The article presents the assessment study of mechanical activation and mechanical alloying effect on the structure, phase state of the powder composition and of the coating based on it. The duration of mechanical activation was varied as follows: 1 h, 2 h, 4 h, 8 h, 16 h, 32 h. It is shown that in order to from a high-entropy FeNiCoAlNb alloy on the workpiece surface the duration of mechanical activation must be at least 4 hours. We described the mechanism of mechanical alloying and ways of accelerating this process.