The invention discloses a preparation method of monodisperse
yolk-shell structured CuO microspheres. The method comprises the following steps: dispersing cupric acetate or cupric acetate and PVP in
ethylene glycol, fully dissolving the cupric acetate or cupric acetate and PVP, transferring the above obtained solution into a high-pressure reaction kettle, carrying out a constant-temperature heating reaction, naturally cooling and
settling a solution obtained after the reaction ends, removing the obtained supernatant, carrying out suction
filtration to obtain a blue
solid product, and
drying the blue
solid product in a
vacuum drying box until the weight is constant in order to obtain a
yolk-shell structured CuO
microsphere precursor with monodisperse characteristic; and carrying out controlled temperature annealing on the obtained precursor in
air atmosphere by using a heating rate-controllable electric resistance furnace, and cooling the annealed precursor to
room temperature in order to obtain the monodisperse
yolk-shell structured CuO microspheres. The method ingeniously using
ethylene glycol as an
organic solvent and a structure guiding agent realizes controllable design of the structure, and also has the advantages of easily available raw materials, low cost, almost no
pollution to environment, realization of easy separation, high purity and good and uniform morphology of the above product, simple preparation process, and easiness in operation, and the product has substantially better photochemical performance than other structures.