I. Carrillo et al., MICROSTRUCTURE OF POLYFURAN PERCHLORATE-DOPED FILMS BY SCANNING AND TRANSMISSION ELECTRON MICROSCOPIES AND ELECTRON-DIFFRACTION/, Macromolecules, 29(17), 1996, pp. 5585-5589
Polyfuran films doped with perchlorate anions (PFu/ClO4) were studied
by scanning and transmission electron microscopies and electron diffra
ction in order to analyze their morphology and microstructure. Film ge
neration was carried out electrochemically at constant potential, E(d)
= 2.6 V (Ag/Ag+), onto platinum electrodes in acetonitrile/sodium per
chlorate medium. The study of the superficial films morphology reveale
d an ordered nodular structure in the films growth face, the nodular s
ize depending on E(d). Alignment of nodules followed a direction paral
lel to the substrate. Crystalline structures immersed in amorphous dom
ains were found in planar sections and cross-sections of PFu/CLO(4) fi
lms by transmission electron microscopy and selected area micro-electr
on diffraction. Planar sections close to thefilm growth surface exhibi
ted randomly oriented crystals, while single crystals with lamellar st
ructures were detected in deeper layers. Electron diffraction patterns
obtained in planar and transversal sections were consistent with a he
xagonal unit cell: a = 0.68 nm and c = 0.62 nm, alpha = beta = 90 degr
ees, and gamma = 120 degrees. The existence of moire patterns in plana
r sections confirms the laminar structure proposed for PFu/ClO4 films.