• 제목/요약/키워드: X-ray Diffraction Method

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증기급속응축법 제조 귀금속 나노분말의 결정학적 특성 연구 (Characterization of Crystal Structure for Nanosized Noble Metal Particles Fabricated by ERC(Evaporation and Rapid Condensation) Method)

  • 유연태
    • 한국재료학회지
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    • 제13권5호
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    • pp.285-291
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    • 2003
  • The nanosized silver and gold particles are prepared by ERC method in which metal vapors with high temperature is rapidly quenched by coolants such as liquid nitrogen or liquid argon. In order to monitor the crystal structural changes on the internal and the surface of the nanosized noble metal particles, lattice parameter, internal strain and Debye-Waller factor are investigated, and the calculation of X-ray diffraction scattering intensity is performed. The lattice parameters of silver and gold particles agree with those of bulk materials, and crystal internal strain of the metal particles is not changed by rapid cooling. The Debye-Waller factor of gold particles is increased with decreasing particle size because of the surface softening phenomenon of nanosized particles, but the crystal structural change on the surface of the particles is not detected from the comparison the calculated X-ray diffraction profile with the experimental profile on gold particles with the particle size of 4 nm.

전기저항 점용접부의 용접잔류응력 해석에 관한 연구 (A Study on the Welding Residual Stress Analysis of the Spot Welding Point)

  • 손일선;배동호
    • 대한용접접합학회:학술대회논문집
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    • 대한용접접합학회 1999년도 특별강연 및 춘계학술발표대회 개요집
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    • pp.233-236
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    • 1999
  • The welding residual stress should be considered in fatigue stress analysis because it develope during the process of the electric resistance spot welding and it causes bad affect on the fatigue crack initiation and growth at nugget edge of spot welded points. Therefore the accurate estimation of residual stress is crucial. In this study, nonlinear finite element analysis on welding residual stress generated during the process of the spot welding was conducted, and their results were compared with the experimental data measured by X-ray diffraction method. From the results, it was found that welding residual stress existed as tension in the nugget center and as compression around the nugget edge.

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Refinement of the structure of naproxen, (+)-6- methoxy-$\alpha$-methyl-2-naphthaleneacetic acid

  • Kim, Yang-Bae;Song, Hyun-June;Park, Il-Yeong
    • Archives of Pharmacal Research
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    • 제10권4호
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    • pp.232-238
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    • 1987
  • The molecular structure of naproxen determined by X-ray diffraction technique was refine to the final R-value geing 0.042. The compound was recrystallized from ethanol solution in monoclinic crystal system, space group $P2_1$ , with Z = 2, a = 13.375(5) $\AA$, b = 5.793(2) $\AA$, c = 7.914 $\AA$, $\beta$=93.91(3)$\AA$ and $d_{obs}$ = 1.26, $d_{calc}$ = 1.25 g/cm$^{3}$. The structure was solved by direct method and refined by block diagonal least squares procedure for 747 relfections (F .leq. 6.sigma.(F)). The molecules are connected by two intermolecular OH--O type hydrogen bonds.

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대향타겟식 스퍼터법으로 제작된 AIN 박막의 결정학적 특성 (Crystallographic properties of AIN thin film prepared by lacing targets sputtering method)

  • 양진석;금민종;손인환;최형욱;김경환
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2000년도 하계학술대회 논문집
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    • pp.464-466
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    • 2000
  • AIN thin films have been prepared by reactive sputtering method, using facing targets sputtering system with a DC power supply which can deposit a high quality thin film and control deposition condition in all range of nitrogen. The crystallographic characteristics of AIN thin films on N$_2$/Ar ratio was investigated by alpha-step and X-ray diffraction. As a result, the AIN film deposited at the pressure ratio of the nitrogen of 30% revealed strong X-ray diffraction intensity under substrate temperature 25$^{\circ}C$ and applied current 0.4A.

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X-선 산란을 이용한$SnO_{2}$ 박막의 결정구조 정밀화 (Crystal Structure Refinement of $SnO_{2}$ Thin Film Using X-ray Scattering)

  • 김용일;남승훈;박종서
    • 대한기계학회:학술대회논문집
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    • 대한기계학회 2003년도 추계학술대회
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    • pp.1939-1943
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    • 2003
  • The precise structural analysis of $SnO_{2}$ thin film, which was prepared by PECVD and thickness 2400 ${\AA}$, was tried to do the structural refinement using X -ray diffraction data. The observed diffraction patterns of $SnO_{2}$ thin film had the strongly preferred orientation effect. WIMV method was used to correct the preferred orientation effect. The final weighted R-factor, $R_{WD}$ was 7.92 %. The lattice parameters, a = b == 4.7366(1) ${\AA}$ and c = 3.1937(1) ${\AA}$, were almost in accordance with ones of $SnO_{2}$ powder.

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The Crystal Structure of Cinmetacin ($C_{21}H_{19}NO_4$), A Non-steroidal Antiinflammatory Agent

  • Kim, Yang-Bae;Park, Il-Yeong;Park, Yang-Hwan
    • Archives of Pharmacal Research
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    • 제12권1호
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    • pp.52-57
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    • 1989
  • The structure of cinmetacin was determined by single crystal X-ray diffraction analysis. The compound was recrystallized from a mixture of acetone and water in orthorhombic, space group $P2_12_12_1$, with Z=4, a=35.681(8), b=9.482(2), c:5.071(1) ${\AA}$, $D_x=1.352 g/cm^3$, and $D_m=1.35g/cm^3$. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.036 for 1441 observed reflections ($F{\geq}3{\sigma}(F)$). The carboxyl group of the molecule is nearly perpendicular to the indole ring. The dihedral angle between indole ring and phenyl group is $64.5^{\circ}$. The molecules are linked together via O(1)-H ----O(3) hydrogen bonds, and arranged along 2-fold screw axis in the crystal. The intermolecular contacts are the normal van der Waals' forces.

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APPLICATION STUDY OF CHEMOINFOMETRICAL NEAR-INFRARED SPECTROSCOPY IN PHARMACEUTICAL INDUSTRY

  • Otsuka, Makoto;Kato, Fumie;Matsuda, Yoshihisa
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.2111-2111
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    • 2001
  • A chemoinfometrical method for evaluating the quantitative determination of crystallinity one 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 and compared with the conventional powder X-ray diffraction method was performed. [Method] The pPure a and g forms of indomethacin (IMC) were prepared by reportedusing published methods. Six kinds of standard samples obtained by physically mixing of a and g forms. After the powder X-ray diffraction profiles of samples have been measured, the intensity values were normalized to against the intensity of silicon powder as the as an external standard. The calibration curves for quantification of crystal content were based upon the total relative intensity of four diffraction peaks from of the form g crystal. FT-NIR spectra of six calibration sample sets were recorded 5 times with the NIR spectrometer (BRAN+LUEBBE). Chemoinfometric analysis was performed on the NIR spectral data sets by applying the principal component regression (PCR). [Results] The relation between the actual and predicted polymorphic contents of form g IMC measured using by the X-ray diffraction method shows a good straight linen linear relation., and it has slope of 0.023, an intercept of 0.131 and a correlation coefficient of 0.986. PCR analyses wereis was performed based on normalized NIR spectra sets offer standard samples of known content of IMC g form. IMC. A calibration equation was determined to minimize the root mean square error of the predictionthe prediction. Figure 1 shows a plot of the calibration data obtained by NIR method between the actual and predicted contents of form g IMC. The predicted values were reproducible and had a smaller standard deviation. Figure 2 shows that the plot for the predicted transformation rate (%) of form a IMC to form g as measured by X-ray diffractomeoy against to those as measured by NIR method. The plot has a slope of 1.296, an intercept of 1,109, and a correlation coefficient of 0.992. The line represents a satisfactory correlation between the two predicted values of form g IMC content. Thus NIR spectroscopy is an effective method for the evaluation to the pharmaceutical products of quantitative of polymorph.

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Additive manufacturing and mechanical properties evolution of biomedical Co-Cr-Mo alloys by using EBM method

  • Chiba, Akihiko;Kurosu, Shingo;Matsumoto, Hiroaki;Li, Yunping;Koizumi, Yuichiro
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2012년도 춘계학술발표대회
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    • pp.56.1-56.1
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    • 2012
  • The microstructures and mechanical properties of Co-29Cr-6Mo alloy with C and N additions, produced by additive manufacturing using electron beam melting (EBM) method, were studied using X-ray diffraction, electron back scatter diffraction, transmission electron microscope, Vickers hardness tests, and tensile tests, focusing on the influences on the build direction and the various heat treatments after build. It is found that the microstructures for the as built specimens were changed from columnar to equiaxed grain structure with average grain size of approximately $10-20{\mu}m$ due to the heat treatment employing the reverse transformation from a lamellar (hcp + $Cr_2N$) phase to an fcc. Our results will contribute to the development of biomedical Ni-free Co-Cr-Mo-N-C alloys, produced by EBM method, with refined grain size and good mechanical properties, without requiring any hot workings.

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Composition Dependence on Structural and Optical Properties of MgxZn1-xO Thin Films Prepared by Sol-Gel Method

  • Kim, Min-Su;Noh, Keun-Tae;Yim, Kwang-Gug;Kim, So-A-Ram;Nam, Gi-Woong;Lee, Dong-Yul;Kim, Jin-Soo;Kim, Jong-Su;Leem, Jae-Young
    • Bulletin of the Korean Chemical Society
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    • 제32권9호
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    • pp.3453-3458
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    • 2011
  • The $Mg_xZn_{1-x}O$ thin films with the various content ratio ranging from 0 to 0.4 were prepared by sol-gel spincoating method. To investigate the effects of content ratio on the structural and optical properties of the $Mg_xZn_{1-x}O$ thin films, scanning electron microscopy (SEM), X-ray diffraction (XRD), and photoluminescence (PL) were carried out. With increase in the content ratio, the grain size of the $Mg_xZn_{1-x}O$ thin films was increased, however, at the content ratio above 0.2, MgO particles with cubic structure were formed on the surface of the $Mg_xZn_{1-x}O$ thin films, indicating that the Mg content exceeded its solubility limit in the thin films. The residual stress of the $Mg_xZn_{1-x}O$ thin films is increased with increase in the Mg mole fraction. In the PL investigations, the bandgap and the activation energy of the $Mg_xZn_{1-x}O$ thin films was increased with the Mg mole fraction.