XPS-UHV system combined with electrochemistry
Custom-designed UHV system that consists of two independent UHV chambers: a preparation/analysis chamber and an electrochemical (EC) chamber.
In the preparation/analysis chamber, several evaporators and gas valves are available, as well as an argon sputter gun, for the preparation of the samples. This chamber is also equipped with an Omicron 4-Grid SPECTALEED, an EA 125 Omicrom electron analyzer with five chaneltrons and a non-monochromatized anode (Al Kα/Mg Kα) X-ray source for X-ray photoemission spectroscopy (XPS) measurements and counts with a High precision VT manipulator (RT – 1000 K) capable of x,y,z translations and polar rotation (around the manipulator axis itself).
The EC chamber is connected to the preparation/analysis chamber through an UHV-EC transfer system, which consists of two manipulators (horizontal and vertical) that allow the coupling with the EC cell. The EC cell is a custom made PEEK (polyether ether ketone) cell equipped with a Pt wire (counter electrode) and an Ag/AgCl/Cl-(3M KCl) electrode placed in a Luggin capillary (reference electrode). The cell is controlled by an Autolab potentiostat running with NOVA Software. The EC measurements can be performed in different solutions that are pumped into the EC cell through a tubing system using a syringe pump (N-1010, Pump Systems Inc.), which allows an accurate control of the flow.
This UHV-EC system allows to combine in situ XPS and electrochemical measurements in order to determine the chemical changes induced in the materials due to the electrochemical work.