Carbonate formation
is a prevailing challenge in synthesis of BaTiO
3
, especially
through wet chemical synthesis routes. In this
work, we report the phase evolution during thermal annealing of an
aqueous BaTiO
3
precursor solution, with a particular focus
on the structures and role of intermediate phases forming prior to
BaTiO
3
nucleation.
In situ
infrared spectroscopy,
in situ
X-ray total scattering, and transmission electron
microscopy were used to reveal the decomposition, pyrolysis, and crystallization
reactions occurring during thermal processing. Our results show that
the intermediate phases consist of nanosized calcite-like BaCO
3
and BaTi
4
O
9
phases and that the intimate
mixing of these along with their metastability ensures complete decomposition
to form BaTiO
3
above 600 °C. We demonstrate that the
stability of the intermediate phases is dependent on the processing
atmosphere, where especially enhanced CO
2
levels is detrimental
for the formation of phase pure BaTiO
3
.