The aim of this study is the compassion investigation of Ni-Al2O3 nanocomposite high corrosion resistance coatings. The content of alumina nanoparticles has the most important effect on these coatings. In this investigation the composition of electrolyte was modified by adding of methanol organic solvents. The concentration of alumina nanoparticles in the bath was 10gL-1. The coating were produced by pulse current and under ultrasonic agitation .After the electroplating process, the coatings cross sectioned and the amount of incorporated alumina nanoparticles and the morphology of each coating was analysed by Energy X-ray spectroscopy (EDX) coupled with an Scanning Electron Microscopy (SEM). The results showed that with increasing the methanol organic solvent to the Watts solution the zeta potential of the nanoparticles increased from -4.1mV to +24.5mV and subsequently, the content of alumina reinforcement nanoparticles increased from 4.6vol. % to 11vol. %. It has been assumed that methanol surfactant may act as a surface agent that affected the hydrated layer on the nanoparticles and it promoted the co-deposition of nano alumina particles with nickel.