Abstract: Si powder and SiO₂ powder as raw materials for synthesizing 1-D β-SiC nanomaterial th ough a chemical vapor reaction approach are treated with high-energy milling process.On the basis of several primary experiments,the influence of milling rotating speed,milling time,mass ratio of milling-ball/powder,blending ratio of milling balls on granularity of the podwer is investigated via the orthogonal experiments and the optimum processes were determined as follows that for Si powder,the rotating speed is 300r/min,milling time is 4 hours,mass ratio of milling-ball/powder is 5:1,blending ratio of ϕ20mm:ϕ10mm:ϕ6mm:ϕ2mm is 1:50:180:400,and for SiO₂ powder the rotating speed is 350r/min,milling time is 4.4 hours,mass ratio of milling-ball/powder is 15:1,blending ratio of ϕ20mm:ϕ10mm:ϕ6mm:ϕ2mm is also 1:50:180:400.According to the results of granularity analysis and transmission electric microscope(TEM) characterization,the granularity distribution of as-gained products is homogeneous,and specific surface is increased significantly,which supports the synthesis of high quality 1-D β-SiC nanomaterial.