In-situ Electrochemistry

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AFM - In-situ Cyclic Voltammetry

 

-Electrodeposition of copper from tetraammonium EDTA solution-

 
   
 
   

 A drop of solution (about 150ml) was self-contained on the glassy carbon electrode due to the high wetting angle, thus no need for an o-ring.  Care taken to ensure that both counter (CE) and reference electrodes (RE) are in contact with the solution.  The 15x15mm AFM images at 2.44Hz scanning rate were continuously recorded with the simultaneous potential sweep at scanning rate 5mV s-1.  The AFM imaging was done in the intermittent-contact mode with Si3N4 AFM tips.  After the completion of the cv experiment, the composite AFM-cv image was constructed by aligning the temporal coordinates of the AFM images and the cv scan, thus enabling the correlation between the electrochemical reactions and the morphological changes at the surface. Figure represents a typical composite AFM-cv image recorded.  Solution composition: 0.005M Cu2++ 0.012M tetraammonium EDTA;  pH 9.

 
   
The schematics of the experimental setup:

 

 

 
   

The experimental setup:

Atomic force microscope:   Digital Instruments, Nanoscope IIIa

Electrochemical Cell      :    AFM electrochemical cell

Working electrode (WE) :   Glassy carbon

Counter electrode (CE)   :   Copper wire

Reference electrode (RE):    Leak-free micro Ag/AgCl (Cypress Systems),

                                           E0 = +0.222V vs. NHE