The work aims to prepare bond course of thermal barrier coating of NiAl intermetallic compound. The composite structure powder of Ni/Al, Ni/Al+0.5 at%ZrC and Ni/Al+0.07 at% was prepared by utilizing mechanical alloying technology. Firstly composite coatings of Ni/Al, Ni/Al+0.5 at%ZrC and Ni/Al+0.07 at% were prepared on nickel base superalloy (IN738) sustrate by cold spraying of ball-milled Ni/Al alloy powders. Then the intermetallic compounds were annealed in protective atmosphere Ar. The results showed that a submicron lamellar structure of Ni/Al+ZrC composite structure powder could be obtained after ball milling for 8 h at low temperture. Composite coating of as-sprayed Ni/Al alloy maintained structure of the powder and formed compact NiAl intermetallic compound after 10 h of heat preservation at 1080 ℃. Ni/Al powder doped with ZrC (0.07 at% and 0.5 at%) is more uniform than that not doped with ZrC. Part of NiAl intermetallic compound is formed in powder doped with ZrC while none formed in powder not doped with ZrC. Nearly non-oxidized bond course of Ni/Al powder can be prepared by cold spraying. Submicron lamellar structure in original as-sprayed coating almost disappears and becomes uniform structure after heat treatment.