Abstract. The effects of reaction material ratio and feed order on the composition of the product are investigated by the reaction of zinc sulfate, bismuth nitrate and sodium hydroxide as raw materials in the ultrasonic system. The product is identified as 2 5 8Bi Zn O by X-ray fluorescence and chemical titration, and the product can be characterized by TEM, SEM and TG-DTA. In this paper, the basic principle and experimental method of X -ray diffractometer are also introduced for the analysis of the sample structure in details. Finally, we expound the principle, application range and related parameters of the physical property measurement system (PPMS) of the experimental instrument for measuring the magneto and electric properties of the Zinc -Bismuth Complex Oxide samples.