The purpose of this work was hydrogen permeation of ceramic or metal/ceramic membrane using γ-Al2O3 by synthesizing. The γ-Al2O3 was synthesized by using the sol-gel process with aluminum isopropoxide and primary distilled water as the precursor and solvent. The γ-Al2O3-based membranes were prepared using HPS. The phase transformation, thermal evolution, surface are and morphology of γ-Al2O3 and γ-Al2O3-based membranes were characterized by XRD, TG-DTA, BET and FE-SEM. The hydrogen permeation of γ-Al2O3-based membranes was examined at room temperature comparing with other paper using nickel composited membrane on alumina ceramic support.