Mesoporous alumina and magnesia were prepared using various polymers, poly(ethylene glycol) (PEG), poly(vinyl alcohol) (PVA), poly(N-(2-hydroxypropyl) methacrylamide) (PHPMA), and poly(dimethylacrylamide) (PDMAAm), as porogenic structure matrices. Mesoporous alumina exhibits large Brunauer-Emmett-Teller (BET) surface areas up to 365 m 2 g −1 , while mesoporous magnesium oxide possesses BET surface areas around 111 m 2 g −1 . Variation of the polymers has little impact on the structural properties of the products. The calcination of the polymer/metal oxide composite materials benefits from the fact that the polymer decomposition is catalyzed by the freshly formed metal oxide.