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O-EC-NAP Operando Electrochemical Cell

Operando Electrochemical Cell for NAP-XPS investigations of electrochemical processes at the interface between electrode and electrolyte

The O-EC-NAP cell allows for NAP-XPS measurements of electrochemical processes electrode - electrolyte interfaces. It has a three electrodes (WE, RE, CE) and is mounted on its own 4-axes manipulator. By rotating the manipulator, the area of interest for NAP-XPS measurements can be easily located. The O-EC-NAP cell can be used with or without a window. In order to minimize evaporation of the electrolyte from the investigation area during the measurements, an additional buffer cell serves as a sacrifice trough for maintaining the vapor pressure value constant during the experiments. Additionally, the buffer cell catches any spilled electrolyte and prevents that the electrolyte drops into the chamber.

The 4-axes manipulator is equipped with all electrical connection for the electrodes as well as the liquid pipelines for filling and draining the O-EC-NAP cell. A peristaltic pump is used for liquid transfer between a reservoir and the EC-cell.

The O-EC-NAP Operando Electrochemical Cell module comes with its own vacuum chamber, pumps and frame and therefore can be attached to almost any NAP-XPS system with backfilling configuration. The first delivered cell was connected to a multimethod NAP-XPS system that combines NAP-XPS, IRRAS and electrochemical investigation techniques for ultimate flexibility in the characterization of various samples and processes.


  • operando electrochemical cell for NAP-XPS measurements of liquid-solid interfaces with 3 electrodes setup: working, reference and counter electrode
  • high versatility: it can be used with or without a window
  • extreme flexibility: it can be attached to almost any NAP-XPS system with backfilling configuration
  • in-situ refillable by using a peristaltic pump







  1. (2019) <p>New Insight into the Gas-Sensing Properties of CuOx Nanowires by Near-Ambient Pressure XPS</p>

    This article presents an investigation of the sensing properties of chemiresistors based on Cu2O/CuO core–shell nanowires containing p–p′ heterojunctions. The nanowires were synthesized by a conventional hydrothermal method and used for the detection of ethanol and nitrogen dioxide, reducing and oxidizing agents, respectively. To unravel the chemical processes connected with gas detection, an in situ approach was applied. This approach was based on near-ambient pressure X-ray photoelectron spectroscopy combined with simultaneous monitoring of sensor responses. The in situ measurements were performed during exposure to the analytes at a total pressure of 0.05–1.05 mbar and 450 K and were correlated with chemiresistor response measurements carried out at a standard pressure and under an ambient atmosphere. The study revealed that heterojunction treatment with ethanol vapors, accompanied by partial reduction of the nanowires, is the key step to obtaining chemiresistors with good sensing performance. While the untreated heterojunctions exhibited poor n-type sensing responses, the treated ones showed significantly improved p-type responses. The treated sensors were characterized by a stable baseline, high reversibility, detection limits estimated as 50 ppm for ethanol and 100 ppb for nitrogen dioxide, and with response times in tens of seconds. In all cases, we propose a band scheme of Cu2O/CuO heterojunctions and a gas-sensing mechanism.

    P. Hozák, M. Vorokhta, I. Khalakhan, K. Jarkovská, K. Jarkovská
    J. Cibulková, P. Fitl, J. Vlček, J. Fara, D. Tomeček, M. Novotný, M. Vorokhta, J. Lančok, I. Matolínová, and M. Vrňata
    J. Phys. Chem. C 2019, 123, 49, 29739–29749
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  2. (2018) <p>Electrifying model catalysts for understanding electrocatalytic reactions in liquid electrolytes</p>

    Electrocatalysis is at the heart of our future transition to a renewable energy system. Most energy storage and conversion technologies for renewables rely on electrocatalytic processes and, with increasing availability of cheap electrical energy from renewables, chemical production will witness electrification in the near future1,2,3. However, our fundamental understanding of electrocatalysis lags behind the field of classical heterogeneous catalysis that has been the dominating chemical technology for a long time. Here, we describe a new strategy to advance fundamental studies on electrocatalytic materials. We propose to ‘electrify’ complex oxide-based model catalysts made by surface science methods to explore electrocatalytic reactions in liquid electrolytes. We demonstrate the feasibility of this concept by transferring an atomically defined platinum/cobalt oxide model catalyst into the electrochemical environment while preserving its atomic surface structure. Using this approach, we explore particle size effects and identify hitherto unknown metal–support interactions that stabilize oxidized platinum at the nanoparticle interface. The metal–support interactions open a new synergistic reaction pathway that involves both metallic and oxidized platinum. Our results illustrate the potential of the concept, which makes available a systematic approach to build atomically defined model electrodes for fundamental electrocatalytic studies.

    F. Faisal, C.Stumm, M. Bertram, F. Waidhas, Y. Lykhach, S.Cherevko, F. Xiang, M. Ammon,
    M. Vorokhta, B. Šmíd, T. Skála, N. Tsud, A. Neitzel, K. Beranová, K. C. Prince, S. Geiger,
    O. Kasian, T. Wähler, R. Schuster, M. A. Schneider, V. Matolín, K. J. J.
    Nature Materials volume 17, pages 592–598 (2018)
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  3. (2018) <p>Investigation of gas sensing mechanism of SnO2 based chemiresistor using near ambient pressure XPS</p>

    In this article, we present the results of an investigation into chemical processes which take place at the surface of SnO2-based chemiresistor in various atmospheres (1 mbar of argon, 1 mbar of oxygen, 0.1 mbar of ethanol, 1 mbar of oxygen + 0.1 mbar of ethanol mixture) at common working temperatures (450 and 573 K). The key method for nanoscale analysis was the Near Ambient Pressure X-ray Photoelectron Spectroscopy. In parallel the resistance and DC-responses of SnO2 layer were in-situ monitored providing information about macroscale processes during gas sensing. The change in the sensor resistance after exposure to the ethanol-containing atmospheres together with the disappearance of the band bending effect and observation of different carbonaceous groups including ethoxy groups and acetaldehyde molecules on the sensor surface in the XPS spectra supported the theory of chemical interaction of ethanol with the chemisorbed oxygen. The NAP-XPS spectra also showed that the nanostructured tin oxide is partially reduced even after being exposed to pure oxygen at 573 K. Exposing this surface to the mixture of O2/EtOH did not significantly increase the surface reduction probably due to slow kinetics of the ethanol reduction process and fast kinetics of the oxygen re-oxidation process. However, it was demonstrated that the surface of sensor is slowly getting contaminated by carbon.

    M. Vorokhta, I. Khalakhan, M. Vondráček, D. Tomeček, M. Vorokhta, E. Marešová, J. Nováková, J. Vlček, P. Fitl, M. Novotný, P. Hozák, J. Lančok, M. Vrňata, I. Matolínová, and V. Matolín
    Surface Science, Volume 677, November 2018, Pages 284-290
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