© 2021, Korean Carbon Society.Carbon xerogels (CXs) with three-dimensional (3D) structure, unusual surface, physical, electrical and mechanical properties and their electrically conductive polymer polypyrrole (PPy) composites were synthesized as electrode materials for supercapacitors. The effect of different resorcinol/formaldehyde (R/C) ratios, whether solvent exchange with or without acetone and polypyrrole addition on the physicochemical (FTIR, XRD, BET, SEM and TGA) and electrochemical properties (CV, 1000 cycles) of the synthesized materials were investigated. It was observed that the R/C ratio and the solvent exchange process prior to drying affect the specific surface areas and the pore size distributions, thereby positively affecting the specific capacitance. PPy film thickness was observed to be effective in the specific capacitance of the electrode in PPy composite synthesis. Among the synthesized materials, the highest specific capacitance values belong to polypyrrole/carbon xerogel composites. As a result of the analysis and calculations, it was found that the highest specific capacitance belongs to CX2/PPy composite with 599 Fg−1 at 5 mVs−1. CX2/PPy composite has been found to have a capacitance retention rate of 80.30% at the end of 1000 cycles.