Nb-Ti alloys were hydrogenated to prepare fine and contamination-free powders. Cracks were introduced in the alloys when they were annealed at 1473 K and cooled in a hydrogen atmosphere. The fragments produced by hydrogen-induced cracking are brittle and the friability enhanced with the Ti content of the alloy, which is beneficial for further refinement of particle size. We also demonstrate that Nb-Ti powders with the average particle size less than 1 m can be produced by ball milling at a temperature lower than 203 K. Furthermore, hydrogen-free powders can then be obtained by annealing above the temperature corresponding to hydrogen desorption from Nb solid solution.