High Resolution Observation of Liquid Water in Polymer Electrolyte Fuel Cell Using X-Ray Nano Computed Tomography
Authors: Watanabe Toshiki , Takeuchi Akihisa , Uesugi Masayuki , Uchiyama Tomoki , Asaoka Takahiko , Tsuji Yoichiro , Imai Hideto , Sakurai Yoshiharu , Uchimoto Yoshiharu 
Published: November 2022

Polymer electrolyte fuel cells (PEFCs) are attracting attention as energy device of low environmental impact because of their high generation efficiency and their emitting only water. The gas supplied to the PEFC is humidified, and water is produced at the cathode catalytic layer by the electrochemical reaction between oxygen and protons. The gas diffusion layer (GDL) and micro porous layer (MPL) in PEFC plays an important role in the transport of oxygen and water. When liquid water accumulates in the GDL, the supply of oxygen to the cathode is inhibited, resulting in poor generation performance. In order to maintain the performance of PEFCs, it is important to manage the water in the cell.
Attempts have been made to visualize the liquid water in GDLs and MPLs for better GDL and MPL design; X-ray micro computed tomography (micro-CT) is one powerful tool for this. Visualization of liquid water in GDLs and MPLs using micro-CT has so far revealed the behavior of the produced water[1,2]. However, in previous studies, it has been difficult to visualize liquid water in the catalyst layer, which is the reaction field where the water is produced. This is because the spatial resolution of micro-CT is larger than a µm, which is insufficient for analyzing liquid water in the catalytic layer. X-ray CT measurements with a resolution of at least 150 nm are needed to measure the distribution of liquid water in the cross section of the catalyst layer. In this study, a measurement system to reveal the distribution of liquid water in the catalyst layer was developed using a 150 nm-spatial-resolution X-ray CT with a synchrotron radiation x-ray microscope called X-ray nano-CT.
A GDL specimen prepared cut to a disk shape with 1 mm diameter. The GDL specimen mounted on a copper stage with high thermal conductivity connected Peltier element module. The micro-CT and nano-CT measurements were carried out in BL20XU beamline at SPring-8, Japan. An X-ray beam energy was 30 keV with a double crystal monochromator. The nano-CT measurements were performed using Zernike phase contrast with voxel size of 38.4 nm. We measured the micro-CT and nano-CT of the dry condition of the GDL specimen. Then, the GDL specimen injected liquid water was scanned. Injection of liquid water into the GDL specimen is not easy because of water-repellent of GDLs. Helium gas saturated water vapor at 40 °C was sprayed to the GDL at 30 ml/min, then the GDL cooled to 10 °C using a Peltier element module and the vapor was condensed inside of the GDL. The measurement setup is shown in Figure 1. This water injection in GDL method was based on the method reported by Kato et al [2].
Figure 2 shows the optical system of the nano-CT used in this study. The optical system of this nano-CT provides a condenser zone plate for sample illumination, a Fresnel zone plate for enlarged image, and phase ring for Zernike phase contrast. These optics allow CT with a high spatial resolution of 150 nm to be measured even for materials with low X-ray absorption.
A three-dimensional structure of GDL was revealed by CT measurements in each scale order. The distribution of liquid water in GDL were visualized with nanoscale spatial resolution (Figure 3). We have successfully visualized the three-dimension distribution of liquid water in the GDL with nm order scale using nano-CT. The newly established nano-CT with a spatial resolution of 150 nm order is extremely useful for elucidating liquid-water behavior in PEFCs containing catalyst layers, which was not clear before.

Acknowledgements

This work is based on results obtained from a NEDO FC-Platform project commissioned by the New Energy and Industrial Technology Development Organization (NEDO). This study was partially supported by the Synchrotron radiation experiments performed at BL20XU of SPring-8 with the approval of the Japan Synchrotron Radiation Research Institute (JASRI) (Proposal numbers 2021A2009, 2021B1015).

References:

1) U. U. Ince, H. Markötter, N. Ge, M. Klages, J. Haußmann, M. Göbel, J. Scholta, A. Bazylak, I. Manke, Int. J. Hydrog. Energy, 45, 12161–12169 (2020)
2) S. Kato, S. Yamaguchi, W. Yoshimune, Y. Matsuoka, A. Kato, Y. Nagai, T. Suzuki, Electrochem. Commun.,
111, 106644 (2020)

Figure 1