A series of the MoO3/γ-Al2O3 samples is prepared by mechanically mixing MoO3 with γ-Al2O3 powder. The solid state dispersion of the MoO3 in to the porous γ-Al2O3 is studied by SEM, XRD, XPS, TG/DTA, and positron annihilation spectroscopy. The positron annihilation lifetime spectra of the MoO3/γ-Al2O3 are measured as a function of the mass ratio of MoO3, heating temperature, heating time and in a way that the MoO3 is loaded gradually, separately. The experimental results show the process of the thermal dispersion of the MoO3 into the γ-Al2O3 support. It is shown that the MoO3 disperses into the outer surface first, and then into the secondary pores and the micro pores. The gradual Loading can make MoO3 effectively dispersed into γ-Al2O3. Grinding can also affecte the thermal dispersion process.