Accelerating Real-Time Analysis of Gas Diffusion Electrodes Using Different Coupled Mass Spectrometry Techniques
Authors: Reichmann Ina , Lloret Segura Vicent , Ehebele Konrad , Mayrhofer Karl J. J. , Cherevko Serhiy 
Published: February 2024

Due to the rapid development of new catalysts, simple electrochemical screening methods are needed to evaluate the activity and stability of catalyst layers. Setups for these applications already exist: the so-called Scanning Flow Cells (SFCs) unify real-time electrochemical activity and dissolution stability analysis in a high-throughput fashion and find applications in a broad range of topics, such as battery research, 1 oxygen evolution reaction catalysts performance,2 and photo-electrochemistry.3 Yet, the low current densities reached in the system hinder the direct comparison of the results to real devices.4

Gas diffusion electrode (GDE) based setups present a promising alternative to Aqueous Model Systems (AMS) due to their ability to achieve higher current densities. Compared to two electrode full cells (fuel cell or water electrolyser), GDE half-cells are operated in a three-electrode configuration with liquid electrolyte. However, as in fuel cells, gasses reach the catalyst layer through a flow field, achieving relevant current densities up to 2 A cm-2. The GDE half- cell offers the advantage of studying the isolated reaction of the working electrode by applying controlled potentials with a reference electrode. While the GDE offers a simplified approach, the assembly process can be time-consuming, and the overall catalyst throughput analysis could be further optimised.5,6

In this context, we present a novel setup that enables the rapid examination of catalyst layers for fuel cells, providing more realistic conditions while simultaneously investigating degradation processes. The setup consists of an optimised SFC based on lower internal resistance and an additional flow field to purge the catalyst layer with different gasses. As the common SFC, the presented Scanning Gas Diffusion Electrode half cell (S-GDE) can be connected to an Inductively Coupled Plasma Mass Spectrometer (ICP-MS) to quantify the dissolution of metals in real-time. Furthermore, the gas-sensitive Mass Spectrometer can be connected to the gas stream of the cell, enabling the detection of volatile products via on-line electrochemical mass spectrometry (OLEMS). The simple replacement of catalyst layers in the S-GDE allows fast analysis of multiple catalysts consecutively. Still, as the aim is to facilitate high-throughput electrochemistry, developing the S-GDE is ongoing. Furthermore, the optimised cell can reach higher current densities than cells of a similar design, allowing accelerated stress tests (ASTs) and the performance of polarisation curves.
The S-GDE will offer a new perspective on realistic catalyst layers, their performance, and catalyst/support degradation processes, e.g. Pt dissolution and carbon corrosion. The increasing demand for new catalyst materials highlights the need for their rapid evaluation under realistic conditions, taking into account not only their electrochemical performance but also their stability.

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Jenewein KJ, Kormányos A, Knöppel J, Mayrhofer KJJ, Cherevko S. Accessing In Situ Photocorrosion under Realistic Light Conditions: Photoelectrochemical Scanning Flow Cell Coupled to Online ICP-MS. ACS Measurement Science Au. 2021;1(2):74–81.

Ehelebe K, Escalera-López D, Cherevko S. Limitations of aqueous model systems in the stability assessment of electrocatalysts for oxygen reactions in fuel cell and Current Opinion in Electrochemistry. 2021;29:100832.

Ehelebe K, Knöppel J, Bierling M, Mayerhöfer B, Böhm T, Kulyk N, et Platinum Dissolution in Realistic Fuel Cell Catalyst Layers. Angewandte Chemie (International ed in English). 2021;60(16):8882–8.

Ehelebe K, Seeberger D, Paul MTY, Thiele S, Mayrhofer KJJ, Cherevko S. Evaluating Electrocatalysts at Relevant Currents in a Half-Cell: The Impact of Pt Loading on Oxygen Reduction Reaction. Journal of The Electrochemical Society. 2019;166(16):F1259-F68.

Figure 1: The S-GDE unifies the real conditions approach of the GDE and the high throughput approach of the SFC and the connection to two mass spectrometer enables the real time detection of dissolved catalyst (ICP-MS) and volatile products (OLEMS).

Figure 1