In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis

Samantha E. Russell; Susan E. Henkelis; Simon M. Vornholt; Daniel N. Rainer; Karena W.  Chapman; Russell E. Morris

doi:10.1039/d1ma00335f

In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis

Samantha E. Russell, Susan E. Henkelis, Simon M. Vornholt, Daniel N. Rainer, Karena W. Chapman, Russell E. Morris

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Abstract

The assembly–disassembly–organisation–reassembly (ADOR) process is an important tool to access zeolite structures that are otherwise unfeasible via hydrothermal methods. In situ flow pair distribution function (PDF) analysis has been used to probe the mechanism of the disassembly and organisation steps, with the disassembly a rapid step that is often difficult to capture. Zeolite UTL was hydrolysed by 6 M hydrochloric acid, with PDF measurements used to monitor framework alterations as the reaction proceeded. The resulting disassembly mechanism shows an initial rapid removal of germanium from the germanium-rich double 4 rings (d4r), followed by silicon rearrangement and gradual silanol condensation to form IPC-2P.

Original language	English
Number of pages	7
Journal	Materials Advances
Volume	Advance Article
Early online date	13 Oct 2021
DOIs	https://doi.org/10.1039/d1ma00335f
Publication status	E-pub ahead of print - 13 Oct 2021

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10.1039/d1ma00335fLicence: CC BY

Russell_2021_MatAdv_In-situ-glow-pair-distribution_CC
Copyright © 2021 The Author(s). This Open Access Article is licensed under a Creative Commons Attribution 3.0 Unported Licence.
Final published version, 5.3 MBLicence: CC BY

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
Advanced Photon Source, PDF measurements at beamline 11-ID-B
Russell, S. E. (PI) & Henkelis, S. E. (Researcher)
15/06/18 → 18/06/18
Project: Standard
Hemilabile switchable metal-organic: Hemilabile and switchable metal-organic frameworks
Morris, R. E. (PI)
EPSRC
1/03/13 → 28/02/16
Project: Standard

In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis (dataset)
Russell, S. E. (Creator), Henkelis, S. E. (Creator), Vornholt, S. M. (Creator), Rainer, D. N. (Creator), Chapman, K. (Creator) & Morris, R. E. (Creator), University of St Andrews, 19 Nov 2021
DOI: 10.17630/11c13889-77d8-471c-83e1-b65af6026042
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title = "In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis",

abstract = "The assembly–disassembly–organisation–reassembly (ADOR) process is an important tool to access zeolite structures that are otherwise unfeasible via hydrothermal methods. In situ flow pair distribution function (PDF) analysis has been used to probe the mechanism of the disassembly and organisation steps, with the disassembly a rapid step that is often difficult to capture. Zeolite UTL was hydrolysed by 6 M hydrochloric acid, with PDF measurements used to monitor framework alterations as the reaction proceeded. The resulting disassembly mechanism shows an initial rapid removal of germanium from the germanium-rich double 4 rings (d4r), followed by silicon rearrangement and gradual silanol condensation to form IPC-2P.",

author = "Russell, {Samantha E.} and Henkelis, {Susan E.} and Vornholt, {Simon M.} and Rainer, {Daniel N.} and Chapman, {Karena W.} and Morris, {Russell E.}",

note = "The authors S. E. R., S. M. V., and R. E. M. would like to thank the European Research Council for funding opportunities under the Advanced Grant 787073. S. E. H., S. M. V. and D. N. R. would like to thank the EPSRC for funding (EP/K503162/1) (EP/K005499/1) (EP/N509759/1). R. E. M. further acknowledges the OP VVV “Excellent Research Teams” grant under project no. CZ.02.1.01/0.0/0.0/15_003/0000417 – CUCAM. ",

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T1 - In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis

AU - Russell, Samantha E.

AU - Henkelis, Susan E.

AU - Vornholt, Simon M.

AU - Rainer, Daniel N.

AU - Chapman, Karena W.

AU - Morris, Russell E.

N1 - The authors S. E. R., S. M. V., and R. E. M. would like to thank the European Research Council for funding opportunities under the Advanced Grant 787073. S. E. H., S. M. V. and D. N. R. would like to thank the EPSRC for funding (EP/K503162/1) (EP/K005499/1) (EP/N509759/1). R. E. M. further acknowledges the OP VVV “Excellent Research Teams” grant under project no. CZ.02.1.01/0.0/0.0/15_003/0000417 – CUCAM.

PY - 2021/10/13

Y1 - 2021/10/13

N2 - The assembly–disassembly–organisation–reassembly (ADOR) process is an important tool to access zeolite structures that are otherwise unfeasible via hydrothermal methods. In situ flow pair distribution function (PDF) analysis has been used to probe the mechanism of the disassembly and organisation steps, with the disassembly a rapid step that is often difficult to capture. Zeolite UTL was hydrolysed by 6 M hydrochloric acid, with PDF measurements used to monitor framework alterations as the reaction proceeded. The resulting disassembly mechanism shows an initial rapid removal of germanium from the germanium-rich double 4 rings (d4r), followed by silicon rearrangement and gradual silanol condensation to form IPC-2P.

AB - The assembly–disassembly–organisation–reassembly (ADOR) process is an important tool to access zeolite structures that are otherwise unfeasible via hydrothermal methods. In situ flow pair distribution function (PDF) analysis has been used to probe the mechanism of the disassembly and organisation steps, with the disassembly a rapid step that is often difficult to capture. Zeolite UTL was hydrolysed by 6 M hydrochloric acid, with PDF measurements used to monitor framework alterations as the reaction proceeded. The resulting disassembly mechanism shows an initial rapid removal of germanium from the germanium-rich double 4 rings (d4r), followed by silicon rearrangement and gradual silanol condensation to form IPC-2P.

U2 - 10.1039/d1ma00335f

DO - 10.1039/d1ma00335f

M3 - Article

SN - 2633-5409

VL - Advance Article

JO - Materials Advances

JF - Materials Advances

ER -

In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis

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Projects

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

Advanced Photon Source, PDF measurements at beamline 11-ID-B

Hemilabile switchable metal-organic: Hemilabile and switchable metal-organic frameworks

Datasets

In situ flow pair distribution function analysis to probe the assembly-disassembly-organisation-reassembly (ADOR) mechanism of zeolite IPC-2 synthesis (dataset)

Cite this