A new heterogeneous Fenton catalyst, Fe-Cu bimetallic oxides supported aluminum-containing MCM-41, was synthesized by co-precipitation method. The physicochemical characteristics of the synthesized samples were evaluated by various techniques such as XRD, TEM, nitrogen physisorption, zeta potential and XPS. The incorporation of metal species did not alter the well-ordered hexagonal mesostructure of MCM-41 support. Compared with the monometallic or the Al absent catalysts, this new bimetallic oxides supported aluminum-containing MCM-41 catalyst exhibited a higher activity and stability in phenol mineralization. The effects of temperature, pH and H2O2 dosage were investigated in terms of the TOC conversion. At pH 4, 60 degrees C and 0.049 mol/L of H2O2 dosage, a 47% TOC reduction has been achieved. With incorporating aluminum, the increase in surface oxygen-containing groups was observed by zeta potential analysis, the downshift binding energy of active metals was found by XPS measurement, and an enhancement of H2O2 utilization ratio was achieved. On the basis of our findings, the beneficial role of Al has been explained. (C) 2011 Elsevier B.V. All rights reserved.