Corncob has a high percentage of cellulose (40.95 ± 0.38%) and hemicellulose (38.94 ± 1.72%) and low lignin content (16.54 ± 0.38%) which has a great potential of bioconversion to bioethanol. The objective of this research was to evaluate the effect of pre-treatment, freezing and the combination of these in corn corona fiber in cellulase hydrolysis, changes in macrostructure and lignocellulosic compounds after pre-treatments. Corncob fiber (FCH) was pre-treated by freezing -20 ° C for 12 h (FCHC); With 0.25M H2SO4 at 121 ° C for 20 minutes (FCHA) and also by the combination of both pre-treatments (FCHAC). To the pre-treated samples, enzymatic hydrolysis with 150 Ucellulase / gsubstrate in 10 ml of acetate was performed at 100 rpm for 72 h, at 37 ° C and pH 5.5. The results showed that after the pre-treatments, the FCHAC contained higher cellulose (64.12 ± 1.03%), lower hemicellulo...