Studies on the use of natural fibers as replacement to man-made fiber in fiber-reinforced co mposites have increased and opened up further industrial possibilities. Natural fibers have the advantages of low density, low cost, and biodegradability. However, the main d isadvantages of natural fibers in co mposites are the poor co mpatibility between fiber and matrix and the relative high mo isture sorption. Therefore, chemical treat ments are considered in modify ing the fiber surface properties. In this study, Sisal fibers were modified using alkali and benzoyl pero xide solution of different concentration for different time intervals. Morphological changes, thermal stability and crystallinity of fibers were investigated using scanning electron microscope (SEM), TGA and XRD technique. Thermal stability of sisal fibers were decreased on mercerization. Whereas, sisal fibers treated with benzoyl pero xide the enhanced thermal stability. In case of XRD studies, sisal fibers show enhanced crystallin ity.