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

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Chemical Vapor Deposition of β-LiGaO2 Films on Si(100) Using a Novel Single Precursor

  • Sung, Myung M.;Kim, Chang G.;Kim, Yun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.480-484
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    • 2004
  • $LiGaO_2$ films have been grown on Si (100) substrates using a new single precursor $[Li(OCH_2CH_2OCH_3)_2-Ga(CH_3)_2]_2$ under high vacuum conditions $(5{\times}10^{-6}Torr)$. The $[Li(OCH_2CH_2OCH_3)_2Ga(CH_3)_2]_2$ was synthe-sized and characterized by using spectroscopic methods and single-crystal X-ray diffraction analysis. The chemical composition, crystalline structure, and morphology of the deposited films were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, and scanning electron microscopy. The results show that polycrystalline $LiGaO_2$ films preferentially oriented in the [010] direction can be deposited on Si (100) at 500-550$^{\circ}C$ by metal organic chemical vapor deposition (MOCVD). The single precursor $[LiOCH_2CH_2OCH_3)_2-Ga(CH_3)_2]_2$ has been found suitable for chemical vapor deposition of $LiGaO_2$ thin films on Si substrates.

Application Study of Chemoinfometrical Near-Infrared Spectroscopic Method to Evaluate for Polymorphic Content of Pharmaceutical Powders (일본의 근적외선분광법에 대한 제약회사 응용 및 현황)

  • Otsuka, Makoto
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2002.11a
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    • pp.97-117
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    • 2002
  • A chemoinfometrical method for quantitative determination of crystal content of indomethacin (IMC) polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the conventional powder X-ray diffraction method was performed. Pure $\alpha$ and ${\gamma}$ forms of IMC were prepared using published methods. Powder X-ray diffraction profiles and NIR spectra were recorded for six kinds of standard materials with various content of ${\gamma}$ form IMC. The principal component regression (PCR) analyses were performed based on normalized NIR spectra sets of standard samples of known content of IMC ${\gamma}$ form. A calibration equation was determined to minimize the root mean square error of the prediction. The predicted ${\gamma}$ form content values were reproducible and had a relatively small standard deviation. The values of ${\gamma}$ form content predicted by two methods were in close agreement. The results were indicated that NIR spectroscopy provides for an accurate quantitative analysis of crystallinity in polymorphs compared with the results obtained by conventional powder X-ray diffractometry.

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Application of Inverse Pole Figure to Rietveld Refinement: III. Rietveld Refinement of $SnO_2$ Thin Film using X-ray Diffraction Data

  • Kim, Yong-Il;Jung, Maeng-Joon;Kim, Kwang-Ho
    • The Korean Journal of Ceramics
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    • v.6 no.4
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    • pp.354-358
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    • 2000
  • The SnO$_2$film was deposited on a corning glass 1737 substrate by plasma enhanced chemical vapor deposition using a gas mixture of SnCl$_4$, $O_2$, and Ar. The film thickness was measured using $\alpha$-step and was about 9400$\AA$. The conventional X-ray diffractometry and pole figure attachment were used to refine the crystal structure of SnO$_2$ thin film. Six pole figures, (200), (211), (310), (301), (321), and (411), were measured with CoK$_\alpha$ radiation in reflection geometry. The X-ray diffraction data were measured at room temperature using CuK$_\alpha$ radiation with graphite monochromator. The agreement between calculated and observed patterns for the normal direction of SnO$_2$ thin film was not satisfactory due to the severely preferred orientation effect. The Rietveld refinement of heavily textured SnO$_2$ thin film was successfully achieved by adopting the pole density distribution of each reflection obtained from the inverse pole figure as a correction factor for the preferred orientation effect. The R-weighted pattern, R$_wp$, was 15.30%.

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Vapor Phase Epitaxy of Magnesium Oxide on Si(001) Using a Single Precursor

  • Lee, Sun-Sook;Lee, Sung-Yong;Kim, Chang G.;Lee, Sang-Heon;Nah, Eun-Ju;Kim, Yunsoo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.122-122
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    • 2000
  • Magnesium oxide is thermodynamically very stable, has a low dielectric constant and a low refractive index, and has been widely used as substrate for growing various thin film materials, particulary oxides of the perovskite structure. There has been a considerable interest in integrating the physical properties of these oxides with semiconductor materials such as GaAs and Si. In this regard, it is considered very important to be able to grow MgO buffer layers epitaxially on the semiconductors. Various oxide films can then be grown on such buffer layers eliminating the need for using MgO single crystal substrates. Vapor phase epitaxy of magnesium oxide has been accomplished on Si(001) substrates in a high vacuum chamber using the single precursor methylmagnesium tert-butoxide in the temperature range 750-80$0^{\circ}C$. For the epitaxy of the MgO films, SiC buffer layers had to be grown on Si(001). The films were characterized by reflection high energy electron diffraction (RHEED) in situ in the growth chamber, and x-ray diffraction (XRD), x-ray pole figure analysis, scanning electron microscopy (SEM), and x-ray photoelectron spectroscopy (XPS) after the growth.

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Structure Identification of 1,2-Disubstituted Chiral Calix[4]arene : X-Ray and NMR Analysis of 25-(3,5-Dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene

  • 박영자;신정미;남계춘;김종민;국승근
    • Bulletin of the Korean Chemical Society
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    • v.17 no.7
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    • pp.643-647
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    • 1996
  • 1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

Magnetic Properties and Impedance Spectroscopic Studies of Multiferroic Bi1-xNdxFeO3 Materials

  • Thang, Dao Viet;Thao, Du Thi Xuan;Minh, Nguyen Van
    • Journal of Magnetics
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    • v.21 no.1
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    • pp.29-34
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    • 2016
  • Nd-doped $BiFeO_3$ materials were synthesized via a sol-gel method. The crystal structure, magnetic properties, and complex impedance spectroscopy of multiferroic $Bi_{1-x}Nd_xFeO_3$ (BNFO) materials were investigated by X-ray diffraction (XRD), Raman scattering, vibrating sample magnetometer (VSM), and complex impedance spectroscopy. Our results show that the lattice crystal constants (a, c) and the ratio c/a of BNFO materials decreased with increasing Nd concentration. All samples exhibited weak ferromagnetism at room temperature, and the magnetization of samples was enhanced by the presence of $Nd^{3+}$ ions. There was an enhancement in the spontaneous magnetization of BFO with increasing Nd concentration, which is attributable to the collapse of the spin cycloid structure.

A Study on the Fatigue-Fractured Surface of Normalized SS41 Steel and M.E.F. Dual Phase Steel by an X-ray Diffraction Technique (X-선 회절에 의한 SS41 불림재와 M.E.F. 복합 조직강의 피로 파단면 해석에 관한 연구)

  • Oh, Sae-Wook;Park, Young-Chul;Park, Soo-Young;Kim, Deug-Jin;Hue, Sun-Chul
    • Journal of the Korean Society for Nondestructive Testing
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    • v.16 no.1
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    • pp.10-18
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    • 1996
  • This study verified the relationship between fracture mechanics parameters and X-ray parameters for normalized SS41 steel with homogeneous crystal structure and M.E.F. dual phase steel(martensite encapsulated islands of ferrite). The fatigue crack propagation test were carried out and X-ray diffraction technique was applied to fatigue fractured surface. The change in X-ray parameters(residual stress, half-value breadth) according to the depth of fatigue fractured surface were investigated. The depth of maximum plastic zone, $w_y$, were determined on the basis of the distribution of the half-value breadth for normalized SS41 steel and that of the residual stress for M.E.F. dual phase steel. $K_{max}$ could be estimated by the measurement of $w_y$.

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The Crystal and Molecular Structure of BENTAZONE, $C_{10}H_{12}N_2O_3S$ (BENTAZONE, $C_{10}H_{12}N_2O_3S$의 결정 및 분자구조)

  • 박권일;조성일
    • Korean Journal of Crystallography
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    • v.8 no.2
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    • pp.144-148
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    • 1997
  • the molecular and crystal 3-dimensional structure of bentazone, C10H12N2O3S, has been determined from single crystal x-ray diffraction study. Crystal system is monoclinic: a=8.7817(9)Å, b=9.6059(9) Å, c=13.574(9) Å, β=97.269(1)', V=1136.1(6)Å, space group : P21/c, z=4. The molecular structure model was solved by direct method and refined by full matrix least squares. The final reliable factor, R, is 0.045 for 1396 independent reflections(Fo2>4σFo2). A molecule has a staggered conformation with thiocarbazin ring and isopropyl functional group and the molecules by hydrogen bonds are cross stacked along the c-axis.

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Crystallization and Preliminary X-Ray Crystallographic Analysis of PAS Factor from Vibrio vulnificus

  • Lee, Jun Hyuck;Kim, Soo Young;Rho, Seong-Hwan;Im, Young Jun;Kim, Young Ran;Kim, Mun-Kyoung;Kang, Gil Bu;Rhee, Joon Haeng;Eom, Soo Hyun
    • Molecules and Cells
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    • v.20 no.3
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    • pp.361-363
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    • 2005
  • Plasmid Achromobacter secretion (PAS) factor is a putative secretion factor that induces the secretion of periplasmic proteins. PAS factor from Vibrio vulnificus was crystallized at 294 K by the hanging drop vapor-diffusion method. It was isolated as a monomer during the purification procedures. The native crystal belongs to the F222 space group with unit cell parameters a = 56.1, b = 74.4, $c=80.0{\AA}$, ${\alpha}={\beta}={\gamma}=90^{\circ}$. The crystal was soaked in cryoprotectant containing 1 M NaBr for 1 h for MAD phasing. The diffraction limit of the Br-MAD data set was $1.9{\AA}$ using synchrotron X-ray irradiation at beam line BL-18B at the Photon Factory, Japan.

Effect of a Laser Ablation on High Voltage Discharge Plasma Area for Carbon Nitride Film Deposition (고전압 방전 플라즈마에 의한 질화탄소 박막 증착 시 플라즈마 영역에 가한 레이저 애블레이션의 효과)

  • 김종일
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.15 no.6
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    • pp.551-557
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    • 2002
  • Carbon nitride films have been deposited on Si(100) substrate by a high voltage discharge plasma combined with laser ablation in a nitrogen atmosphere. The films were grown both with the without the presence of an assisting focused Nd:YAG laser ablation. The laser ablation of the graphite target leads to vapor plume plasma expending into th ambient nitrogen arc discharge area. X-ray photoelectron spectroscopy and Auger electron spectroscopy were used to identify the binding structure and the content of the nitrogen species in the deposited films. The nitrogen content of the films was found to increase drastically with an increase of nitrogen pressure. The surface morphology of the films was studied using a scanning electron microscopy. Data of infrared spectroscopy and x-ray photoelectron spectroscopy indicate the existence of carbon-nitrogen bonds in the films. The x-ray diffraction measurements have also been taken to characterize the crystal properties of the obtained films.