• Title/Summary/Keyword: X-ray crystal diffraction

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In-situ Determination of Structural Changes in Polyethylene upon Creep and Cyclic Fatigue Loading (크리프와 반복 피로하중에 의한 폴리에틸렌의 실시간 구조 변화)

  • Jeon, Hye-Jin;Ryu, Seo-Kgn;Pyo, Soo-Ho;Choi, Sun-Woong;Song, Hyun-Hoon
    • Polymer(Korea)
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    • v.36 no.1
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    • pp.88-92
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    • 2012
  • Long-term performance of polymer under constant sustained load has been the main research focus, which created a need for the accelerated test method providing proper lifetime assessment. Cycling fatigue loading is one of the accelerated test method and has been of great interest. Microstructure change of high density polyethylene under cyclic fatigue loading and creep was examined utilizing a tensile device specially designed for creep and fatigue test and also can be attachable to the X-ray diffractometer. In this way, the crystal morphology change of polyethylene under creep and cyclic fatigue load was successfully monitored and compared. Despite the marked differences in macroscopic deformation between the creep and cyclic fatigue tests, crystal morphology such as crystallinity, crystal size, and $d$-spacing was as nearly identical between the two test cases. Specimens pre-deformed to different strains, i.e., before yield point (BYP), at yield point (YP) and after yield point (AYP), however, showed markedly different changes in crystal morphology, especially between AYP and the other two specimens.

A Study on the Alkaline Degradation Properties of Silk Fabrics for Costume Heritage Restoration (유물 복원을 위한 실크 직물의 알칼리에 의한 열화 특성 연구)

  • Jeon Cho-Hyun;Kwon Young-Suk;Lee Sang-Joon;Cho Hyun-Hok
    • Textile Coloration and Finishing
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    • v.17 no.4 s.83
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    • pp.41-47
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    • 2005
  • Costume heritages of an excavated silk fabrics should be preserved without damage. In order to artificially restore the excavated silk fabrics, alkaline aqueous solution, as a simulated corpse, and two kinds of silk fabrics were used. Two kinds of silk fabrics were treated by aqueous alkaline solution according to strength retention value(100, 80, 60, 40, 20$\%$). The fine structure and physical properties of alkaline treated silk fabrics were investigated with various techniques such as wide-angle X-ray diffraction, tensile test, weight loss, shrinkage, SEM. and yellowness. As the alkaline treatment time increased tensile strength of silk fabrics decreased. However, weight loss and shrinkage slightly increased. The diffraction intensity of $\beta-form$ crystal declined and $\alpha-form$ crystal diffraction intensity disappeared with the treatment.

The effect of additives on the electrocrystallization of Zn-Ni alloy deposit (아연-니켈 합금도금 전착성에 미치는 첨가제 영향)

  • 김현태;정원섭
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.456-464
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    • 1997
  • The effect of the additives on the Zn-Ni alloy electrocrystallization from a chloride bath was investigated by means of electrochemical methodes, scanning electron microscopy and measurement of surface appearance, X-ray diffraction patterns. The additives tested were the surfactant of naphtalene-derivative, saccharin and aliphatic alcohol. The resistance of electrodeposit increased by adding the additives, whereas the effect of additives on resistance was different with current density. The nickel content of alloy deposit was increased by the addition of alcohol, while decreased by the surfactant. The surface roughness, appearance and morphology of deposit were also influenced by the type of additive. The fine, compact grains and good surface roughness could be obtained from the surfactant or alcohol -added bath, and the surfactant or saccharin improved the surface appearance.

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Crystal Structure and Thermal Decomposition Studies on Cobalt (II) Complex of 4-Chloro-2-((E)-(Isopropylimino)methyl)phenol (4-Chloro-2-((E)-(Isopropylimino)methyl)phenol 코발트(II) 착물에 대한 결정 구조 및 열분해 연구)

  • Pu, Xiao-Hua
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.341-345
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    • 2011
  • The Schiff base cobalt(II) complex, bis[4-chloro-2-((E)-(isopropylimino) methyl) phenol]cobalt(II), has been prepared and characterized by single-crystal X-ray diffraction analyses. The phenomenological, kinetic and mechanistic aspects of the cobalt (II) complex have been studied by TG/DTG techniques. On the basis of the experimental data, the kinetic parameters such as activation energy, pre-exponential factor and entropy of activation were computed, and then the most probable mechanism function was estimated as $g({\alpha})={\alpha}^2$ 2. Hence the rate controlling process at all stages of decomposition is onedimensional diffusion (Parabolic model).

Growth of $CaF_{2}:R^{+3}$ (R=Nd, Er) layers by molecular beam epitaxy (Molecular beam epitaxy법에 의한 희토류 이온$(Nd^{3+},\;Er^{3+})$ 첨가 $CaF_{2}$ 박막의 성장)

  • ;Yefen Chen;Tsuguo Fukuda
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.1
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    • pp.1-5
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    • 1999
  • The rare-earth ions ($R^{3+}$, R=Nd, Er) doped $CaF_{2}$ layers have been grown on $CaF_{2}$ (111) substrate by molecular beam epitaxy. The surface structure and the crystallinity of $CaF_{2}:R^{3+}$ layers depending on the doping concentration of $R^{3+}$ and layer thickness were studied by reflection high-energy electron diffraction (RHEED). In aspect of application as buffer layer in semiconductor-related hybrid structure, the lattice displacement between $CaF_{2}:R^{3+}$ layers and $CaF_{2}$ (111) substrate was investigated by X-ray rocking curve analysis.

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Preparation and photocatalytic activity of ACF/$TiO_2$ composites by using titanium n-butoxide and acid modified activated carbon fiber

  • Oh, Won-Chun;Kwon, Ho-Joug;Chen, Ming-Liang;Zhang, Feng-Jun;Ko, Weon-Bae
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.19 no.3
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    • pp.144-151
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    • 2009
  • Photocatalytic degradation of methylene blue (MB) in aqueous solution was investigated using $TiO_2$ coated on various acid modified activated carbon fiber (ACF). The ACFs/$TiO_2$ composites were prepared from titanium n-butoxide (TNB) as titanium precursor and various acid modified ACFs. The prepared samples are heat treated at 973 K. Then the ACF/$TiO_2$ composites were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX). Moreover, photocatalytic degradation of MB by the ACF/$TiO_2$ composites was determined under UV irradiation. The results shows that the photocatalytic activity of ACF/$TiO_2$ composites ($AT1{\sim}AT4$) prepared with TNB and various acid modified ACF was much better than that of ACF/$TiO_2$ composite (AT) prepared with TNB and non-acid modified ACF, and the effects improved with order of sample AT3 > AT4 > AT1 > AT2.

Synthesis of graphene nano-sheet without catalysts and substrates using fullerene and spark plasma sintering process

  • Jun, Tae-Sung;Park, No-Hyung;So, Dea-Sup;Lee, Joon-Woo;Lim, Hak-Sang;Ham, Heon;Shim, Kwang Bo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.1
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    • pp.27-30
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    • 2013
  • Catalyst-free graphene nano-sheets without substrates have been synthesized using fullerene and a high direct current (dc) pulse in the spark plasma sintering (SPS) process. Graphene nano-sheets were synthesized directly in the gas phase of carbon atoms which are generated from fullerene at a temperature of $600^{\circ}C$. Characterization has been carried out by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), Raman spectroscopy (Raman), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD).

Development of an Auto Sample Centering Algorithm at the Macromolecular Crystallography Beam Line of the Pohang Light Source (단백질 결정학 빔 라인에서의 자동 샘플 정렬 알고리즘 개발)

  • Jang, Yu-Jin
    • The Transactions of the Korean Institute of Electrical Engineers D
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    • v.55 no.7
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    • pp.313-318
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    • 2006
  • An automatic sample centering system is underway at the protein crystallography beam line of the Pohang Light Source to improve the efficiency of the crystal screening process. A sample pin which contains a protein crystal is mounted on a goniometer head. Then the crystal should be moved to the center of X-ray beam by controlling the motorized goniometer to obtain diffraction data. Since the X-ray beam is located at the center of the image obtained from the CCD camera when the image of the sample pin is in focus, an auto-focusing algorithm is a very important part in the auto-sample-centering system. However the results of applying several well-known auto focusing algorithms directly to the images are not satisfactory owing to the following factors: misalignment of CCD camera, non-uniform cryo-stream in the background of the image and the supporter of the loop. The performance of an auto-focusing algorithm can be increased if the algorithm is applied to only the loop region identified. Non-uniform cryo-stream and a various illumination condition and a stain, which is shown in the image, are main obstacles to loop region identification. In this paper, a simple loop region identification algorithm, which can solve these problems, is proposed and the effective ness of the proposed scheme is shown by applying the auto-focusing algorithm to the loop region identified.

Synthesis and Crystal Structures of Copper(II) Complexes with Schiff Base Ligands: [Cu2(acpy-mdtc)2(HBA)(ClO4)]·H2O and [Cu2(acpy-phtsc)2(HBA)]·ClO4

  • Koo, Bon Kweon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3233-3238
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    • 2013
  • Two new Cu(II) complexes, $[Cu_2(acpy-mdtc)_2(HBA)(ClO_4)]{\cdot}H_2O$ (1) (acpy-mdtc- = 2-acetylpyridine S-methyldithiocarbamate and $HBA^-$ = benzilic acid anion) and $[Cu_2(acpy-phtsc)_2(HBA)]{\cdot}ClO_4$ (2) (acpy-$phtsc^-$ = 2-acetylpyridine 4-phenyl-3-thiosemicarbazate) have been synthesized and characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, and single crystal X-ray diffraction. The X-ray analysis reveals that the structures of 1 and 2 are dinuclear copper(II) complexes bridged by two thiolate sulfur atoms of Schiff base ligand and bidentate bridging $HBA^-$ anion. For 1, each of the two copper atoms has different coordination environments. Cu1 adopts a five-coordinate square-pyramidal with a $N_2OS_2$ donor, while Cu2 exhibits a distorted octahedral geometry in a $N_2O_2S_2$ manner. For 2, two Cu(II) ions all have a five-coordinate square-pyramidal with a $N_2OS_2$ donor. In each complex, the Schiff base ligand is coordinated to copper ions as a tridentate thiol mode.

A Highly Stereoselective Synthesis and Crystal Structure of (E)-4'-Amino-3,4,5- trimethoxystilbene ((E)-4'-Amino-3,4,5-trimethoxystilbene의 선택적인 합성 및 결정 구조)

  • Li, Xia-Bing;Zhang, Xi-Quan;Gu, Hong-Mei;Li, Bao-Lin
    • Journal of the Korean Chemical Society
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    • v.55 no.2
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    • pp.251-255
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    • 2011
  • A new and highly stereoselective synthesis of (E)-4'-amino-3,4,5-trimethoxystilbene was achieved by using 3,4,5-trimethoxybenzaldehyde and p-nitrotoluene as starting materials through condensation under solvent-free condition and followed by the reducing of nitro group with the system of $NH_2NH_2/FeCl_3$/C in ethanol. The crystal structure of (E)-4'-amino-3,4,5-trimethoxystilbene was also determined by X-ray diffraction analysis.