The role of the ionic liquid C6C1ImTFSI in the sol–gel synthesis of silica studied using in situ SAXS and Raman spectroscopy
Artikel i vetenskaplig tidskrift, 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

superconducting detectors

hightemperature superconductors

x-ray scattering

silica

ionic liquids

Författare

Moheb Nayeri

Kemi och kemiteknik, Tillämpad kemi, Teknisk ytkemi

Kim Nygård

Göteborgs universitet

Maths Karlsson

Chalmers, Teknisk fysik, Kondenserade materiens fysik

M. Maréchal

Le Commissariat à l’énergie atomique et aux énergies alternatives (CEA)

Université Grenoble Alpes

CNRS Centre National de la Recherche Scientifique

Manfred Burghammer

European Synchrotron Radiation Facility

Michael Reynolds

European Synchrotron Radiation Facility

Anna Martinelli

Kemi och kemiteknik, Tillämpad kemi, Teknisk ytkemi

Physical Chemistry Chemical Physics

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

Vol. 17 9841-9848

Ämneskategorier

Fysikalisk kemi

Materialkemi

Kemi

DOI

10.1039/C5CP00709G