R. Nyffenegger et al., INSITU INVESTIGATION OF ELECTROPOLYMERIZED POLYANILINE FILMS BY SCANNING-TUNNELING-MICROSCOPY, Synthetic metals, 55(1), 1993, pp. 402-407
Electrolytic Scanning Tunneling Microscopy (STM) was used to investiga
te in situ the nm- to mum-scale morphology of Polyaniline films prepar
ed by potentiodynamic electrochemical polymerization of aniline in pre
sence of p-phenylenediamine in 1M HClO4 and 1M HCl. The measurements w
ere assisted by ex situ Scanning Electron Microscopy. By choosing an a
ppropriate potential of the tunneling tip, it is possible to perform S
TM directly in the electropolymerization solution and to image film gr
owth sequences. In the sub-mum-scale, the films exhibit a granular mor
phology, where the average diameter of the granular growth patterns is
affected by the polymerization electrolyte. In the mum-scale it is ob
served that the 3D morphology of the films is markedly influenced by t
he voltammetric scan rate during electropolymerization, leading to mor
e compact films with less fibrous features at very high scan rates of
50 V/s.