Proton-Exchange Membrane Fuel Cells is a promising emission free energy technology. New generation of hybrid membrane for hydrogen fuel cells were produced from commercial sPEEK membranes, chemically and mechanically stabilized with a Sol-Gel (SG) phase. To study the process-structure-properties relationship of our alternative membranes we coupled Atomic Force Microscopy and Raman microspectroscopy on membranes prepared by cryo-ultramicrotomy without epoxy embedding. This paper demonstrates the powerfulness of co-localized AFM-Raman analysis, revealing the inner structure of hybrid membranes. We obtained quantitative data on the diffusion/condensation of SG precursors inside the sPEEK membrane. Co-localized analyses revealed the formation of skin layers with lower SG concentration on both sides of the membrane. The diffusion of species from the SG phase at the cross-section surface was observed at the first step of fabrication (insufficient SG condensation) and disappeared after hydrothermal treatments (improved SG condensation). The nano-mechanical data revealed a densification of the SG phase through the fabrication process.

质子交换膜燃料电池是一种很有前途的无排放能源技术。用于氢燃料电池的新一代混合膜是由商用sPEEK膜生产的，并通过Sol-Gel（SG）相进行了化学和机械稳定处理。为了研究我们替代膜的过程-结构-性能关系，我们将原子力显微镜和拉曼光谱法结合在通过低温超薄切片术制备的无环氧包埋膜上。本文展示了共定位AFM-拉曼分析的强大功能，揭示了杂化膜的内部结构。我们获得了sPEEK膜内部SG前体的扩散/冷凝的定量数据。共定位分析表明，在膜的两侧均形成了具有较低SG浓度的皮肤层。在制造的第一步（SG凝结不足）中观察到了物种从SG相的横截面扩散（在SG凝结不足的情况下），并且在水热处理后消失了（SG凝结得到改善）。纳米力学数据揭示了在整个制造过程中SG相的致密化。