MXene, as a suitable and alternative 2D nanofiller incorporated into a proton exchange membrane (PEM), has recently received considerable attention because of desired mechanical stability, promising conductivity, and active surface functional groups. However, agglomeration or sedimentation in PEMs, as well as the water
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MXene, as a suitable and alternative 2D nanofiller incorporated into a proton exchange membrane (PEM), has recently received considerable attention because of desired mechanical stability, promising conductivity, and active surface functional groups. However, agglomeration or sedimentation in PEMs, as well as the water retention capacity under low humidity of MXene, are limiting factors in the field of PEMs. In this paper, modified MXene and TiO
2 nanoparticles used as functional nanofillers were incorporated into sulfonated poly (ether ether ketone) (SPEEK) to prepare novel SPEEK-based composite PEMs. The effects of the nanofiller contents on self-humidifying and protonic conductivity of the composite PEMs were also investigated under different temperatures. When the contents of functionalized MXene and modified TiO
2 are 5 wt.%, proton conductivity, water uptake and methanol permeability of the composite PEMs can be up to 0.143 S/cm, 60% and 2.27 × 10
−7 cm
2/s, respectively, which represent increases of about 192%, about 38% and a decrease of 47%, respectively, compared with that of primary SPEEK PEM. Under the synergistic action of functionalized MXene providing a higher number of exchangeable proton sites, modified TiO
2 with inherent hydrophilicity enhancing water retention and Pt providing catalytic sites for the H
2/O
2 reaction to generate water in situ, the self-humidifying capability and proton conductivity of the composite PEMs were improved significantly.
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