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Facile Low Temperature Hydrothermal Synthesis of BaTiO3 Nanoparticles Studied by In Situ X-ray Diffraction

1
Department of Materials Science and Engineering, NTNU Norwegian University of Science and Technology, 7491 Trondheim, Norway
2
Swiss-Norwegian Beamlines at European Synchrotron Research Facility, 38043 Grenoble, France
*
Author to whom correspondence should be addressed.
Crystals 2018, 8(6), 253; https://doi.org/10.3390/cryst8060253
Received: 30 April 2018 / Revised: 5 June 2018 / Accepted: 15 June 2018 / Published: 17 June 2018
(This article belongs to the Special Issue Synthesis, Properties and Applications of Metal Oxides Nanoparticles)
Ferroelectric materials are crucial for today’s technological society and nanostructured ferroelectric materials are important for the 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. View Full-Text
Keywords: BaTiO3; hydrothermal synthesis; in situ; X-ray diffraction; nanoparticles BaTiO3; hydrothermal synthesis; in situ; X-ray diffraction; nanoparticles
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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.

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