We present the formation mechanism and structure of the superconducting pha
ses in the Bi-Sr-Ca-Cu-O system by TEM and SEM observations. Oxalate coprec
ipitation was used as preparation method. The average particle size, distri
bution and the presence of different phases and shapes of the particles wer
e evaluated. All samples were well crystallized, showing grains in submicro
nic range. After thermal treatments, the complex samples showed mica-like c
rystals uniform dispersed and also an orientation tendency. The superlattic
e was composed of building blocks and successive planes. The TEM observatio
ns were in agreement with the diffraction patterns that revealed a mixture
of 2212 and 2223 superconducting phases. With the building blocks in the sy
stem, it is possible to form many incommensurate phases that destroy the sy
mmetry. Careful control of the preparation conditions is essential to produ
ce a well-ordered commensurate phase, suitable for the precise determinatio
n of the complete superstructure by X-ray diffraction. (C) 2000 Elsevier Sc
ience Ltd. All rights reserved.