Composite particles represented as TiV 2 . 1 Ni 0 . 3 -Raney Ni(R) were prepared by ball-milling a TiV 2 . 1 Ni 0 . 3 alloy with Raney Ni in the presence of 0.01 M sodium hypophosphite (NaH 2 PO 2 ) aqueous solution as a reducing agent. The composite particles had different morphology from original TiV 2 . 1 Ni 0 . 3 alloy particles and TiV 2 . 1 Ni 0 . 3 -Raney Ni composite particles prepared by the ball-milling in the absence of the NaH 2 PO 2 aqueous solution. In charge-discharge cycle tests, the TiV 2 . 1 Ni 0 . 3 -Raney Ni(R) composite electrode showed the maximum discharge capacity of 620 mAh g - 1 , while its cycle durability was similar to the TiV 2 . 1 Ni 0 . 3 alloy electrode, which was explained from depth profiles of constituent elements by Auger electron spectroscopy (AES). In thermogravimetry (TG) and differential thermal analysis (DTA), two steps of dehydriding for hydrided TiV 2 . 1 Ni 0 . 3 -Raney Ni(R) composite started from much lower temperature than hydrided TiV 2 . 1 Ni 0 . 3 alloy, and the amount of hydrogen absorbed in this composite was still larger than that absorbed in the TiV 2 . 1 Ni 0 . 3 -Raney Ni composite.