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In this study, a nickel film with nano-crystalline grains, high hardness and smooth surface was electrodeposited using a post supercritical carbon dioxide (CO2) mixed Watts electrolyte. Although the hardness was not as high as its Sc-CO2 counterpart, the thin coating contained significantly less number of nano-sized pinholes. By measuring the escape concentration of the dissolved CO2 in post Sc-CO2 mixed electrolyte with the elapsed time, it was believed that the residue of dissolved CO2 bubbles should closely relate to the improvement in hardness and surface roughness over its conventional plating counterpart. Therefore, shortening the duration of electroplating with the raise of current density up to 0.5 A/cm2 could effectively retain more post Sc-CO2 mixing effect. This study not only confirms the roles of dissolved CO2 bubbles in electrolyte but also provides a potential process to overcome most issues associated with the cost in building high-pressure chamber for large size products and continuous plating using supercritical method.