Grendal, O.G.; Blichfeld, A.B.; Skjærvø, S.L.; van Beek, W.; Selbach, S.M.; Grande, T.; Einarsrud, M.-A. Facile Low Temperature Hydrothermal Synthesis of BaTiO3 Nanoparticles Studied by In Situ X-ray Diffraction. Crystals2018, 8, 253.
Grendal, O.G.; Blichfeld, A.B.; Skjærvø, S.L.; van Beek, W.; Selbach, S.M.; Grande, T.; Einarsrud, M.-A. Facile Low Temperature Hydrothermal Synthesis of BaTiO3 Nanoparticles Studied by In Situ X-ray Diffraction. Crystals 2018, 8, 253.
Ferroelectric materials are crucial for today’s technological society, and nanostructured ferroelectric materials are important for downscaling of devices. Controlled and reproducible synthesis of these materials are therefore of immense importance. Hydrothermal synthesis is a well-established synthesis route, with a large parameter space for optimization, but a better understanding of nucleation and growth mechanisms is needed for full utilization and control. Here we use in situ X-ray diffraction to follow the nucleation and growth of BaTiO3 formed by hydrothermal synthesis using two different titanium precursors, an amorphous titania precipitate slurry and a Ti-citric acid complex solution. Sequential Rietveld refinement was used to extract the time dependency of lattice parameters, crystallite size, strain and atomic displacement parameters. Phase pure BaTiO3 nanoparticles 10 - 15 nm in size were successfully synthesized at different temperatures (100, 125, and 150 °C) from both precursors after reaction times ranging from a few seconds, to several hours. The two precursors resulted in phase pure BaTiO3 with similar final crystallite size. Finally, two different growth mechanisms were revealed, where the effect of surfactants present during hydrothermal synthesis is discussed as one of the key parameters.
BaTiO3; hydrothermal synthesis; in situ; X-ray diffraction; nanoparticles
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