Griffin, S., Briuglia, M. L., ter Horst, J. H. and Forgan, R. S. (2020) Assessing crystallisation kinetics of Zr metal-organic frameworks through turbidity measurements to inform rapid microwave-assisted synthesis. Chemistry: A European Journal, 26(30), pp. 6910-6918. (doi: 10.1002/chem.202000993) (PMID:32227534) (PMCID:PMC7318326)
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Abstract
Controlling the crystallisation of metal‐organic frameworks (MOFs), network solids of metal ions or clusters connected by organic ligands, is often hindered by the significant number of synthetic variables inherent to their synthesis. Coordination modulation, the addition of monotopic competing ligands to solvothermal syntheses, can allow tuning of physical properties (particle size, porosity, surface chemistry), enhance crystallinity, and select desired phases, by modifying the kinetics of self‐assembly, but its mechanism(s) are poorly understood. Herein, we use turbidity measurements to assess the effects of modulation on the solvothermal synthesis of the prototypical Zr terephthalate MOF UiO‐66 and apply the knowledge gained to its rapid microwave synthesis. The studied experimental parameters ‐ temperature, reagent concentration, reagent aging, metal precursor, water content, and modulator addition ‐ all influence the time taken for onset of nucleation, and subsequently allow microwave synthesis of UiO‐66 in as little as one minute. The simple, low cost turbidity measurements align closely with previously reported in situ synchrotron X‐ray diffraction studies, proving their simplicity and utility for probing the nucleation of complex materials while offering significant insights to the synthetic chemist.
| Item Type: | Articles |
|---|---|
| Status: | Published |
| Refereed: | Yes |
| Glasgow Author(s) Enlighten ID: | Griffin, Sarah and Forgan, Professor Ross |
| Authors: | Griffin, S., Briuglia, M. L., ter Horst, J. H., and Forgan, R. S. |
| College/School: | College of Science and Engineering > School of Chemistry |
| Journal Name: | Chemistry: A European Journal |
| Publisher: | Wiley |
| ISSN: | 0947-6539 |
| ISSN (Online): | 1521-3765 |
| Published Online: | 30 March 2020 |
| Copyright Holders: | Copyright © 2020 The Authors |
| First Published: | First published in Chemistry: A European Journal 26(30): 6910-6918 |
| Publisher Policy: | Reproduced under a Creative Commons License |
| Data DOI: | 10.5525/gla.researchdata.996 |
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