Fabrication and characterization of porous titanium-based PbO₂ electrode through the pulse electrodeposition method: Deposition condition optimization by orthogonal experiment

Porous titanium-based PbO₂ electrodes were successfully fabricated by pulse electrodeposition method. The primary pulse electrodeposition parameters, including pulse frequency (f), duty ratio (γ), average current density (J_a) and electrodeposition time (t) were considered in this study. An orthogonal experiment was designed based on those four factors and in three levels. SEM images and XRD results suggest that the surface morphology and structure of PbO₂ electrodes could be easily changed by varying pulse electrodeposition parameters. Orthogonal analysis reveals that the increase of f and J_a could decrease the average grain size of PbO₂ electrodes, which is conducive to create more active sites and promote the generation of hydroxide radicals. The electrochemical degradation of Azophloxine was carried out to evaluate the electrochemical oxidation performance of pulse electrodeposited electrodes. The results indicate that the influences of four factors can be ranked as follow: J_a > γ≈ t > f. The higher f, larger J_a and longer t could facilitate the optimization of the integrated electrochemical degradation performance of prepared PbO₂ electrode. The accelerated life time is dominated by J_a and t, coincident with the average weight increase of β-PbO₂ layer. The optimal parameters of pulse electrodeposition turn out to be: f = 50 Hz, γ = 30%, J_a = 25 mA cm⁻², t = 60 min. Together, the consequences of the experiments give assistance to uncover and roughly conclude the mechanism of pulse electrodeposition.