Results of X-ray and electrochemical analyses of properties of Ti-Zr-Ni powders obtained by the volumetric electric-spark dispersion method in water, alcohol, kerosene, liquid nitrogen and liquid argon are presented. The influence of working fluids and parameters of discharge pulses on the chemical composition, phase-structural state, electrochemical characteristics and electrical capacity of the obtained powders is considered. The effect of annealing in various media on the electrochemical properties of powders has been studied. (c) 2005 Elsevier B.V. All rights reserved.