A variety of characterization techniques have been employed to study the growth and structure of nickel carbon thin films fabricated by ionized magnetron sputter deposition. A two target magnetron system is used along with an RF powered coil, to create a secondary plasma, with a DC bias applied at the substrate. By varying the bias it is possible to control the energy of the depositing species as well as a range of other plasma properties and therefore the resulting film microstructure. It has been observed that a change from the metastable hexagonal nickel carbide phase to the stable face centered cubic structure of nickel can be induced. This change in metal crystallinity was accompanied by a change in carbon ordering. The ability to control the film structure and morphology without the need for substrate heating opens up the possibility of depositing a range of structures onto polymers.