Thin Solid Films, Vol.324, No.1-2, 30-36, 1998
Phase control of MoxN films via chemical vapor deposition
Polycrystalline single phase (gamma-Mo2N and delta-MoN) and two phase (gamma-Mo2N + delta-MoN) films have been deposited via chemical vapor deposition on prepared 50 mu m thick polycrystalline Ti substrates using both molybdenum pentachloride (MoCl5) and molybdenum hexacarbonyl (Mo(CO)(6)), diluted in either N-2 or Ar, and anhydrous ammonia (NH3) in a cold-wall, vertical pancake-style reactor. X-ray diffraction data showed that polycrystalline, single phase gamma-Mo2N films were deposited between 400-450 degrees C with the MoCl5 precursor and between 350-500 degrees C with the Mo(CO)(6) precursor. Above these respective temperatures and up to 700 degrees C, a two-phase mixture of gamma-Mo2N and delta-MoN was observed. At 700 degrees C, single phase delta-MoN films were deposited by employing the Mo(CO)(6) precursor and 1.5 slm of NH3; however, a two phase mixture of approximate to 95 at.% delta-MoN and approximate to 5 at.% gamma-Mo2N was observed in films prepared using the MoCl5 precursor. Regardless of the precursor, decreases in the NH3 flow rate were matched by decreases in delta-MoN percentages at each temperature where delta-MoN was present. Increasing in the deposition rate also resulted in decreasing delta-MoN percentages at each deposition temperature. Scanning electron micrographs (SEM) indicated that the porous microstructure of the films were dependent on both the deposition temperature and the precursor employed. Energy dispersive X-ray (EDX) data indicated that films deposited at and above 400 degrees C with the MoCl5 precursor did not contain detectable levels of chlorine. Higher carbon levels were detected in films deposited with the Mo(CO)(6) precursor than with the MoCl5 precursor.