Vein-Like Ni-BTC@Ni₃S₄ with Sulfur Vacancy and Ni³⁺ Fabricated In Situ Etching Vulcanization Strategy for an Electrochemical Sensor of Dopamine

In this study, a novel Ni-BTC@Ni 3 S 4 composite was fabricated by solvothermal reaction using an in situ etching vulcanization strategy and characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), electron paramagnetic resonance (EPR), and Brunauer–Emmett–Teller (BET) analyses. The existence of a sulfur vacancy and Ni 3+ in the as-prepared vein-like Ni-BTC@Ni 3 S 4 greatly promoted the electrochemical sensing activity of the materials. Herein, a simple electrochemical sensor (Ni-BTC@Ni 3 S 4 /CPE) has been fabricated and used for the detection of dopamine (DA). The current signal of the Ni-BTC@Ni 3 S 4 /CPE-modified electrode was linear with the concentration of DA in the range of 0.05–750 μM ( R 2 = 0.9995) with a sensitivity of 560.27 μA·mM –1 ·cm –2 and a detection limit of 0.016 μM. At the same time, the sensor has good stability and anti-interference ability. This study could provide a new idea and strategy for the structural regulation of composite electrode-modified materials and sensitive sensing detection of small biological molecules.