A new technique for the deposition of nickel metal films by gas‐phase pyrolysis of nickel tetracarbonyl gas is described. A pulsed CO2laser is used to form a reaction zone adjacent to a cold substrate, resulting in a rapidly quenched film. The technique relies on dielectric breakdown of a mixture of source and carrier gases and therefore lends itself to a variety of source gases and chemistries. Adherence data and compositional and structural analyses are presented.