Study of the Microstructure of iViaterials by Synchrotron Radiation Wavelength-Modulated Diffraction Method

同步辐射波长调制衍射法研究iVaterials的微观结构

• 批准号: 14550659
• 负责人: IWASAKI Hiroshi
• 金额: $ 2.05万
• 依托单位: Ritsumeikan University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 2002
• 资助国家: 日本
• 起止时间: 2002 至 2003
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-14550659/
• 关键词: Synchrotron Radiation; X-ray Diffraction; Crystal Structure Analysis; Anomalous Scattering; Multilayer Monochromator; X線回析

We established utilizing the continuous nature of spectrum and the high brightness of synchrotron radiation a new diffraction method "wavelength-modulated diffraction" and showed that it is possible to derive information on the microstructure of materials that is not obtainable by other methods. From the intensity profile of Bragg reflections recorded using radiation of a band of wavelength in the vicinity of the absorption edge of an atom in organic crystal, phases of the structure factors were derived.In the present research, the method has been extended so that parallel radiation beam of a band of wavelength isproduced by reflection by a depth'graded multilayer at the X-ray diffraction beamline at the Ritsumeikan Synchrotron Radiation Center and used to record intensity profiles of Bragg reflections. With a single crystal of a ferrocene derivative known to have an enantiomorphous structure as a sample and the wavelength band set so as to include the absorption edge of the iron atom, clear contrast has been observed at the edge between the Friedel pairs of reflections and the chirality of the structure has been unequivocally determined. It has also been shown that the method has a wide range of application in diffraction crystallography.

我们利用光谱的连续性和同步辐射的高亮度建立了一种新的衍射方法“波长调制衍射”，并表明它有可能获得其他方法无法获得的材料微观结构信息。利用有机晶体中原子吸收边附近一波段的辐射记录布拉格反射的强度分布，导出了结构因子的相位。在本研究中，扩展了该方法，在立命馆同步辐射中心的x射线衍射光束线上，通过深度梯度多层反射产生一波段的平行辐射光束，并用于记录布拉格反射的强度分布。以已知具有对映异构结构的二茂铁衍生物单晶为样品，并设置包含铁原子吸收边的波长带，在弗里德尔反射对的边缘处观察到明显的对比，明确地确定了该结构的手性。结果表明，该方法在衍射晶体学中具有广泛的应用前景。

项目成果

T.Koganezawa, H.Iwasaki, N.Nakamura, Y.Yoshimura, T.Shoji: "A Wide-B andp ass Monochromator and Jts Application to the Determination of Absolute Structure"J.Appl.Cryst.. 37. 136-142 (2004)

T.Koganezawa、H.Iwasaki、N.Nakamura、Y.Yoshimura、T.Shoji：“宽频带单色仪及其在绝对结构测定中的应用”J.Appl.Cryst.. 37. 136-142

T.Koganezawa: "Phase Determination by Wavelength-Modulated Diffraction. II."Acta Cryst.. A58(Suppl). C84 (2002)

T.Koganezawa：“通过波长调制衍射进行相位测定。II”Acta Cryst.. A58（增刊）。

T.Koganezawa: "A Diffraction System with an X-ray Beam of a Band of Wavelength"Proc.Intern.Conf.Synchrotron Radiation Instrumentation. (印刷中). (2004)

T. Koganezawa：“具有一定波长带的 X 射线束的衍射系统”Proc.Intern.Conf.Synchrotron Radiation Instrumentation（正在出版）。

T.Koganezawa, H.Iwasaki, N.Nakamura, Y.Yoshimura, T.Shoji: "A Diffraction System with an X-ray Beam of a Band of Wavelength"Proc. 8th Intern. Conf. Synchrotron Radiation Instrurnentatior. (in press). (2004)

T.Koganezawa、H.Iwasaki、N.Nakamura、Y.Yoshimura、T.Shoji：“具有波长带 X 射线束的衍射系统”Proc。

T.Koganezawa, H.Iwasaki, N.Nakamura, Y.Yoshimura: "Synchrotron Radiation Wavelength-Modulated Diffraction Method and Its Recent Developments"Rigaku Denki Journal. 34. 4-14 (2003)

T.Koganezawa、H.Iwasaki、N.Nakamura、Y.Yoshimura：“同步辐射波长调制衍射方法及其最新进展”Rigaku Denki Journal。