Synthesis and Electrocatalytic Mechanism of SrO/Monolayer C ₃ N ₄ Composite for Vanillin Detection

Synthesis at low temperature and interface characteristics in electrocatalysis for nanocomposites are alternative challenge up to date. A SrO nanoparticles (NPs)/g‐C ₃ N ₄ nanosheets (SrO/ng‐C ₃ N ₄ ) composite was prepared by a feasible one‐pot synthesis at 80 °C without post‐sintering, where SrO NPs (with diameters of 20 ∼ 50 nm) were loaded onto ng‐C ₃ N ₄ nanosheets to form an efficient electrocatalyst. By the aid of XPS and FT‐IR analysis, it confirms that SrO NPs were anchored in proximity to the s‐triazine units of ng‐C ₃ N ₄ via SrN bonds. Based on the surface charge characteristics, the electrostatic adsorption between SrO/ng‐C ₃ N ₄ and vanillin as a catalysant was verified. C ₇ H ₅ O ₂ ⁻ anions after the hydrolyzation and ionization of vanillin in PBS solution were adsorbed on the surface of positively charged SrO/ng‐C ₃ N ₄ before electro‐oxidation. The electrocatalytically active centers, i.e., oxygen vacancies on the surface of SrO NPs, facilitate in the oxidation of vanillin, and further the overpotential of the electrocatalyst by SrO/ng‐C ₃ N ₄ toward vanillin is reduced. A detail eletro‐oxidation process of vanillin was identified by UV–vis spectra and differential pulse voltammetry analysis. Based on the Laviron equation, two electrons transfer from vanillin during the oxidation reaction, and speculates the reaction mechanism. Under optimal conditions, vanillin oxidation current is linear to its concentration in the range of 2.0 × 10 ⁻⁸ to 1.4 × 10 ⁻⁵ M, with a detection limit of 6.7 nM (S/N = 3). The limit value complies with the requirements of the World Health Organization and the Chinese Health Standard. As‐prepared sensor applied for the quantification of vanillin in milk samples is long‐term stable, selective, and feasible.