This investigation involves the development and implementation of NiFe2O4/g-C3N4 (NFCN) heterogeneous structures for the photocatalytic elimination of crystal violet (CV) using sol-gel assisted ultrasonication method. The synthesized sample was characterized by XRD, UV-vis spectroscopy, FTIR, HR-SEM, EDX, and XPS. An effective combination of pure nickel ferrite (NF), g-C3N4 (CN), and their composite NFCN with minimal Fe2O3 phases was verified by XRD analysis. Optical studies revealed that the NFCN composite's outermost region is red shifted towards the visible light range associated with pure NF, which proved highly beneficial for photocatalytic applications. FTIR spectra confirmed that the nanocomposite exhibits the absorbing bands of both CN and NF. According to HR-SEM, the NF nanoparticles have been embedded onto the CN surface, which indicates the creation of NF-CN heterogeneous structures. CV was degraded by the analysed nanocomposite NFCN (30 mg/litre) in 180 min, at a rate of 65%. This result indicated that h(+), center dot OH, and center dot O-2(-) play a role in the breakdown of dyes. The primary objective of this investigation is to get more insight into the process of creating beneficial photocatalysts for the breakdown of naturally occurring contaminants.