In situ X-ray reflectivity and GISAXS study of mesoporous silica films grown from sodium silicate solution precursors

Andi Di, Julien Schmitt, Naomi Elstone, Thomas Arnold, Karen J. Edler

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3 Citations (SciVal)

Abstract

An environmentally friendly and inexpensive silica source, sodium silicate solution, was applied to synthesize a free-standing mesoporous silica film at the air/liquid interface, exploiting the co-assembly of cetyltrimethylammonium bromide and polyethylenimine. The effect of the composition of the solution used for the film formation on the mesostructure of the as-synthesized silica films, characterized by small angle X-ray scattering (SAXS), was investigated. The initial film formation time is estimated by the change in surface pressure with time. Additionally, a possible formation process of the mesostructured silica film is proposed using data from in situ grazing incidence small angle X-ray scattering (GISAXS) and X-ray reflectivity (XRR) measurements. A free-standing film with a wormlike structure was formed at the interface and reorganized into a 2D hexagonal ordered structure while drying at room temperature, after removal from the air/solution interface. The ordered 2D hexagonal structure, however, could only be retained to some extent during calcination, in samples where nitrate ions are present in the film formation solution.

Original languageEnglish
Article number112018
Pages (from-to)112018
JournalMicroporous and Mesoporous Materials
Volume341
Early online date25 May 2022
DOIs
Publication statusPublished - 31 Aug 2022

Bibliographical note

Funding Information:
A. Di would like to thank the China Scholarship Council and the University of Bath for funding her PhD studies. N. Elstone thanks the UK Engineering and Physical Sciences Research Council (EPSRC), for a PhD studentship in the Centre for Doctoral Training in Sustainable Chemical Technologies at the University of Bath (EP/L016354/1). The authors thank Diamond Light Source (UK) for the award of beamtime on beamline I07 (experiment SI52101-1), and the ISIS Neutron and Muon Source for beamtime on CRISP (DOI: 10.5286/ISIS.E.RB13425). The authors would like to acknowledge Dr Johnathan Rawle for his assistance with the reduction of GISAXS data and Dr Stephen Holt for assistance with the experiment on CRISP. Data supporting this paper are available through the University of Bath research data archive system, DOI: https://doi.org/10.15125/BATH-01151.

Funding Information:
A. Di would like to thank the China Scholarship Council and the University of Bath for funding her PhD studies. N. Elstone thanks the UK Engineering and Physical Sciences Research Council (EPSRC) , for a PhD studentship in the Centre for Doctoral Training in Sustainable Chemical Technologies at the University of Bath (EP/L016354/1). The authors thank Diamond Light Source (UK) for the award of beamtime on beamline I07 (experiment SI52101-1), and the ISIS Neutron and Muon Source for beamtime on CRISP (DOI: 10.5286/ISIS.E.RB13425). The authors would like to acknowledge Dr Johnathan Rawle for his assistance with the reduction of GISAXS data and Dr Stephen Holt for assistance with the experiment on CRISP. Data supporting this paper are available through the University of Bath research data archive system, DOI: https://doi.org/10.15125/BATH-01151 .

ASJC Scopus subject areas

  • General Chemistry
  • General Materials Science
  • Condensed Matter Physics
  • Mechanics of Materials

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