PURPOSE: To produce flakes of an inorganic substance having excellent smoothness and high gloss, by applying a liquid or organic solvent solution of a metallic compound characterized by the existence of an acyloxy group to a flat surface, hydrolyzing the compound, and peeling the resultant thin film of the metallic compound.

CONSTITUTION: The liquid or organic solvent solution of a metallic compound having acyloxy group is applied to a flat surface, and the coating film is hydrolyzed with water or steam to obtain a thin film of metallic compound. The thin film is peeled from the flat surface, and if necessary, calcined to a metallic oxide thin film to obtain the objective flakes of an inorganic substance. The metal in the metallic compound having acyloxy group is a metal belonging to the groups IIIb, IVa or IVb of the periodic table, preferably one or more metals selected from Al, Si, Ti, Sn and Zr.