Maize stalk has become one of the major sources of fibers from the agricultural residues. Use of these fibers as a reinforcement in the polymer is described in this paper. The present work is focused on establishing the properties such as physical, chemical, morphological structure and thermal properties of maize stalk fiber using different characterization techniques. Simple hand layup method was followed for processing the composite material. Chemical treatments of fibers were carried out to study the interaction of fibers with the matrix. The results revealed that maize fibers can also be used as a traditional fiber as reinforcement in a natural fiber reinforced composite materials.