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

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Structure Identification of 1,2-Disubstituted Chiral Calix[4]arene : X-Ray and NMR Analysis of 25-(3,5-Dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene

  • 박영자;신정미;남계춘;김종민;국승근
    • Bulletin of the Korean Chemical Society
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    • v.17 no.7
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    • pp.643-647
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    • 1996
  • 1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

The Immediate Effects of Five-Toed Shoes on Foot Structure

  • Yi, Kyung-Ock
    • Korean Journal of Applied Biomechanics
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    • v.21 no.4
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    • pp.397-403
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    • 2011
  • The purpose of this study is to analyze the immediate effects of five toed shoes on foot structure. Subjects consisted of 26 college-aged women with pes planus. X-ray analysis of student feet were performed both barefooted and with five toed shoes. Dependent variables were hallux valgus angle, calcaneal inclination angle, 1st metatarsal declination angle, and intermetartarsal angle. Independent t-test was used for statistical analysis along with SAS. Overall, there were statistically significant changes of test subject's dependent variables when wearing five toed shoes. Specifically, the hallux valgus angle decreased, the calcaneal inclination angle and 1st metatarsal inclination angle increased, and intermetatasal angles both increased and decreased, shifting towards normal range. In every case the dependent variables shifted towards a more normal range while subjects wore five toed shoes. This study only examined the immediate corrective effects of five toed shoes on foot structure, but long-term studies are needed to understand the prolonged effects of five toed shoes on foot structure.

Preparation and Structure Properties of LaBa2Cu2O9, LaBa22CaCu3O12 and LaBa2Ca2Cu5O15 Perovskites

  • Kareem Ali Jasim;Hind Abdulmajeed Mahdi;Rafah Ismael Noori;Marwa Ayad Abdulmajeed
    • Korean Journal of Materials Research
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    • v.33 no.9
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    • pp.367-371
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    • 2023
  • In this study we examine variations in the structure of perovskite compounds of LaBa2Cu2O9, LaBa22CaCu3O12 and LaBa2Ca2Cu5O15 synthesized using the solid state reaction method. The samples' compositions were assessed using X-ray fluorescence (XRF) analysis. The La: Ba: Ca: Cu ratios for samples LaBa2Cu2O9, LaBa22CaCu3O12 and LaBa2Ca2Cu5O15 were found by XRF analysis to be around 1:2:0:2, 1:2:1:3, and 1:2:2:5, respectively. The samples' well-known structures were then analyzed using X-ray diffraction. The three samples largely consist of phases 1202, 1213, and 1225, with a trace quantity of an unknown secondary phase, based on the intensities and locations of the diffraction peaks. According to the measured parameters a, b, and c, every sample has a tetragonal symmetry structure. Each sample's mass density was observed to alter as the lead oxide content rose. Scanning electron microscope (SEM) images of the three phases revealed that different Ca-O and Cu-O layers can cause different grain sizes, characterized by elongated thin grains, without a preferred orientation.

In Situ X-ray Absorption Spectroscopic Study for α-MoO3 Electrode upon Discharge/Charge Reaction in Lithium Secondary Batteries

  • Kang, Joo-Hee;Paek, Seung-Min;Choy, Jin-Ho
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3675-3678
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    • 2010
  • In-situ X-ray absorption spectroscopy (XAS) was used to elucidate the structural variation of $\alpha-MoO_3$ electrode upon discharge/charge reaction in a lithium ion battery. According to the XAS analysis, hexavalent Mo atoms in $\alpha-MoO_3$ framework are reduced as the amount of intercalated lithium ions increases. As lithium de-intercalation proceeds, most of pre-edge peaks are restored again. However, according to the Fourier transforms of the extended X-ray absorption fine structure (EXAFS) spectra, lithium de-intercalation reaction is partially irreversible upon the charge reaction, which is one of the main reasons why the capacity of $\alpha-MoO_3$ electrode decreases upon successive discharge/charge cycles.

Properties of $Zn_xSnO_2$ Nanorods Synthesized by Hytrothermal Method

  • Yeo, Chang-Su;Lee, Gwan-Ho;Kang, Hee-Kyoung;Lee, Kyung-Hee;Yu, Byung-Yong;Song, Jong-Han;Chae, Kuen-Hwa
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.313-313
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    • 2012
  • ZnO and $SnO_2$, well-known wide direct band-gap semiconductors, have been considered as the most promising functional materials due to their highly sensitive gas sensing and excellent optical properties. ZnO/$SnO_2$ epitaxial hetrostructure exhibited unique luminescence properties in contrast with individual tetra-pod ZnO and $SnO_2$ nanostructures. Polycrystalline $SnO_2$-based samples $Zn_xSn_{1-x}O_2$(x=0, 0.01, 0.03, 0.05) were prepared by solid state reaction and eco-friendly hydrothermal techniques. Scanning electron microscopy equipped with electron dispersive x-ray spectra confirms the formation of near stoichiometric $Zn_xSn_{1-x}O_2$ nanorods of diameter ~10 nm. X-ray diffraction analysis revealed the rutile structure, except for x=0.07, which may have a small part of $Zn_2SnO_4$ as a secondary phase.

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6H-SiC epitaxial growth and crystal structure analysis (6H-SiC 에피층 성장과 결정구조 해석)

  • Kook-Sang Park;Ky-Am Lee
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.2
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    • pp.197-206
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    • 1997
  • A SiC epilayer on the 6H-SiC crystal substrate was grown by chemical vapor deposition (CVD). The crystal structure of the SiC epilayer was investigated by using the X-ray diffraction patterns and the Roman scattering spectroscopy. The SiC epilayer on the 6H-SiC substrate was grown to be homoepilayer by CVD. In order to distinguish a certain SiC polytype mixed in the SiC crystal grown by the modified Lely method, we have calculated the X-ray diffraction intensities and Brags angles of the typical SiC crystal powders. By comparing the measured X-ray diffraction pattern with the calculated ones, it was identified that the SiC crystal grown by the modified Lely method was the 6H-SiC crystal mixed some 15R-SiC.

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Synthesis, Structure, and Thermal Property of Poly(trimethylene terephthalate- co-trimethylene 2,6-naphthalate) Copolymers

  • Jeong, Young-Gyu;Jo, Won-Ho;Lee, Sang-Cheol
    • Fibers and Polymers
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    • v.5 no.3
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    • pp.245-251
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    • 2004
  • Poly(trimethylene terephthalate-co-trimethylene 2,6-naphthalate)s (P(TT-co-TN)s) with various copolymer composition were synthesized, and their chain structure, thermal property and crystalline structure were investigated by using $^1$H-NMR spectroscopy, differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD), respectively. It was found from sequence analysis that all the P(TT-co-TN) copolymers synthesized have a statistical random distribution of TT and TN units. It was also observed from DSC thermograms that the glass transition temperature increases linearly with increasing the TN comonomer content, whereas the melting temperature of copolymer decreases with increasing the corresponding comonomer content in respective PTT- and PTN-based copolymer, showing pseudo-eutectic melting behavior. All the samples melt-crystallized isothermally except for P(TT-co-66 mol % TN) exhibit multiple melting endotherms and clear X-ray diffraction patterns. The multiple melting behavior originates from the dual lamellar population and/or the melting-recrystallization-remelting. The X-ray diffraction patterns are largely divided into two classes depending on the copolymer composition, i.e., PTT and PTN $\beta$-form diffraction patterns, without exhibiting cocrystallization.

Phase Analysis of Mechanically Alloyed $\sigma$-VFe Alloy Powders by Neutron and X-ray Diffraction (기계적 합금화한 $\sigma$-VFe합금의 중성자 및 X선 회절에 의한 상분석)

  • 이충효;조재문;이상진;심해섭;이창희
    • Korean Journal of Materials Research
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    • v.11 no.8
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    • pp.664-664
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    • 2001
  • The mechanical alloying (MA) effect in $\sigma$-VFe intermetallic compound was studied by neutron and X-ray diffraction. The structure of MA $\sigma$-VFe powders were characterized by the X- ray diffraction with Cu- $K\alpha$ radiation and neutron diffraction with monochromatic neutrons of $1.835\AA$ using a high resolution powder diffractometer (HRPD). Mechanical alloying of $\sigma$-VFe compound gives rise to a dramatic structural change. After 60 hours of MA, the Fe-Fe distribution of the $\sigma$- phase VFe tetragonal structure with 30 atoms in a unit cell is found to change into that of the $\sigma$-(V,Fe) solid solution with bcc structure, which is a stable phase at elevated temperature above $1200^{\circ}C$. A comparison of X-ray diffraction data for the $\alpha$-phase has been also made with the corresponding neutron diffraction data. The (101) and (111) diffraction peaks of the $\sigma$-phase was clearly observed only in neutron diffraction pattern, which is believed to be a characteristic feature due to the chemical atomic ordering of $\sigma$- VFe phase.

Structural and Magnetic Properties of the Brownmillerite $Ca_2Al_xFe_{2-x}O_5$ System

  • 김귀야;로권선;여철현
    • Bulletin of the Korean Chemical Society
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    • v.16 no.10
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    • pp.934-938
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    • 1995
  • A series of solid solutions in the Ca2AlxFe2-xO5 (x=0.00, 0.50, 0.66, 1.00 and 1.34) system with brownmillerite structure has been synthesized at 1100 ℃ under an atmospheric air pressure. The solid solutions are analysed by powder x-ray diffraction analysis, Mohr salt titration, thermal analysis, and Mossbauer spectroscopic analysis. The x-ray diffraction analysis assigns the compositions of x=0.00 and 0.50 to the space group Pcmn and those of x=0.66, 1.00, and 1.34 to the Ibm2. Mo&ssbauer spectra have shown the coordination state and disordering of Al3+ and Fe3+ ions. The substituting preference of Al3+ ions for the tetrahedral site decreases with increasing x value. Magnetic susceptibility of the system has been measured in the temperature range of 5 K to 900 K. The solid solutions of the compositions of x=0.00, 0.50 and 0.66 have shown a thermal hysteresis and the thermoremanent magnetization gap decreases with increasing x value in the above systems. However the compositions of x=1.00 and 1.34 do not show the hysteresis. The exchange integral is calculated from Fe3+ ion occupancy ratio. The integral decreases with x value and thus the magnetic transition temperature decreases with the increasing x value.

Studies on the Crystal Structure of Benzidine Perchlorate by X-ray Diffraction method (II) Crystal Structure Analysis (X-線 廻折法을 利用한 벤지딘過鹽素酸鹽의 結晶構造에 關한 硏究 (II)結晶構造의 解析)

  • Koo, Chung-Hoe;Shin, Hyun-So;Kang, Man-Hyong
    • Journal of the Korean Chemical Society
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    • v.14 no.1
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    • pp.123-126
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    • 1970
  • The approximate crystal structure of benzidine monoperchlorate has been determined by single crystal X-Ray diffraction technique and patterson method. As the molecule has a center of symmetry in it and location of perchlorate ion is symmetrically on the mirror plane in the unit cell, perchlorate ion is forming hydrogen bond with two -$NH_2$ groups in the different molecule. Thus, one molecule of benzidine and perchloric acid combines 1:1 by mole ratio.

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