti 양극 산화 피막에 미치는 영향)

  • Kim, Kye-Sung;Chung, Won-Sub;Shin, Heon-Cheol;Choe, Young-Son;Cho, Young-Rae
    • Korean Journal of Metals and Materials
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    • v.46 no.6
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    • pp.370-376
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    • 2008
  • The formation of anodic oxide film of titanium (Ti) was studied at a variety of electrolyte concentrations and current density to clarify their effects on morphology, microstructure and composition of Ti oxide layer. For the analysis of the Ti oxide films, a scanning electron microscopy (SEM), X-ray diffractometer (XRD), and X-ray photoelectron spectroscopy (XPS) were used. The results showed that the concentration of phosphoric acid played a crucial role in the crystalline structure of the Ti oxide layer while the current density gave a critical effect on the thickness and diameter of its pore. In particular, the crystalline anatase phase with a thickness larger than $2{\mu}m$, which is quite desirable for a dental implant application, could be readily prepared at the phosphoric acid concentration of 0.5 M and current density higher than $2.0A/dm^2$.

Synthesis and X-Ray Structure of 25-Acetoxy-26,27,28-trimethoxycalix[4]arene

  • Park, Yeong Ja;No Kwanghyun;Song Boo-Hee;Rhim Soo Kyung
    • Bulletin of the Korean Chemical Society
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    • v.15 no.12
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    • pp.1108-1112
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    • 1994
  • 25-Acetoxy-26,27,28-trimethoxycalix[4]arene was synthesized by the treatment of calix[4]arene trimethyl ether with acetyl chloride in the presence of NaH. The solution conformation was inferred as a partial cone conformation based on the $^1H$-and $^{13}C$ NMR spectra. The crystal structure has been determined by X-ray diffraction method. The crystals are monoclinic, space group $P2_1$/n, a=8.186 (1), b=17.137 (2), c=19.878 (3) ${\AA}$, ${\beta}$=95.67 (1)$^{\circ}$, Z=4, V=2774.90 ${\AA}^3$, $D_c$= 1.22 g $cm^{-3}$, $D_m$=1.23 g $cm^{-3}$. The intensity data were collected on an Enraf-Noninus CAD-4 Diffractometer with a graphite monochromated $Cu-K{\alpha}$ radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.054 for 3675 observed reflections. The molecule possesses a partial cone conformation with one flattened phenyl unit, in which one anisol ring, distal to the ester ring, is inverted. The acetoxyphenyl ring is flattened.

Photocurrent Characteristics of Zinc-Oxide Films Prepared by Using Sputtering and Spin-Coating Methods

  • Park, Sungho;Kim, Byung Jun;Kang, Seong Jun;Cho, Nam-Kwang
    • Journal of the Korean Physical Society
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    • v.73 no.9
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    • pp.1351-1355
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    • 2018
  • The photocurrent characteristics of zinc-oxide (ZnO) thin-film transistors (TFTs) prepared using radio-frequency sputtering and spin-coating methods were investigated. Various characterization methods were used to compare the physical and the chemical properties of the sputtered and the spin-coated ZnO films. X-ray photoelectron spectroscopy was used to investigate the chemical composition and state of the ZnO films. The transmittance and the optical band gap were measured by using UV-vis spectrometry. The crystal structures of the prepared ZnO films were examined by using an X-ray diffractometer, and the surfaces of the films were investigated by using scanning electron microscopy. ZnO TFTs were prepared using both sputter and solution processes, both of which showed photocurrent characteristics when illuminated by light. The sputtered ZnO TFTs had a photoresponsivity of 3.08 mA/W under illumination with 405-nm light while the solution-processed ZnO TFTs had a photoresponsivity of 5.56 mA/W. This study provides useful information for the development of optoelectronics based on ZnO.

Structure of Yb Complex with 3-nitro-1,2,4-triazol-5-one (3-nitro-1,2,4-triazol-5-one의 Yb 착물 구조)

  • 김광주;김재경;오기환
    • Journal of the Korea Institute of Military Science and Technology
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    • v.4 no.1
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    • pp.198-206
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    • 2001
  • The structure of Yb complex with 3-nitro-1,2,4-triazol-5-one(NTO), $[Yb(NTO)3(H2O)4].5H2O$ has been investigated by X-ray diffraction method. Crystallographic data for the title compound : monoclinic, C2/c, $a=36.925(2){\AA},$ b=6.6770(4)${\AA},$ c=25.6376(15)${\AA},$ {\beta}=130.978(1)^{\circ},$ V=4772.0(5)${\AA}^3,$ Z=8, $D_c,=1.952\; Mg/m^3.$ The intensity data were collected on a Broker SMART diffractometer equipped with a CCD area detector using Mo $K\alpha$ radiation. The structure was solved by direct method and refined by full-matrix least-squares calculations to a final R value of 0.0424 for 4727 independent reflections and 335 parameters. The three carbonyls of three NTO anions and four ligand water molecules which are formed the pentagonal bipyramid are coordinated with $Yb^{3+}$ and also five water molecules are included in the form of the crystal water in the molecular structure.

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[ $C_{28}H_{41}N_4O_4Br\;{\cdot}\;2H_2O$ ] (C_{28}H_{41}N_4O_4Br\;{\cdot}\;2H_2O$의 결정구조)

  • Kim Moon-Jib;Lee Jung-Ah;Jo Kyung-Jin;Choi Ki-Young
    • Korean Journal of Crystallography
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    • v.15 no.2
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    • pp.93-98
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    • 2004
  • The structure of C_{28}H_{41}N_4O_4Br\;{\cdot}\;2H_2O$ has been determined by X-ray deffraction methods. The crystal system is triclinic, space group Pl, unit cell constants, a=9.000(1) $\AA$, b=9.312(3) $\AA$, c=9.344(2) $\AA$, $\alpha=89.37(20)^{\circ},\;\beta=68.81(3)^{\circ},\;\gamma=84.70(4)^{\circ},\;V=726.7(8){\AA},\;T=298K,\;Z=1,\;D_c=1.402Mgm^{-3}$. The intensity data were collected on an Enraf-Nonius CAD4 Diffractometer with graphite monochromated $MoK\alpha$ radiation $(\lambda=0.71073\;{\AA}$. The molecular structure was solved by direct methods and refined by full-matrix least squares to a final $R=5.95\%$ for 2521 unique observed $F_0>4\sigma(F_0)$reflections and 370 parameters.

Synthesis and Molecular Structure of p-tert-butylcalix[4]arene Hexanoate

  • Park, Young-Ja;Kwanghyun No;Cho, Sun-Hee
    • Korean Journal of Crystallography
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    • v.10 no.1
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    • pp.1-8
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    • 1999
  • Two conformational isomers of p-tert-butylcalix[4]arene hexanoate were prepared from the reaction of-p-tert-butylcalix[4]arene and hexanoly chloride in the presence of AlCl3 in CH2Cl2 and their structures were determined by NMR spectra and X-ray diffraction as a cone and a 1,3-alternate conformer, respectively. The crystal of cone conformer (C68H96O8·(CH3)2CO) is triclinic, P, a=15.066(1) , b=16.063(1) , c=16.365(1) , α=79.75(2)o, β=109.95(2)o, γ=80.32(0)o, V=3602.7(4) 3, Z=2. The intensity data were collected on Simens SMART diffractometer/CCD area detector. The structure was solved by direct method and refined by least-squares calculations to a final R value of 0.144 for 4638 observed reflections. The molecular conformation is distorted symmetric cone with the flattening A and D phenyl rings. The crystal of 1,3-alternate conformer (C68H96O8·2CHCl3) is orthorhombic, Pca21, a=34.586(5) , b=10.207(3) , c=20.394(4) , V=7199(3) 3, Z=4. The intensity data were collected on an Enraf-Noninus CAD-4 Diffractometer with a graphite monochromated Mo-K radiation. The structure was solved by direct method and refined by least-squares calculations to a final R value of 0.152 for 2241 observed reflections. The molecule has a pseudo mirror symmetric 1,3-alternate conformation.

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