This work deals with the synthesis of SiO2@TiO2 supported palygorskite fibers and their use as a filler for proton exchange membrane fuel cells in order to improve their performance. SiO2@TiO2‐palygorskite nanostructured particles were synthesized separately with original route to ensure the growth of TiO2 and then of SiO2 on the surface of the clay. Accordingly, the introduction of the synthetic filler (SiO2@TiO2‐paly) into the electrolyte membrane (Nafion) aims to improve mechanical, thermal, and proton conductivity properties. The TiO2 nanoparticles were generated via a sol–gel process on the external surface of palygorskite. Then, SiO2 nanoparticles were synthetized using a similar sol–gel process, onto the TiO2‐palygorskite particles to produce the final SiO2@TiO2‐palygorskite particles. The physico‐chemical properties of the nanostructured particles were studied by X‐ray diffractometry, Fourier transform infrared, scanning electron microscopy, and transmission electron microscopy. Nafion based composite membranes were prepared using SiO2@TiO2‐palygorskite and TiO2‐palygorskite as a control standard. The composite membranes show improved mechanical properties, thermal stability, water retention, and proton conductivity compared to the neat Nafion membrane. Proton conductivities (at 100°C and 100% relative humidity) increased from 65.0 mS/cm for neat Nafion to 70.4 mS/cm and to 128.6 mS/cm when incorporated TiO2‐Paly (6% in weight) and SiO2@TiO2‐Paly (6% in weight), respectively.

Sulfonated poly(ether ether ketone) (SPEEK) with a low sulfonation degree was blended using nanofiller layered double hydroxide (LDH, Mg2AlCl)/sepiolite nanostructured material as additive to use as an electrolyte membrane for fuel cell application. Characterization assessments, that is, mechanical stability, thermal gravimetric analysis, ion exchange capability, swelling properties, water uptake capacities, electrochemical impedance spectroscopy analysis, and Fourier transform infrared spectroscopy of the composite membranes were conducted. The presence of LDH/sepiolite nanoarchitectured material within SPEEK was found to have the highest water retention and proton conductivity value at high temperature rather than LDH/SPEEK and pristine SPEEK membranes.

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