Practical XRay Diffraction uocgr：实际的X射线衍射uocgr.pptVIP

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Practical XRay Diffraction uocgr：实际的X射线衍射uocgr.ppt

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Practical XRay Diffraction uocgr：实际的X射线衍射uocgr

Crystallite Size Broadening Peak Width B(2q) varies inversely with crystallite size The constant of proportionality, K (the Scherrer constant) depends on the how the width is determined, the shape of the crystal, and the size distribution The most common values for K are 0.94 (for FWHM of spherical crystals with cubic symmetry), 0.89 (for integral breadth of spherical crystals with cubic symmetry, and 1 (because 0.94 and 0.89 both round up to 1). K actually varies from 0.62 to 2.08 For an excellent discussion of K, JI Langford and AJC Wilson, “Scherrer after sixty years: A survey and some new results in the determination of crystallite size,” J. Appl. Cryst. 11 (1978) p102-113. Remember: Instrument contributions must be subtracted * 46.7 46.8 46.9 47.0 47.1 47.2 47.3 47.4 47.5 47.6 47.7 47.8 47.9 2 q (deg.) Intensity (a.u.) 46.7 46.8 46.9 47.0 47.1 47.2 47.3 47.4 47.5 47.6 47.7 47.8 47.9 2 q (deg.) Intensity (a.u.) Methods used to Define Peak Width Full Width at Half Maximum (FWHM) the width of the diffraction peak, in radians, at a height half-way between background and the peak maximum Integral Breadth the total area under the peak divided by the peak height the width of a rectangle having the same area and the same height as the peak requires very careful evaluation of the tails of the peak and the background FWHM * Williamson-Hull Plot y-intercept slope K≈0.94 Grain size broadening Grain size and strain broadening Gausian Peak Shape Assumed * 66 67 68 69 70 71 72 73 74 2 q (deg.) Intensity (a.u.) Which of these diffraction patterns comes from a nanocrystalline material? These diffraction patterns were produced from the exact same sample The apparent peak broadening is due solely to the instrumentation 0.0015° slits vs. 1° slits Hint: Why are the intensities different? * Remember, Crystallite Size is Different than Particle Size A particle may be made up of several different crystallites Crystallite size often matches grain size, but there are exceptions *