Cellulose whiskers were obtained by means of sulfuric acid hydrolysis of curauá fibers. Before hydrolysis, the natural fibers were treated with an alkaline solution to remove the non-cellulosic content. Fiber degradation evolution and cellulose whisker formation were analyzed by structural and morphological analysis. The original fiber structure underwent a fragmentation mechanism after being exposed for 3 min to sulfuric acid. Cellulose whiskers were lixiviated from the fiber surface after 10 min of hydrolysis, developing two scenarios: one where the whiskers became unattached from the original fiber, and the other which remained attached. The cellulose whiskers presented a needle-like geometry with an approximate diameter of 11 nm and average length of 185 nm, after 30 min of acid hydrolysis. 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