As　an　excellent　photocatalytic　material,　ZnxCd1-xS　is　widely　used　in　photocatalytic　H2　production　due　to　its　good　visible　light　response　and　suitable　band　position.　Based　on　our　previous　studies,　this　paper　systematically　studies　the　relationship　of　Zn0.5Cd0.5S　(ZCS)　material　between　microstructure　and　photocatalytic　activity.　By　controlling　the　synthesized　temperature,　S　sources　and　solvents,　a　series　of　ZCS　nanomaterials　with　different　morphology　and　crystalline　phase　have　been　prepared　by　hydrothermal,　solvothermal　and　ion-exchange　methods.　When　several　sacrificial　agents　are　added　in　photocatalytic　H2　production,　ZCS　performs　the　highest　activity　synthesized　by　solvothermal　method,　about　12.15　mmol　g−1　under　4　h＇s　visible　light　illumination.　To　explore　the　difference　of　ZCS　samples　in　photocatalytic　performance,　many　factors　are　considered,　such　as　crystal　size,　crystallinity,　separation　of　photogenerated　charge　carriers　(PCCs),　specific　surface　area　and　defect　sites,　which　play　important　roles　in　the　improving　photocatalytic　activity.　This　work　provides　a　new　direction　for　the　design　of　photocatalyst　from　the　microstructural　regulation　to　achieve　highly　efficient　activity.　©　2024　Elsevier　Ltd