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A Series of LiCl/γ-Al2O3 samples were prepared by mixing and then heating at 400℃ for 30 hours. 7Li MAS NMR was used to investigated their structures. The 7Li MAS NMR signal of LiCl in the dispersion phase was observed for the first time, and its chemical shift was at 0.25ppm.After the dispersion threshold of LiCl on γ-Al2O3 was achieved, the 7Li signal in the crystallme phase LiCl appears at -1.01ppm and its intensity increases with the increasing in LiCl loading.From the 2D nutation NMR spectra, it can be seen that the electric field gradient surrounding the lithium nuclei in the dispersion state is larger and so the quadrupole interaction is stonger than that in the crystalline state. The dispersion threshold indicated by NMR is in agreement with that deduced from XRD, which is about 0.136gLiCl/gγ-Al2O3.