• 제목/요약/키워드: X-ray structure analysis

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

  • 김철배;조현종;이성경;박광용
    • 공업화학
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    • 제20권3호
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    • pp.335-338
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    • 2009
  • 유기발광다이오드의 청색 발광 물질로 많은 관심을 받고 있는 디스티릴아릴렌 화합물들의 합성 과정에서 핵심적인 중간체인 브로모트리페닐에틸렌 화합물들은 브로모벤조페논과 벤질포스포네이트의 반응을 통하여 얻어진다. 이 반응은 분리하기 어려운 (Z)-와 (E)-기하이성질체가 60 : 40의 비율로 생성한다. 본 연구에서는 2-프로탄올을 이용한 재결정법을 통하여 (Z)-이성질체를 간단하게 분리하였다. X-ray를 이용하여 (Z)-이성질체의 결정 구조를 살펴본 결과, tert-부틸페닐 고리와 브로모페닐 고리 간의 dihedral angle은 $56.5(4)^{\circ}$이며 브로모페닐 고리와 페닐 고리 간의 dihedral angle은 $74.1(4)^{\circ}$였다.

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

  • 김신애;김성훈;소지용;이정수;이창희
    • 한국광물학회지
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    • 제20권4호
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    • pp.351-356
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    • 2007
  • 수소원자를 포함한 강유전체 $Li(NH_4)SO_4$의 중수소 치환형인 $Li(ND_4)SO_4$ 단결정에 대해 X-선과 중성자 회절법으로 결정구조를 연구하였다. 이 결정은 상온에서 사방정계이고 공간군은 $P2_1nb$이다. 격자상수는 $a=5.2773(5)\;{\AA},\;b=9.1244(23)\;{\AA},\;c=8.7719(11)\;{\AA}$이며 Z=4이다. 한국원자력연구원의 연구용 원자로인 하나로에 설치된 중성자 4축 단결정 회절장치로 중성자데이터를 수집하였으며, X-선 회절데이터는 일본 동북대학교 물리학과에서 측정하였다. X-선 회절법으로 수집한 1450개의 독립 회절반점에 대하여 최소자승법으로 정밀화하여 최종 신뢰도값 R=0.070을 얻었으며, 중성자 회절법으로는 745개의 회절반점에 대하여 R=0.049을 얻었다. X-선 회절데이터 분석 결과 결정구조 내의 수소원자 중 1개의 위치만을 얻었으나, 중성자 회절법으로는 $NH_4$ 사면체의 수소/중수소원자의 위치는 물론 H를 치환해서 들어간 D의 점유율을 정련하여 측정시료의 평균화학식이 $LiND_{3.05}H_{0.95}SO_4$임을 밝혔다.

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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    • 제11권5호
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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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    • 제14권2호
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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.

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

  • 이지원;이언석
    • 한국콘텐츠학회논문지
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    • 제16권12호
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    • pp.70-77
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    • 2016
  • 본 연구에서는 거머리의 미세한 해부구조를 3차원적으로 분석 가능한 방사광의 경 엑스선 이미징을 통하여 객관적 분석법 및 생체모사기술 구축을 위한 기초자료를 구축하고자 하였다. 우리는 방사광을 이용하여 거머리의 미세 구조영상을 얻을 수 있었고, 3차원적인 해부학적 분석이 가능함을 확인하였다. 또한 방사광을 통해 얻은 데이터는 내부구조의 미세조직까지 관찰 가능하기 때문에 성분 분석 및 생리적, 기능적 측면으로도 연구의 토대가 될 것으로 사료된다. 더 나아가 추후 거머리로부터 생체모사기술 연구 분야 등에 기여할 수 있을 것이라 기대된다.

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

  • 홍순혁;이동우;조석수;주원식
    • 한국정밀공학회지
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    • 제19권2호
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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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    • 제14권1호
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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
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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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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    • 제30권1호
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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.