A new ternary solid solution, Cu 3-x Ni xþy N, is prepared by gas-pulsed CVD at 260 8C. Gas pulses of the precursor mixtures Cu(hfac) 2 þ NH 3 and Ni(thd) 2 þ NH 3 , separated by intermittent ammonia pulses, are employed for the deposition of Cu 3 N and Ni 3 N, respectively. A few monolayers of the nitrides are grown in each CVD pulse and then mixed by diffusion to produce the solid solution. The metal content of the solid solution can be varied continuously from 100% to about 20% Cu, which means that the electrical properties can be varied from 1.6 eV (band gap of Cu 3 N) to metallic (Ni 3 N). This is of interest for various applications, e.g., solar energy, catalysis, and microelectronics.