The invention relates to a preparation method of 
metal mono-atoms and belongs to the technical field of 
materials science and 
engineering. The 
metal mono-atoms prepared through the method may include: Pt, Ag, Au, Pd, Rh, Ir, Ru, Co, Ni and Cu, and 
metal mono-atoms supported on TiO2, 
zinc oxide, 
cerium oxide, aluminum 
oxide, 
silicon oxide, 
ferric oxide, 
manganese oxide, C3N4, 
mesoporous carbon, ultrathin carbon films, 
graphene, carbon nano tubes or 
molecular sieve materials, etc. The method includes the steps of: preparing a precursor solution in a certain concentration, and freezing the solution; and under an ice phase, 
processing ice cubes by means of 
external field or reaction between reactants in the ice cubes, and when the ice cubes are molten, a mono-atom solution is finally produced; mixing the mono-atom solution with different materials, performing ultrasonic treatment, 
filtration, cleaning and 
drying to finally obtain the mono-atoms supported on various materials. The preparation method is quick, has high product density, allows 
mass production, is high in efficiency and has wide application range, and compared with a co-
precipitation method and an impregnation method, the method has significant advantages.