This video presents, for the first time, a comprehensive investigation of the influence of pre- and post-fabrication parameters for the electroactive properties of electrospun chitosan/PVA-based micro- and nanofibers. Chitosan/PVA fibers were fabricated using electrospinning, characterized, and tested as electroactive materials. Solutions with different acetic acid contents (50, 60, 70, and 80 v/v%) were used, and the rheological properties of the solutions were analyzed.