Emphasis has been given on applying green chemistry principle to get desire product, bio-composites have been prepared using sisal fiber and Maize starch by using homemade mold. Bio-composites have huge demand in many sectors from Building construction to auto sector due to conscious awareness regarding environment and therefore there is a need of an hour to synthesize Biocomposites materials. The materials and methods used for enhancement of properties of biocomposites materials have been given in details in this paper.Furthermore, characterization and testing have also been mentioned. Crystalline structure and Tg have been found out by SEM method and TGA method respectively. XRD chart has been given firm surface morphology and amount of crystallinity has been found to be maximum for S1.5 composite as compared to other two composites and it may be due to the thoroughly wetting the fibers by the matrix phase for S1.5 composite. SEM charts have been showing the hard surface morphology of the product. TGA/DTA analysis has been showing that the ratio of starch increases is directly proportional to Tg value. Therefore, more the percentage ratio of starch in product more the free mobility and molecular volume, which impacts the higher up Tg value.