The experimental data concerning nanoscale hydrides of transition metals, obtained by synthesis in combustion wave are presented. The systems TI-H, Zr-H, Ti-N-H, Zr-N-H. Ti-Zr-N-H were studied. In all samples, the dimensions of grains were as low as 50 nm. The peculiarities of self-propagating high-temperature synthesis processing and structure causes of this phenomena are discussed. The relations between cubic structure of TiH2 hydride and hexagonal structure of Ti-hydridonitride were demonstrated. (C) 2001 International Association for Hydrogen Energy. Published by Elsevier Science Ltd. All rights reserved.