The electrodes of a polymer electrolyte fuel cell (PEFC) are composite porous layers consisting of carbon and platinum nanoparticles and a polymer electrolyte binder. The proper composition and arrangement of these materials for fast reactant transport and high electrochemical activity is crucial to achieving high performance, long lifetimes, and low costs. Here, the microstructure of a PEFC electrode using nanometer‐scale X‐ray computed tomography (nano‐CT) with a resolution of 50 nm is investigated. The nano‐CT instrument obtains this resolution for the low‐atomic‐number catalyst support and binder using a combination of a Fresnel zone plate objective and Zernike phase contrast imaging. High‐resolution, non‐destructive imaging of the three‐dimensional (3D) microstructures provides important new information on the size and form of the catalyst particle agglomerates and pore spaces. Transmission electron microscopy (TEM) and mercury intrusion porosimetry (MIP) is applied to evaluate the limits of the resolution and to verify the 3D reconstructions. The computational reconstructions and size distributions obtained with nano‐CT can be used for evaluating electrode preparation, performing pore‐scale simulations, and extracting effective morphological parameters for large‐scale computational models.

We report a three‐dimensional (3D), pore‐scale analysis of morphological and transport properties for a polymer electrolyte fuel cell (PEFC) catalyst layer. The 3D structure of the platinum/carbon/Nafion electrode was obtained using nano‐scale resolution X‐ray computed tomography (nano‐CT). The 3D nano‐CT data was analyzed according to several morphological characteristics, with particular focus on various effective pore diameters used in modeling gas diffusion in the Knudsen transition regime, which is prevalent in PEFC catalyst layers. The pore diameter metrics include those based on chord length distributions, inscribed spheres, and surface area. Those pore diameter statistics are evaluated against computational pore‐scale diffusion simulations with local gas diffusion coefficients determined from the local pore size according to the Bosanquet formulation. According to our comparison, simulations that use local pore diameters defined by inscribed spheres provide effective diffusion coefficients that are consistent with chord‐length based estimations for an effective Knudsen length scale. By evaluating transport rates in regions of varying porosity within the nano‐CT data, we identified a Bruggeman correction scaling factor for the effective diffusivity.

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