Optimization-Driven Engineering of Electrodeposited Nanographenide–Conductive Polymer/Prussian Blue Nanoarchitectures for Robust Electrochemical Sensing

The development of high-performance electrochemical sensors requires precise integration of electrode active materials that provide both superior electrocatalytic activity and long-term structural stability. Herein, we report a systematically optimized, one-pot electrochemical deposition approach for the fabrication of nanographenide-based nanoarchitectures, incorporating either a conducting polymer (PEDOT-NG) or Prussian blue (PB-NG). Derived from optimization-driven structural refinement-including applied potential, electrodeposition time, and precursor concentration-the robust nanoarchitecture exhibits a hierarchical morphology that provides an expanded electroactive surface area, accelerating charge transfer and enhancing electrochemical catalytic activity. The optimized PEDOT-NG exhibits exceptional sensitivity for the simultaneous determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA), achieving wide linear ranges with low detection limits of 4.1, 0.12, and 0.18 μM, respectively. The PB-NG achieves a limit of detection of 4.39 μM, driven by highly reversible and stable redox kinetics. This performance is underpinned by narrowed peak-to-peak separations (ΔE) and reduced redox potentials. These results underscore the pivotal role of precise parametric control in developing high-performance electrochemical sensors. Furthermore, this work establishes a comprehensive strategy for designing resilient electrode active materials, thereby paving the way for next-generation electrochemical platforms tailored for diverse and robust sensing environments.