Hydrothermal syntheses on the stoichiometric composition 3MgO . 2SiO(2
) plus excess H2O can reproduce the various rolled structures of natur
al serpentines. However, synthetic polygonal serpentine has not been r
eported yet, probably due to difficulties in TEM sample preparation. W
e describe herein an embedding preparation technique followed by ion m
illing, which allows HRTEM axial imaging of synthetic serpentine fibre
s. Selected-area electron diffraction (SAED) patterns of single fibres
could also be recorded. Like their natural counterparts synthetic fib
res with a diameter greater than 100 nm unambiguously display polygona
l arrangements of 15- and 30-sector types, and various stacking sequen
ces including regular multi-layer polytypes. These results suggest tha
t the origin of polygonization is probably controlled by temperature a
nd/or growth (kinetic) parameters.