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Polymer electrolyte fuel cells (PEMFCs) are key to developing the hydrogen economy, particularly in the transportation sector. The focus on heavy-duty vehicles has driven research toward improving the efficiency and durability of catalyst layers and understanding the role of the ionomer binder. The characterization of these ionomers is important not only in their cast forms but also in inks and dispersions. Small-angle scattering (SAS) techniques have become one of the primary tools for analyzing ionomer systems in solution. While SAS can provide valuable structural information about ionomer aggregates, relevant size and shape information requires model fitting to obtain. While many scattering form factor models have been applied to uncover the behavior of aggregates in ionomer dispersions, the role of the fitting range in the fit quality has not been extensively discussed. In this work, we illustrate the effect of varying fitting ranges for three commonly used form factors. 

Abstract Increasing catalytic activity and durability of atomically dispersed metal–nitrogen–carbon (M–N–C) catalysts for the oxygen reduction reaction (ORR) cathode in proton‐exchange‐membrane fuel cells remains a grand challenge. Here, a high‐power and durable Co–N–C nanofiber catalyst synthesized through electrospinning cobalt‐doped zeolitic imidazolate frameworks into selected polyacrylonitrile and poly(vinylpyrrolidone) polymers is reported. The distinct porous fibrous morphology and hierarchical structures play a vital role in boosting electrode performance by exposing more accessible active sites, providing facile electron conductivity, and facilitating the mass transport of reactant. The enhanced intrinsic activity is attributed to the extra graphitic N dopants surrounding the CoN₄moieties. The highly graphitized carbon matrix in the catalyst is beneficial for enhancing the carbon corrosion resistance, thereby promoting catalyst stability. The unique nanoscale X‐ray computed tomography verifies the well‐distributed ionomer coverage throughout the fibrous carbon network in the catalyst. The membrane electrode assembly achieves a power density of 0.40 W cm⁻²in a practical H₂/air cell (1.0 bar) and demonstrates significantly enhanced durability under accelerated stability tests. The combination of the intrinsic activity and stability of single Co sites, along with unique catalyst architecture, provide new insight into designing efficient PGM‐free electrodes with improved performance and durability.