A new method is developed for obtaining powder nanocomposites consisting of a metallic or intermetallic matrix and ceramic nanometer particles as a reinforcing phase. This method involves the following consecutive processes: short-time mechanical activation of the mixture of powder reagents in a high-energy planetary ball mill, self-propagating high-temperature synthesis, and additional mechanical activation of the synthesis products. Specific features of the reinforcing phase synthesis in matrices are examined by an example of TiB 2 -Cu and TiB 2 -TiNi systems. Compaction conditions that allow obtaining volume nanostructural materials with high strength characteristics are found.