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In this work, a pair of biopolymer materials has been used to prepare high ion-conducting electrolytes for energy storage application (ESA). The chitosan:methylcellulose (CS:MC) blend was selected as a host for the ammonium thiocyanate NH₄SCN dopant salt. Three different concentrations of glycerol was successfully incorporated as a plasticizer into the CS–MC–NH₄SCN electrolyte system. The structural, electrical, and ion transport properties were investigated. The highest conductivity of 2.29 × 10⁻⁴ S cm⁻¹ is recorded for the electrolyte incorporated 42 wt.% of plasticizer. The complexation and interaction of polymer electrolyte components are studied using the FTIR spectra. The deconvolution (DVN) of FTIR peaks as a sensitive method was used to calculate ion transport parameters. The percentage of free ions is found to influence the transport parameters of number density (<i>n</i>), ionic mobility (<i>µ</i>), and diffusion coefficient (<i>D</i>). All electrolytes in this work obey the non-Debye behavior. The highest conductivity electrolyte exhibits the dominancy of ions, where the ionic transference number, <i>t_ion</i> value of (0.976) is near to infinity with a voltage of breakdown of 2.11 V. The fabricated electrochemical double-layer capacitor (EDLC) achieves the highest specific capacitance, <i>C_s</i> of 98.08 F/g at 10 mV/s by using the cyclic voltammetry (CV) technique.