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Comprehensive Solid-State Characterization of Rare Earth Flouride Nanoparticles

Lucier, Bryan E.G.; Johnston, Karen E.; Arnold, Donna C.; Lemyre, Jean-Luc; Beaupré, Ariane; Blanchette, Maxime; Ritcey, Anna M.; Schurko, Robert W.

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Bryan E.G. Lucier

Donna C. Arnold

Jean-Luc Lemyre

Ariane Beaupré

Maxime Blanchette

Anna M. Ritcey

Robert W. Schurko


The combination of multinuclear solid-state NMR spectroscopy and powder X-ray diffraction has been applied to characterize the octahedron-shaped crystalline nanoparticle products resulting from an inverse micelle synthesis. Rietveld refinements of the powder X-ray diffraction data from the nanoparticles revealed their general formula to be (H3O)Y3F10·xH2O. 1H magic-angle spinning (MAS) NMR experiments provided information on sample purity and served as an excellent probe of the zeolithic incorporation of atmospheric water. 19F MAS NMR experiments on a series of monodisperse nanoparticle samples of various sizes yielded spectra featuring three unique 19F resonances arising from three different fluorine sites within the (H3O)Y3F10·xH2O crystal structure. Partial removal of zeolithic water from the internal cavities and tunnels of the nanoparticles led to changes in the integrated peak intensities in the 19F MAS NMR spectra; the origin of this behavior is discussed in terms of 19F longitudinal relaxation. 19F–89Y variable-amplitude cross-polarization (VACP) NMR experiments on both stationary samples and samples under MAS conditions indicated that two distinct yttrium environments are present, and on the basis of the relative peak intensities, the population of one of the two sites is closely linked to the nanoparticle size. Both 19F MAS and 19F–89Y VACP/MAS experiments indicated small amounts of an impurity present in certain nanoparticles; these are postulated to be spherical amorphous YF3 nanoparticles. We discuss the importance of probing molecular-level structure in addition to microscopic structure and how the combination of these characterization methods is crucial for understanding nanoparticle design, synthesis, and application.


Lucier, B. E., Johnston, K. E., Arnold, D. C., Lemyre, J., Beaupré, A., Blanchette, M., …Schurko, R. W. (2013). Comprehensive Solid-State Characterization of Rare Earth Flouride Nanoparticles. Journal of Physical Chemistry C, 118(2), 1213-1228.

Journal Article Type Article
Acceptance Date Aug 14, 2013
Online Publication Date Nov 18, 2013
Publication Date Nov 18, 2013
Deposit Date Sep 30, 2016
Publicly Available Date Aug 28, 2018
Journal Journal of Physical Chemistry C
Print ISSN 1932-7447
Electronic ISSN 1932-7455
Publisher American Chemical Society
Peer Reviewed Peer Reviewed
Volume 118
Issue 2
Pages 1213-1228


Accepted Journal Article (4 Mb)

Copyright Statement
This document is the Accepted Manuscript version of a Published Work that appeared in final form in Journal of physical chemistry C copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see

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