Metal vapor method was employed to design a new method for preparation of nickel-containing supported catalysts on different metal oxides such as Al2O3, MgO, ZSM-5. The activation of carbon-carbon bonds in some n-alkanes and cycloalkanes was investigated. Results have shown that these catalysts retained very high activity, selectivity and stability toward hydrocracking and isomerization of hydrocarbons. Since metal vapor method yielded metal particles in a highly dispersed state, these particles were unique and demonstrated considerable decrease in the cleavage temperature of C-C bonds in hydrocarbons. The most significant difference was observed in the presence of bimetallic Ni-Re/ZSM-5 catalyst: it caused almost complete conversion of tested hydrocarbons at 463-493 K under normal pressure. n-Heptane could be converted virtually to isobutane and propane only. Hydrocracking of high alkanes (C-16) on these catalysts produced high liquid products and lower gas products.