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

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Crystal Structure of an Acetylene Sorption Complex of Dehydrated Fully Mn(II)-Exchanged Zeolite X

  • 배명남;김양
    • Bulletin of the Korean Chemical Society
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    • v.19 no.10
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    • pp.1095-1099
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    • 1998
  • The crystal structure of an acetylene sorption complex of dehydrated fully Mn(Ⅱ)-exchanged zeolite X, Mn46Si100Al92O384·30C2H2 (a=24.705(3) Å) has been determined by single-crystal X-ray diffraction techniques. The structure was solved and refined in the cubic space group Fd3 at 21(l) ℃. The complex was prepared by dehydration at 380 ℃ and 2 x 10-6 Torr for 2 days, followed by exposure to 300 Torr of acetylene gas for 2 h at 24 ℃. The structure was refined to the final error indices, R1=0.060 and R2=0.054 with 383 reflections for which I > 3σ(Ⅰ). In the structure, Mn2+ ions are located at two different crystallographic sites; sixteen Mn2+ ions at site I are located at the centers of the double six rings and thirty Mn2+ ions are found at site Ⅱ in the supercage, respectively. Each of these latter Mn2+ ions is recessed ca. 0.385(2) Å into the supercage from its three-oxygen plane. Thirty acetylene molecules are sorbed per unit cell. Each Mn2+ ion at site Ⅱ lies on a threefold axis in the supercage of the unit cell, close to three equivalent trigonally arranged zeolite framework oxygen atoms (Mn(Ⅱ)-O=2.135(9) Å) and symmetrically to both carbon atoms of a C2H2 molecules. At these latter distances, the Mn(Ⅱ)-C interactions are weak (Mn(Ⅱ)-C=2.70(5) Å), probably resulting from electrostatic attractions between the divalent cations and the polarizable π-electron density of the acetylene molecules.

Three Crystal Structures of Dehydrated $Cd^{2+}$ and $Rb^+$ Exchanged Zeolite A, $Cd_xRb_{12-2x}-A,$ x=4.0, 5.0 and 5.95

  • Song, Yeong-Sim;Kim, Un-Sik;Kim, Yang;Kim, Duk-Soo
    • Bulletin of the Korean Chemical Society
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    • v.11 no.4
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    • pp.328-331
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    • 1990
  • Three crystal structures of dehydrated Cd(II) and Rb(I) exchanged zeolite A, $Cd_{4.0}Rb_{4.0}-A (a = 12.204(3) {\AA}), Cd_{5.0}Rb_{2.0}-A (a = 12.202(1) {\AA}),$ and $Cd_{5.95}Rb_{0.1}-A (a = 12.250(2) {\AA}),$ have been determined by single-crystal X-ray diffraction techniques. Their structures were solved and refined in the cubic space group Pm3m at $21(1)^{\circ}C.$ All crystals were ion exchanged in flowing streams of mixed $Cd(NO_3)_2·4H_2O$ and $RbNO_3$ aqueous solution with total concentration of 0.05 M. All crystals were dehydrated at ca. $450^{\circ}C$ and $2×10^{-6}$ Torr for 2 days. In all of these structures, $Cd^{2+}$ ions are found on threefold axes, each nearly at the center of a 6-oxygen ring. The first three $Rb^+$ ions per unit cell preferentially associate with 8-oxygen rings, and additional $Rb^+$ ions, if present, are found on threefold axes in the large cavity. The final $R_1$ and $R_2$ values for the three structures are 0.087 and 0.079, 0.059 and 0.067, and 0.079 and 0.095, respectively.

The properties of AlGaN epi layer grown by HVPE (HVPE에 의해 성장된 AlGaN epi layer의 특성)

  • Jung, Se-Gyo;Jeon, Hun-Soo;Lee, Gang-Seok;Bae, Seon-Min;Yun, Wi-Il;Kim, Kyoung-Hwa;Yi, Sam-Nyung;Yang, Min;Ahn, Hyung-Soo;Kim, Suck-Whan;Yu, Young-Moon;Cheon, Seong-Hak;Ha, Hong-Ju
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.1
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    • pp.11-14
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    • 2012
  • The AlGaN layer has direct wide bandgaps ranging from 3.4 to 6.2 eV. Nowadays, it is becoming more important to fabricate optical devices in an UV region for the many applications. The high quality AlGaN layer is necessary to establish the UV optical devices. However, the growth of AlGaN layer on GaN layer is difficult due to the lattice mismatch and difference thermal expansion coefficient between GaN layer and AlGaN layer. In this paper, we attempted to grow the LED structure on GaN template by mixed-source HVPE method with multi-sliding boat system. We tried to find the optical and lattice transition of active layer by control the Al content in mixed-source. For the growth of epi layer, the HCl and $NH_3$ gas were flowed over the mixed-source and the carrier gas was $N_2$. The temperature of source zone and growth zone was stabled at 900 and $1090^{\circ}C$, respectively. After the growth, we performed the x-ray diffraction (XRD) and electro luminescence (EL) measurement.

Crystal structure of $Ba(Mg_{1/3}Nb_{2/3})O_3$ - $La(Mg_{2/3}Nb_{1/3})O_3$ Complex perovskite compound ($Ba(Mg_{1/3}Nb_{2/3})O_3$ - $La(Mg_{2/3}Nb_{1/3})O_3$ 복합 페로브스카이트 화합물의 결정구조)

  • Paik, Jong-Hoo;Lee, Mi-Jae;Choi, Byung-Hyun;Lee, Jong-Won;Jee, Mi-Jung;Lim, Eun-Kyeong;Nahm, Sahn;Lee, Hwack-Joo
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2003.11a
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    • pp.283-287
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    • 2003
  • Crystal structure of $(Ba_{1-x}La_x)[Mg_{(1+x)/3}Nb_{(2-x)/3}]O_3$ (BLMN) ceramics with $0{\leq}x{\leq}1$ was investigated using synchrotron X-ray powder diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). When La content, x, is above 0.1, the 1:2 ordered hexagonal structure found in $Ba(Mg_{1/3}Nb_{2/3})O_3$ (BMN) was transformed into 1:1 ordered cubic structure. The 1:1 ordered cubic structure was maintained up to x=0.7. However, when x exceeded 0.7, BLMN was transformed 1:1 ordered structure which has cation displacement and in-phase and anti-phase tilt of octahedra.

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Growth and characterization of ZnIn$_2$S$_4$ single crystal thin film using Hot Wall Epitaxy method (Hot Wall Epitaxy (W)에 의한 ZnIn$_2$S$_4$ 단결정 박막 성장과 특성)

  • 윤석진;홍광준
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07a
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    • pp.266-272
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    • 2002
  • The stochiometric mixture of evaporating materials for the ZnIn$_2$S$_4$ single crystal thin film was prepared from horizontal furnace. To obtain the ZnIn$_2$S$_4$ single crystal thin film, ZnIn$_2$S$_4$ mixed crystal was deposited on throughly etched semi-insulating GaAs(100) in the Hot Wall Epitaxy(HWE) system. The source and substrate temperature were 610 $^{\circ}C$ and 450 $^{\circ}C$, respectively and the growth rate of the ZnIn$_2$S$_4$ single crystal thin film was about 0.5 $\mu\textrm{m}$/hr. The crystalline structure of ZnIn$_2$S$_4$ single crystal thin film was investigated by photo1uminescence and double crystal X-ray diffraction(DCXD) measurement. The carrier density and mobility of ZnIn$_2$S$_4$ single crystal thin film measured from Hall effect by van der Pauw method are 8.51${\times}$10$\^$17/ cm$\^$-3/, 291 $\textrm{cm}^2$/V$.$s at 293 $^{\circ}$K, respectively. From the photocurrent spectrum by illumination of perpendicular light on the c - axis of the ZnIn$_2$S$_4$ single crystal thin film, we have found that the values of spin orbit splitting ΔSo and the crystal field splitting ΔCr were 0.0148 eV and 0.1678 eV at 10 $^{\circ}$K, respectively. From the photoluminescence measurement of ZnIn$_2$S$_4$ single crystal thin film, we observed free excition (E$\_$X/) typically observed only in high quality crystal and neutral donor bound exciton (D$^{\circ}$,X) having very strong peak intensity. The full width at half maximum and binding energy of neutral donor bound excition were 9 meV and 26 meV, respectively. The activation energy of impurity measured by Haynes rule was 130 meV.

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Growth and Optoelectrical Properties for $AgGaSe_2$ Single Crystal Thin Films ($AgGaSe_2$ 단결정 박막 성장과 광전기적 특성)

  • Hong, Kwang-Joon;You, Sang-Ha
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2004.11a
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    • pp.171-174
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    • 2004
  • The stochiometric $AgGaSe_2$ polycrystalline mixture of evaporating materials for the $AgGaSe_2$ single crystal thin film was prepared from horizontal furnace. To obtain the single crystal thin films, $AgGaSe_2$ mixed crystal and semi-insulating GaAs(100) wafer were used as source material and substrate for the Hot Wall Epitaxy (HWE) system, respectively. The source and substrate temperature were fixed at $630^{\circ}C$ and $420^{\circ}C$, respectively. The thickness of grown single crystal thin films is $2.1{\mu}m$. The single crystal thin films were investigated by photoluminescence and double crystal X-ray diffraction(DCXD) measurement. The carrier density and mobility of $AgGaSe_2$ single crystal thin films measured from Hall effect by van der Pauw method are $4.89{\times}10^{17}\;cm^{-3},\;129cm^2/V{\cdot}s$ at 293K, respectively. From the photocurrent spectrum by illumination of perpendicular light on the c - axis of the $AgGaSe_2$ single crystal thin film, we have found that the values of spin orbit splitting ${\Delta}S_o$ and the crystal field splitting ${\Delta}C_r$ were 0.1762 eV and 0.2494 eV at 10 K, respectively. From the photoluminescence measurement of $AgGaSe_2$ single crystal thin film, we observed free excition $(E_X)$ observable only in high quality crystal and neutral bound exciton $(D^o,X)$ having very strong peak intensity And, the full width at half maximum and binding energy of neutral donor bound excition were 8 meV and 14.1 meV, respectively. By Haynes rule, an activation energy of impurity was 141 meV.

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Studies on the Crystal Growth in ZnO-AI$_2$O$_3$-SiO$_2$Glass (ZnO-Al$_2$O$_3$-SiO$_2$ 유리에서의 결정성장에 관한 연구)

  • 이종근;이병하
    • Journal of the Korean Ceramic Society
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    • v.12 no.1
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    • pp.23-28
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    • 1975
  • The object of this study is to find the optimum conditions for crystal growth and kinds of crystal in ZnO-Al2O3-SiO2 glass composition. At first, the base glass composed of ZnO (44.7%), Al2O3(14.0%) and SiO2(41.3%) was melted in propane gas furnace at 1450-150$0^{\circ}C$ for an hour, and then it was poured into the stainless steel mould heated previously at $600^{\circ}C$ to obtain the thin glass test piece. Four crystal forms from base glass such as stuffed keatite, zinc orthosilicate, zinc aluminosilicate, and cristobalite were crystallized during heat treatment between 80$0^{\circ}C$ and 110$0^{\circ}C$. For the investigation of crystal growth, X-ray diffractometer and thermal differential analysis were used and the growth rate of the four crystal forms were obtained by the method of Archimedes specific gravity and intensity comparison of X-ray diffraction peak. The results obtained were as follows. 1) Stuffed keatite peaks which started to appear after two hours at 80$0^{\circ}C$ were maximum after 11 hours and this crystal breaks down to willemite irreversibly at about 100$0^{\circ}C$. 2) Development of gahnite started at 85$0^{\circ}C$ and increased with temperature growth. 3) Stuffed keatite which had been transformed slowly into willemite at 100$0^{\circ}C$ was decreased with time and willemite increased until four hours. 4) Cristobalite began to be developed after treatment of 110$0^{\circ}C$.

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Structure and chemical composition of $CsB_{3}O_{5}$ (CBO) optical surface

  • V.V. Atuchin;V.G. Kesler;L.D. Pokrovsky;N. Yu. Maklakova;M. Yoshimura;N. Ushiyama;T. Matsui;K. Kamimura;Y. Mori;T. Sasaki
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.1
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    • pp.19-23
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    • 2003
  • Polished surface of $CsB_{3}O_{5}$ (CBO) has been observed by reflection high energy electron diffraction (RHEED) and X-ray photoelectron spectroscopy (XPS). For comparison, electronic properties of CBO powder have been studied by XPS. It has been found that the crystal surface is covered by thick amorphous layer with chemical composition closely related to that of CBO. Great enrichment of top surface by cesium, ~30 % in reference to the bulk of the modified layer, has been displayed by depth profiling.

Dialytic pH Condition for Obtaining Silk I Type Structure (Silk I형 결정을 얻기 위한 투석의 pH조건)

  • ;小西 孝
    • Journal of Sericultural and Entomological Science
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    • v.39 no.1
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    • pp.67-72
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    • 1997
  • As a condition for obtaining the silk I type crystal that has stability and high reproducibility, after dissolving silk fibroin crystalline part (Fcp), the changes of recrystallized crystal structure according to dialytic pH were examined by x-ray diffraction and differential thermal analysis. The Fcp was obtained from the aqueous solution of silk fibroin enzymatic proteolyzed by chymotrypsin. The crystal structure of Fcp showed silk II type. When the Fcp was dissolved by 10M LiBr aqueous solution, the Fcp1 showed the silk II type at pH 9. However, besides the silk II type, the silk I type structure begins to appear at pH 8 and only the silk I type structure was found below pH 6. On the other hand, the Fcp2 that calcium chloride was used in the dissolution found only the silk I type crystal structure below pH8.

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Optical properties of vanadium dioxide thin films on c-Al2O3 (001) substrates by in-situ RF magnetron sputtering

  • Han, Seung Ho;Kang, So Hee;Kim, Hyeongkeun;Yoon, Dae Ho;Yang, Woo Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.5
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    • pp.224-229
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    • 2013
  • Vanadium oxide thin films were deposited on $c-Al_2O_3$ (001) substrate by in-situ RF magnetron sputtering. Oxygen partial pressure was adjusted to prepare thermochromic $VO_2$ phase. X-ray diffraction patterns and scanning electron microscopy convincingly showed that plate-like $V_2O_5$ grains were changed into round-shape $VO_2$ grains as oxygen partial pressure decreased. After the optimized deposition conditions were fixed, the effect of substrate temperature and orientation on the optical properties of $VO_2$ thin films was analyzed.