The invention belongs to the technical fields of ceramic and fireproof material, providing a method used for preparing Al4SiC4 powder. The method comprises the specific processes as follows: metal Al powder, Si powder, carbon black or graphite are taken as raw materials; the metal Al powder, Si powder and carbon black or graphite are uniformly mixed according to the molar ratio of 4:1:4.2-4.5; the mixture of the metal Al powder, Si powder and carbon black or graphite is arranged in the ball-grinding tank of a high-energy ball-grinder where aluminum stearate used as a dispersant is added; the ball material ratio is 10-15:1; the ball-grinding is carried out for 20-40 hours under a vacuum argon state, the rotation speed is 800-1000r/min; therefore, the Al4SiC4 powder is gained. The method has simple preparation process, stable process parameter, easy controlling, high ball-grinding efficiency and complete raw material reaction, and can prepare the high-purity powder containing no Al3C4 phase.