Thin mesoporous films of TiO₂ (anatase) particles (or similar types of nanoparticles) are assembled at electrode surfaces via layer-by-layer deposition techniques. Depending on the particle size and the number of deposition cycles, functionalized films of typically 30 to 300 nm thickness are formed and characterised by atomic force microscopy (AFM), scanning electron microscopy (SEM), voltammetric, and impedance methods.

Depending on the type of mesoporous membrane and the adsorbed redox system, electrochemical processes close to the electrode surface (Process 1) or throughout the mesoporous film (Process 2) are observed. In some cases Process 2 is inhibited by slow electron conduction through TiO₂ and in the presence of a soluble redox mediator strong amplification of voltammetric signals is observed.