Operando X-ray EC Flow Cell - Model A
The Operando X-ray Electrochemical Flow Cell Model A is a vacuum-compatible operando electrochemical flow cell designed for fluorescence-mode X-ray spectroscopy and reflection-mode X-ray scattering measurements of thin-film and mechanically fragile working electrodes.
The working electrode is mounted without screws. The screw-free assembly minimizes local mechanical stress in the active measurement area and allows very thin, etched or mechanically sensitive substrates to be installed safely. Soft tantalum electrical contacts and compliant sealing gaskets distribute the clamping force over the sample surface. This enables reliable electrical connection and sealing without applying concentrated pressure to the working electrode.
The working electrode is not included with the cell. Very thin glassy carbon plates can be used as working electrodes. The cell is also compatible with locally etched glassy carbon substrates, microfabricated chips and other flat electrode substrates, provided that their dimensions and chemical resistance are suitable for the experiment. Two independent electrical contacts are provided for the working electrode: one contact touches the front surface of the working electrode, while the second contact touches the rear surface of the working electrode. This arrangement allows the electrical connection to be adapted to different electrode and chip designs.
The distance between the working electrode and the counter electrode can be continuously adjusted from 0 to 4 mm. The position is controlled using a micrometer screw with a scale resolution of 20 µm. The adjustable spacing can be used to control the electrolyte layer thickness, uncompensated resistance and mass-transport conditions between the electrodes.
The counter electrode is a 5 mm diameter glassy carbon rod. Its surface can be polished between experiments using suitable polishing suspensions. This allows the exposed surface to be renewed and helps maintain reproducible electrochemical conditions.
The cell uses a micro leak-free Ag/AgCl reference electrode. The compact reference electrode format is suitable for operation in the restricted internal volume of the cell and allows the reference electrode to be positioned close to the working electrode.
The electrolyte can flow through the space between the working and counter electrodes. The cell is designed for operation in vacuum environments. The main structural components are manufactured from Grade 1 titanium and PEEK. These materials provide mechanical stability, chemical resistance and compatibility with demanding synchrotron experimental environments.
Application note
The cell is primarily designed for operando X-ray Absorption Spectroscopy (XAS) in fluorescence mode, including both X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS) measurements. Owing to its fluorescence-optimized geometry, vacuum compatibility and adjustable electrode spacing, the cell is also suitable for several other synchrotron X-ray techniques.
In addition to XAS, the cell is compatible with X-ray Fluorescence (XRF), X-ray Emission Spectroscopy (XES), Resonant X-ray Emission Spectroscopy (RXES), High-Energy-Resolution Fluorescence-Detected X-ray Absorption Spectroscopy (HERFD-XAS) and, depending on the experimental setup, Resonant Inelastic X-ray Scattering (RIXS).
The cell may also be used with selected X-ray scattering and diffraction techniques, including Reflection X-ray Diffraction (Reflection XRD) and Wide-Angle X-ray Scattering (WAXS). Depending on the available beamline geometry and sample positioning capabilities, compatibility with Grazing-Incidence X-ray Diffraction (GIXRD), Grazing-Incidence Wide-Angle X-ray Scattering (GIWAXS), Grazing-Incidence Small-Angle X-ray Scattering (GISAXS) and X-ray Reflectivity (XRR) may also be achievable.
The cell is not intended for transmission-mode measurements, including transmission XAS, transmission XRD or transmission SAXS/WAXS, as its geometry is specifically optimized for fluorescence detection and reflection-based experiments.
Although the cell has been designed to maximize compatibility with a wide range of synchrotron X-ray techniques, the suitability for a particular experiment depends on the beamline configuration and the complete experimental setup. Before purchasing the cell, users should verify that the available incident beam geometry, detector position, spectrometer acceptance, sample environment, vacuum chamber dimensions, angular access, working distance and mechanical clearances are compatible with the cell. Certain experimental stations may impose geometric or instrumental constraints that limit or prevent the use of specific techniques, even though they are generally compatible with the cell design.
This cell includes complimentary beamline compatibility support. If the standard cell configuration is not fully compatible with a specific beamline or experimental setup, redox.me will evaluate the limitations and, whenever technically feasible, modify the cell or provide dedicated adapters to ensure compatibility. This service is provided free of charge and is intended to simplify integration with different synchrotron beamlines while minimizing the need for custom engineering by the user.
For troubleshooting instruction see the redox.me blog post
Specification
WE type: flat plate, thin film substrate, etched substrate or microfabricated chip
recommended WE dimensions: 10 mm × 10 mm
minimum WE dimensions: 8 mm × 8 mm
maximum WE dimensions: 13 mm × 13 mm
WE included: no
number of WE contacts: 2
WE contact arrangement: front-side and rear-side contacts
WE contact material: tantalum
WE assembly: screw-free
CE material: glassy carbon rod
CE diameter: 5 mm
RE: micro leak-free Ag/AgCl
WE-to-CE distance: continuously adjustable from 0 to 4 mm
micrometer scale resolution: 20 µm
electrolyte operation: static or flow
maximum fluorescence/scattering collection angle: 76° from WE surface normal
X-ray detection mode: fluorescence and reflection geometries
transmission-mode compatibility: no
vacuum compatibility: yes
tubing OD: 1/16 inch
Intrastat data
HS Code: 90275000
Country of Origin: Sweden
NET weight: 200g
Product includes
1 x lid screw (Ti G1)
1 x lid (Ti G1)
2 x gasket, 0.5 mm thick FKM or FFKM
2 x tantalum foil contact, 0.05 mm thick
1 x cell body with fittings (PEEK)
1 x index mark (Ti G1) with PEEK screw
1 x CE mount (Ti G1)
1 x Glassy Carbon counter electrode, 5 mm dia.
1 x micrometer thimble (PEEK)
3 x electrode contacts (PEEK, gold-plated Cu pins)
1 x micro leak-free Ag/AgCl
1 x RE termination plug
1 x set of O-rings (FKM or FFKM)
1 x ball head
Related products
BEC 50 mL - Basic Electrochemical Cell
Peristaltic pump
