• 제목/요약/키워드: 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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    • 제17권7호
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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
    • 한국운동역학회지
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    • 제21권4호
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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
    • 한국재료학회지
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    • 제33권9호
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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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    • 제31권12호
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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
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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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 에피층 성장과 결정구조 해석 (6H-SiC epitaxial growth and crystal structure analysis)

  • Kook-Sang Park;Ky-Am Lee
    • 한국결정성장학회지
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    • 제7권2호
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    • pp.197-206
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    • 1997
  • 6H-SiC 위에 SiC 에피층이 화학 기상 증착(CVD)에 의하여 성장되었다. 성장된 SiC 에피층의 결정구조는 X-선 회절과 Raman 분광을 사용하여 조사되었으며, 이 에피층은 6H-SiC로서 성장되었음을 확인하였다. 수정된 Lely법으로 성장된 한 SiC 결정 분말의 결정구조를 확인하기 위하여 전형적인 SiC polytype들의 X-선 회절상을 계산하였으며, 측정된 X-선 회절상과 비교하여 이 SiC 결정에는 15R-SiC가 약간 혼재되어 있음을 확인하였다.

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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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    • 제5권3호
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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.

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

  • 이충효;조재문;이상진;심해섭;이창희
    • 한국재료학회지
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    • 제11권8호
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    • pp.664-664
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    • 2001
  • $\sigma$-VFe 금속간화합물에 대한 기계적 합금화(MA) 효과를 중성자 및 X선 회절법으로 조사하였다. MA 분말의 구조분석은 X선 회절(Cu-K$\alpha$) 린 중성자회절(HRPD, λ=1.835$\AA$)을 이용하여 행하였다. $\sigma$-VFe화합물의 MA시 큰 구조변화가 관찰되었으며, MA 60시간의 경우 Fe-Fe 훤자분포는 unit cell에 30개의 원자를 포함하고 있는 $\sigma$상의 tetragonal구조에서 $120^{\circ}C$이상에서 안정하게 존재하는 $\alpha$-(V,Fe) 고용체의 bcc 구조로 상변화함을 알 수 있었다. 또한 $\alpha$-VFe 화합물에 대한 중성자 및 X선 회절패턴의 비교분석을 행하였으며 그 결과 $\sigma$상이 가지는 화학적 규칙성에 기인하는 (101)과 (111) 회절 피크가 중성자 회절에서 뚜렷하게 관찰됨을 알 수 있었다.

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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    • 제16권10호
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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.

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 (Studies on the Crystal Structure of Benzidine Perchlorate by X-ray Diffraction method (II) Crystal Structure Analysis)

  • 구정회;신현소;강만형
    • 대한화학회지
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    • 제14권1호
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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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