Abstract: This paper introduced a comprehensive experiment on the preparation and characterization of the BiVO4 powder.BiVO4 photocatalysts powder were prepared by the chemical precipitation method and characterized about their crystal structure,morphology,particle size distribution and photocatalytic activity.The results show that the BiVO4 samples with spherical particles are monoclinic sheelite structure.The particle size distribution is relatively uniform.The photocatalytic degradation of methyl orange over BiVO4 was in accordance with the first order reaction kinetics.This experiment with simple route includes a lot of knowledge and covers many basic experimental skills such as synthesis,structural characterization and performance test.Moreover,it is easy for students to learn and operate,thus it can be applied as a comprehensive experiment of practical teaching course of material science and engineering major.