Cassava stillage residue (CSR), a kind of agro-industrial plant fiber, was modified by coupling agent (CA), mechanical activation (MA), and MA-assisted CA (MACA) surface treatments, respectively. The untreated and different surface treated CSRs were used to prepare plant fibers/polymer composites (PFPC) with poly(vinyl chloride) (PVC) as polymer matrix, and the properties of these CSR/PVC composites were compared. Surface treated CSR/PVC composites possessed better mechanical properties, water resistance and dimensional stability compared with the untreated CSR/PVC composite, attributing to the improvement of interfacial properties between CSR and PVC matrix. MACA-treated CSR was the best reinforcement among four types of CSRs (untreated, MA-treated, CA-treated, and MACA-treated CSRs) because MACA treatment led to the significant improvement of dispersion, interfacial adhesion and compatibility between CSR and PVC. MACA treatment could be considered as an effective and green method for enhancing reinforcement efficiency of plant fibers and the properties of PFPC. (C) 2014 Elsevier B.V. All rights reserved.