XRD数据Rietveld_精修与GSAS.ppt

Is the compound known?Crystallographic Structure Databases ICSD (Minerals and Inorganics) http://www.fiz-karlsruhe.de/ Minerals and Inorganic Over 60000 entries Cambridge Structure Data Bank） http://www.ccdc.cam.ac.uk Organics Organometallics Over 250000 entries ICDD diffraction data http:/ Inorganic Organic Over 140000 entries NIST Crystal Data /srd/nist3.htm Inorganic Organic Over 230000 entries 278916 Patterns already! A new structural database (2003) aimed at freely retrieving data Profile Factor 越小越好 Weighted Profile Factor ～ 10 % Expected Weighted Profile Factor Goodness of fit indicator ～ 1 晶体结构精修结果正确性判据 晶体结构精修结果正确性判据 Bragg Factor Crystallographic RF factor Rietveld结构精修 根据初始的结构模型，计算出衍射图谱，通过与实验图谱进行全谱对比，进一步优化结构模型的方法。 结构精确的作用： Lattice Parameters Quantitative phase Analysis Atomic Positions Grain size，Strain Atomic Occupancy Incommensurate Structure Debye Temperatures Crystallinity Magnetic structures Phase transitions Structure factors …… History Review Rietveld originally introduced the Profile Refinement method (Using step-scanned data rather than integrated Powder peak intensity) (1966,1967) Rietveld developed first computer Program for the analysis of neutron data for Fixed-wavelength diffractometers (1969) Malmos Thomas first applied the Rietveld refinement method (RR) for analysis of x-ray powder data collected on a Ginier Hagg focusing Camera (1977) Khattack Cox first applied the RR to x-ray powder data collected on a diffractometer (1977) Conference on Diffraction Profile Anlysis Sponsored by IUCr in Poland, suggested the term “Rietveld Method”(1978) Wiles and Yang developed a general computer program (D.B.W) for both x-ray neutron diffraction data (fixed wavelength)(1981) Von Dreele, Jorgensen and Windsor extended to the program to the neutron diffraction data (1982) Fitch et al, 193 refined parameters,UO2 DAs.4D2O (1982) Gregori Aminoff Priz