Nanostructured and composite powders have been prepared by mechanochemical reaction from mixtures of Ti, BN, and powders. The raw materials have reacted to form a uniform mixture of TiN, and or depending on the amount of used in the starting mixtures, and the reaction proceeded through so-called mechanically activated self-sustaining reaction (MSR). Fine TiN and crystallites less than a few tens of nanometer were homogeneously dispersed in the amorphous or matrix after milling for 12 hours. These amorphous matrices became crystalline phases after annealing at high temperatures as expected, but the original microstructure did not change significantly