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A biocomposite was successfully prepared by blending montmorillonite (MMT)/hemicellulose from oil palm empty fruit bunches (OPEFB) with carboxymethyl cellulose (CMC) through solution casting. The composite was characterized by scanning electron microscopy (SEM), Fourier transmission infrared spectroscopy (FT-IR), and X-ray diffraction (XRD). The results displayed good compatibility between the mixtures of the blended MMT/hemicellulose and CMC due to the hydrogen bonding and electrostatic interaction. There was an improvement in the thermal analysis through their thermogravimetry analysis (TGA), derivative thermogravimetry (DTG), and differential scanning calorimetry (DSC), mechanical properties (tensile strength and tensile modulus), and water vapor permeability (WVP). The best values of tensile strength and tensile modulus of 47.5 MPa and 2.62 MPa, respectively, were obtained from 60H-40CMC-MMT nanocomposite films. The results showed that the mixture of the blended MMT/hemicelluloses and CMC produced a robust nanocomposite film with improved physical and mechanical properties, demonstrating that it is a promising candidate for green packaging applications. [ABSTRACT FROM AUTHOR]