• Title/Summary/Keyword: X-ray Structure Analysis

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Formation Mechanism of Pores in Ni-P Coated Carbon Fiber Prepared by Electroless Plating Upon Annealing (무전해 니켈-인 도금법을 이용하여 도금된 탄소 섬유의 열처리 과정에서 나타나는 다공성 구조 생성 메커니즘 분석)

  • Ham, Seung Woo;Sim, Jong Ki;Kim, Young Dok
    • Applied Chemistry for Engineering
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    • v.24 no.4
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    • pp.438-442
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    • 2013
  • In the present work, electroless plating was used for coating thin films consisting mainly of Ni and P on carbon fiber. Structural changes appeared upon the post-annealing at various temperatures of the Ni-P film on carbon fiber was studied using various analysis methods. Scanning, a flat surface structure of Ni-P film on carbon fiber was found after electroless plating of Ni-P film on carbon fiber without post-annealing, whereas annealing at $350^{\circ}C$ resulted the formation of porous structures. With increasing the annealing temperature to $650^{\circ}C$ with an interval of $50^{\circ}C$, the pore size increased, but the density decreased. X-ray diffraction (XRD) showed the existence of metallic Ni, and Ni-P compounds before post-annealing, whereas the post-annealing resulted in the appearance of NiO peaks, and the decrease in the intensity of the peak of metallic Ni. Using X-ray photoelectron spectroscopy (XPS), phosphorous oxides were detected on the surface upon annealing at $650^{\circ}C$, and $700^{\circ}C$, which can be attributed to the phosphorous compounds originally existing in the deeper layers of the Ni films, which undergo sublimation and escape from the film upon annealing. Escape of phosphorous species from the bulk of Ni-P film upon annealing could leave a porous structure in the Ni films. Porous materials can be of potential applications in diverse fields due to their interesting physical properties such as high surface area, and methods for fabricating porous Ni films introduced here could be easily applied to a large-scale production, and therefore applicable in diverse fields such as environmental filters.

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)

  • Lee, Chung-Hyo;Jo, Jae-Mun;Lee, Sang-Jin;Sim, Hae-Seop;Lee, Chang-Hui
    • Korean Journal of Materials Research
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    • v.11 no.8
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    • pp.661-665
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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.

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Synthesis, Stability Constants, X-ray Structure and Electrochemical Studies of Copper (II) 1, 14-Bis (2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane.tetrahydrochloride Complex (1, 14-Bis(2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane.tetrahydro-chloride 구리착물의 합성, 안정도상수, X-ray 구조 및 전기화학적 연구)

  • Kim, Sun-Deuk;Kim, Jun-Kwang;Kim, Seong-Yun
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.173-178
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    • 2000
  • A new open-chain ligand containing two phenol groups, 1, 14-Bis (2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane(bsated) was synthesized as its tetrahydrochloride salt and characterized by elemental analysis, mass, infrared and NMR. Its proton dissociation constants ($logK^n{_H}$) and stability constants ($logK_{ML}$) toward $Co^{2+}$, $Ni^{2+}$, $Cu^{2+}$ and $Zn^{2+}$ were determined at $25^{\circ}C$ and 0.10M($KNO_3$) ionic strength in aqueous solution by potentiometry. The X-ray structure of its copper (II) complex [Cu(bsated)]$(ClO_4)_2$ was reported: Monoclinic space group $P2_1/n$, $a=17.856(4){\AA}$, $b=17.709(1){\AA}$, $c=8.539(2){\AA}$, $V=2700(2){\AA}$ with Z=4. Electrochemical studies of [Cu(bsated)]$(ClO_4)_2$ complex in dimethyl sulfoxide (DMSO) solution containing tetrabutylammonium perchlorate (supporting electrolyte) were carried out by cyclic voltammograms (CV) and normal pulse voltammetry (NPV).

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Hydrothermal Synthesis, Crystal Structure of Four Novel Complexes Based on Thiabendazole Ligand

  • Wei, Shui-Qiang;Lin, Cui-Wu;Yin, Xian-Hong;Huang, Yue-Jiao;Luo, Pei-Qi
    • Bulletin of the Korean Chemical Society
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    • v.33 no.9
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    • pp.2917-2924
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    • 2012
  • Four novel metal-organic complexes $[Cd_2(IP)_2(TBZ)_2(H_2O)_2]{\cdot}(H_2O)$ (1), $[Zn_4(IP)_4(TBZ)_4]{\cdot}2(H_2O)$ (2), $[Zn_2(BTC)(TBZ)_2(CO_2H)]$ (3), [Co(PDC)(TBZ)] (4) (where IP = isophthalate; TBZ = thiabendazole; BTC = 1,3,5-benzenetricarboxylate; PDC = pyridine-3,4-dicarboxylate) have been prepared and characterized by IR spectrum, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. X-ray structure analysis reveals that 1, 2, and 3 are one-dimensional chain polymers, while 4 is a two-dimensional network polymer. The TBZ acts as a typical chelating ligand coordinated to the metal center in all complexes. The 1D chain architecture of 1 is constructed from isophthalates and cadmium atoms. A simultaneous presence of chelating, monodentate and bidentate coordination modes of IP ligands is observed in complex 2. In complex 3, the 16-membered rings are alternately arranged forming an infinite 1D double-chain structure. The 2D skeleton of 4 is formed by cobalt ions as nodes and PDC dianions as spacers, through coordination bonds. The hydrogen bonds and ${\pi}-{\pi}$ stacking play important roles in affecting the final structure where complexes 1 and 3 have 2D supramolecular networks, while complexes 2 and 4 have 3D supramolecular architectures.

The structure analysis of $Y_1Ba_2Cu_3O_x$ high Tc superconductor based on rietveld method (리트벨트 해석법을 이용한 $Y_1Ba_2Cu_3O_x$ 고온 초전도체의 구조분석)

  • 채기병;소대화
    • Electrical & Electronic Materials
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    • v.8 no.6
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    • pp.780-786
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    • 1995
  • For the execution of RIETAN program adopting Rietveld Analysis Method, the sample superconductor is made according to the solid state synthesis method at 920.deg. C for 24hrs, and was examined for the optimization of parameters needed to analyze Rietveld method with the input of the measured pattern data after measuring the pattern resulted from the X-ray diffraction. It was proven that the lattice constant of the superconductor which was consisted of Pmmm orthorhombic crystal structure in the analyzed space group correspond to the presented theoretical lattice constant a=3.8887(8).angs., b=3.8238(4).angs., c=11.7079.angs.. Therefore, it was examined and confin-ned that the R factor, which was compensated after analyzing the structure of superconductor resulted from this experimented data with the computer simulation, was refined to $R_{wp}$=8.83[%], $R_{P}$=6.47[%], $R_{I}$=10.08[%], $R_{F}$=7.19[%], $R_{E}$=3.76[%]. On the basis of these experimental data, the significant parameter such as the scale factor(S) and the zero point shift(Z) and FWHM value(U,V,W) were optimized as follows; S=2.0827E-3, Z=0.2146, U=4.2761E-2, V=1.7983E-2, and W=2.6768E-2.2.2.2.2.2.

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Crystal and Block Structures of Hexagonal Ferrites (육방정 페라이트의 결정과 Block 구조)

  • Shin, Hyung-Sup
    • Journal of the Korean Ceramic Society
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    • v.49 no.3
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    • pp.205-215
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    • 2012
  • It has been studied the crystal and block structures of the hexagonal ferrites with M, W, Y and Z types prepared by various coprecipitation-oxidation method. The structures have been refined with a Rietveld analysis of the powder X-ray diffraction pattern with high precision ($R_{WP}$ <0.09, $R_I$ <0.03). The density difference between the S-blocks was proportioned to the cobalt contents in hexagonal ferrites, but that between the R or T-blocks was relatively small. Compared with the blocks and cation-oxygen polyhedra in BaM ($BaFe_{12}O_{19}$), those were bulky to the normal direction for the c-axis in $Co_2W$ ($BaCo_2Fe_{16}O_{27}$) and to the parallel direction for the c-axis in $Co_2Y$ ($Ba_2Co_2Fe_{12}O_{22}$) and $Co_2Z$ ($Ba_3Co_2Fe_{24}O_{41}$). The S-blocks of $Co_2W$, $Co_2Y$, and $Co_2Z$ were unstable and distorted. Because the T-block of $Co_2Z$ was unstable, the T-block was decomposed into the Ba-rich phase and $Co_2W$ at high temperatures above $1200^{\circ}C$. A standard powder X-ray diffraction pattern for $Co_2Z$ was proposed as well.

A Study on Formation of Ni-Tl-P deposits by Electroless Plating (무전해도금에 의한 Ni-Tl-P 피막형성에 관한 연구)

  • 류일광;추현식
    • Journal of the Korean institute of surface engineering
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    • v.33 no.2
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    • pp.126-134
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    • 2000
  • This study investigated the bath compositions and plating conditions and crystal structure used for achieving nickel-thallium-phosphorus deposits by means electroless plating. The electroless nickel-thallium-phosphorus deposits were achieved with a bath using sodium hypophosphite as the reducing agent and sodium citrate as the complexing agent. The depositing rate was 10.5mg.$cm^{2-1}$ .$hr^{-1 }$ from the optimistic bath composition, 0.1M nickel sulfate, 0.005M thallium sulfate, 0.2M sodium hypophosphite, and 0.05M sodium citrat and the recommended plating conditions, pH 5.5 and $90^{\circ}C$. The composition of alloy deposits determined by X-ray analysis (EDS) that the Thallium was increased with major increasing concentration of complexing agent and thallium ion in bath solution, it decreased according to the increasing concentrations of reduction agent in the bath solution, Bit Phosphorus showed a contrary to the thallium. It was observed from X-ray diffraction analysis, Scanning Electron Microscopy and Transmission Electron Microscopy. The crystalline structure of deposits was amorphous at the first deposited state but it was changed $Ni-T1-Ni_{5}$ $P_2$ polycrystalline when subjected to 1 hour heat treatment of more than $350^{\circ}C$. TEM observation demonstrated that the microstructure was identical to the result of the XRD at as deposited but it became $Ni-Tl-Ni_{5}$ $P_2$ polycrystalline when heated. And grain size was 10-50nm.

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Preparation and characterization of isotropic pitch-based carbon fiber

  • Zhu, Jiadeng;Park, Sang Wook;Joh, Han-Ik;Kim, Hwan Chul;Lee, Sungho
    • Carbon letters
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    • v.14 no.2
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    • pp.94-98
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    • 2013
  • Isotropic pitch fibers were stabilized and carbonized for preparing carbon fibers. To optimize the duration and temperature during the stabilization process, a thermogravimetric analysis was conducted. Stabilized fibers were carbonized at 1000, 1500, and $2000^{\circ}C$ in a furnace under a nitrogen atmosphere. An elemental analysis confirmed that the carbon content increased with an increase in the carbonization temperature. Although short graphitic-like layers were observed with carbon fibers heat-treated at 1500 and $2000^{\circ}C$, Raman spectroscopy and X-ray diffraction revealed no significant effect of the carbonization temperature on the crystalline structure of the carbon fibers, indicating the limit of developing an ordered structure of isotropic pitch-based carbon fibers. The electrical conductivity of the carbonized fiber reached $3.9{\times}10^4$ S/m with the carbonization temperature increasing to $2000^{\circ}C$ using a four-point method.

One-Pot Synthesis, Crystal Structures and Thermal Properties of Two Three-Dimensional Cobalt(II) Complexes

  • Tao, Bo;Lei, Wen;Cheng, Feiran;Xia, Hua
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1929-1933
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    • 2012
  • Two cobalt(II) compounds $[Co(2,2{^\prime}-bipy)(H_2O)_2(SO_4)]_n$ (1) and $[Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6]{\cdot}2H_2O$ (2) (2,2'-bipy = 2,2'-bipyridine, $H_4btec$ = 1,2,4,5-benzenetetracarboxylic acid), have been simultaneously synthesized by a one-pot slow solvent evaporation reaction. Their structures were determined by single-crystal X-ray diffraction and further characterized by X-ray powder diffraction (XRPD), IR, elemental and thermogravimetric analysis (TGA). The structural analysis reveals that compound 1 exhibits an infinite 1D chain structure with the octahedral Co(II) centers bridging by the tetrahedral ${\mu}_2-SO{_4}^{2-}$ ligands, while compound 2 possesses a dinuclear $Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6$ unit and the two adjacent octahedral Co(II) ions are linked by the bismonodentately coordinated btec ligand. Additionally, compound 2 exhibits blue fluorescent emission in the solid state at room temperature.