Bismuth
layer-structured oxides with natural superlattices have
attracted great attention because of their fascinating functional
properties, such as ferroelectricity, ferromagnetism, multiferroicity,
etc., introduced by the abundant structural tunability and high doping
tolerance. To realize multifunctionalities, double or triple transition
ion intercalation is usually required, while large-size (>10 μm
in diameter) multi-transition-ion-intercalated single crystals with
spontaneous crystallization are not yet obtained so far. In this work,
tens of micron Fe-doped bismuth titanate single crystals have been
successfully synthesized for the first time by the differential-temperature
supercritical hydrothermal method. Bi4Fe
x
Ti3 – x
O12 – δ single crystals with a lateral
length of ∼40 μm and thickness of ∼4 μm
are the largest bulk single crystals for the Fe-doped bismuth layer-structured
oxide single crystals under spontaneous crystallization as reported
so far. Their growth mechanism is discussed, which involves dissolution,
mass transport, and recrystallization. In addition, the magnetic properties
of the supercritical hydrothermal method samples were also investigated.
This work sheds light on the feasibility to grow larger bismuth layer-structured
oxide single crystals containing multiple transition metal ions.