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Crystallisation kinetics of metal organic frameworks from in situ time-resolved x-ray diffraction
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El Osta, Racha, Feyand, Mark, Stock, Norbert, Millange, Franck and Walton, Richard I. (2013) Crystallisation kinetics of metal organic frameworks from in situ time-resolved x-ray diffraction. Powder Diffraction, Volume 28 (Number S2). S256-S275. doi:10.1017/S0885715613000997 ISSN 0885-7156.
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Official URL: http://dx.doi.org/10.1017/S0885715613000997
Abstract
A time-resolved powder diffraction study of the crystallisation of porous metal organic framework materials with the CPO-27 structure ([M2(dhtp)(H2O)2]·8H2O where, dhtp=2,5-dioxoterephthalate) using the energy dispersive X-ray diffraction method is described. Crystallisation under solvothermal conditions is performed between 70 - 110 °C from clear solutions of metal salts (M=Co2+ or Ni2+) and 2,5-dihydroxyterephthalic acid in a mixture of THF-water in sealed reaction vessels, using both conventional and microwave heating. Integration of Bragg peak areas with time provides accurate crystallisation curves, which are modelled using the method of Gualtieri to determine rate constants for nucleation and for growth and then, by Arrhenius analysis, activation energies. Crystallisation is determined to be one-dimensional, consistent with the elongated morphology of the crystals produced in these reactions. With conventional heating the Co-containing CPO-27 crystallises more rapidly than the isostructural Ni-containing analogue and analysis of the kinetic parameters would suggest a complex multi-step crystallisation process. The effect of microwave heating is upon activation energies: the values for both nucleation and for crystal growth are lowered compared to reactions using conventional heating.
Item Type: | Journal Article | ||||
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | ||||
Journal or Publication Title: | Powder Diffraction | ||||
Publisher: | Cambridge University Press | ||||
ISSN: | 0885-7156 | ||||
Official Date: | 2013 | ||||
Dates: |
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Volume: | Volume 28 | ||||
Number: | Number S2 | ||||
Page Range: | S256-S275 | ||||
DOI: | 10.1017/S0885715613000997 | ||||
Status: | Peer Reviewed | ||||
Publication Status: | Published | ||||
Access rights to Published version: | Restricted or Subscription Access | ||||
Funder: | European Community | ||||
Grant number: | [228862] |
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