The hydrogen energy had recognized clean and high efficiency energy source. The research field of hydrogen energy was production, storage, application and transport. The commercial storage method was using high pressure tanks but it was not safety. However metal hydride was very safety due to high chemical stability. Mg and Mg alloys are attractive as hydrogen storage materials because of their lightweight and high absorption capacity (about 7.6 wt%). Their range of applications could be further extended if their hydrogenation properties and degradation behavior could be improved. The main emphasis of this study was to find an economical manufacturing method for Mg-Ti-Ni-H systems, and to investigate their hydrogenation properties. In order to examine their hydrogenation behavior, a Sievert's type automatic pressure-compositionisotherm (PCI) apparatus was used and experiments were performed at 423, 473, 523, 573, 623 and 673 K. The results of the thermogravimetric analysis (TGA) revealed that the absorbed hydrogen contents were around 2.5wt.% for (Mg8Ti2)-10 wt.%Ni. With an increasing Ni content, the absorbed hydrogen content decreased to 1.7 wt%, whereas the dehydriding starting temperatures were lowered by some 70-100 K. The results of PCI on (Mg8Ti2)-20 wt.%Ni showed that its hydrogen capacity was around 5.5 wt% and its reversible capacity and plateau pressure were also excellent at 623 K and 673 K.