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

Di, Andi ; Schmitt, Julien LU ; Elstone, Naomi ; Arnold, Thomas and Edler, Karen J. LU orcid (2022) In Microporous and Mesoporous Materials 341.
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... (More)

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.

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author
; ; ; and
publishing date
type
Contribution to journal
publication status
published
subject
in
Microporous and Mesoporous Materials
volume
341
article number
112018
pages
11 pages
publisher
Elsevier
external identifiers
  • scopus:85132323519
ISSN
1387-1811
DOI
10.1016/j.micromeso.2022.112018
language
English
LU publication?
no
additional info
Publisher Copyright: © 2022 The Authors
id
e821ed27-475a-4131-ba00-c291a30bada5
date added to LUP
2022-07-12 13:54:30
date last changed
2022-07-25 13:07:35
@article{e821ed27-475a-4131-ba00-c291a30bada5,
  abstract     = {{<p>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 <i>in situ</i> 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.</p>}},
  author       = {{Di, Andi and Schmitt, Julien and Elstone, Naomi and Arnold, Thomas and Edler, Karen J.}},
  issn         = {{1387-1811}},
  language     = {{eng}},
  publisher    = {{Elsevier}},
  series       = {{Microporous and Mesoporous Materials}},
  title        = {{<i>In situ</i> X-ray reflectivity and GISAXS study of mesoporous silica films grown from sodium silicate solution precursors}},
  url          = {{http://dx.doi.org/10.1016/j.micromeso.2022.112018}},
  doi          = {{10.1016/j.micromeso.2022.112018}},
  volume       = {{341}},
  year         = {{2022}},
}