Proceedings of MATSUS Spring 2025 Conference (MATSUSSpring25)
DOI: https://doi.org/10.29363/nanoge.matsusspring.2025.389
Publication date: 16th December 2024
We have developed new environmental liquid cells for Hard X-ray Photoelectron Spectroscopy (HAXPES) experiments at the HAXPES endstation of the GALAXIES beamline at the SOLEIL synchrotron radiation facility using on-purpose designed thin (15-25 nm) low-stress silicon nitride membranes. The membranes were fabricated at IMB-CNM-CSIC from 100 mm silicon wafers using standard lithography techniques and in order to facilitate fast positioning of the X-ray beam on the membrane, platinum alignment marks have been added to the chips hosting the membranes. We have selected rectangular membranes in order to achieve an optimal balance between producing large enough membranes ensuring mechanical stability as well as conforming to the elliptical shape of the synchrotron radiation beam, about 30 µm (V) × 100 µm (H), since in this configuration the strain depends mainly on the short dimension of the rectangle. Optimizing such dimensions, we have fabricated membranes with dimensions of about 20-90 um (V) x 530-600 um (H). The geometry of the HAXPES endstation, with horizontal polarization parallel to the analyzer axis and the intrinsic 54.7 degrees angle arising from the chemical etching of silicon for the fabrication of the membranes, imposes incidence angles of about 45 degrees.
Two types of liquid cells have been built: (i) a static one mounted on an Omicron-type sample holder with the liquid confined in the cell container, and (ii) a circulating liquid cell, inspired on an existing electrochemical cell installed at the LUCIA beamline [1]. The cells have been successfully tested in first exploratory experiments with aqueous solutions of salts (Na+, Cs2+, Cl-), with dispersions of gold nanoparticles and in electrochemical experiments using a coin-cell configuration [2]. The membranes are mechanically robust and withstand the 1 bar pressure difference between the liquid inside the cell and vacuum and the intense synchrotron radiation beam during data acquisition if correctly handled. The lifetime of the membranes is beyond the time scale of the performed experiments in our tests (more than 6 hours). Our results open the door to regular HAXPES studies of liquids under circulation and potentially to other techniques using synchrotron radiation such as e. g., X-ray absorption and transmission.
This project has received funding from the European Union's Horizon 2020 research and innovation programme, under grant agreement No. 101007417 NFFA-Europe Pilot and the Spanish Ministry of Science and Innovation (MCIN) under contract No. PID2021-124568NB-I00. The ICN2 is funded by the CERCA program/Generalitat de Catalunya. The ICN2 is supported by the Severo Ochoa Centres of Excellence programme, grant CEX2021-001214-S, funded by MCIN/AEI. Support through the María de Maeztu grant CEX2023-001397-M funded by MICIU/AEI is acknowledged. We acknowledge funding from Generalitat de Catalunya through the 2021-SGR-00644 project. We also acknowledge the scientific exchange and support of the Centre for Molecular Water Science (CMWS). This project has received funding from the European Union's Horizon 2020 research and innovation programme under grant agreement No. 957189. The project is part of BATTERY 2030+, the large-scale European research initiative for inventing the sustainable batteries of the future. We thank SOLEIL for the provision of beam time (proposal Nos. 20220156 and 20230319). We acknowledge support for the publication fee by the CSIC Open Access Publication Support Initiative through its Unit of Information Resources for Research (URICI).
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