Hydrogen sorption properties and some corresponding changes in the crystallization of amorphous TM33Zr67 (TM=Fe, Co, Ni) alloys have been investigated. Relatively large amount of hydrogen was found to dissolve into the amorphous alloys
during electrochemical hydrogen charging. The microstructural evolution during annealing of H-charged Ni33Zr67 was studied as well. The weaker bonded hydrogen desorbs in a large temperature range (440–625 K) before the crystallization
of the amorphous alloys to start. A hydride phase (ZrH2) was found to form during annealing the H-charged amorphous Ni33Zr67 alloy. During heating at constant heating rate the hydride decomposes at about 715 K and formation of Zr2Ni immediately takes place. The final microstructure of the Zr2Ni, crystallized from the H-charged matrix, is noticeably finer compared to the material crystallized from the H-free amorphous
alloy, most probably due to the higher temperature of Zr2Ni formation in the H-charged amorphous alloy than in the H-free sample.