Abstract: Reasonable metallographic sample preparation method is the guarantee to obtain clear and high quality microstructure image, and is the basis of metallographic study of materials. The metallographic preparation techniques and specific methods of high purity tungsten, high nitrogen stainless steel, automobile steel plate and coating material were analyzed, and the problems encountered in the process of cutting, inlaying, grinding and polishing and etching in sample preparation were solved. The results show that the hardness of high purity tungsten is high, so grinding and polishing time should be ensured. High nitrogen stainless steel agent can obtain uniform microstructure by etching with ferric chloride and glycerin hydrochloride mixture. The sample preparation of automobile steel plate should ensure that the sample is upright and not inclined, and avoid scratches during polishing. During the cutting, inlaying and grinding and polishing process of coating material sample preparation, the protective work should be done to ensure the integrity of coating.