ZnAlFe layered double hydroxides (LDHs) were synthesized by the co-precipitation method at different M(II)/M(III) ratio. The solids were calcined at 723 K obtaining the respective mixed oxides with high specific surface areas (138-70 m(2)/g) and semiconductor properties (band gap values of 2.54-2.04 eV). The photocatalytic activity of these materials was tested for the photodegradation of aqueous solutions containing phenol and p-cresol (40 ppm), in presence of a UV light source. A disappearance of 98% of phenol and a total photodegradation of p-cresol were obtained after 6 and 4 h, respectively. (C) 2009 Elsevier B.V. All rights reserved.