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The X-ray Bulk Liquid Electrochemistry Sample Holder integrates a sealed microfluidic liquid cell with true bulk reference and counter electrodes positioned off-chip, enabling accurate electrochemical control within the X-ray microscope. Real reference electrodes (e.g., Ag/AgCl) provide stable potentials, while bulk counter electrodes (e.g., Pt) support consistent current flow, eliminating the instability and drift common in on-chip systems.
During operation, electrolyte flows through the liquid cell while electrochemical cycling is performed on the working electrode under direct X-ray illumination. This architecture decouples electrochemical performance from geometric and material limitations of on-chip microfabricated electrodes, delivering reproducible current voltage responses with well-defined redox peaks closely matching bulk electroanalytical behavior while simultaneously enabling nanometer resolution imaging in liquid environments.