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From Micro to Nano: A Toolbox for Tuning Crystal Size and Morphology of Benzotriazolate-Based Metal–Organic Frameworks

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Chair of Solid State and Materials Chemistry, Institute of Physics, University of Augsburg, Universitaetsstrasse 1, D-86159 Augsburg, Germany
*(H.B.) E-mail: [email protected]
*(D.V.) E-mail: [email protected]
Cite this: Cryst. Growth Des. 2016, 16, 6, 3190–3197
Publication Date (Web):April 29, 2016
https://doi.org/10.1021/acs.cgd.6b00038
Copyright © 2016 American Chemical Society

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    Abstract

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    Scaling down the size of metal–organic framework (MOF) particles is a challenging but important task for extending the spectrum of potential MOF applications. Herein, we describe downsizing particles of MFU-4, a benzobistriazolate-based Zn(II)-MOF, which can be prepared by either solvothermal or microwave-assisted synthesis. We report on combining various synthetic strategies leading to a production of nanosized MOF crystals of well-defined sizes and shape. Our approaches include varying reaction time, temperature, solvent choice, and amount of additives (alkali hydroxides or selected amines) in order to gain control over the nucleation process. As a result, the crystal sizes can be tuned over a broad range, from 40 nm large globular particles up to 5 μm cubic crystals with narrow size distributions. Additionally, the article offers a comparison of different techniques used to determine the particle size of crystals. These include dynamic light scattering, X-ray powder diffraction (from Scherrer equation), and transmission electron microscopy.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.cgd.6b00038.

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    CCDC 1440258 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, or by emailing [email protected], or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033.

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