Hollow　ZnO　core/ZnS　shell　structure　(ZnO/ZnS　HCSS)　has　been　successfully　synthesized　via　a　microwave-assisted　hydrothermal　approach.　It　is　found　that　such　a　ZnO/ZnS　HCSS　exhibits　higher　photocatalytic　activity　than　pure　ZnO　and　ZnS　toward　the　liquid-phase　degradation　of　methyl　orange　(MO)　under　UV　irradiation.　What　is　more　noteworthy,　it　is　also　demonstrated　that　ZnO/ZnS　HCSS　photocatalyst　overcomes　the　photocorrosion　in　comparison　to　pristine　ZnO　by　mean　of　cycling　tests　toward　MO.　The　detailed　degradation　process　of　MO　over　ZnO/ZnS　HCSS　is　investigated　by　liquid　chromatography　mass　spectrometry　method.　And　then,　the　roles　of　active　species　in　the　photocatalytic　process　are　discussed　by　using　different　types　of　active　species　scavengers.　Meanwhile,　combined　with　the　electron　spin　resonance　and　photocurrent　test,　the　degradation　mechanism　of　the　photocatalysts　is　proposed.　It　is　hoped　that　the　work　could　provide　valuable　information　on　the　design　of　specific　structure　materials　with　more　excellent　properties　and　set　the　foundation　for　the　further　industrial　application.　(C)　2014　Elsevier　B.V.　All　rights　reserved.