621.762Methods have been applied from scanning electron microscopy, hydrogen thermal desorption, XRD, and differential thermal analysis on the effects of grain size and alloying with boron as regards the thermal stability and decomposition temperatures of hydride phases in mechanical alloys in the Ti − B − H system. The alloys were prepared by high-energy processing for 50 h in a planetary ball mill with mixtures of TiH 1.9 + 9 mass% B + 13 mass% Ti and also with TiH 1.9 + 50 mass% TiB 2 at speeds of 1000 rpm, in addition to mixtures of TiH 1.9 + 40 mass% B and TiH 1.9 + 50 mass% TiB 2 , which were treated for 20 min at speeds of 1680 rpm. The dispersal on mechanical treatment and the addition of boron to the titanium hydride powder have substantial effects on the thermal stability. The processing of the mixture TiH 1.9 + 9 mass% B + 13 mass% Ti lasting 50 h in argon gave temperatures for the dissociation of the Ti(B, H) x hydride phase in the mechanical alloy lower by 300 deg than the decomposition temperature for the initial titanium hydride TiH 1.9 . The mechanisms have been identified for the effects of the dispersal and boron alloying on the thermal stability of the titanium hydride.