Optimizing the Construction and Activation of 3D-Printed Electrochemical Sensors: An Experimental Design Approach for...

This work presents an optimization of the construction, treatment, and activation of 3D-printed electrochemical sensors (E-3D). For this, was used a 2³-full factorial design examining three key variables at two levels: electrode height, electrode diameter, and printing speed. Moreover, it evaluates various physical, chemical, and electrochemical methods to treat and activate the E-3D surface. The techniques of electrochemical impedance spectroscopy and cyclic voltammetry (CV) shows that the sequential physical, chemical, and electrochemical treatments lead to the highest treatment efficiency and activation. Raman spectroscopy and atomic force microscopy characterize untreated and treated E-3D sensor surfaces. The optimal treatment and activation methodology was applied to the electroanalysis of paracetamol (PAR) and caffeine (CAF) simultaneously using CV and differential pulse anodic stripping voltammetry (DPASV). DPASV measurements reveal limits of detection of 0.44 and 0.58 μmol L^-1 in a 0.5 mol L^-1 H₂SO₄ medium for PAR and CAF, respectively, with the treated and activated E-3D sensor. The principal achievement of this work was emphasizing the critical role of surface treatment and activation in enhancing the performance of the developed electrodes, thereby advancing technological applications of 3D-printed electrochemical sensors.