To　improve　the　electrochemical　properties　of　Ni-Mo　alloys,　the　Ni-Mo/ZrO2　co-coating　is　obtained　by　adding　nano　ZrO2　particles　into　Ni-Mo　plating　solutions.　The　microstructure　and　chemical　activity　of　Ni-Mo/ZrO2　alloy　electrode　are　discussed　and　compared　with　that　of　Ni-Mo　and　Ni/ZrO2　electrodes.　The　experimental　results　show　that　the　Ni-Mo/ZrO2　plating　microstructure　is　composed　of　amorphous　and　nanocrystal　phases,　mixed　with　nano-ZrO2　particles　which　can　affect　the　morphology　of　the　plating　surface.　When　the　electrolysis　current　is　lower　than　250　mA/cm2,　the　Ni-Mo/ZrO2　co-coating　has　a　better　hydrogen　evolution　catalytic　activity　than　Ni-Mo　and　Ni/ZrO2　alloy　electrodes,　and　its　anti-corrosive　performance　is　more　outstanding　than　that　of　the　latter　two　electrodes　which　is　related　to　the　Ni-Mo　amorphous　basement.　The　element　Mo,　which　can　be　easily　oxidated　and　formed　to　oxide,　increases　the　structure　stability　of　the　compound　plating　surface.　In　addition,　the　nano-ZrO2　particle　also　has　an　outstanding　anti-corrosive　properties　in　itself.