Exploiting in situ NMR spectroscopy to understand non-traditional methods for zeolite synthesis

Nicole L. Kelly; Emma A. L. Borthwick; Gaynor B. Lawrence; Paul S. Wheatley; Colan E. Hughes; Kenneth D. M. Harris; Russell E. Morris; Sharon E. Ashbrook

doi:10.1039/D4SC07931K

Exploiting in situ NMR spectroscopy to understand non-traditional methods for zeolite synthesis

Nicole L. Kelly, Emma A. L. Borthwick, Gaynor B. Lawrence, Paul S. Wheatley, Colan E. Hughes, Kenneth D. M. Harris^*, Russell E. Morris^*, Sharon E. Ashbrook^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

Abstract

Zeolite-formation mechanisms have long been the subject of intensive study, with most work concentrating on hydrothermal mechanisms. However, non-traditional zeolite syntheses that do not rely on hydrothermal crystallisation have provided a number of new routes to interesting and unexpected new materials, but their formation mechanisms remain poorly understood. Here, we show how simultaneous in situ liquid- and solid-state ²⁹Si NMR spectroscopy can reveal the mechanism of the formation of a zeolite from a layered silicate precursor. The study provides evidence for the species that are intercalated into the layered material and establishes those that are involved in building the inter-layer, zeolitic connections as a function of time during the zeolite formation process.

Original language	English
Number of pages	11
Journal	Chemical Science
Volume	Advance Article
Early online date	6 Feb 2025
DOIs	https://doi.org/10.1039/D4SC07931K
Publication status	E-pub ahead of print - 6 Feb 2025

Access to Document

10.1039/D4SC07931KLicence: CC BY

Kelly_2025_CS_Exploiting-NMR-spectroscopy-zeolite-synthesis_CC
© 2025 The Authors. This article is licensed under a Creative Commons Attribution 3.0 Unported Licence (https://creativecommons.org/licenses/by/3.0/).
Final published version, 2.15 MBLicence: CC BY

1 Active
3 Finished

ZeoMOFs: ZeoMOFS
Morris, R. E. (PI) & Ashbrook, S. E. (CoI)
EPSRC
1/10/22 → 30/09/25
Project: Standard
Light Element Analysis Facility (LEAF): Light Element Analysis Facility (LEAF)
Irvine, J. T. S. (PI), Baker, R. (CoI) & Miller, D. N. (CoI)
EPSRC
5/04/20 → 4/04/23
Project: Standard
H2020 ERC Advanced Grant 2017 ADOR: H2020 ERC Advanced Grant 2017 ADOR
Morris, R. E. (PI)
European Research Council
1/10/18 → 30/09/23
Project: Fellowship

Exploiting In Situ NMR Spectroscopy to Understand Non-Traditional Methods for Zeolite Synthesis (dataset)
Kelly, N. (Creator), Borthwick, E. A. L. (Creator), Lawrence, G. (Creator), Wheatley, P. S. (Creator), Hughes, C. E. (Creator), Harris, K. D. M. (Creator), Morris, R. E. (Creator) & Ashbrook, S. E. (Creator), University of St Andrews, 19 Feb 2025
DOI: 10.17630/4d38d0ea-6238-4ae8-9055-ed92a03979c6
Dataset

File

Cite this

@article{e41cd6a9156d4e8a8a3c8ce827a9bd92,

title = "Exploiting in situ NMR spectroscopy to understand non-traditional methods for zeolite synthesis",

abstract = "Zeolite-formation mechanisms have long been the subject of intensive study, with most work concentrating on hydrothermal mechanisms. However, non-traditional zeolite syntheses that do not rely on hydrothermal crystallisation have provided a number of new routes to interesting and unexpected new materials, but their formation mechanisms remain poorly understood. Here, we show how simultaneous in situ liquid- and solid-state 29Si NMR spectroscopy can reveal the mechanism of the formation of a zeolite from a layered silicate precursor. The study provides evidence for the species that are intercalated into the layered material and establishes those that are involved in building the inter-layer, zeolitic connections as a function of time during the zeolite formation process.",

author = "Kelly, {Nicole L.} and Borthwick, {Emma A. L.} and Lawrence, {Gaynor B.} and Wheatley, {Paul S.} and Hughes, {Colan E.} and Harris, {Kenneth D. M.} and Morris, {Russell E.} and Ashbrook, {Sharon E.}",

note = "Funding: This research was funded by the European Research Council under Advanced Grant 787073 and by the UKRI (EPSRC) under grant number EP/W034824/1. The authors would like to thank the Allan Handsel Postgraduate Research Scholarship for Chemistry for studentship funding for E. A. L. B. The UK High-Field Solid-State NMR Facility used in this research was funded by EPSRC and BBSRC (EP/T015063/1), in addition to (for results at 850 MHz) the University of Warwick including via part funding through Birmingham Science City Advanced Materials Projects 1 and 2 supported by Advantage West Midlands (AWM) and the European Regional Development Fund (ERDF). Collaborative assistance from the Facility Manager Team (Dinu Iuga and Trent Franks, University of Warwick) is acknowledged. We also gratefully acknowledge funding from the EPSRC for microscopy through grant numbers EP/L017008/1, EP/R023751/1 and EP/T019298/1.",

year = "2025",

month = feb,

day = "6",

doi = "10.1039/D4SC07931K",

language = "English",

volume = "Advance Article",

journal = "Chemical Science",

issn = "2041-6520",

publisher = "Royal Society of Chemistry",

}

TY - JOUR

T1 - Exploiting in situ NMR spectroscopy to understand non-traditional methods for zeolite synthesis

AU - Kelly, Nicole L.

AU - Borthwick, Emma A. L.

AU - Lawrence, Gaynor B.

AU - Wheatley, Paul S.

AU - Hughes, Colan E.

AU - Harris, Kenneth D. M.

AU - Morris, Russell E.

AU - Ashbrook, Sharon E.

N1 - Funding: This research was funded by the European Research Council under Advanced Grant 787073 and by the UKRI (EPSRC) under grant number EP/W034824/1. The authors would like to thank the Allan Handsel Postgraduate Research Scholarship for Chemistry for studentship funding for E. A. L. B. The UK High-Field Solid-State NMR Facility used in this research was funded by EPSRC and BBSRC (EP/T015063/1), in addition to (for results at 850 MHz) the University of Warwick including via part funding through Birmingham Science City Advanced Materials Projects 1 and 2 supported by Advantage West Midlands (AWM) and the European Regional Development Fund (ERDF). Collaborative assistance from the Facility Manager Team (Dinu Iuga and Trent Franks, University of Warwick) is acknowledged. We also gratefully acknowledge funding from the EPSRC for microscopy through grant numbers EP/L017008/1, EP/R023751/1 and EP/T019298/1.

PY - 2025/2/6

Y1 - 2025/2/6

N2 - Zeolite-formation mechanisms have long been the subject of intensive study, with most work concentrating on hydrothermal mechanisms. However, non-traditional zeolite syntheses that do not rely on hydrothermal crystallisation have provided a number of new routes to interesting and unexpected new materials, but their formation mechanisms remain poorly understood. Here, we show how simultaneous in situ liquid- and solid-state 29Si NMR spectroscopy can reveal the mechanism of the formation of a zeolite from a layered silicate precursor. The study provides evidence for the species that are intercalated into the layered material and establishes those that are involved in building the inter-layer, zeolitic connections as a function of time during the zeolite formation process.

AB - Zeolite-formation mechanisms have long been the subject of intensive study, with most work concentrating on hydrothermal mechanisms. However, non-traditional zeolite syntheses that do not rely on hydrothermal crystallisation have provided a number of new routes to interesting and unexpected new materials, but their formation mechanisms remain poorly understood. Here, we show how simultaneous in situ liquid- and solid-state 29Si NMR spectroscopy can reveal the mechanism of the formation of a zeolite from a layered silicate precursor. The study provides evidence for the species that are intercalated into the layered material and establishes those that are involved in building the inter-layer, zeolitic connections as a function of time during the zeolite formation process.

U2 - 10.1039/D4SC07931K

DO - 10.1039/D4SC07931K

M3 - Article

SN - 2041-6520

VL - Advance Article

JO - Chemical Science

JF - Chemical Science

ER -

Exploiting in situ NMR spectroscopy to understand non-traditional methods for zeolite synthesis

Abstract

Access to Document

Fingerprint

Projects

ZeoMOFs: ZeoMOFS

Light Element Analysis Facility (LEAF): Light Element Analysis Facility (LEAF)

H2020 ERC Advanced Grant 2017 ADOR: H2020 ERC Advanced Grant 2017 ADOR

Datasets

Exploiting In Situ NMR Spectroscopy to Understand Non-Traditional Methods for Zeolite Synthesis (dataset)

Cite this