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Exploiting in-situ NMR to monitor the formation of a metal-organic framework

DOI: 10.1039/D0SC04892E DOI Help

Authors: Corey L. Jones (Cardiff University) , Colan E. Hughes (Cardiff University) , Hamish H.-m. Yeung (NIMS) , Alison Paul (Cardiff University) , Kenneth D. M. Harris (Cardiff University) , Timothy L. Easun (University of Nottingham)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Chemical Science

State: Published (Approved)
Published: November 2020
Diamond Proposal Number(s): 16450

Open Access Open Access

Abstract: The formation processes of metal–organic frameworks are becoming more widely researched using in situ techniques, although there remains a scarcity of NMR studies in this field. In this work, the synthesis of framework MFM-500(Ni) has been investigated using an in situ NMR strategy that provides information on the time-evolution of the reaction and crystallization process. In our in situ NMR study of MFM-500(Ni) formation, liquid-phase 1H NMR data recorded as a function of time at fixed temperatures (between 60 and 100 °C) afford qualitative information on the solution-phase processes and quantitative information on the kinetics of crystallization, allowing the activation energies for nucleation (61.4 ± 9.7 kJ mol−1) and growth (72.9 ± 8.6 kJ mol−1) to be determined. Ex situ small-angle X-ray scattering studies (at 80 °C) provide complementary nanoscale information on the rapid self-assembly prior to MOF crystallization and in situ powder X-ray diffraction confirms that the only crystalline phase present during the reaction (at 90 °C) is phase-pure MFM-500(Ni). This work demonstrates that in situ NMR experiments can shed new light on MOF synthesis, opening up the technique to provide better understanding of how MOFs are formed.

Subject Areas: Chemistry, Materials

Instruments: I12-JEEP: Joint Engineering, Environmental and Processing


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