Purpose: The aim of this paper is to determine the influence of the alloying time and composition on the structure of Ti-Si-C alloy.Design/methodology/approach: The powders of the Ti-Si-C alloys were obtained by mechanical alloying method in a planetary Fritsh Pulverisette 5 mill under inert argon atmosphere. In order to investigate the structure scanning electron microscopy, transmission electron microscopy and optical microscopy were used. Phase transformations during mechanical alloying process were determined by means of diffractometer. The distribution of particle sizes of powder materials was determined by a laser analyser.Findings: The application of the mechanical alloying method gives opportunity to produce nanocrystalline and amorphous phase. The laboratory test show that, by using this method, one can produce alloys with intentional chemical constitution and desirable structure.Research limitations/implications: : The powder metallurgy techniques make it possible to obtain Ti-Si-C massive materials by means of milling, followed by compacting and sintering. All of the experiments presented in this article are made on a laboratory scale. Further investigations should be concentrated on the developing of powder sintering method.Originality/value: This scientific research will be helpful for the composition plan for higher Ti3SiC2 content of powder synthesis. The synthesis of Ti-Si-C powder gives opportunity for the development of dispersion-strengthened alloys. The Ti-Si-C alloys have been considered to be potentially important for high temperature applications as either a structural or functional material.