User`s guide

Electrochemistry 15

Agilent 5500 SPM User’s Guide 220

Insert the counter and reference electrodes into the sample plate

block (Figure 146). Push the spring-loaded clamp forward from

behind, insert the electrode and release the clamp.

9 Position the electrodes so that they will make good contact with the

electrolyte but will not touch the sample substrate or each other.

10 Use a multimeter to check for good conductivity between the

reference electrode and sample plate clamp, and between the counter

electrode and sample plate clamp.

11 With the multimeter verify that the reference and counter electrode

are not shorted to another electrode or to the substrate.

12 Verify that the AFM probe or STM tip will pass through the

electrodes without any contact.

13 Fill the liquid cell enough to submerge the sample. Check for leaks

and reposition the cell if necessary.

14 Verify that the counter electrode feedback is turned off in the

software and that the potentials are set appropriately for the

particular experiment.

15 Connect the sample plate to the microscope using the 3-pin

connector of the EC/MAC Cable.

16 Load the sample plate onto the microscope.

17 Approach the sample.

Troubleshooting

The most frequently encountered problem is leakage from around the

bottom of the liquid cell. It is generally more of a problem with solvents

that “wet” the substrate well, such as methanol. This causes leakage

current and erratic imaging. Make sure that the sample is flat and large

enough to fit underneath the liquid cell without gaps. Check that the

O-ring is clean and pliable. Tightening the sample plate screws will

increase pressure on the cell. Do not overtighten as this may crack the

liquid cell.

Electrochemistry Definitions

1 In STM Mode the tip is always virtual ground. Virtual ground means

that the potential of the probe is actively kept at ground by the