The present work reports the usage of nanocrystalline plasma electrolytic saturation (PES) by applying pulsed current in an organic electrolyte based on Glycerol. Response surface methodology was applied to optimize the operating conditions for small nanocrystallite sizes of coatings. The levels studiedwere peak of applied cathodic voltage range between 500 and 700V, peak of applied anodic voltage between 200 and 400V and the ratio of duty cycle of cathodic direction to duty cycle of anodic direction at 0.25–0.35. The usage of high applied cathodic voltages and low anodic voltages and also low ratio of duty cycle of cathodic direction to duty cycle of anodic direction is more suitable for achieving lower sizes of complex nanocrystallites. The samples with high height to width ratio of distribution curves of nanocrystallites have simultaneously, smaller average sizes and lower length to diameter ratio of nanocrystallites.
