Zn(BH4)2 was prepared by milling ZnCl2 and NaBH4 in a planetary ball mill in an Ar atmosphere, and XRD analysis, SEM observation, FT-IR analysis, DTA, and TGA were performed for synthesized Z (BH4)2 samples. 90 wt% MgH2+ 1.67 wt% Zn(BH4)2(+NaCl)+5 wt% Ni+1.67 wt% Ti+1.67 wt% Fe (named 90MgH2+1.67Zn(BH4) (+NaCl)+5Ni+1.67Ti+1.67Fe) samples were also prepared by milling in a planetary ball mill in an H2 atmosphere. The gas absorption and release properties of the Zn(BH4)2(+NaCl) and 90MgH2+1.67Zn(BH4)2(+NaCl)+5Ni+1.67Ti+1.67Fe samples were investigated. An FT-IR analysis showed that Zn(BH4)2 formed in the Zn(BH4)2(+NaCl) samples prepared by milling ZnCl2 and NaBH4. At the first cycle at 320 oC, 90MgH2+1.67Zn(BH4)2(+NaCl)+5Ni+1.67Ti+1.67Fe absorbed 2.95 wt% H for 2.5 min and 4.93 wt% H for 60 min under 12 bar H2, and released 1.46 wt% H for 10 min and 4.57 wt% H for 60 min under 1.0 bar H2.