In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

Samuel A. Morris; Giulia P. M. Bignami; Yuyang Tian; Marta Navarro-Rojas; Daniel S. Firth; Jiri Cejka; Paul S. Wheatley; Daniel M. Dawson; Wojciech A. Slawinski; David S. Wragg; Russell E. Morris; Sharon E. Ashbrook

doi:10.1038/nchem.2761

In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

Samuel A. Morris, Giulia P. M. Bignami, Yuyang Tian, Marta Navarro-Rojas, Daniel S. Firth, Jiri Cejka, Paul S. Wheatley, Daniel M. Dawson, Wojciech A. Slawinski, David S. Wragg, Russell E. Morris, Sharon E. Ashbrook

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Abstract

The assembly–disassembly–organization–reassembly (ADOR) mechanism is a recent method for preparing inorganic framework materials and, in particular, zeolites. This flexible approach has enabled the synthesis of isoreticular families of zeolites with unprecedented continuous control over porosity, and the design and preparation of materials that would have been difficult—or even impossible—to obtain using traditional hydrothermal techniques. Applying the ADOR process to a parent zeolite with the UTL framework topology, for example, has led to six previously unknown zeolites (named IPC-n, where n = 2, 4, 6, 7, 9 and 10). To realize the full potential of the ADOR method, however, a further understanding of the complex mechanism at play is needed. Here, we probe the disassembly, organization and reassembly steps of the ADOR process through a combination of in situ solid-state NMR spectroscopy and powder X-ray diffraction experiments. We further use the insight gained to explain the formation of the unusual structure of zeolite IPC-6.

Original language	English
Pages (from-to)	1012-1018
Number of pages	7
Journal	Nature Chemistry
Volume	9
Issue number	10
Early online date	17 Apr 2017
DOIs	https://doi.org/10.1038/nchem.2761
Publication status	Published - Oct 2017

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Morris_insitu_IPC6_AAM
© 2017 the Authors. This work has been made available online in accordance with the publisher’s policies. This is the author created, accepted version manuscript following peer review and may differ slightly from the final published version. The final published version of this work is available at: https://doi.org/10.1038/nchem.2761
Accepted author manuscript, 6.07 MB

EXONMR: EU FP7 Consolidator 2013 EXONMR
Ashbrook, S. E. (PI)
European Research Council
1/04/14 → 30/09/19
Project: Standard
Nanoparticle: Nanoparticle Approaches to Zeolitic Catalysts
Morris, R. E. (PI)
EPSRC
15/01/14 → 2/08/15
Project: Standard
Assembly Disassembly Reassembly: Assembly disassembly reassembly - New routes to extended structures and their impact
Morris, R. E. (PI)
EPSRC
1/08/13 → 31/07/18
Project: Fellowship

Sharon E. Ashbrook
- semast-andrews.acuk
- School of Chemistry - Deputy Head of School, Professor
- EaSTCHEM
Person: Academic

Data underpinning "In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6"
Morris, S. A. (Creator), Bignami, G. P. M. (Creator), Tian, Y. (Creator), Navarro-Rojas, M. (Creator), Firth, D. S. (Creator), Cejka, J. (Creator), Wheatley, P. S. (Creator), Dawson, D. M. (Creator), Slawinski, W. A. (Creator), Wragg, D. S. (Creator), Morris, R. E. (Creator) & Ashbrook, S. E. M. (Creator), University of St Andrews, 10 Nov 2017
DOI: 10.17630/47861a6e-f7c4-466e-9108-d4adb104f74d
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@article{53f7b71eb4314707b363464539b46ded,

title = "In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6",

abstract = "The assembly–disassembly–organization–reassembly (ADOR) mechanism is a recent method for preparing inorganic framework materials and, in particular, zeolites. This flexible approach has enabled the synthesis of isoreticular families of zeolites with unprecedented continuous control over porosity, and the design and preparation of materials that would have been difficult—or even impossible—to obtain using traditional hydrothermal techniques. Applying the ADOR process to a parent zeolite with the UTL framework topology, for example, has led to six previously unknown zeolites (named IPC-n, where n = 2, 4, 6, 7, 9 and 10). To realize the full potential of the ADOR method, however, a further understanding of the complex mechanism at play is needed. Here, we probe the disassembly, organization and reassembly steps of the ADOR process through a combination of in situ solid-state NMR spectroscopy and powder X-ray diffraction experiments. We further use the insight gained to explain the formation of the unusual structure of zeolite IPC-6.",

author = "Morris, {Samuel A.} and Bignami, {Giulia P. M.} and Yuyang Tian and Marta Navarro-Rojas and Firth, {Daniel S.} and Jiri Cejka and Wheatley, {Paul S.} and Dawson, {Daniel M.} and Slawinski, {Wojciech A.} and Wragg, {David S.} and Morris, {Russell E.} and Ashbrook, {Sharon E.}",

note = "R.E.M. and M.N. thank the Royal Society and the E.P.S.R.C. (Grants EP/L014475/1, EP/K025112/1 and EP/K005499/1) for funding work in this area. R.E.M. and J.{\v C}. acknowledge the Czech Science Foundation for the project P106/12/G015 and OP VVV {"}Excellent Research Teams{"}, project No. CZ.02.1.01/0.0/0.0/15_003/0000417 - CUCAM. S.E.A. would like to thank the ERC (EU FP7 Consolidator Grant 614290 “EXONMR”) and the Royal Society and Wolfson Foundation for a merit award. The UK 850 MHz solid-state NMR Facility used in this research was funded by EPSRC and BBSRC (contract reference PR140003), as well as 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). W.A.S. and D.S.W. acknowledge the Research Council of Norway and NOTUR are acknowledged for providing the computer time at the Norwegian supercomputer facilities (under the project number NN2875k).",

year = "2017",

month = oct,

doi = "10.1038/nchem.2761",

language = "English",

volume = "9",

pages = "1012--1018",

journal = "Nature Chemistry",

issn = "1755-4330",

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TY - JOUR

T1 - In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

AU - Morris, Samuel A.

AU - Bignami, Giulia P. M.

AU - Tian, Yuyang

AU - Navarro-Rojas, Marta

AU - Firth, Daniel S.

AU - Cejka, Jiri

AU - Wheatley, Paul S.

AU - Dawson, Daniel M.

AU - Slawinski, Wojciech A.

AU - Wragg, David S.

AU - Morris, Russell E.

AU - Ashbrook, Sharon E.

N1 - R.E.M. and M.N. thank the Royal Society and the E.P.S.R.C. (Grants EP/L014475/1, EP/K025112/1 and EP/K005499/1) for funding work in this area. R.E.M. and J.Č. acknowledge the Czech Science Foundation for the project P106/12/G015 and OP VVV "Excellent Research Teams", project No. CZ.02.1.01/0.0/0.0/15_003/0000417 - CUCAM. S.E.A. would like to thank the ERC (EU FP7 Consolidator Grant 614290 “EXONMR”) and the Royal Society and Wolfson Foundation for a merit award. The UK 850 MHz solid-state NMR Facility used in this research was funded by EPSRC and BBSRC (contract reference PR140003), as well as 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). W.A.S. and D.S.W. acknowledge the Research Council of Norway and NOTUR are acknowledged for providing the computer time at the Norwegian supercomputer facilities (under the project number NN2875k).

PY - 2017/10

Y1 - 2017/10

N2 - The assembly–disassembly–organization–reassembly (ADOR) mechanism is a recent method for preparing inorganic framework materials and, in particular, zeolites. This flexible approach has enabled the synthesis of isoreticular families of zeolites with unprecedented continuous control over porosity, and the design and preparation of materials that would have been difficult—or even impossible—to obtain using traditional hydrothermal techniques. Applying the ADOR process to a parent zeolite with the UTL framework topology, for example, has led to six previously unknown zeolites (named IPC-n, where n = 2, 4, 6, 7, 9 and 10). To realize the full potential of the ADOR method, however, a further understanding of the complex mechanism at play is needed. Here, we probe the disassembly, organization and reassembly steps of the ADOR process through a combination of in situ solid-state NMR spectroscopy and powder X-ray diffraction experiments. We further use the insight gained to explain the formation of the unusual structure of zeolite IPC-6.

AB - The assembly–disassembly–organization–reassembly (ADOR) mechanism is a recent method for preparing inorganic framework materials and, in particular, zeolites. This flexible approach has enabled the synthesis of isoreticular families of zeolites with unprecedented continuous control over porosity, and the design and preparation of materials that would have been difficult—or even impossible—to obtain using traditional hydrothermal techniques. Applying the ADOR process to a parent zeolite with the UTL framework topology, for example, has led to six previously unknown zeolites (named IPC-n, where n = 2, 4, 6, 7, 9 and 10). To realize the full potential of the ADOR method, however, a further understanding of the complex mechanism at play is needed. Here, we probe the disassembly, organization and reassembly steps of the ADOR process through a combination of in situ solid-state NMR spectroscopy and powder X-ray diffraction experiments. We further use the insight gained to explain the formation of the unusual structure of zeolite IPC-6.

U2 - 10.1038/nchem.2761

DO - 10.1038/nchem.2761

M3 - Article

SN - 1755-4330

VL - 9

SP - 1012

EP - 1018

JO - Nature Chemistry

JF - Nature Chemistry

IS - 10

ER -

In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

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Projects

EXONMR: EU FP7 Consolidator 2013 EXONMR

Nanoparticle: Nanoparticle Approaches to Zeolitic Catalysts

Assembly Disassembly Reassembly: Assembly disassembly reassembly - New routes to extended structures and their impact

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Sharon E. Ashbrook

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Data underpinning "In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6"

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