Al-27 MAS NMR was used on structural studies of AlON spinel. The results su
ggested that NMR can offer more accurate information about microstructure a
nd coordination when X-ray diffraction display the same spectra. The Al-27
MAS NMR spectra of the samples of gamma-AlON spinel crystal with different
composition were acquired. The results confirmed that AlN4, AlO4 and AlO6 s
tructures exist in AlON spinel. The number of the nitrogen atoms that subst
itute oxygen atoms and enter into anion positions increases with the conten
t of nitrogen increasing. However, the substitution has no influence on the
structure of the crystal, thus no influence on the X-ray diffraction spect
ra.