In recent years, as a result of increasing environmental concerns, biodegradable materials have gained great attention. With the rapid development of electronic technology, the importance of innovation and development of low-cost, sustainable, transient bioelectronics materials is increasing. In this research, the preparation of Poly(Vinyl Alcohol) (PVA), Chitosan (CS), and Multi-Walled Carbon nanotube (MWCNT) biocomposite films have been described. The solution mixing, ultrasonic mixing, and spin coating techniques were used to prepare the PVA/CS/MWCNT biocomposite thin films. UV–Vis absorption spectroscopy and two-point probe resistivity measurement techniques were used to study the optical and electrical properties of the biocomposite thin films. Optical band gap energies ( Eg) of PVA/CS/MWCNT biocomposites were obtained using the Tauc and Absorbance Spectrum Fitting (ASF) methods. Results obtained with both methods were found to be exactly the same. Experimental results have shown that with increasing MWCNT concentration, electrical conductivity (σ) increases from 1.75x10−16 S to 2.94x10−3 S, and Eg decreases significantly. At the same time, the fundamental optical parameters such as band tail (Urbach) energy ( Eu), refractive index ( n), absorption ( α), and extinction ( k) coefficient of the PVA/CS/MWCNT biocomposites were investigated in the UV-VIS range. The improvement observed in the optical and electrical properties of PVA/CS/MWCNT biocomposite films shows that these composites could be used as bioelectronics materials.