This Letter demonstrates the first attempt of using sol-gel technique in combination with argon plasma calcination for the preparation of mesoporous silica films. CTAB is used as an organic template to generate the porous structure upon removal by the argon plasma treatment. Field emission scanning electron microscope, Fourier transform infrared spectroscopy, small angle X-ray scattering, N-2-sorption experiment and nanoindentation technique are used for characterization. Results show that the obtained films have identical chemical structure and comparable mechanical properties with those prepared using thermal calcination. The plasma parameters have distinct influences on the thickness and mesoporous property of the films. (C) 2004 Elsevier B.V. All rights reserved.