[en] A versatile high pressure X-ray sample cell has been developed for conducting in situ time-resolved X-ray scattering experiments in the pressure and temperature regime required (pressures up to 210 bars and temperatures up to 120 °C) for chemical reactions in supercritical fluids. The large exit opening angle of the cell allows simultaneous performance of SAXS-WAXS experiments. Diamond windows are used in order to benefit from the combination of maximum strength, minimal X-ray absorption and chemical inertia. The sample cell can also be utilised for X-ray spectroscopy experiments over a wide range of photon energies. Results of the online synthesis of a block copolymer, poly(methyl methacrylate-block-poly(benzyl methacrylate), by Reversible Addition-Fragmentation Chain Transfer (RAFT) in a supercritical CO2 dispersion polymerisation will be discussed. The contribution of the density fluctuations, as function of temperature, to the X-ray scattering signal has been quantified in order to allow appropriate background subtractions
Disciplines :
Physics
Author, co-author :
Hermida-Merino, Daniel
Portale, Giuseppe
Fields, Peter
Wilson, Richard
Basset, Simon
Jennings, James
Dellar, Martin
Gommes, Cédric ; Université de Liège - ULiège > Département de chimie appliquée > Département de chimie appliquée
Howdle, Steven
Bras, Wim
Vrolijk, Benno
Language :
English
Title :
A high pressure cell for supercritical CO2 on-line chemical reactions studied with x-ray techniques
Publication date :
2014
Journal title :
Review of Scientific Instruments
ISSN :
0034-6748
eISSN :
1089-7623
Publisher :
American Institute of Physics, New York, United States - New York
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