 This study evaluated the effect of different pretreatments on the microstructure, thermal, and physical properties of activated carbons, ACs, prepared from Amazon Piazava fibers using CO2 activation at 800 degrees Celsius. Pretreatments included meserization, corona discharge, and extractive removal. The resulting ACs exhibited nanoscale pores, lower crystallinity, and higher thermal stability than the untreated sample, making them potential adsorbent materials for various applications. This article was authored by Johnnie's Pascastro, Joao Rodrigo Coimbra-Noble, Maria Lucia Bianchi, and others.