• Title/Summary/Keyword: wide angle X-ray diffraction

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Current Status of the Synchrotron Small-Angle X-ray Scattering Station BL4C1 at the Pohang Accelerator Laboratory

  • Jorg Bolze;Kim, Jehan;Huang, Jung-Yun;Seungyu Rah;Youn, Hwa-Shik;Lee, Byeongdu;Shin, Tae-Joo;Moonhor Ree
    • Macromolecular Research
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    • v.10 no.1
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    • pp.2-12
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    • 2002
  • The small-angle X-ray scattering (SAXS) beamline BL4C1 at the 2.5 GeV storage ring of the Pohang Accelerator Laboratory (PAL) has been in its first you of operation since August 2000. During this first stage it could meet the basic requirements of the rapidly growing domestic SAXS user community, which has been carrying out measurements mainly on various polymer systems. The X-ray source is a bending magnet which produces white radiation with a critical energy of 5.5 keV. A synthetic double multilayer monochromator selects quasi-monochromatic radiation with a bandwidth of ca. 1.5%. This relatively low degree of monochromatization is sufficient for most SAXS measurements and allows a considerably higher flux at the sample as compared to monochromators using single crystals. Higher harmonics from the monochromator are rejected by reflection from a flat mirror, and a slit system is installed for collimation. A charge-coupled device (CCD) system, two one-dimensional photodiode arrays (PDA) and imaging plates (IP) are available its detectors. The overall performance of the beamline optics and of the detector systems has been checked using various standard samples. While the CCD and PDA detectors are well-suited for diffraction measurements, they give unsatisfactory data from weakly scattering samples, due to their high intrinsic noise. By using the IP system smooth scattering curves could be obtained in a wide dynamic range. In the second stage, stating from August 2001, the beamline will be upgraded with additional slits, focusing optics and gas-filled proportional detectors.

Cure and Thermal Degradation Kinetics of Epoxy/Organoclay Nanocomposite

  • Park, Jae-Jun
    • Transactions on Electrical and Electronic Materials
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    • v.13 no.4
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    • pp.204-207
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    • 2012
  • Epoxy nanocomposite was synthesized through the exfoliation of organoclay in an epoxy matrix, which was composed of diglycidyl ether of bisphenol A (DGEBA), 4,4'-methylene dianiline (MDA) and malononitrile (MN). Organoclay was prepared by treating the montmorillonite with octadecyl trimethyl ammonium bromide (ODTMA). The exfoliation of the organoclay was estimated by wide angle X-ray diffraction (WAXD) analysis. In order to measure the cure rate of DGEBA/MDA (30 phr)/MN (5 phr)/organoclay (3 phr), differential scanning calorimetry (DSC) analysis was performed at various heating rates, and the data were interpreted by Kissinger equation. Thermal degradation kinetics of the epoxy nanocomposite were studied by thermogravimetric analysis (TGA), and the data were introduced to the Ozawa equation. The activation energy for cure reaction was 45.8 kJ/mol, and the activation energy for thermal degradation was 143 kJ/mol.

Long-term AC Electrical Treeing Behaviors of Epoxy/Layered Silicate Nanocomposites Prepared by a 3-Roll Mill

  • Park, Jae-Jun
    • Transactions on Electrical and Electronic Materials
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    • v.13 no.2
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    • pp.85-88
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    • 2012
  • Studies on the effects of layered silicate content on the AC electrical treeing and breakdown behaviors of epoxy/layered silicate nanocomposites were carried out in needle-plate electrode geometry. Wide-angle X-ray diffraction (WAXD) analysis and transmission electron microscopy (TEM) observation showed that 1 wt% of the multilayered silicate was fully exfoliated into nano-sized monolayers in the epoxy matrix however, over 3 wt% of the silicate was in an intercalated state. When 1 wt% layered silicates were incorporated, an electrical tree was initiated in 439 min and propagated at a speed of 2.3 ${\mu}m$/min after applying 781.4 kV/mm, representing a decreased in starting initiation time by a factor of 11.0 and increase in propagation speed by a factor 8.2 in comparison with neat epoxy resin. These values were in great decline after the layered silicate content was increased to 3wt% which implies that the exfoliated silicate blocked the tree initiation and propagation processes effectively. However the effect was largely decreased in the intercalated state.

Synthesis of PMMA/Clay Nanocomposite via Emulsion Polymerization (유화중합을 이용한 PMMA/Clay 나노컴포지트의 제조)

  • Kim, Cheol-Woo;Wu, Jong-Pyo
    • Journal of the Korean Applied Science and Technology
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    • v.20 no.3
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    • pp.243-250
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    • 2003
  • Poly(methyl methacrylate)/clay nanocomposite particles with particle size of 275${\sim}$292 nm range were successfully prepared using emulsion polymerization. The content of montmorillonite based on the methyl methacrylate monomer was chosen as 30 wt.%. 2,2-azobis(isobuthylamidine hydrochloride) and n-dodecyltrimethylammonium chloride were used as an initiator and a surfactant in cationic emulsion system. Potassium persulfate and sodium lauryl sulfate were used as an initiator and a surfactant in anionic emulsion system. The evidence of intercalated /exfoliated structure of montmorillonite in the nanocomposite prepared in our experiment was confirmed by wide angle x-ray diffraction patterns of $d_{001}$ plane. Thermal behavior of nanocomposite was traced using DSC and TGA. It was found that the nanocomposite particle prepared by cationic emulsion system showed intercalated structured. We also found that the nanocomposite particle obtained from anionic emulsion system resulted in the fully exfoliated structure.

m-Aramid Films in Diverse Coagulants

  • Kim, Ji-Young;Jung, Ji-Won;Kim, Sam-Soo;Lee, Jae-Woong
    • Textile Coloration and Finishing
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    • v.21 no.4
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    • pp.63-67
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    • 2009
  • m-Aramid dissolved in N,N-dimethylacetamide (DMAc), were coagulated in different coagulants such as water, methanol, ethanol, propanol and butanol. Various concentrations and temperatures of the coagulants were also used to evaluate dyeing properties of coagulated m-aramid films. Field emission scanning electron microscopy (FE-SEM) was employed to investigate the surface morphology of m-aramid films. Wide angle X-ray diffraction (WAXD) was conducted in order to measure crystallinity change of mcaramid fibers and films. WAXD patterns showed that crystallinity of m-aramid fibers was reduced after film formation. In addition, color depth (K/S value) was measured and the results revealed that the film coagulated in water possessed fairly enhanced color depth.

Preparation and Characterization of Enrofloxacin/Carbopol Complex in Aqueous Solution

  • Chun, Myung-Kwan;Choi, Hoo-Kyun
    • Archives of Pharmacal Research
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    • v.27 no.6
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    • pp.670-675
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    • 2004
  • Since the bitter taste of enrofloxacin apparently limit the patient compliance in the oral formulations of the antibacterial agent, the masking of the taste is essential for the improvement of the therapeutic effectiveness. Therefore, this study was carried out to examine the feasibility of taste masking of enrofloxacin by the retardation of its dissolution rate using the formation of complex between the drug and Carbopol. The complexation between Carbopol and enrofloxacin was confirmed by turbidity, UV spectrophotometry, wide angle X-ray diffraction, and differential scanning calorimetry. The enrofloxacin content in the complexes was 34% (Carbo-enrofloxacin complex I) and 57% (Carbo-enrofloxacin complex II) depending on the prepara-tion method. The dissolution rate of enrofloxacin from the complex increased as the pH was reduced. The dissolution rate of enrofloxacin from the Carbo-enrofloxacin complex I was significantly lower than that of the enrofloxacin powder. Therefore, these observations suggest that Carbo-enrofloxacin complex I can be used to mask the taste of enrofloxacin.

Effect of Organically Modified Layered Silicate on Thermal, Mechanical, and Electrical Properties of Epoxy-Based Nanocomposites

  • Park, Jae-Jun;Kwon, Soon-Seok;Lee, Jae-Young
    • Transactions on Electrical and Electronic Materials
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    • v.12 no.4
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    • pp.135-139
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    • 2011
  • In an effort to develop new electrical insulation materials, four different kinds of organically modified layered silicate were incorporated into an epoxy matrix to prepare nanocomposites for electrical insulation. Five wt% of organically modified layered silicates were processed in a planetary centrifugal mixer in an epoxy matrix, and the thermal, mechanical, and electrical properties of the cured epoxy/layered silicate were investigated. The morphology of the nanoscale silicate dispersed in the epoxy matrix was observed using transmission electron microscopy, and the interlayer distance was measured by wide-angle X-ray scattering diffraction analysis.

A Study on the Acid Degradation Properties of Cellulose Fabrics for Costume Heritage Restoration (유물 복원을 위한 천연 셀룰로오스 직물의 산에 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.35-40
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    • 2005
  • Researches to preserve and restore the excavated cellulose fabrics as costume heritages have been carried out. In this study, in order to artificially restore an excavated cellulose fabrics, acid-treated cellulose fabrics were prepared. Three kinds of cellulose fabrics were used for an experiment. Three kinds of cellulose fabrics were treated by the acid aqueous solution for the various strength retention ($100\%,\;80\%,\;60\%,\;40\%,\;20\%$). The fine structure and physical properties of acid treated cellulose fabrics were investigated with various techniques such as wide-angle X-ray diffraction, tensile test, weight loss, shrinkage, SEM etc. Tensile strength and strain of cellulose fabrics decreased with increasing acid treatment time. However, weight loss and shrinkage increasing slightly. The crystal diffraction intensity was not changed. SEM results of acid-treated cellulose fabrics show that the surface was damaged.

Photo-Degradation Behavior of Silk Fabrics (견직물의 광열화 거동)

  • Lee, Hack-Jung;Kwon, Young-Suk;Jang, Jeong-Dae;Lee, Sang-Joon;Cho, Hyun-Hok
    • Textile Coloration and Finishing
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    • v.18 no.6 s.91
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    • pp.37-42
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    • 2006
  • Researches to preserve and restore the remaining fabrics as costume heritages have been carried out. In this study, in order to artificially restore an excavated silk fabrics, degummed silk fabrics and safflower dyed silk fabrics were prepared for an experiment. These fabrics were photo-degraded by the Xenon arc beam to have various strength retention(100%, 80%, 60%, 40%, 20%). The fine structure and physical properties of Xenon arc treated fabrics were investigated with various techniques such as tensile test, weight loss, wide-angle X-ray diffraction, yellowness, color, SEM etc. Tensile strength and the crystal diffraction intensity of silk fabrics decreased as Xenon arc hem treatment time increased. Weight loss increased slightly. Strength retention was decreased as the Xenon arc beam treatment time goes by. (Yellowness of the undyed silk fabrics and $L^*$ of the dyed silk fabrics increased. Whiteness of the undyed silk fabrics and $b^* of the dyed silk fabrics decreased.) SEM results of the silk fabrics treated Xenon arc beam show that surface was a little damaged.

Cocrystallization of Poly(1,4-cyclohexylenedimethylene terephthalate-co-hexamethylene terephthalate) Copolymers

  • Jeong, Young-Gyu;Jo, Won-Ho;Lee, Sang-Cheol
    • Macromolecular Research
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    • v.12 no.5
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    • pp.459-465
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    • 2004
  • We have synthesized poly(l,4-cyclohexylenedimethylene terephthalate-co-hexamethylene terephthalate) [P(CT-co-HT)] random copolymers having various comonomer contents, from 0 to 100 mol% HT, by melt-condensation and have investigated their crystallization behavior by using differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD). We observed that P(CT-co-HT)s exhibit clear melting and crystallization peaks in their DSC thermograms and sharp diffraction peaks in their WAXD patterns for all of their copolymer compositions as a result of cocrystallization of the CT and HT units, even though the copolymers are statistically random copolymers. When we plotted the melting and crystallization temperatures of P(CT-co-HT)s and the d-spacings of all the reflections against the copolymer composition, we observed a eutectic point at ca. 80 mol% HT, which suggests that a crystal transition occured from a PCT-type crystal to a PHT-type crystal. Both the DSC and WAXD results support the notion that P(CT-co-HT) copolymers undergo an isodimorphic cocrystallization.