The endstation at the solid-liquid branch hosts the Electrochemistry (EC) cell which is designed for performing photoemission measurements of the solid-liquid interfaces in a dip-and-pull geometry of liquid-gas interfaces using liquid microjet.
The EC cell is a large volume vacuum vessel with two manipulators. Top manipulator holds the sample or microjet; bottom manipulator holds beaker or catcher. Cell access is done via 300 mm front “door” (load-lock style). Sample exchange is done via removing the sample holder from manipulator.
Specs Phoibos-NAP spectrometer is used as a detector of electrons and equipped with a 2D Delayline Detector.
An Ar or N2 glove box can be attached to the endstation for moisture and oxygen-free sample transfer.
Electrochemistry Cell
| Base pressure | 5 x 10-6 mbar Cell not bakeable |
| Pressure range | 5 x 10-6 mbar – 30 mbar |
| Top (sample) manipulator | X, Y, Z, R motorised |
| Bottom (beaker) manipulator | X, Y, Z motorised |
| Electrode info | Typical working electrode dimension: 7mm x 50mm (w x h). Leakless Ag/AgCl reference electrodes are available on request. Contact beamline staff to discuss sample/electrode requirements if uncertain. |
| EC sample holder | 3-electrode setup: WE, RE, and CE placed one after other. WE and CE can be measured by XPS Sample holder can be easily removed from manipulator for electrode/sample exchanging |
| Beaker/Catcher holder | Can hold beakers up to 50 mm diameter and up to 60 mm height. Available beakers of 30, 60, 100, and 150 ml volume. Users can bring their own beakers. Heating or cooling can be provided via temperature-controlled platform on which beaker stands. |
| Potentiostat | Bio-Logic SP200. E range +/- 10V. I range +/- 500 mA. |
| Glove box | A custom glove box can be attached to allow handling/loading of samples in inert/dry Ar or N2atmospheres (typically 3ppm O2 and H2O) |
| Availability | Available |
Liquid Microjet
| Liquid microjet | A jet insert can replace EC sample holder. Jet typically operates at equilibrium liquid pressure (24 mbar for water at RT). Nozzles of 15, 20, 25, 40 µm size are available. Samples delivered using sample loops of 50 ml volume and a HPLC pump. Capillary mixing of 2 liquids is available. Jet manipulator has heating/cooling jacket. Catcher (bottom manipulator) size: 300 ml. Catcher can be heated and cooled. |
| Availability | Available |
Time resolved catalysis
Fast piezoelectric valves can be installed to provide short chemical perturbations to a sample in the form of gas pulses. Synchronization of the valves with the delay-line detector allows the response of the sample to measured with microsecond time resolution. This capability is new and is offered in collaboration with the beamline staff – please contact us to discuss.
| Sample mounting | Samples mounted on omicron plates (as per the solid-gas endstation) on a 3 axis x,y,z manipulator. |
| Sample heating | Up to ~550 C via a resistive heater |
| Sample preparation | No UHV sample preparation is available. Samples must be prepared outside and transferred via air (or inert atmosphere using the glove box). The preparation chamber in the solid-gas endstation can be used for ex-situ sample preparation. |
| Base pressure | 5e-6 mbar |
| Time resolution | µs-s |