33 Search Results

This work investigates the use of roll-to-roll coating methods for the production of iridium oxide catalyst layers for proton exchange membrane water electrolyzers. Catalyst layers were produced using two coating methods: slot die and gravure. By varying the solids content of the catalyst ink and coating process variables loadings between 0.08 and 0.64 mg_Ir cm⁻² were prepared with relatively high spatial uniformity. However, at loadings below 0.2 mg_Ir cm⁻² microscopy reveals voids in the catalyst layer due to similar length scales of catalyst agglomerates and overall layer thickness. Electrochemical testing shows that these voids do not impact initial membrane electrodemore » assembly performance but lead to increased performance losses after potential cycling compared to spray coated catalyst layers.« less

Understanding water, evolved gas, and ionic transport in membrane-electrode-assemblies (MEAs) is essential for the development of high performance and durable anion exchange membrane water electrolyzers (AEMWEs). This study evaluates the MEA conditioning process, operating conditions, and short-term stability in a 1 M potassium hydroxide (KOH) electrolyte, focusing on the underlying transport phenomena. We observe a significant initial voltage loss in continuous cell operation, which could be associated with gas bubble accumulation, transport layer or flow field passivation, and changes in the catalyst oxidation state. Further, we investigate the effects of materials and operational configurations, including the membrane type and thickness,more » and the electrolyte flow rate, including KOH being fed to both electrodes as well as to the anode only. Furthermore, the effect of membrane drying temperature on ex situ as well as in situ electrochemical performance is evaluated. Finally, we discuss 700 h of AEMWE operation at 1 A/cm², highlighting the underlying degradation phenomena.« less

This work focuses on porous transport electrodes (PTEs), which integrate the anodic catalyst with the adjacent Ti porous transport layer (PTL). Challenges in catalyst deposition on PTLs, particularly at low loadings, motivated this study to evaluate various fabrication methods and characterization approaches. This work investigated Pt-treated PTLs coated with Ir-based catalysts using several common methods, including airbrush coating, rod coating, ultrasonic spray coating, electrodeposition, and sputter deposition, with catalyst loadings ranging from 2.9 to 0.1 mg/cm², providing the opportunity for comparisons across a large set of samples produced by different methods. Two widely accessible characterization techniques: X-ray computed tomography (XCT)more » and scanning electron microscopy energy dispersive X-ray spectroscopy (SEM-EDS) were explored. Initial evaluation of selected samples with XCT provided qualitative insights into catalyst distribution, however comprehensive quantitative analysis was limited. SEM-EDS enabled detailed information on the catalyst distribution both qualitatively and quantitatively using two metrics. Atomic and surface area % ratios of Pt:Ir and Ti:Ir revealed trends in catalyst loading and losses into the PTL pores, as well as evaluating the homogeneity of catalyst coatings. The analysis demonstrated that ultrasonic spray coating, electrodeposition, and sputter coating produced the most homogeneous coatings, with minimal catalyst losses observed for electrodeposition and sputter coating. By adapting common techniques with novel, standardized methodologies, this work establishes a universally applicable framework for cross-study comparison of PTEs. The SEM-EDS approach provides a practical, accessible tool for PTE characterization and contributes a reference dataset supporting both research development and rapid quality control.« less

The proton exchange membrane integrity can be compromised during hot-press fabrication of membrane electrode assemblies (MEAs) causing premature cell failures during operation. In this work, infrared (IR) thermography was used as a diagnostic tool to spatially visualize hydrogen (H₂) crossover and identify process-induced-membrane irregularities (PIMs). These irregularities were identified as seed locations for MEA failures. Fine tuning of hot-press conditions was used to mitigate premature cell failures informed by accelerated stress testing (AST). The impact of PIMs on the initial performance, high-frequency resistances, open-circuit voltage, and H₂ crossover are reported. Nafion XL and 212 membranes, hot-pressed with a force ofmore » 16 kg/cm² and temperature of 120°C, were found to be consistently irregularity-free. Irregularity-free MEAs using Nafion 211, 212, and XL membranes demonstrated AST lifetime improvements of 58, 64 and 400%, respectively, compared to those fabricated with non-optimized conditions. In conclusion, this work highlights the importance of fabrication parameters on premature cell failures.« less

Electrode cracks in polymer electrolyte membrane fuel cells (PEMFCs) are correlated with early onset failures. Here, in this work we investigate the influence of cracked gas diffusion electrodes (GDEs) on the durability of the membrane electrode assembly (MEA) using a combined chemical-mechanical accelerated stress test (AST). Electrode crack dimensions were systematically tuned using ink formulations and material selection strategies. A parameter to describe the crack width areal density (Φ_CW) was used to quantify the degree of discontinuity in the electrode surfaces. Open circuit voltage (OCV) transient analyses were used to benchmark and characterize the failure mechanisms in the MEAs asmore » a function of the Φ_CW. While smaller electrode-level cracks, on the order of microns, yielded a 28 % decrease in operating lifetime, larger cracks that propagated from a discontinuous, microporous layer (MPL) coating, decreased the operating lifetime by 56 %. This work emphasizes the need for material processing strategies that consider defect tolerances to limit membrane failures in PEMFCs.« less

A major factor driving fuel cell costs is the quantity of precious metal required. Therefore, it is important to understand a timeframe where inks can be reused. Here, in this work, we explore differences between a freshly prepared catalyst ink and one that has been stored for over a year – comparing ink properties, cathode catalyst layer microstructure, and their respective fuel cell performance. Ink studies revealed smaller agglomerate sizes and a decrease in shear viscosity for the aged ink. Longer storage time also results in fewer cracks and a more uniform ionomer distribution, as evidenced by microscopy characterization ofmore » rod-coated electrodes. Lastly, polarization curves show improved performance at higher current densities for the electrode prepared from the aged ink. We rationalize such effect in terms of enhanced ionomer adsorption onto the catalyst over time.« less

X-ray photoelectron spectroscopy (XPS) is one of the most common techniques used to analyze the surface composition of catalysts and support materials used in polymer electrolyte membrane (PEM) fuel cells and electrolyzers, providing important insights for further improvement of their properties. Characterization of catalyst layers (CLs) is more challenging, which can be at least partially attributed to the instability of ionomer materials such as Nafion during measurements. This work explores the stability of Nafion during XPS measurements, illuminating and addressing Nafion degradation concerns. The extent of Nafion damage as a function of XPS instrumentation, measurement conditions, and sample properties wasmore » evaluated across multiple instruments. Results revealed that significant Nafion damage to the ion-conducting sulfonic acid species (>50% loss in sulfur signal) may occur in a relatively short time frame (tens of minutes) depending on the exact nature of the sample and XPS instrument. This motivated the development and validation of a multipoint XPS data acquisition protocol that minimizes Nafion damage, resulting in reliable data acquisition by avoiding significant artifacts from Nafion instability. The developed protocol was then used to analyze both thin film ionomer samples and Pt/C-based CLs. Comparison of PEM fuel cell CLs to Nafion thin films revealed several changes in Nafion spectral features attributed to charge transfer due to interaction with conductive catalyst and support species. This study provides a method to reliably characterize ionomer-containing samples, facilitating fundamental studies of the catalyst-ionomer interface and more applied investigations of structure-processing-performance correlations in PEM fuel cell and electrolyzer CLs.« less

This work investigates the influence of ballmilling (sometimes also referred to as jar roller milling) time on cathode catalyst layer (CL) inks and electrode properties using formulations and coating methods relevant for industrial manufacturing. Four CL inks with the same composition were milled for 24, 48, 72, or 96 h. Rheological investigation of these inks showed a reduction of elastic moduli and steady-shear viscosity with continuous ink milling, which is correlated to a decrease in particle-particle interactions as well as formation of smaller agglomerates. Optical microscopy (OM) analysis of the fabricated electrodes revealed a trend in surface crack formation; formulationsmore » milled for 24 h contained the lowest average surface crack area percentages of 0.370% at heavy-duty loadings of ~0.300 mg_Pt cm^-2, compared to 2.418% for the ink milled for 96 h. Further characterization of the CL through transmission electron microscopy (TEM) imaging showed a decrease in the mean agglomerate and pore size with milling time. Furthermore, these smaller electrode features were consistent with reduced fracture resistance and, hence, development of larger stresses during drying. Our results highlight the need to consider ink processing as an important component in defect-free CL manufacturing.« less