A Strategy for Probing the Evolution of Crystallization Processes by Low-Temperature Solid-State NMR and Dynamic Nuclear Polarization

Vioglio, Paolo Cerreia; Thureau, Pierre; Juramy, Marie; Ziarelli, Fabio; Viel, Stéphane; Williams, P. Andrew; Hughes, Colan E.; Harris, Kenneth D. M.; Mollica, Giulia

Abstract

Crystallization plays an important role in many areas, and to derive a fundamental understanding of crystallization processes, it is essential to understand the sequence of solid phases produced as a function of time. Here, we introduce a new NMR strategy for studying the time evolution of crystallization processes, in which the crystallizing system is quenched rapidly to low temperature at specific time points during crystallization. The crystallized phase present within the resultant “frozen solution” may be investigated in detail using a range of sophisticated NMR techniques. The low temperatures involved allow dynamic nuclear polarization (DNP) to be exploited to enhance the signal intensity in the solid-state NMR measurements, which is advantageous for detection and structural characterization of transient forms that are present only in small quantities. This work opens up the prospect of studying the very early stages of crystallization, at which the amount of solid phase present is intrinsically low.

Citation

Vioglio, P. C., Thureau, P., Juramy, M., Ziarelli, F., Viel, S., Williams, P. A., Hughes, C. E., Harris, K. D. M., & Mollica, G. (2019). A Strategy for Probing the Evolution of Crystallization Processes by Low-Temperature Solid-State NMR and Dynamic Nuclear Polarization. Journal of Physical Chemistry Letters, 10(7), 1505-1510. https://doi.org/10.1021/acs.jpclett.9b00306

• Journal Article Type: Article
• Acceptance Date: Mar 14, 2019
• Online Publication Date: Mar 14, 2019
• Publication Date: Apr 4, 2019
• Deposit Date: Nov 18, 2024
• Journal: The Journal of Physical Chemistry Letters
• Electronic ISSN: 1948-7185
• Publisher: American Chemical Society
• Peer Reviewed: Peer Reviewed
• Volume: 10
• Issue: 7
• Pages: 1505-1510
• DOI: https://doi.org/10.1021/acs.jpclett.9b00306
• Keywords: Amorphous materials, Crystallization, Nuclear magnetic resonance spectroscopy, Polarization, Solution chemistry
• Public URL: https://nottingham-repository.worktribe.com/output/41934175
• Publisher URL: https://pubs.acs.org/doi/10.1021/acs.jpclett.9b00306