Nowadays, there are many surface treatment methods for aluminium alloys; the most commonly used of these is the chemical dip galvanizing process, which is complicated due to its use of large quantities of corrosive drugs. In order to simplify the process, this paper proposes a new electromagnetic induction heating activation method instead of the zinc dipping process. The method works as follows: The substrate is first degreased and then activated. The activation process starts by soaking the degreased substrate in an activation solution, taking it out after ten minutes, and placing it into an induction heating unit. The activation solution is sprayed onto the surface of the substrate while heating, using the energy generated by high temperatures to complete the activation reaction. The surface of the activated substrate forms a nanoscale film of nickel, which is finally utilised as a catalytic centre for ENP (an advanced surface treatment process that deposits a very uniform layer). The optimisation of important parameters of the non-destructive activation process was determined using the L9 Taguchi method. The main parameters ranged from 0.15 L/min to 0.25 L/min for spray rate, 200 °C to 400 °C for heat treatment temperature, and 1:4, 1:5, and 1:6 for Ni2+ and H2PO4− ion concentration ratios. The above data were derived from a single variable and were analysed using Minitab 20 software. Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), energy spectrometry (EDS), and ultrasonic experiments were used to characterize and analyse the surface morphology, composition, and bond strength of the coatings. The results show that the nanoscale nickel particles can completely cover the surface of the substrate, forming a layer of nano-film. After activation and ultrasonic cleaning for 30 s at an ultrasonic frequency of 40 KHz and a power of 80 W, the surface nano-film was not destroyed, which proves that it had a high bonding strength. After the application of the plating, the plated surface had a compact microstructure, and the continuity was good. Therefore, compared with the currently commonly used zinc dipping process, this process has the advantages of being a low-cost, simple operation, and non-destructive and environmentally friendly activation process for the substrate.