The　amorphous-nanocrystal　Ni-Mo　deposits　were　obtained　by　electrodeposition　in　alkaline　nickel　carbonate　solution.　X-ray　diffraction　(XRD),　scanning　electron　microscopy　(SEM)　and　modern　technologies　were　used　to　describe　the　content,　microstructure　and　morphology　of　the　deposits.　The　electrochemical　characteristics　of　Ni-Mo　deposits　were　electrolyzed　in　33°C,　7　mol/L　NaOH　electrolytic　solutions.　The　results　showed　that　when　I　was　100　mA　cm-2,　the　hydrogen　evolution　potential　of　Ni-Mo21.76　was　lower　than　amorphous　Ni-Mo26.36　and　250mV　lower　than　the　nanocrystal　Ni　cathode.　And　the　Ni-Mo　deposits　with　more　amorphous　phase　content　would　be　in　lower　hydrogen　evolution　overpotential,　a　higher　exchange　current　density,　and　a　better　electrolytic　stability.　These　due　to　the　amorphous　combined　with　nanocrystal,　lager　contact　surface　and　binding　energy　of　Ni-Mo　structure.　©　(2016)　Trans　Tech　Publications,　Switzerland.