Correlative chemical and structural nanocharacterization of a pseudo-binary 0.75Bi(Fe0.97Ti0.03)O3–0.25BaTiO3 ceramic

McCartan, S. J., Calisir, I., Paterson, G. W. , Webster, R. W.H., Macgregor, T. A., Hall, D. A. and MacLaren, I. (2021) Correlative chemical and structural nanocharacterization of a pseudo-binary 0.75Bi(Fe0.97Ti0.03)O3–0.25BaTiO3 ceramic. Journal of the American Ceramic Society, 104(5), pp. 2388-2397. (doi: 10.1111/jace.17599)

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Abstract

Fast‐cooling after sintering or annealing of BiFeO3‐BaTiO3 mixed oxide ceramics yields core‐shell structures that give excellent functional properties, but their precise phase assemblage and nanostructure remains an open question. By comparing conventional electron energy loss spectroscopy (EELS) with scanning precession electron diffraction (SPED) mapping using a direct electron detector, we correlate chemical composition with the presence or absence of octahedral tilting and with changes in lattice parameters. This reveals that some grains have a 3‐phase assemblage of a BaTiO3‐rich pseudocubic shell; a BiFeO3‐rich outer core with octahedral tilting consistent with an R3c structure; and an inner core richer in Ba and even poorer in Ti, which seems to show a pseudocubic structure of slightly smaller lattice parameter than the shell region. This last structure has not been previously identified in these materials, but the composition and structure fit with previous studies. These inner cores are likely to be non‐polar and play no part in the ferroelectric properties. Nevertheless, the combination of EELS and SPED clearly provides a novel way to examine heterogeneous microstructures with high spatial resolution, thus revealing the presence of phases that may be too subtle to detect with more conventional techniques.

Item Type:Articles
Additional Information:S.J.M would like to acknowledge the CDT in Photonic Integration and Advanced Data Storage (PIADS) for the funding of his PhD through the EPSRC grant (EP/L015323/1). We gratefully acknowledge funding from EPSRC which has supported the development of the detector (through “Fast Pixel Detectors: a paradigm shift in STEM imaging” (EP/M009963/1) and Impact Acceleration Accounts (EP/K503903/1 and EP/R511705/1)). Funding from EPSRC (EP/R511705/1) and NanoMEGAS supported integration of the Merlin for EM detector with the ASTAR system.
Status:Published
Refereed:Yes
Glasgow Author(s) Enlighten ID:Macgregor, Mr Thomas and Paterson, Dr Gary and Webster, Mr Robert and MacLaren, Dr Ian
Authors: McCartan, S. J., Calisir, I., Paterson, G. W., Webster, R. W.H., Macgregor, T. A., Hall, D. A., and MacLaren, I.
College/School:College of Science and Engineering > School of Physics and Astronomy
Journal Name:Journal of the American Ceramic Society
Publisher:Wiley
ISSN:0002-7820
ISSN (Online):1551-2916
Published Online:02 December 2020
Copyright Holders:Copyright © 2020 The Authors
First Published:First published in Journal of the American Ceramic Society 104(5): 2388-2397
Publisher Policy:Reproduced under a Creative Commons License

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Project CodeAward NoProject NamePrincipal InvestigatorFunder's NameFunder RefLead Dept
172610External engagement manager: CDT Photonic Integration for Advanced Data StorageJohn MarshEngineering and Physical Sciences Research Council (EPSRC)EP/L015323/1ENG - Electronics & Nanoscale Engineering
171131Fast Pixel Detectors: a paradigm shift in STEM imagingIan MacLarenEngineering and Physical Sciences Research Council (EPSRC)EP/M009963/1P&S - Physics & Astronomy
190531Impact Acceleration Account (IAA - EPSRC)Jonathan CooperEngineering and Physical Sciences Research Council (EPSRC)EP/K503903/1Research and Innovation Services
304896EPSRC-IAA: Early Stage Commercialisation of a PET Imaging Agent for the Detection of Cardiovascular Disease and CancerAndrew SutherlandEngineering and Physical Sciences Research Council (EPSRC)EP/R511705/1Chemistry
304896EPSRC-IAA: Early Stage Commercialisation of a PET Imaging Agent for the Detection of Cardiovascular Disease and CancerAndrew SutherlandEngineering and Physical Sciences Research Council (EPSRC)EP/R511705/1Chemistry