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Ball milling of a coarse powder and co-precipitation of CaCl2 and NH4F were employed to produce two nanostructured fluorites with comparable domain size but drastically different defect concentration. The combined use of X-ray diffraction line profile analysis and solid-state NMR shows the effects of inhomogeneity in the milling process and clearly points out the different effect of lattice defects on the NMR spin-lattice relaxation.
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