《MIT-XRD分析晶体粒径》.ppt

Estimating Crystallite SizeUsing XRD Scott A Speakman, Ph.D. 13-4009A speakman@ /xray Warning These slides have not been extensively proof-read, and therefore may contain errors. While I have tried to cite all references, I may have missed some– these slides were prepared for an informal lecture and not for publication. If you note a mistake or a missing citation, please let me know and I will correct it. I hope to add commentary in the notes section of these slides, offering additional details. However, these notes are incomplete so far. Goals of Today’s Lecture Provide a quick overview of the theory behind peak profile analysis Discuss practical considerations for analysis Demonstrate the use of lab software for analysis empirical peak fitting using MDI Jade Rietveld refinement using HighScore Plus Discuss other software for peak profile analysis Briefly mention other peak profile analysis methods Warren Averbach Variance method Mixed peak profiling whole pattern Discuss other ways to evaluate crystallite size Assumptions: you understand the basics of crystallography, X-ray diffraction, and the operation of a Bragg-Brentano diffractometer A Brief History of XRD 1895- R?ntgen publishes the discovery of X-rays 1912- Laue observes diffraction of X-rays from a crystal when did Scherrer use X-rays to estimate the crystallite size of nanophase materials? The Scherrer Equation was published in 1918 Peak width (B) is inversely proportional to crystallite size (L) P. Scherrer, “Bestimmung der Gr?sse und der inneren Struktur von Kolloidteilchen mittels R?ntgenstrahlen,” Nachr. Ges. Wiss. G?ttingen 26 (1918) pp 98-100. J.I. Langford and A.J.C. Wilson, “Scherrer after Sixty Years: A Survey and Some New Results in the Determination of Crystallite Size,” J. Appl. Cryst. 11 (1978) pp 102-113. The Laue Equations describe the intensity of a diffracted peak from a single parallelopipeden crystal N1, N2, and N3 are the number of unit cells along the a1, a2, and a3 directi