The role of the ionic liquid C6C1ImTFSI in the sol–gel synthesis of silica studied using in situ SAXS and Raman spectroscopy
Journal article, 2015

The sol–gel synthesis of a silica based ionogel using the ionic liquid 1-hexyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (C6C1ImTFSI) as the solvent has been followed in situ by combined μ-focused X-ray scattering and μ-Raman spectroscopy. By covering the momentum transfer range 0.2 < q < 30 nm−1 we probe the evolution of the characteristic peaks of the ionic liquid, associated with the existence of polar and non-polar domains, as a function of reaction time. Our detailed analysis of the small angle X-ray scattered (SAXS) pattern reveals that the nano-structure of the ionic liquid is partially retained during the sol–gel synthesis, as indicated by the broader yet distinguishable SAXS signatures. We also observe that the signature associated with the non-polar and polar domains shift to higher and lower q-values, respectively. Interestingly, this behavior correlates with the evolution of the chemical composition of the sol as probed by Raman spectroscopy. More precisely, we observe that both the nano-structural changes and the production of polar molecules arrest at the point of gelation. This is rationalized by the tendency of the reagents and products of the sol–gel reaction to locate in different portions of the nano-structure of the ionic liquid.

nanostructures

hybrid devices

ionic liquids

hightemperature superconductors

silica

x-ray scattering

superconducting detectors

Author

Moheb Nayeri

Chalmers, Chemistry and Chemical Engineering, Applied Chemistry, Applied Surface Chemistry

Kim Nygård

University of Gothenburg

Maths Karlsson

Chalmers, Applied Physics, Condensed Matter Physics

M. Maréchal

Université Grenoble Alpes

Centre national de la recherche scientifique (CNRS)

The French Alternative Energies and Atomic Energy Commission (CEA)

Manfred Burghammer

European Synchrotron Radiation Facility (ESRF)

Michael Reynolds

European Synchrotron Radiation Facility (ESRF)

Anna Martinelli

Chalmers, Chemistry and Chemical Engineering, Applied Chemistry, Applied Surface Chemistry

Physical Chemistry Chemical Physics

1463-9076 (ISSN) 1463-9084 (eISSN)

Vol. 17 15 9841-9848

Subject Categories

Physical Chemistry

Materials Chemistry

Chemical Sciences

DOI

10.1039/C5CP00709G

More information

Latest update

9/7/2018 1