An　electrodeposited　Ni-Mo　alloy　coating　with　18.68%　(atomic　fraction)　Mo　content　was　obtained　in　an　alkaline　nickel　carbonate　solution.　It　was　found　from　X-ray　diffraction　(XRD)　that　the　deposition　was　composed　of　amorphous　and　nanocrystalline　phases　and　compounds.　Crystallization　dynamics　from　differential　scanning　calorimetry　(DSC)　showed　that　the　deposition　crystallization　activation　energy　(E)　was　about　3.84×105　kJ　·　mol　-1　and　the　crystallization　temperature　was　440　°C.　Compared　with　amorphous　Ni-Mo　alloy　depositions,　the　deposition　crystallization　temperature　was　increased　by　about　13　°C.　It　was　found　from　the　heat　treatment　process　that　a　small　amount　of　nanocrystallines　in　the　deposition　could　prevent　the　possibility　of　crystallization　and　improve　the　thermal　stability　and　increase　the　crystallization　temperature　of　the　co-composite.　New　phases　would　take　on　in　the　deposited　Ni81.32Mo18.68　alloy　during　the　heat　treatment　process　when　annealed　at　450　°C.　This　improved　the　density　of　the　deposition　coating　and　prevented　a　change　in　the　amorphous　phase.　The　thermal　stability　of　the　co-deposited　coating　was　also　improved.　©　Editorial　office　of　Acta　Physico-Chimica　Sinica.