A series of MgO-rich MgAl 2 O 4 samples were prepared by co-precipitation in the presence of CTAB, Triton X-100, and glucose or a combination of CTAB and glucose, which act as templates. The effects of different types and amounts of single template, as well as adding order of the mixed templates, on the specific surface area and particle size were investigated by BET and XRD analyses. The addition of the single template can lead to the increase of the specific surface area, wherein the samples using glucose as templates own the maximum specific surface area of 198 m 2 /g; as for the use of mixed templates, results revealed that adding CTAB first, followed by the addition of glucose, is better, giving a surface area of 223 m 2 /g.