Synthesis and morphological investigation of pulsed current formed nano-structured lead dioxide

An electro-forming method was used for the preparation of nano-structured lead dioxide on lead substrate in 4.8 M H₂SO₄. A two electrode system composed of two similarly prepared lead electrodes was employed. A constant current was applied between two electrodes for a short time, followed by a relaxation period. A dark oxidation film of suitable stability and homogeneity was formed on the anode electrode. Different parameters including pulse height, pulse time (t_on) and relaxation time (t_off) were optimized. A change in morphology of lead dioxide from globular to nanofibriliar was observed when the pulse time and relaxation time varied from 0.01 to 10 and 0.1 to 5 s, respectively, at a pulse height of 25 mA cm⁻². A variation in pulse height caused a variation in diameter and length of nanofibers formed at a pulsed time of 0.1 s and relaxation time of 5 s. The scanning electron microscopy (SEM) showed that lead dioxide particles obtained under these conditions have nanofibriliar morphology with an average diameter in the range between 20 and 50 nm and length of 500–1000 nm.