The determination of the flat band
potential of metal oxide nanoparticles is essential to understand
their electrochemical behavior in aqueous environments. The electrochemical
behavior determines the possible applications and governs the environmental
impact of a nanomaterial. Hence, a new electrode fabrication method
is demonstrated that allows determining the flat band potential of
nanoparticles in porous nanoparticle electrodes via electrochemical
impedance spectroscopy. In such electrodes, the electrolyte is in
contact with the substrate material and contributes significantly
to the ac response of the entire electrode. To block the substrate–electrolyte
contact, the nanoparticle layers were imbibed in a liquid diacrylate
monomer, followed by polymerization. To reestablish the contact between
the outermost polymer-covered particles and the electrolyte, an O2 plasma treatment was conducted. Based on this new electrode
fabrication procedure, the flat band potential of TiO2,
WO3, and Co3O4 nanoparticles in porous
electrodes was determined with high precision. We believe that this
new and economical method will offer an alternative to expensive ultraviolet
photoelectron spectroscopy measurements at synchrotron facilities.