Optimizing surfactant removal from a soft-templated ordered mesoporous carbon precursor: an in situ SAXS study
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in: Journal of applied crystallography, Jahrgang 56.2023, Nr. 3, 02.05.2023, S. 801-809.
Publikationen: Beitrag in Fachzeitschrift › Artikel › Forschung › (peer-reviewed)
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TY - JOUR
T1 - Optimizing surfactant removal from a soft-templated ordered mesoporous carbon precursor
T2 - an in situ SAXS study
AU - Rauscher, Max
AU - Seyffertitz, Malina
AU - Kohns, Richard
AU - Stock, Sebastian
AU - Amenitsch, Heinz
AU - Huesing, Nicola
AU - Paris, Oskar
N1 - Publisher Copyright: © 2023 International Union of Crystallography. All rights reserved.
PY - 2023/5/2
Y1 - 2023/5/2
N2 - In situ small-angle X-ray scattering (SAXS) was employed to identify critical parameters during thermal treatment for template removal of an ordered mesoporous carbon precursor synthesized via a direct soft-templating route. The structural parameters obtained from the SAXS data as a function of time were the lattice parameter of the 2D hexagonal structure, the diameter of the cylindrical mesostructures and a power-law exponent characterizing the interface roughness. Moreover, detailed information on contrast changes and pore lattice order was obtained from analysis of the integrated SAXS intensity of the Bragg and diffuse scattering separately. Five characteristic regions during heat treatment were identified and discussed regarding the underlying dominant processes. The influence of temperature and O2/N2 ratio on the final structure was analyzed, and parameter ranges were identified for an optimized template removal without strongly affecting the matrix. The results indicate that the final structure and controllability of the process are optimum for temperatures between 260 and 300°C with a gas flow containing 2 mol% of O2.
AB - In situ small-angle X-ray scattering (SAXS) was employed to identify critical parameters during thermal treatment for template removal of an ordered mesoporous carbon precursor synthesized via a direct soft-templating route. The structural parameters obtained from the SAXS data as a function of time were the lattice parameter of the 2D hexagonal structure, the diameter of the cylindrical mesostructures and a power-law exponent characterizing the interface roughness. Moreover, detailed information on contrast changes and pore lattice order was obtained from analysis of the integrated SAXS intensity of the Bragg and diffuse scattering separately. Five characteristic regions during heat treatment were identified and discussed regarding the underlying dominant processes. The influence of temperature and O2/N2 ratio on the final structure was analyzed, and parameter ranges were identified for an optimized template removal without strongly affecting the matrix. The results indicate that the final structure and controllability of the process are optimum for temperatures between 260 and 300°C with a gas flow containing 2 mol% of O2.
KW - SAXS
KW - In Situ Behandlung
KW - carbon
KW - Mesoporous carbon
KW - calcination
KW - ordered mesoporous carbon
UR - http://www.scopus.com/inward/record.url?scp=85171530192&partnerID=8YFLogxK
U2 - 10.1107/S1600576723003886
DO - 10.1107/S1600576723003886
M3 - Article
AN - SCOPUS:85171530192
VL - 56.2023
SP - 801
EP - 809
JO - Journal of applied crystallography
JF - Journal of applied crystallography
SN - 1600-5767
IS - 3
ER -