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

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HRTEM Analysis of Apatite Formed on Bioactive Titanium in Modified-SBF (수정된 유사체액 내에서 티타늄에 생성된 아파타이트의 고분해능 전자현미경에 의한 분석)

  • Kim, Hyun-Ook;Kim, Woo-Jeong;Lee, Kap-Ho;Hon, Sun-Ig
    • Korean Journal of Materials Research
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    • v.17 no.8
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    • pp.408-413
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    • 2007
  • Process of the hydroxyapapite(HA) precipitation on bioactive titanium metal prepared by NaOH in a modified-simulated body fluid(mSBF) was investigated by high resolution transmission electron microscope (HRTEM) attached with energy dispersive X-ray spectrometer(EDX). The amorphous titanate phase on titanium surface is form by NaOH treatment and an amorphous titanate incorporated calcium and phosphate ions in the liquid to form an amorphous calcium phosphate. With increasing of soaking time in the liquid, the HA particles are observed in amorphous calcium phosphate phase with a Ca/P atomic ratio of I.30. The octacalcium phosphate (OCP) structure is not detected in HRTEM image and electron diffraction pattern. After a long soaking time, the HA particles grow as needle-like shape on titanium surface and a large particle-like aggregates of needle-like substance were observed to form on titanium surface within needle-like shape. A long axis of needle parallels to c-direction of the hexagonal HA structure.

Olefin Separation Performances and Coordination Behaviors of Facilitated Transport Membranes Based on Poly(styrene-b-isoprene-b-styrene)/Silver Salt Complexes

  • Lee, Dong-Hoon;Kang, Yong-Soo;Kim, Jong-Hak
    • Macromolecular Research
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    • v.17 no.2
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    • pp.104-109
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    • 2009
  • Solid-state facilitated, olefin transport membranes were prepared by complexation of poly(styrene-b-iso-prene-b-styrene) (SIS) block copolymer and silver salt. Facilitated olefin transport was not observed up to a silver mole fraction of 0.14, representing a threshold concentration, above which transport increased almost linearly with increasing silver salt concentration. This was because firstly the silver ions were selectively coordinated with the C=C bonds of PI blocks up to a silver mole fraction of 0.20, and secondly the coordinative interaction of the silver ions with the aliphatic C=C bond was stronger than that with the aromatic C=C bond, as confirmed by FT-Raman spectroscopy. Small angle X-ray scattering (SAXS) analysis showed that the cylindrical morphology of the neat SIS block copolymer was changed to a disordered structure at low silver concentrations ($0.01{\sim}0.02$). However, at intermediate silver concentrations ($0.15{\sim}0.20$), disordered-ordered structural changes occurred and finally returned to a disordered structure again at higher silver concentrations (>0.33). These results demonstrated that the facilitated olefin transport of SIS/silver salt complex membrancs was significantly affected by their coordinative interactions and nano-structural morphology.

Effect of Al Precursor Type on Mesoporous Alumina Particles Prepared by Spray Pyrolysis (분무열분해공정에 의한 메조기공 알루미나 제조에 있어 Al 전구체 영향)

  • Kim, Joo-Hyun;Jung, Kyeong-Youl;Park, Kyun-Young
    • Journal of Powder Materials
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    • v.17 no.3
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    • pp.209-215
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    • 2010
  • Mesoporous alumina particles were prepared by spray pyrolysis using cetyltrimethyl-ammonium bromide (CTAB) as a structure directing agent and the effect of Al precursor types on the texture properties was studied using $N_2$ adsorption isotherms, small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The surface area and the microstructure of alumina particles were significantly influenced by the Al precursor type. The largest BET surface area was obtained when Al chloride was used, whereas alumina particles prepared from Al acetate had the largest pore volume. According to small-angle X-ray scattering (SAXS) analysis, the alumina powders prepared using nitrate and acetate precursors had a clear single SAXS peak around $2{\theta}=1.0{\sim}1.5^{\circ}$, indicating that regular mesopores with sponge-like structure were produced. On the basis of TEM, SAXS, and $N_2$ isotherm results, the chloride precursor was most profitable to obtain the largest surface area ($265\;m^2/g$), whereas, the nitrate precursor is useful for the preparation of non-hollow mesoporous alumina with regular pore size, maintaining high surface area (${\sim}233\;m^2/g$).

Preparation of ZnO Nanorod Grown on the PAN Surface and Its Sulfur Removal Characteristics (PAN 섬유 표면에서 성장하는 ZnO 나노로드의 제조 및 이를 이용한 황화합물 제거 특성)

  • LEE, JAEYOUNG;HAN, KYEONGSIK;JEONG, INSOO;LEE, HONGKI
    • Transactions of the Korean hydrogen and new energy society
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    • v.29 no.3
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    • pp.243-250
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    • 2018
  • Zinc oxide (ZnO) nanorods were grown on a palladium (Pd) activated polyacrylonitrile (PAN) fiber where Pd activation was carried out in advance by the following dry process: palladium(II) bis(acetylacetonate), $Pd(acac)_2$ was sublimed, penetrated into the surface of PAN fiber and spontaneously reduced to Pd nanoparticles at $180^{\circ}C$ for various times under a nitrogen atmosphere. ZnO nanorod morphology was observed by a scanning electron microscopy (SEM) and the elemental composition was confirmed by energy-dispersive X-ray spectroscopy (EDS). The crystalline structure of ZnO nanorods was analyzed by X-ray diffraction (XRD) analysis showing Wurtzite structure consisting of hexagonal lattice. Sulfur removal characteristics were evaluated.

CO-Tolerant PtMo/C Fuel Cell Catalyst for H2 Oxidation

  • Bang, Jin-Ho;Kim, Ha-Suck
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3660-3665
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    • 2011
  • CO-tolerant PtMo/C alloy electrocatalyst was prepared by a colloidal method, and its electrocatalytic activity toward CO oxidation was investigated. Electrochemical study revealed that the alloy catalyst significantly enhanced catalytic activity toward the electro-oxidation of CO compared to Pt/C counterpart. Cyclic voltammetry suggested that Mo plays an important role in promoting CO electro-oxidation by facilitating the formation of active oxygen species. The effect of Mo on the electronic structure of Pt was investigated using X-ray absorption spectroscopy to elucidate the synergetic effect of alloying. Our in-depth spectroscopic analysis revealed that CO is less strongly adsorbed on PtMo/C catalyst than on Pt/C catalyst due to the modulation of the electronic structure of Pt d-band. Our investigation shows that the enhanced CO electrooxidation in PtMo alloy electrocatalyst is originated from two factors; one comes from the facile formation of active oxygen species, and the other from the weak interaction between Pt and CO.

A Carbazole-Attached NO2S2-Macrocycle Exhibiting Hg2+ and Cu2+ Selectivity

  • Lee, Seul-Gi;Kang, Eun-Ju;Lee, Shim Sung
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1429-1434
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    • 2013
  • A synthesis and cation-induced fluorescent behavior of the carbazole-attached $NO_2S_2$-macrocycle (L) is described and structurally characterized by single crystal X-ray analysis. The photoluminescence spectrum of L in 80% $CH_3CN/CH_2Cl_2$ displays a peak maximum at 431 nm (blue emission). In the metal-induced fluorometric experiment, L showed a drastic chelation-enhanced fluorescence quenching (CHEQ) effect only with $Hg^{2+}$ and $Cu^{2+}$. In ESI-mass study, a 1:1 stoichiometry for complexation of L with $Hg^{2+}$ was confirmed, suggesting the unique sensing behavior of the proposed ligand L due to the selective complexation affinity for $Hg^{2+}$. The observed results indicate that L is a promising turn-off type fluoroionophore for $Hg^{2+}$ and $Cu^{2+}$ detections. Additionally, the $Ag^+$ complex of the precursor macrocycle was prepared and its solid structure was crystallographically characterized.

Preparation and Structure of $Re(≡NC_6H_5)(DPPE)CI_3$, $[DPPE=Ph_2PCH_2CH_2PPh_2]$ ($Re(≡NC_6H_5)(DPPE)CI_3$화합물의 합성 및 구조)

  • 박병규;정건수
    • Korean Journal of Crystallography
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    • v.6 no.2
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    • pp.93-97
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    • 1995
  • Re(≡NC6H5)(PPh3)2CI3, I, reacted with, 1,2-bis(diphenylphosphino)ethane (DPPE) to give fac-Re(≡NC6H5)(DPPE)CI3, II. The product has been characterized by 1H-NMR, elemental analysis, and X-ray crystallography. II Crystalizes in the monoclinic space group Pc, with cell parameters a=11.083(3)Å, b=10.930(1)Å, c=14.081(2)Å, β=108.37(2)°, Z=2. Least-squares refinement of the structure led to a R(wR2)factor of 0.0254(0.0607) for 2888 unique reflections of I>2σ(I) and for 352 variables.

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Preparation and Structure of $Re(NC_6F_5)(PPh_3)_2Cl_3 $ ($Re(NC_6F_5)(PPh_3)_2Cl_3 $화합물의 합성 및 구조)

  • 박병규;김영웅
    • Korean Journal of Crystallography
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    • v.7 no.2
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    • pp.113-119
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    • 1996
  • Reaction of Re(O)(PPh3)2Cl3,I, with 2,3,4,5,6-pentafluoroaniline (C6F5NH2), produced Re(NC6F5)(PPh3)2Cl3, II. The product has been characterized by 1H-NMR, elemental analysis, and X-ray diffraction. II crystallizes in the orthorhombic system, space group Pna21 with cell parameters a=18.763Å, b=14.737(2)Å, c=16.707(3)Å, Z=4. Least-square refinement of the structure led to an R(wR2)factor of 0.0455(0.1148) for 3319 unique reflections of I > 2σ(I) and for 174 variables.

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Crystallization and X-ray crystallographic analysis of the PH-like domain of lipid transfer protein anchored at membrane contact sites from Saccharomyces cerevisiae

  • Tong, Junsen;Im, Young Jun
    • Biodesign
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    • v.5 no.4
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    • pp.136-140
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    • 2017
  • Lam6 is a member of sterol-specific ${\underline{l}ipid$ transfer proteins ${\underline{a}}nchored$ at ${\underline{m}ebrane$ contact sites (LAMs). Lam6 localizes to the ER-mitochondria contact sites by its PH-like domain and the C-terminal transmembrane helix. Here, we purified and crystallized the Lam6 PH-like domain from Saccharomyces cerevisiae. To aid crystallization of the Lam6 PH-like domain, T4 lysozyme was fused to the N-terminus of the Lam6 PH-like domain with a short dipeptide linker, GlySer. The fusion protein was crystallized under the condition of 0.1 M HEPES-HCl pH 7.0, 10% (w/v) PEG 8000, and 0.1 M $Na_3$ Citrate at 293K. X-ray diffraction data of the crystals were collected to $2.4{\AA}$ resolution using synchrotron radiation. The crystals belong to the orthorhombic space group $P2_12_12_1$ with unit cell parameters $a=59.5{\AA}$, $b=60.1{\AA}$, and $c=105.6{\AA}$. The asymmetric unit contains one T4L-Lam6 molecule with a solvent content of 58.7%. The initial attempt to solve the structure by molecular replacement using the T4 lysozyme structure was successful.

Structure Analyses of Rubber/Filler System under Shear Flow by Using Time Resolved USAXS Method

  • Nishitsuji, Shotaro;Takenaka, Mikihito;Amino, Naoya;Ishikawa, Yasuhiro
    • Elastomers and Composites
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    • v.54 no.2
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    • pp.156-160
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    • 2019
  • The changes in the dispersion of carbon black in liquid polyisoprene under shear flow with time have been investigated by time-resolved ultra small-angle X-ray scattering (USAXS) method. The analyses of USAXS profile immediately after the start of shear flow clarified that the aggregates of carbon black with a mean radius of gyration of 14 nm and surface fractal dimension of 2.5 form the fractal network structure with mass-fractal dimension of 2.9. After the application of the shear flow, the scattering intensity increases with time at the observed whole entire q region, and then the a shoulder appears at $q=0.005nm^{-1}$, indicating that the agglomerate is broken and becomes smaller by shear flow. The analysis by the Unified Guinier/Power-law approach yielded several characteristic parameters, such as the sizes of aggregate and agglomerate, mass-fractal dimension of agglomerate, and surface fractal dimension of the primary particle. While the mean radius of gyration of the agglomerate decreases with time, the mean radius of gyration of the aggregate, mass fractal dimension, and surface fractal dimension don't change with time, indicating that the aggregates peel off the surface of the agglomerate.