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X-ray Analys is of the Thermotropic Liquid Crystalline Copolyester Poly(1 -phenylethylpphenylene-tere phthalate) (열방성 액정폴리에스터Poly(1-phenylethyl.p-phenyleneterephthalate)의 X-선 결정구조해석)

  • 홍성권
    • Korean Journal of Crystallography
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    • v.2 no.2
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    • pp.13-21
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    • 1991
  • X-ray methods have been used to determine the chain conformation and packing of the thermotropic liquid crystalline copolyester prepared from 50% tarephthaloyl chloride(TPA) and 50% (1-phenylethyl) hydroquinone(PEHQ). The x-ray patterns of annealed melt-spun fibers contain a series of annealed melt-Pointing to a well ordered crystalline structure, despite the random sense(2 or 3-) of the 1-phenylethyl substiuttion on the TPA-hydroquinone backbone. The crystalline fiber is monoclinic with space group P2l and the unit cell has dimensions 11=12.77 A, b=10.17 A (upique axis), c=12.58 h (fiber axis). and β=90.1° and contains TPA-PEHO units of to or chains. The random substitution of 1-phenylethyl groups was modelled by placing these groups at both the 2and 3 positions and giving each a weight of one-hal(. T he structure has been refined by linked a rom least square methods(LALS) against 16 observed and 21 unobserved reflections. and had a final R value of 0.20. Packing of the side chains is effected by staggering adjacent chains along the b axis by approximately c/2, so that the side chains are interleaved. The phenyl-COO and COO-phenyl torsion angles are -6.1 and 65.6, respectively, such that the main chain phenyls are mutually inclined at 59.5 (the ester groups are assumed to be planar). These torsion angles compare very well with those for the model compounds, notably phenylbenzoate, and can be used in future analyses of the structures of more complex random sequence copolyesters.

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Synthesis of Dimethyl Carbonate from Methanol and Supercritical Carbon Dioxide over K2CO3/ZrO2 Catalysts (메탄올과 초임계 이산화탄소로부터 K2CO3/ZrO2 촉매를 이용한 디메틸카보네이트 (Dimethyl Carbonate) 합성)

  • Hong, Seung Tae;Park, Hyung Sang;Lim, Jong Sung;Yoo, Ki-Pung
    • Korean Chemical Engineering Research
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    • v.46 no.3
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    • pp.550-554
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    • 2008
  • The synthesis of dimethyl carbonate (DMC) from methanol and supercritical carbon dioxide over $K_2CO_3/ZrO_2$ catalysts have been studied. The catalysts were prepared by impregnating $ZrO_2$ with an aqueous $K_2CO_3$ solution. The optimum calcination temperature to disperse K species on the $ZrO_2$ surface was found to be 673 K. Monoclinic $ZrO_2$ was not active, as itself, for the DMC production. However, when the $K_2CO_3$ was impregnated on the $ZrO_2$, the catalytic performance was improved. Besides the catalyst, $CH_3I$ was used as a promoter. The $CH_3I$ promoter as well as the $K_2CO_3/ZrO_2$ catalyst was found to take an important role to improve the production of DMC. The optimum quantities for the catalyst and the promoter were estimated. The effect of the catalyst and the promoter for the DMC synthesis from methanol and supercritical carbon dioxide was investigated and the reaction mechanism was proposed.

Preparation of CaO-SiO2-B2O3 Glass-ceramics and Evaluation of Bioactivity Using in-vitro Test (CaO-SiO2-B2O3계 결정화 유리의 제조와 in-vitro법을 이용한 생체활성 평가)

  • Ryu, Hyun-Seung;Seo, Jun-Hyuk;Kim, Hwan;Hong, Kug-Sun;Kim, Deug-Joong;Lee, Jae-Hyup;Lee, Dong-Ho;Chang, Bong-Soon;Lee, Choon-Ki
    • Journal of the Korean Ceramic Society
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    • v.39 no.5
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    • pp.490-497
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    • 2002
  • Sintering property, mechanical property and bioactivity of $CaO-SiO_2-B_2O_3$ glass-ceramics were investigated. This glass-ceramics was sintered at 750-830${\circ}$ and showed nearly pore-free microstructure. The glass-ceramics consisted of three phases, i.e. monclinic-wollastonite, calcium borate and borosilicate glass matrix. The mechanical strength was higher than that of other bioactive ceramics, especially compressive strength(2813 MPa) and fracture toughness($3.12 MPa{\cdot}m^{1/2}$). Bioactivity of the glass-ceramics depends on amount of $CaB_2O_4$ and borosilicate glass matrix. It might be likely that more soluble $CaB_2O_4$ raises supersaturation of Ca ion in SBF solution and borosilicate glass forms Si-OH group that presents nucleation site of hydroxycarbonate apatite(HCA) layer. So, glassceramics of more $CaB_2O_4$ and borosilicate glass showed better bioactivity.

Petrology on the Late Miocene Basalts in Goseong-gun, Gangwon Province (강원도 고성군 일대의 후기 마이오세 현무암의 암석학적 연구)

  • Koh Jeong Seon;Yun Sung-Hyo
    • Journal of the Korean earth science society
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    • v.26 no.1
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    • pp.78-92
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    • 2005
  • Petrographical and petrochemical analyses for late Miocene basalts in Goseong-gun area. Gangwon province, were carried out to interpret the characteristics and the origin of magma. The basaltic rocks occurred as plug-dome in the summit of several small mountain and developed columnar jointing with pyroxene-megacryst bearing porphyritic texture. And the basalt contains xenoliths of biotite granite (basement rocks), gabbro (lower crustal origin) and Iherzolite(upper mantle origin). The basalts belong to the alkaline basalt field in TAS diagram and partly belong to picrobasalt and trachybasalt field. On the tectonomagmatic discrimination diagram f3r basalt in the Goseong-gun area. they fall into the fields for the within plate and oceanic island basalt. The characteristics of trace elements and REEs shows that primary magma for the basalt magma would have been derived from partial melting of garnet-peridotite mantle. This late Miocene basalt volcanism is related to the hot spot within the palte.

Fabrication and Its Characteristics of YSZ Composite with Added Transition Metal Oxides (천이금속산화물이 첨가된 YSZ 복합체의 제조 및 그 특성)

  • 최성운;박재성
    • Journal of the Institute of Electronics Engineers of Korea TE
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    • v.39 no.4
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    • pp.341-349
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    • 2002
  • Electrical, mechanical and sinterability properties of yttria-stabilized zirconia doped with 5.35wt% $Y_2$O$_3$(Y$_2$O$_3$- containing stabilized zirconia : YSZ) were studied as a function of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ addition. The ratio of monoclinic phase to tetragonal phase was changed by the addition of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ to 8.00 wt% and sintered density decreased with increasing $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ addition. Fracture toughness increased with the increase of monoclinic to tetragonal phase ratio and was maximum at about 18%. When transition metals such as CoO, Fe$_2$O$_3$ or MnO$_2$ was added more than 1.5 wt%, the electrical conductivity of YSZ increased. But $Al_2$O$_3$ hardly affected the electrical conductivity of YSZ. The addition of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ into YSZ resulted in the more complex behavior of fracture toughness and hardness variation and the specimen with 1.5wt%-Fe$_2$O$_3$, 3.0wt%-Al$_2$O$_3$ and 1.5wt%-CoO showed the monoclinic to tetragonal phase ratio of 18% and the highest toughness of 10.8 MPa.m$^{1}$2/ and Vickers hardness of 1201 kgf/mm$^2$.

Crystal Structure of Bithional Sulfoxide, $C_{12}H_6Cl_4O_3S$ (비치오놀 설폭사이드, C12H6Cl4O3S의 결정구조)

  • Sin, Hyeon So;Song, Hyeon
    • Journal of the Korean Chemical Society
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    • v.38 no.4
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    • pp.283-287
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    • 1994
  • The crystal stucture of bithional surfoxide, $C_{12}H_6Cl_4O_3S$, has been determined from 2295 independent reflections collected on an automated CAD-4 diffractometer with a graphite-monochromated $Mo-K\alpha$ radiation. The crystal belongs to the monoclinic, space group P2$_1$/n, with a unit cell dimensions a = 12.448(4), b = 9.740(1), c = $11.815(2)\AA$, $\beta$ = $100.06^{\circ}$, $\mu$ = 9.02 cm$^{-1}$, Dm = 1.76 g/cm$^3$, Dc = 1.75 g/cm$^3$, F(000) = 744, and Z = 4. The structure was solved by the direct method and refined by the least-squares method. The final R values was 0.037 for 2295 independent reflections. Overall conformation of the molecule is folded with respect to central surfur atom. Comparing with the molecular conformation of bithional, one of phenyl rings was swinged with about $180^{\circ}.$ This conformational change in the molecule results in the existance of intramolecular-hydrogen bond of S-O(3)---H-O(1) type and its steric hindrance between this moiety and the other phenyl ring. The two best planes of the phenyl rings have a maximum deviation of 0.009 $\AA$ for C(1) atom. The dihedral angle between two phenyl rings is $99.22^{\circ}.$ In the crystal structure, the molecules are packed with intermolecular-hydrogen bond of O(3)---H-O(2).

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Tholeitic volcanism in Cheju Island, Korea (제주도의 솔리아이트 화산활동)

  • 박준범;권성택
    • The Journal of the Petrological Society of Korea
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    • v.5 no.1
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    • pp.66-83
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    • 1996
  • We report petrography, mineral chemistry, and major and trace element chemistry for rare tholeiites in Cheju island where alkalic rocks predominate. Available age data indicate that the tholeiitic magmatism was younger than 0.49Ma, possibly younger than 0.17 Ma. The tholeiites are generally fine-grained, porphyritic rock and show intergranular texture with lath-shaped plagioclase ($An_{61-46}$), orthopyroxene (bronzite) and olivine ($Fo_{78-67}$). Characteristically, two kinds of clinopyroxene (pigeonite and augite) occur only in groundmass. The tholeiites have normative quartz and show limited compositional variations ($SiO_2$=51.0-52.5 wt%; Mg#=54-60). Major and transitional metal element variations of tholeiites are distinct from those of alkaline rocks in MgO diagram, suggestingthat the two rock types cannot be simply related to differentiation process from the same magma. The ratios among $K_2O$, Rb, Ba, Nb and La are similar for both tholeiites and alkali basalts, however the ratios between the elements (P, Y and Yb) having an affinity with garnet and the above elements are higher for tholeiites than for alkali basalts. These trace element ratios suggest that the tholeiites and alkali basalts were produced by different degrees of partial melting from a similar sources material (garnet lherzolite mantle).

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Petrology of Puu Oo lavas from the Big Island, Hawaii (하와이, 빅 아일랜드의 푸우오오 용암에 대한 암석학적 연구)

  • Kwon, Suk-Bom;Jang, Yun-Deuk;Park, Byeong-Jun;Kim, Yeong-Kyoo;Kim, Jung-Jin
    • The Journal of the Petrological Society of Korea
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    • v.16 no.4
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    • pp.217-232
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    • 2007
  • The Puu Oo eruption in Hawaii since 1983 is one of the largest eruptions on Hawaii's volcanic history with prominent compositional variation ($5.6{\sim}10.1wt.%$ in MgO content). Although intense researches of Hawaiian eruption have been conducted for recent years, there is no up-to-date study on Puu Oo lavas that is erupting hot lavas today. in oder to obtain basic information on the geological characteristics of the eruption including any noticeable change in its petrological trend and magma dynamics, we applied several geological approaches such as field survey, systematic sampling, petrography, mineralogy, and geochemistry. Clinopyroxene and Plagioclase phenocrysts are rarely observed on the thin section, however Olivine crysts are much more obvious in the study area. It indicates that Puu Oo is early stage of magma differentiation. Variation diagram of whole rock composition shows that the elements such as $TiO_2,\;Al_2O_3,\;SiO_2$ and $Na_2O$ decrease with increasing MgO. In the trace element Sr, Y Zr and V versus $K_2O$, P18, P19 samples are plotted in primitive area. Variations of the Ni contents during $2003{\sim}2006$ may suggest a sudden change in magma composition probably caused by new magma injection.

Rietveld Refinement and Crystal Structure of K-Ba Substituted Synthetic Hollandite, ($K_{2x}Ba_{1-x}Cr_2Ti_6O_{16}$) (리트벨트법을 이용한 K-Ba 치환 합성 홀란다이트($K_{2x}Ba_{1-x}Cr_2Ti_6O_{16}$)의 결정구조 연구)

  • 최진범;김태현
    • Journal of the Mineralogical Society of Korea
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    • v.14 no.2
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    • pp.128-136
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    • 2001
  • The K-Ba complete solid solution of 7 synthetic hollandite-type minerals ($K_{2x}$ $Ba_{1-x}$ $Cr_2$/$Ti_{6}$ $O_{16}$ , x=0, 0.1, 0.3, 0.5, 0.7, 0.9, 1.0, respectively) are studied by the X-ray powder diffraction and Rietveld refinement to find structural transformation during substitution of $Ba^{2+}$ by $K^{+}$ in A site of the tunnel structure of hollandite. Rietveld indices indicate that $R_{wp}$ with respect to $R^{exp}$ ($R_{wp}$ $R_{exp}$ ) are in the range of 15.66%/20.90% and 14.74%/l9.37%, $R_{B}$ and S(Goodness of Fitness) are 6.45~8.97%, 1.45~1.63, respectively. Unit cell parameters of synthetic hollandites, space group 14/m, are a=10.1194(2)~10.0599(2)$\AA$, c=2.9572(6)~2.9512(7)$\AA$, and V=302.75~298.66$\AA^{3}$. Rutile formed as an impurity in those with more than 50% K contents in hollandite series. Substitution of Ba by K ion in a tunnel structure results in constant decrease of cell parameters, but is not sufficient enough to change the hollandite structure. Our data indicate that transformation of tetragonal 14/m to lower symmetry of monoclinic 12/m in hollandite structure may at least be affected by other cation substitution in same A site and/or by cation substitution in B site.

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A Study on the Mechanical Properties of Single and Multiple layer Thin Film of YSZ Electrolyte Produced by E-beam Coating for Solid Oxide Fuel Cells (전자빔 코팅에 의해 제조된 고체산화물 연료전지용 YSZ 전해질 단층 및 다층박막의 기계적 특성 연구)

  • Im, Hae-Sang;Kim, Hui-Jae;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.9 no.8
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    • pp.792-797
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    • 1999
  • The 8mol.%Y$_2$$O_3$-$ZrO_2$mainly employed as an electrolyte of solid oxide fuel cells(SOFCs) shows excellent electrical properties but has a weakness in the mechanical properties. Since the electrolyte of SOFCs requires both good electrical and mechanical properties, this study was conducted to meet both requirements. The electrolyte thin films were produced on the LSM(cathode material) substrate of a cell and Si wafer. Four electrolyte film types of single layer and the multiple layer, consisting of 3-YSZ(3mol.%$Y_2$$O_3$) with excellent mechanical properties and 8-YSZ with the excellent electric conduction, were produced by electron beam coating technology. Ther crystal structure and the mechanical properties were also analysed. As the results of the study, the 3-YSZ thin film turned out to be in the tetragonal, partially monoclinic phase, while the 8-YSZ thin film showed the cubic phase. The residual stress in the multiple layer was lower than that of the single layer. The microhardness of the multiple layer was similar to that of the existing 8-YSZ single layer both before and after annealing treatment.

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