This study aimed to evaluate the effect of different pretreatments of Amazon piassava (Leopoldinia piassaba) fibers on microstructure, thermal, and physical properties of the ensuing activated carbons (ACs). ACs were prepared from untreated and pretreated piassava fibers by physical activation using CO2 at 800°C. Pretreatments include: mercerization, corona discharge, and removal of extractives. Scanning electron micrographs showed the formation of nanoscale pores after the activation process of the charcoal. ACs from pretreated piassava fibers presented lower crystallinity and higher thermal stability than the untreated sample. ACs from Amazon piassava fibers are potential adsorbent materials for a myriad of applications.