In this study, the Sulfonated graphene oxide (SGO)/Fe 3 O 4 nanosheets were synthesized by hydrothermal method and incorporated into blend sulfonated poly(ether ether ketone) (SPEEK)/poly(vinyl alchole) (PVA) matrix with different weight percent of (SGO)/Fe 3 O 4 nanosheets. The performances of prepared membranes were investigated by water uptake, membrane swelling, mechanical and thermal stability, proton conductivity, methanol permeability and DMFC test. It was found that the water uptake and tensile strength of SPEEK membrane increased and proton conductivity and power density decreased by 2 blending with PVA. Incorporation of SGO/Fe 3 O 4 nanosheets into SPEEK/PVA matrix enhanced mechanical stability, proton conductivity and methanol barrier properties of membrane. The SPEEK/PVA/SGO/Fe 3 O 4 nanocomposite membrane with optimal nanosheets content (5 wt%) exhibits low methanol permeability (8.83 × 10 −7 cm 2 s -1 ), high tensile strength (51.2 MPa), high proton conductivity (0.084 S cm -1 at 25°C) and high power density (122.7 mW cm -2 at 80°C) and suggests its potential application in DMFCs.