Synthesis of a NiO/Bentonite Nanocomposite via Thermal Decomposition of a Schiff Base Precursor

ABSTRACT This study introduces a novel and efficient route for synthesizing a bentonite‐supported nickel oxide (NiO) nanocomposite. A newly synthesized diselenide‐bridged dinuclear nickel(II) complex, with 6,6'‐((1E,1'E)‐((diselenediylbis(4,1‐phenylene))bis (azanylylidene))‐bis(methanylylidene))bis(3‐methoxyphenol) [Ni 2 (SemO) 2 ], was utilized as a single‐source precursor. This complex was immobilized onto natural bentonite and subsequently calcined at 600°C to yield well‐dispersed, face‐centered cubic (FCC) NiO nanoparticles. Unlike conventional impregnation methods that often result in agglomeration, this precursor‐based approach leverages the thermal decomposition of the pre‐adsorbed complex to achieve superior structural control. Comprehensive characterization via x‐ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) analysis confirmed the formation of phase‐pure NiO with a high specific surface area. The resulting nanocomposite exhibits exceptional structural properties that position it as a highly promising candidate for advanced catalytic applications and environmental remediation, offering a distinct advantage over materials prepared through traditional techniques.