Nanocrystalline Inconel 718 and Ni powders were prepared using two approaches: methanol and cryogenic attritor milling. High velocity oxy-fuel (HVOF) spraying of milled Inconel 718 powders was then utilized to produce Inconel 718 coatings with a nanocrystalline grain size. Isothermal heat treatments were carried out to study the thermal stability of the methanol milled and cryomilled Inconel 718 powders, as well as the HVOF Inconel 718 coatings. All nanocrystalline Inconel 718 powders and coatings studied herein exhibited significant thermal stability against grain growth as evidenced by a grain size around 100 nm following annealing at 1273 K for 60 min. In the case of the cryomilled nanocrystalline Ni powders, isothermal grain growth behavior was studied, from which the parameters required for the prediction of the microstructural evolution during a non-isothermal annealing were acquired. The theoretical simulation of grain growth behavior of nanocrystalline Ni during non-isothermal annealing conditions yields results that are in good correspondence with the experimental results.