Magnesium aluminate spinel has a great prospect in catalyst supports due to the porousstructure, good cata-lytic activity, high thermal stability and the presence of two active centers as acid and alkaline. The magnesium alumi-nate spinel powders were synthesized by a hydrothermal process. The samples were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction and N2adsorption-desorption isotherms, respectively. The particle surface with the laminated structure increases with the increase of hydrothermal temperature and hydro-thermal time. The spinel has a worm-like porous structure, and the pores become smaller and well-distributed under hexadecyl trimethyl ammonium bromide condition. The phase of the spinel appears at 450°C and the perfect crystalline structure emerges at 600°C. The percentage of MgAl2O4spinel increases with the increase of heat treatment temperature. The spinel has a great specific surface area (i.e., 245.68–58.65 m2/g) when the calcinating temperature increases from 500 to 1200°C. Moreover, the specific surface area is 195.11 m2/g 1 at.% hexadecyl trimethyl ammonium bromide.
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