In this paper, the design of experiments (DOE) optimization
was
carried out via response surface methodology (RSM) based on central
composite design (CCD) to investigate the impact of four main pulse
reverse electrodeposition factors involved in the deposition of hydrothermally
reduced graphene oxide (rGO) on nickel foam (NF). Furthermore, optimization
with the same method was performed on pH and Se/Ni ion source ratio
to achieve the best electrolyte for cathodic pulse electrodeposition
of Ni–Se on the optimized rGO@NF electrode. Therefore, a high
reduction degree of GO was achieved via hydrothermal reduction before
electrodeposition, which was further enhanced by cathodic reverse
pulses. RSM revealed desirable models for both processes. The X-ray
diffraction (XRD) investigation indicated an amorphous Ni–Se
structure, which holds many advantages for electrocatalytic activity.
Moreover, the optimized Ni–Se@rGO@NF exhibited coin-like nanostructures
on the field emission scanning electron microscopy (FESEM) images,
providing a highly exposed surface area. As demonstrated in electrochemical
investigations, the optimized Ni–Se@rGO@NF required 63, 185
mV, and 1.509 V to attain 10 mA·cm–2 for HER,
OER, and bifunctional water splitting, respectively. Moreover, an
excellent Cdl value of 106.55 mFs
n–1/cm2 for the Ni–Se@rGO@NF suggested
a high accessibility of the optimized electrode.