Abstract: In the procedures of designing polystyrene-polyvinyl alcohol-CH (carbon and hydrogen elements) (PS-PVA-CH) triple-layer microspheres, there are many methods such as drop-tower technique, emulsion micro-encapsulation, dip (spin) coating, interfacial polycondensation, and spraying technique to prepare the PVA coating. Drop-tower technique, emulsion micro-encapsulation and dip (spin) coating are most-commonly used. The advantages, disadvantages and the research progress of the three methods are summarized in this paper. Emulsion micro-encapsulation is suitable for preparing double-layer microspheres of sizes smaller then 500 m, with high survival ratio and good quality. However,the preparation process is easily influenced by artificial factors. Small-sized double-layer microspheres can also be prepared by the drop-tower technique, and the preparation period is short. But there are still some problems such as the difficulty in designing thedroplet generator, uneven PVA coating and the difficulty in preparing large-sized microspheres. Dip (spin) coating technique can be used to prepare PS-PVA microspheres with sizes larger than 1000 m, but the spread of PVA coating is affected by many factors in this method, and the prepared PVA coating is too thin and not uniform.