Enhancing Co3O4 nanoparticles: Investigating the impact of nickel doping and high-temperature annealing on NiCo2O4/CoO heterostructures

In this study, we investigated the phase transition of cobalt spinel (Co3O4) nanoparticles into Co3-xNixO4/CoO heterostructures by introducing varying amounts of nickel (x = 0.0–0.16) and subjecting the particles to high annealing temperatures of 1000 ℃. X-ray diffraction (XRD) analysis confirmed the Co3-xNixO4CoO structure for all samples. Transmission electron microscopy (TEM) provided further insights into the phase or heterostructure of the samples after annealing, revealing the arrangement of the two phases. Fourier-transform infrared spectroscopy measurements demonstrated a band shift around 537 cm-1 with increasing Ni content, while ultraviolet-visible (UV-Vis) measurements indicated the energy band (Eg). Significant morphological changes were observed in scanning electron microscope (SEM) measurements at 0.16 Ni, displaying irregular agglomerates. Our findings suggest that introducing Ni into the Co3O4 structure and increasing the annealing temperature to 1000 ℃ can lead to the formation of a heterostructured system. Furthermore, our study's significance is highlighted by the streamlined synthesis of NiCo2O4/CoO using the sol-gel method followed by calcination. This departure from complex techniques provides an efficient route to acquiring the NiCo2O4/CoO system, a promissory material for advancing supercapacitor research.