The experimental researches on the chemical deposition of Ni-Mo-P amorphous alloys were carried out by adding Na2 MoO4 into acidic solutions. The optimum technology conditions were obtained by orthogonal design experiments. The structures and the relationship between compositions and their thermal stability were studied by energy spectrum (EC), scanning electron micrograph and X-ray diffraction spectrum. Compared with Ni-P amorphous alloys, the Ni-Mo-P amorphous alloys have high crystallization temperature and thermal stability, and the hardness reaches its peak when the annealing temperature is 500 ℃. With the increase of the heat treatment temperature, the surface morphology of the alloys changes.