Nanometer　sized　TiO2　powder　with　large　surface　area　was　synthesized　by　sol-gel　method　using　tetrabutyl　titanate　as　precursor　and　hexadecyltrimethylammonium　bromide　(CTAB)　as　template.　The　photocatalyst　is　characterized　on　particle　size,　crystal　structure,　and　surface　area　by　XRD,　TEM,　BET.　The　results　show　that　the　molar　ratio　of　CTAB　to　Ti　and　temperature　of　calcination　have　great　effect　on　their　particle　size　and　surface　area.　The　photocatalytic　activities　of　hydrogen　evolution　were　compared　on　samples　with　different　preparation　conditions.　The　results　indicate　that　CTAB　obviously　improves　the　hydrogen　evolution　performance　of　photocatalytic　water　splitting,　the　0.15-450　sample　that　the　molar　ratio　of　CTAB　to　Ti　is　about　0.15　and　calcination　temperature　is　450　degrees　C　with　particle　size　of　5.73　nm　and　the　specific　surface　area　of　150　m(2.)h(-1)　is　the　best　with　an　average　hydrogen　evolution　rate　of　12.5　mL(.)h(-1)　in　3　hours.