Electrochemical Characterization

Part of the electrochemical characterization at DiSC ranges from cyclic voltammetry, chronoamperometry, differential pulse voltammetry with standard electrodes and ultramicroelectrodes, to low temperature spectroelectrochemistry.

  Electrochemical apparatus

EG&G Mod 175 potenziostat/galvanostat, LeCroy 9361 oscilloscope, home-built potentiostat with positive feedback loop for compensation of ohmic drop. Wide range of standard or ultramicroelectrodes and home developed double faradic cage are used.

 oscilloscope connected to an electrochemical apparatus in a fume hoodfaraday cage and electrochemical setup in a fume hood

copper faraday cage and electrochemical apparatus in a fume hoodelectrochemical apparatus in a fume hood









location at DiSC: 215-02-107

 


voltammeter with monitor and electrochemical celldifferential pulse voltammetry

 
Autolab PGSTAT 100 potentiostat/galvanostat (EcoChemie, The Netherlands) run by a PC with GPES software is used for the differential pulse voltammetry experiments.

location at DiSC: 210-02-020


home-made electrode sealer machinehome-made electrode sealer machine

location at DiSC: 215-02-107

 

 

 


optical microscopeNikon SMZ800 optical microscope

location at DiSC: 215-02-107



 



contacts: saverio.santi@unipd.it

  Spectroelectrochemistry

Equinox 55 Bruker FT-IR spectrometer interfaced to Optically Transparent Thin-Layer Electrochemical (OTTLE) cell (IDEAS! UvA B.V., University of Amsterdam) equipped with CaF2 windows. Pt working (80% transmittance), Pt auxiliary minigrid electrodes, and pseudo-reference Ag wire are melt-sealed in the insulating polyethylene spacer with optical path of 0.019 cm.

spectrometer equipped with electrochemical cell

detail of the electrochemical cell with clouds of water vapour produced by the liquid nitrogen refrigerator

 

contacts: saverio.santi@unipd.it
location at DiSC: 215-02-108

  XPS-UHV system combined with electrochemistry

XPS-UHV system combined with electrochemistry

 electrochemical cell detail

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.

contact: gaetano.granozzi@unipd.it ; laura.calvillolamana@unipd.it
location at DiSC: 215-01-163



note: This system is also reported in the "Surfaces" section.