AbstractIn this work, the surface of oil palm mesocarp fiber (OPMF) was modified via alkaline-peroxide treatment with hydrogen peroxide under alkaline conditions. The effect of the treatment on the chemical composition and microstructure of the fiber was examined using chemical analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and X-ray diffraction (XRD) analysis. The treatment resulted in the removal of lignin, hemicellulose, and waxy substances from the fiber and increased its surface roughness and crystallinity. The eco-friendly biocomposite was made from poly(butylene succinate) (PBS) and chemically treated fiber at a weight ratio of 30:70, and was fabricated via a melt-blending technique followed by hot-pressed moulding. The results indicated that alkaline-peroxide treatment of the fiber improved the tensile strength, tensile modulus, and elongation at break of the OPMF/PBS biocomposite by 54, 830, and 43%, respectively. The SEM analysis revealed improvement of the interfacial adhesion between the chemically treated fiber and the PBS. This work demonstrates that alkaline-peroxide treatment of fiber is beneficial prior to its use in fabricating biocomposites.