Abstract: The preparation of the SEM sample has essential influence to the SEM section analysis of HDPE/CaCO₃ filled macromolecule materials. In this paper, the influence of the choice of the metal source and the controllable parameter during the preparation of the sputtered SEM sample to the final analysis result has been studied. An optimal condition has been obtained and has been applied to the further analysis of this kind of materials. It has been shown that it is a reasonable and reliable condition for the analysis of this kind of materials.