Nickel foam substrates are frequently utilised as porous 3D substrates for renewable energy applications. The preparation of these substrates usually includes an acid-washing step, but the degree to which this step affects the final electrochemical performance after spray-coating a catalyst ink is unreported. Herein, we report the effects of acid washing through physicochemical and electrochemical characterisation. The electrochemical performance was determined through repeated measurements of catalyst-coated nickel foam substrates both with and without the initial step of acid washing. It was found that acid washing increased the current density by 17.9% for the acid-treated MoS2-coated nickel foam electrode. This increment was affiliated with an electrochemically active surface area that increased by 11.2%, and a Tafel analysis indicated that the acid-treated MoS2-coated electrodes facilitated the initial water dissociation step of the hydrogen evolution reaction with greater ease. Similar effects were also discovered for acid-treated PtIr(1:3)/C-coated nickel foam substrates. The stability was also improved; the degradation rate was reduced by 18.9% for the acid-treated MoS2-coated electrodes. This demonstrates the utility of acid washing nickel foam electrodes.