The effect of three principal, independent, high-velocity oxygen fuel (HVOF)-processing parameters on the properties of NiCoCrAlY coatings deposited using commercial powders is reported here. The design of experiments (DoE) technique at a two-level factorial and a central composite rotatable design was used to analyze and optimize the HVOF spraying process. The deposition parameters investigated were (1) fuel flow, (2) oxygen flow, and (3) stand-off distance. The effect of these processing variables was evaluated using selected responses, including porosity and oxide content, residual stresses, and deposition efficiency. Coatings with low porosity as well as with low residual stress were obtained using high fuel-rich conditions at a stand-off distance between 250 and 300 mm. At shorter and longer stand-off distances, respectively, either excessive flattening of splats or un-molten condition occurred, resulting in high levels of porosity and residual stress. The response surface, the empirical relationships among the variables, and the response parameters allowed the selection of optimum deposition parameters and the improvement of coating properties.