Structural, morphological, optical, and magnetic properties of NiO-added NiCo2O4 electrode materials synthesized by sol-gel, Co-precipitation and ultrasonication methods and their electrochemical supercapacitor response

Abstract

In this study, NiO-added NiCo2O4 composite samples were prepared using three distinct synthesis methods to study the impact of synthesis technique and NiO addition on the electrochemical performance of NiCo2O4. The chosen methods, sol-gel, co-precipitation, and ultrasonication, represent a range of approaches that yield different particle structures and morphologies. The structural and morphological studies of composite samples were investigated using X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM), respectively. XRD analysis revealed the crystalline composition, revealing the presence of two distinct phases: NiO and NiCo2O4. The Rietveld analysis of the composite samples supports the dual phases in the samples. FESEM analysis confirms the change in size and shape of the particles with the synthesis procedure. Optical properties, measured via UV–visible absorbance spectra, demonstrated that the energy gap varied with the synthesis method. The sol-gel samples exhibited the highest energy gap at 2.20 eV. The magnetic properties were measured using the vibration sample magnetometer (VSM), and the results confirm that the synthesis procedure influences magnetic loops and coercivity. The electrochemical performance of the samples in a 3 M potassium hydroxide electrolyte revealed that the co-precipitation method produced the highest capacitance of 398 Fg-1 at a 10 mV/s sweep rate, indicating superior energy storage capacity compared to pure NiCo2O4. Adding NiO phase to the NiCo2O4 matrix is believed to enhance electrochemical performance by creating additional charge at the grain boundaries, leading to a synergistic effect and improved electron and ion transport. The exceptional electrochemical performance of these composite materials suggests that the synthesis methods and the addition of NiO play a critical role in determining the overall efficiency and applicability of battery-type supercapacitors. These findings pave the way for further research into optimizing synthesis parameters to enhance energy storage capacity and inspire the development of advanced spinel metal oxide composite electrodes for supercapacitors and other energy storage applications.