In Situ Small‐Angle X‐ray Scattering Investigation of the Formation of Dual‐Mesoporous Materials |
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Authors: | Dr. Julien Schmitt Dr. Nadia Canilho Dr. Marianne Impéror‐Clerc Prof. Jean‐Luc Blin Dr. Jan Skov Pedersen Dr. Javier Pérez Dr. Bénédicte Lebeau Dr. Loic Vidal Dr. Marie‐José Stébé |
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Affiliation: | 1. Physical Chemistry, Lund University, Lund, Sweden;2. Université de Lorraine, UMR CNRS 7565 SRSMC, Vandoeuvre les Nancy cedex, France;3. Laboratoire de Physique de Solides, UMR CNRS 8502, Bat. 510, Université Paris-Sud, Orsay, France;4. Department of Chemistry and Interdisciplinary Nanoscience Center (iNANO), Aarhus University Gustav Wieds Vej 14, Aarhus C, Denmark;5. Beamline SWING, Synchrotron Soleil, BP 48, Gif-sur-Yvette, France;6. Université de Haute Alsace, Institut de Science des Matériaux de Mulhouse (IS2?M), Equipe Matériaux à Porosité Contr?lée (MPC), UMR CNRS 7361, Mulhouse cedex, France |
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Abstract: | The formation of a 2D‐hexagonal (p6m) silica‐based hybrid dual‐mesoporous material is investigated in situ by using synchrotron time‐resolved small‐angle X‐ray scattering (SAXS). The material is synthesized from a mixed micellar solution of a nonionic fluorinated surfactant, RF8(EO)9 (EO=ethylene oxide) and a nonionic triblock copolymer, P123. Both mesoporous networks, with pore dimensions of 3.3 and 8.5 nm respectively, are observed by nitrogen sorption, transmission electron microscopy (TEM), and SAXS. The in situ SAXS experiments reveal that mesophase formation occurs in two steps. First the nucleation and growth of a primary 2D‐hexagonal network (N1), associated with mixed micelles containing P123, then subsequent formation of a second network (N2), associated with micelles of pure RF8(EO)9. The data obtained from SAXS and TEM suggest that the N1 network is used as a nucleation center for the formation of the N2 network, which would result in the formation of a grain with two mesopore sizes. Understanding the mechanism of the formation of such materials is an important step towards the synthesis of more‐complex materials by fine tuning the porosity. |
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Keywords: | electron microscopy kinetics mesoporous materials small-angle X-ray scattering surfactants |
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