Co (Ni or Cu)-MCM-41 mesoporous molecular sieves with different amount of metal were synthesized by using cetyltrimethyl ammonium bromide as a template and by a novel microwave irradiation method. These samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and N-2 physical adsorption. The experimental results show that Co ( Ni or Cu)-MCM-41 mesoporous molecular sieves were successfully synthesized. When the as-synthesized samples were calcined at 550 degrees C for 10 h, the template was effectively removed. Under microwave irradiation condition, Co-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 745.7-1188.8 m(2)/g and average pore sizes in a range of 2.46-2.75 nm; Ni-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 625.8-1161.3 m(2)/g and average pore sizes of ca. 2.7 nm; Cu-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 601.6-1142.9 m(2)/g and average pore sizes in a range of 2.46-2.76 nm. On the other hand, with increasing the introduced metal amount, the specific surface area and pore volume of the synthesized Co ( Ni or Cu)-MCM-41 mesoporous molecular sieves became small, and the mesoporous ordering of the samples became poor. Under the comparable synthesis conditions, the synthesized Co-MCM-41 mesoporous molecular sieve has a bigger specific surface area and a more uniform pore distribution as compared with the synthesized Ni-MCM- 41 and Cu-MCM-41 mesoporous molecular sieves. (C) 2007 Elsevier B. V. All rights reserved.