Research has been conducted to investigate process control methods to make thinner, yet more cohesive TiN films. An electron cyclotron resonance plasma enhanced reactive sputtering technique was used to deposit TiN films of 1–2 μm thickness on Inconel 718 substrates. A designed experiment was conducted to identify which processing parameters, single or coupled, had significant effects upon the film microstructure and mechanical properties. It was found that Meyer hardness and root mean square (rms) roughness can be changed by varying the deposition conditions of system pressure, substrate temperature, nitrogen flow, and substrate bias. While it was determined that substrate temperature and substrate bias caused a variation in rms roughness, it was found that the interaction of system pressure and substrate temperature had a stronger effect. While system pressure was shown to have a strong effect on hardness, the interaction of system pressure and nitrogen flow caused a greater variation.