The　amorphous/nanocrystalline　Ni-Mo-Ce　alloy　coating　electrode　was　obtained　in　alkaline　solution　from　Ni-Mo　deposited　solution　with　an　appropriate　addition　of　CeCl3.　X-ray　diffraction　(XRD)　and　scanning　electron　microscopy　(TEM)　were　used　to　describe　the　microstructure　and　the　morphology　of　the　deposited　Ni-Mo　alloys　coating.　The　experimental　results　showed　that　the　deposited　Mo　content　was　increasing　but　Ni　decreasing　due　to　the　addition　of　more　Ce.　And　at　the　same　time,　the　microhardness　of　the　deposition　increased　at　first　and　then　decreased.　When　the　addition　Ce　amount　reached　2　g　·　L-1,　the　microhardness　of　the　deposite　was　up　to　the　highest　value.　The　electrolysis　experiments　showed　that　Ni-Mo-Ce　alloys　were　with　excellent　corrosion　resistance　and　better　performance　of　the　catalytic　hydrogen　evolution　than　Ni-Mo　alloys.