• Title/Summary/Keyword: X-ray structure analysis

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Synthesis and X-ray Structure Analysis of (Z)-1-(4-Bromophenyl)-1-phenyl-2-(4-tert-butylphenyl)ethene ((Z)-1-(4-브로모페닐)-1-페닐-2-(4-tert-부틸페닐)에텐의 합성 및 X-선 구조분석)

  • Kim, Chul-Bae;Cho, Hyun-Jong;Lee, Sung-Kyung;Park, Kwangyong
    • Applied Chemistry for Engineering
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    • v.20 no.3
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    • pp.335-338
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    • 2009
  • As important intermediates for blue emitting materials of organic light-emitting diodes, bromotriphenylethylene derivatives for distrylarylenes are prepared by reactions of bromobenzophenone with benzylphosphonates. The reaction produces a 60 : 40 mixture of (Z)- and (E)-geometric isomers that are difficult to be resolved. The (Z)-isomer is successfully isolated by a selective recrystallization process using 2-propanol as a solvent. The X-ray structure analysis of (Z)-isomer shows that dihedral angles between tert-butylphenyl ring and bromophenyl ring and between bromophenyl ring and phenyl ring are $56.5(4)^{\circ}$ and $74.1(4)^{\circ}$, respectively.

Crystal Structure Analysis of $LiN(D_xH_{1-x}){_4}SO_4$ by X-ray and Neutron Diffraction (X-선과 중성자 회절을 이용한 강유전체 단결정 $LiN(D_xH_{1-x}){_4}SO_4$의 결정구조 연구)

  • Kim, Shin-Ae;Kim, Seong-Hoon;So, Ji-Yong;Lee, Jeong-Soo;Lee, Chana-Hee
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.4
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    • pp.351-356
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    • 2007
  • The crystal structure of $Li(ND_4)SO_4$ was analyzed by X-ray and neutron diffraction methods. The crystal is a deuterated $Li(NH_4)SO_4$ and one of the ferroelectric materials with hydrogen atoms. The crystal is orthorhombic at room temperature, $P2_1nb$, with lattice parameters of $a=5.2773(5)\;{\AA},\;b=9.1244(23)\;{\AA},\;c=8.7719(11)\;{\AA}$ and Z=4. Neutron intensity data were collected on the Four-Circle diffractometer (FCD) at HANARO in Korea Atomic Energy Research Institute and X-ray date were given by Prof. Y. Noda of Tohoku University Japan. The structure was refined by full-matrix least-square to final R value of 0.070 for 1450 observed reflections by X-ray diffraction and to final R=0.049 for 745 observed reflections by neutron diffraction. With X-ray data we obtained only one hydrogen atomic position. However, not only all atomic positions of four hydrogen atoms at $NH_4$ but also the occupation factors of D and H were refined with neutron data. From this results we obtained the average chemical structure of this sample, $LiND_{3.05}H_{0.95}SO_4$.

Preparation, Structure, and Photoemission Studies on the High Temperature Superconductor $YBa_2Cu_{3-x}Ni_xO_{7-{\delta}}$

  • Choy, Jin-Ho;Choe, Won-Young
    • Bulletin of the Korean Chemical Society
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    • v.11 no.5
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    • pp.379-383
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    • 1990
  • $YBa_2Cu_{3-x}Ni_xO_{7-{\delta}}$, with x = 0.05, 0.2, 0.4, 0.7 and 1.0 had been prepared by the thermal decomposition of corresponding nitrates. Among them, the sample with x = 0.05 shows above-liquid-$N_2$ temperature superconductivity with $T_c$ of 88.7K. According to the X-ray diffraction analysis, its crystal symmetry was estimated as orthorhombic with the lattice parameters of a = 3.866${\AA}$, b = 3.893${\AA}$, c = 11.715${\AA}$. The chemical composition of the sample was determined by electron probe microanalysis and the chemical composition around its grain boundaries was carefully studied by the X-ray line scanning technique. From the observed binding energy of Ni-$2p_{3/2}$ orbital electron (B.E. = 853 eV) measured by X-ray photoelectron spectroscopy, the valency state of nickel stabilized in $YBa_2Cu_{2.95}Ni_{0.05}O_{7-{\delta}}$ oxide lattice could be determined to be Ni(II).

Analysis of Wide-gap Semiconductors with Superconducting XAFS Apparatus

  • Shiki, S.;Zen, N.;Matsubayashi, N.;Koike, M.;Ukibe, M.;Kitajima, Y.;Nagamachi, S.;Ohkubo, M.
    • Progress in Superconductivity
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    • v.14 no.2
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    • pp.99-101
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    • 2012
  • Fluorescent yield X-ray absorption fine structure (XAFS) spectroscopy is useful for analyzing local structure of specific elements in matrices. We developed an XAFS apparatus with a 100-pixel superconducting tunnel junction (STJ) detector array with a high sensitivity and a high resolution for light-element dopants in wide-gap semiconductors. An STJ detector has a pixel size of $100{\mu}m$ square, and an asymmetric layer structure of Nb(300 nm)-Al(70 nm)/AlOx/Al(70 nm)-Nb(50 nm). The 100-pixel STJ array has an effective area of $1mm^2$. The XAFS apparatus with the STJ array detector was installed in BL-11A of High Energy Accelerator Research Organization, Photon Factory (KEK PF). Fluorescent X-ray spectrum for boron nitride showed that the average energy resolution of the 100-pixels is 12 eV in full width half maximum for the N-K line, and The C-K and N-K lines are separated without peak tail overlap. We analyzed the N dopant atoms implanted into 4H-SiC substrates at a dose of 300 ppm in a 200 nm-thick surface layer. From a comparison between measured X-ray Absorption Near Edge Structure (XANES) spectra and ab initio FEFF calculations, it has been revealed that the N atoms substitute for the C site of the SiC lattice.

A Study of the 3D Anatomical Structure Analysis of Leech Using Hard X-ray Micro Tomography by Synchrotron Radiation (방사광 경 엑스선 마이크로 단층촬영을 이용한 거머리의 해부학적 3차원 구조분석)

  • Lee, Ji Won;Lee, On Seok
    • The Journal of the Korea Contents Association
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    • v.16 no.12
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    • pp.70-77
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    • 2016
  • In this study, we aim to obtain the fundamental data needed for the objective analysis and bio-mimetics of leeches, using x-ray imaging with radiation that allows 3D analysis of the detailed anatomic structures of leeches. It was confirmed that through using radiation, detailed images of leeches can be obtained, allowing 3D analysis of leeches' anatomical structures. Also, since the data obtained through the radiation allows you to observe the micro-structure, it can serve as a good resource for component analysis, as well as physiological and functional research. More, it is hoped to contribute to further research in the areas of bio-mimetics using leeches.

A Study on the X-Ray Fractography of Turbine Blade under Fatigue Load (피로하중을 받는 터빈 블레이드의 X선 프랙토그래픽에 관한 연구)

  • Hong, Soon-Hyeok;Lee, Dong-Woo;Cho, Seok-Swoo;Joo, Won-Sik
    • Journal of the Korean Society for Precision Engineering
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    • v.19 no.2
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    • pp.65-71
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    • 2002
  • Turbine blade is subject to cyclic bending force by steam pressure. Stress analysis by fractography is already established technology as means far seeking cause of fracture and has been widely employed. In the X-ray frctography, plastic deformation and residual stress near the fracture surface can be determined and information of internal structure of material can be obtained. Therefore, to find a fracture mechanism of torsion-mounted blade in nuclear power plant, based on the information from the fracture surface obtained by fatigue test, the correlation of X-ray parameter and fracture mechanics parameter was determined and then the stress intensity factor to actual broken turbine blade was predicted.

The Crystal Structure of Licarin-B $(C_{20}H_{20}O_4)$, A Component of the Seeds of Myristica fragrans

  • Kim, Yang-Bae;Park, Il-Yeong;Shin, Kuk-Hyun
    • Archives of Pharmacal Research
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    • v.14 no.1
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    • pp.1-6
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    • 1991
  • The crystal structure of licarin-B, a component of Myristicae Semen was determined by single crystal X-ray diffraction analysis. Crystal of the compound, which was recrystallized from the mixture of hexane and ether, is monoclinic with a=12.740(1), b=7.219(1), c=9.284(1) ${\AA}$, ${\beta}=94.75(1)^{\circ}$, $D_x=1.26$, $D_m=1.27\;g/cm^3$, space group P21, and Z=2. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.040 for 1532 independent reflections ${F{\ge}3{\sigma}(F)}$. The compound is a dimeric phenylpropanoid, and belongs to the neolignan analogues. The molecules are arranged along with the screw axis. The intermolecular contacts appear to be the normal van der Waals' forces.

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X-Ray Absorption Spectroscopic Study of 120 MeV $Ag^{9+}$ Ion-Irradiated N-Doped ZnO Thin Films

  • Gautam, Sanjeev;Lim, Weon Cheol;Kang, Hee Kyung;Lee, Ki Soo;Song, Jaebong;Song, Jonghan;Asokan, K.;Chae, Keun Hwa
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.315-315
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    • 2013
  • We report the electronic structure modification in the swift heavy ion (SHI) irradiated N-doped ZnO thin films prepared by RF sputtering from ZnO target in different ratio of Ar/$N_2$ gas mixture using highly pure $N_2$ gas. The different N-ZnO thin lms were then irradiated with 120 MeV Ag ion beam with different doses ranging from $1{\times}10^{11}$ to $5{\times}10^{12}$ ions/$cm^2$ and characterized by XRD and near edge X-ray absorption ne structure (NEXAFS) at N and O K-edges. The NEXAFS measurements provide direct evidence of O 2p and Zn 3d orbital hybridization and also the bonding of N ions with Zn and O ions. The minimum value of resistivity of $790{\Omega}cm$, a Hall mobility of $22cm^2V^-1s^-1$ and the carrier concentration of $3.6{\times}10^{14}cm^{-3}$ were yielded at 75% $N_2$. X-ray diffraction (XRD) measurements revealed that N-doped ZnO films had the preferential orientation of (002) plane for all samples, while crystallinity start decreasing at 32.5% $N_2$. The average crystallite size varies from 5.7 to 8.2 nm for 75% and then decreases to 7.8 nm for 80% $Ar:N_2$ ratio.

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Sonochemical Synthesis, Thermal Studies and X-ray Structure of Precursor [Zr(acac)3(H2O)2]Cl for Deposition of Thin Film of ZrO2 by Ultrasonic Aerosol Assisted Chemical Vapour Deposition

  • Hussain, Muzammil;Mazhar, Muhammad;Rauf, Muhammad Khawar;Ebihara, Masahiro;Hussain, Tajammal
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.92-96
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    • 2009
  • A new precursor [$Zr(acac)_{3}(H_{2}O)_{2}$] was synthesized by Sonochemical technique and used to deposit thin $ZrO_{2}$ film on quartz and ceramic substrate via ultrasonic aerosol assisted chemical vapour deposition (UAACVD) at 300 ${^{\circ}C}$ in oxygen environment followed by annealing of the sample for 2-3 minutes at 500 ${^{\circ}C}$ in nitrogen ambient. The molecular structure of the precursor determined by single crystal X-ray analysis revealed that the molecules are linked through intermolecular hydrogen bonds forming pseudo six and eight membered rings. DSC and TGA/FTIR techniques were used to determine thermal behavior and decomposition temperature of the precursor and nature of evolved gas products. The optical measurement of annealed $ZrO_{2}$ film with tetragonal phase shows optical energy band gap of 5.01 eV. The particle size, morphology, surface structure and composition of deposited films were investigated by XRD, SEM and EDX.