Electrochemistry
5
Keysight 5500 SPM User’s Guide
5-6
Critical Applications
1
Soak overnight in a solution of 70 % concentrated sulfuric acid and
30 % hydrogen peroxide (of 30 % v/v concentration).
2
Rinse thoroughly, at least four times, in 18 MW/cm water.
3
Boil for one hour in 18 MW/cm water, changing the water every 15
minutes. You may instead rinse overnight in 18 MW/cm water.
4
Rinse two more times in 18 MW/cm water.
5
Dry under argon or nitrogen gas.
Electrode Cleaning
Electrodes should be carefully cleaned prior to assembling the liquid
cell. This may even include flame annealing of the electrodes prior to
use in certain cases.
Sample Plate Cleaning
Since the sample plate does not directly contact the sample surface or
electrolyte, a general cleaning with methanol or ethanol prior to
assembly is sufficient.
Substrate Cleaning
Substrates should be free of surface contaminants. Gold substrates
should be hydrogen flame annealed prior to imaging for best results.
Assembling and Loading the Liquid Cell
It is recommended that the assembly procedure be carried out in a
laminar flow hood, glove box or other clean environment. The work
surface should be well cleaned prior to assembling, and gloves should
be worn to prevent contaminating the electrodes and liquid cell. Refer to
for a view of the components described below.
1
Place a clean substrate onto the sample plate.
2
Push the liquid cell onto the spring-loaded pins on the sample plate.
Verify that the O-ring is in contact with the substrate at all points.
WARNING
Use extreme caution when handling this solution. It is a strong
oxidizing agent and extremely corrosive.
