Insights to the formation of Zr-based metal–organic frameworks from in situ powder x-ray diffraction

Eja Petersen; Russell Matthew Main; Oxana Magdysyuk; Nicole Kelly; Emma Ann Lamont Borthwick; Aaron Benjamin Naden; Sharon E. Ashbrook; Russell Edward Morris; Romy  Ettlinger

doi:10.1088/2515-7639/ad9b4f

Insights to the formation of Zr-based metal–organic frameworks from in situ powder x-ray diffraction

Eja Petersen, Russell Matthew Main, Oxana Magdysyuk, Nicole Kelly, Emma Ann Lamont Borthwick, Aaron Benjamin Naden, Sharon E. Ashbrook, Russell Edward Morris, Romy Ettlinger^*

^*Corresponding author for this work

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

Abstract

This study sheds light on the kinetics of crystallisation of two Zr-based metal–organic frameworks (MOFs), namely Zr6-MOF-808 and Zr6-MOF-801, using in situ powder x-ray diffraction (PXRD). Once a room temperature synthesis for the two MOFs was designed for the very small scale, a successful series of in situ PXRD experiments over the range of 10 °C–40 °C yielded high quality quantitative information on the kinetics of crystallisation for both MOFs. These findings indicate the importance of the solubility of the linker and its connectivity: while the rate of nucleation and the resulting particle size of the MOF (Zr6-MOF-801), with the less soluble and lower connected linker, was strongly temperature dependent, the growth and particle size of Zr6-MOF-808 was hardly impacted by an increase in temperature. This work highlights the importance of careful preliminary research and helps to improve future MOF synthesis design to efficiently achieve the desired particle size distribution.

Original language	English
Article number	015006
Number of pages	9
Journal	Journal of Physics: Materials
Volume	8
Issue number	1
DOIs	https://doi.org/10.1088/2515-7639/ad9b4f
Publication status	Published - 17 Dec 2024

Keywords

Metal-organic framework
In situ powder x-ray diffraction
Crystallisation kinetics

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Petersen_2025_J._Phys._Mater._8_015006
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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

Insights to the formation of Zr-based metal-organic frameworks from in situ powder X-ray diffraction (dataset)
Petersen, E. E. (Creator), Main, R. M. (Creator), Magdysyuk, O. V. (Creator), Kelly, N. (Creator), Borthwick, E. A. L. (Creator), Naden, A. B. (Creator), Ashbrook, S. E. (Creator), Morris, R. E. (Creator) & Ettlinger, R. (Creator), University of St Andrews, 22 Jan 2025
DOI: 10.17630/15689b05-cd78-4f08-882d-bce6f7561380
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Cite this

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title = "Insights to the formation of Zr-based metal–organic frameworks from in situ powder x-ray diffraction",

abstract = "This study sheds light on the kinetics of crystallisation of two Zr-based metal–organic frameworks (MOFs), namely Zr6-MOF-808 and Zr6-MOF-801, using in situ powder x-ray diffraction (PXRD). Once a room temperature synthesis for the two MOFs was designed for the very small scale, a successful series of in situ PXRD experiments over the range of 10 °C–40 °C yielded high quality quantitative information on the kinetics of crystallisation for both MOFs. These findings indicate the importance of the solubility of the linker and its connectivity: while the rate of nucleation and the resulting particle size of the MOF (Zr6-MOF-801), with the less soluble and lower connected linker, was strongly temperature dependent, the growth and particle size of Zr6-MOF-808 was hardly impacted by an increase in temperature. This work highlights the importance of careful preliminary research and helps to improve future MOF synthesis design to efficiently achieve the desired particle size distribution.",

keywords = "Metal-organic framework, In situ powder x-ray diffraction, Crystallisation kinetics",

author = "Eja Petersen and Main, {Russell Matthew} and Oxana Magdysyuk and Nicole Kelly and Borthwick, {Emma Ann Lamont} and Naden, {Aaron Benjamin} and Ashbrook, {Sharon E.} and Morris, {Russell Edward} and Romy Ettlinger",

note = "Funding: We gratefully acknowledge Dr Aamod V Desai for fruitful discussions. RE and EEP thank the Fonds der Chemischen Industrie for a Liebig Fellowship. This work was supported by the European Research Council grant ADOR (Advanced Grant 787073). The authors acknowledge the EPSRC Light Element Analysis Facility Grant (EP/T019298/1), the EPSRC Strategic Equipment Resource Grant (EP/R023751/1), the EPSRC Core Equipment Grant (EP/V034138/1) and EP/W034824/1. EALB acknowledges the Allan Handsel Postgraduate Research Scholarship for Chemistry for studentship funding.",

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AU - Petersen, Eja

AU - Main, Russell Matthew

AU - Magdysyuk, Oxana

AU - Kelly, Nicole

AU - Borthwick, Emma Ann Lamont

AU - Naden, Aaron Benjamin

AU - Ashbrook, Sharon E.

AU - Morris, Russell Edward

AU - Ettlinger, Romy

N1 - Funding: We gratefully acknowledge Dr Aamod V Desai for fruitful discussions. RE and EEP thank the Fonds der Chemischen Industrie for a Liebig Fellowship. This work was supported by the European Research Council grant ADOR (Advanced Grant 787073). The authors acknowledge the EPSRC Light Element Analysis Facility Grant (EP/T019298/1), the EPSRC Strategic Equipment Resource Grant (EP/R023751/1), the EPSRC Core Equipment Grant (EP/V034138/1) and EP/W034824/1. EALB acknowledges the Allan Handsel Postgraduate Research Scholarship for Chemistry for studentship funding.

PY - 2024/12/17

Y1 - 2024/12/17

N2 - This study sheds light on the kinetics of crystallisation of two Zr-based metal–organic frameworks (MOFs), namely Zr6-MOF-808 and Zr6-MOF-801, using in situ powder x-ray diffraction (PXRD). Once a room temperature synthesis for the two MOFs was designed for the very small scale, a successful series of in situ PXRD experiments over the range of 10 °C–40 °C yielded high quality quantitative information on the kinetics of crystallisation for both MOFs. These findings indicate the importance of the solubility of the linker and its connectivity: while the rate of nucleation and the resulting particle size of the MOF (Zr6-MOF-801), with the less soluble and lower connected linker, was strongly temperature dependent, the growth and particle size of Zr6-MOF-808 was hardly impacted by an increase in temperature. This work highlights the importance of careful preliminary research and helps to improve future MOF synthesis design to efficiently achieve the desired particle size distribution.

AB - This study sheds light on the kinetics of crystallisation of two Zr-based metal–organic frameworks (MOFs), namely Zr6-MOF-808 and Zr6-MOF-801, using in situ powder x-ray diffraction (PXRD). Once a room temperature synthesis for the two MOFs was designed for the very small scale, a successful series of in situ PXRD experiments over the range of 10 °C–40 °C yielded high quality quantitative information on the kinetics of crystallisation for both MOFs. These findings indicate the importance of the solubility of the linker and its connectivity: while the rate of nucleation and the resulting particle size of the MOF (Zr6-MOF-801), with the less soluble and lower connected linker, was strongly temperature dependent, the growth and particle size of Zr6-MOF-808 was hardly impacted by an increase in temperature. This work highlights the importance of careful preliminary research and helps to improve future MOF synthesis design to efficiently achieve the desired particle size distribution.

KW - Metal-organic framework

KW - In situ powder x-ray diffraction

KW - Crystallisation kinetics

U2 - 10.1088/2515-7639/ad9b4f

DO - 10.1088/2515-7639/ad9b4f

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SN - 2515-7639

VL - 8

JO - Journal of Physics: Materials

JF - Journal of Physics: Materials

IS - 1

M1 - 015006

ER -

Insights to the formation of Zr-based metal–organic frameworks from in situ powder x-ray diffraction

Abstract

Keywords

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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

Insights to the formation of Zr-based metal-organic frameworks from in situ powder X-ray diffraction (dataset)

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