The development of gas separation membranes able to work at high temperatures require robust and thin ceramic layers. In this work, zirconia membranes have been prepared by the sol-gel method, following the colloidal sol route. The microporosity and crystallinity of the ZrO 2 material was tested by N 2 adsorption and XRD. The derived active zirconia layers were defect-free as seen by SEM. The optimum firing temperature range was set in the range 400-500 C. He, H 2 , CO 2 , N 2 gas permeation was conducted at temperatures up to 200 C. High permeances were obtained and the microporosity of the zirconia layer was confirmed.