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Small angle X-ray scattering from MCM-41 and its synthesis gels : optimisation of the synthesis parameters

Edler, K. J. LU orcid ; Dougherty, J. ; Durand, R. ; Iton, L. ; Kirton, G. ; Lockhart, G. ; Wang, Z. LU ; Withers, R. and White, J. W. (1995) In Colloids and Surfaces A: Physicochemical and Engineering Aspects 102(C). p.213-230
Abstract

We have found optimised conditions for alkaline synthesis of the large pore molecular sieve, MCM-41, by determining small angle X-ray scattering and adsorption isotherms from materials at various stages of the preparation. The presence of highly curved surfaces, sealed structures, and quasicrystalline hexagonal products coexisting with true MCM-41 are all detected by transmission electron microscopy. Calcination must be carried out with care. The product is most crystalline from unstirred preparations which have been heated at 100°C for no longer than three days. Under these conditions, a maximum BET surface area of 1950 m2 g-1 was attained, with evident crystallinity observed by electron diffraction and... (More)

We have found optimised conditions for alkaline synthesis of the large pore molecular sieve, MCM-41, by determining small angle X-ray scattering and adsorption isotherms from materials at various stages of the preparation. The presence of highly curved surfaces, sealed structures, and quasicrystalline hexagonal products coexisting with true MCM-41 are all detected by transmission electron microscopy. Calcination must be carried out with care. The product is most crystalline from unstirred preparations which have been heated at 100°C for no longer than three days. Under these conditions, a maximum BET surface area of 1950 m2 g-1 was attained, with evident crystallinity observed by electron diffraction and transmission electron microscopy. In the stirred system, which appears to be in a non-equilibrium state, materials after calcination exhibiting Bragg d-spacings of 35 Å, 37 Å and 38 Å have been identified.

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author
; ; ; ; ; ; ; and
publishing date
type
Contribution to journal
publication status
published
keywords
Characterisation, Mesoporous molecular sieve, Synthesis
in
Colloids and Surfaces A: Physicochemical and Engineering Aspects
volume
102
issue
C
pages
18 pages
publisher
Elsevier
external identifiers
  • scopus:0002256775
ISSN
0927-7757
DOI
10.1016/0927-7757(95)03241-5
language
English
LU publication?
no
id
248f6381-6189-45ac-9466-1c7ec04f2c46
date added to LUP
2022-07-12 15:53:59
date last changed
2022-08-12 12:56:00
@article{248f6381-6189-45ac-9466-1c7ec04f2c46,
  abstract     = {{<p>We have found optimised conditions for alkaline synthesis of the large pore molecular sieve, MCM-41, by determining small angle X-ray scattering and adsorption isotherms from materials at various stages of the preparation. The presence of highly curved surfaces, sealed structures, and quasicrystalline hexagonal products coexisting with true MCM-41 are all detected by transmission electron microscopy. Calcination must be carried out with care. The product is most crystalline from unstirred preparations which have been heated at 100°C for no longer than three days. Under these conditions, a maximum BET surface area of 1950 m<sup>2</sup> g<sup>-1</sup> was attained, with evident crystallinity observed by electron diffraction and transmission electron microscopy. In the stirred system, which appears to be in a non-equilibrium state, materials after calcination exhibiting Bragg d-spacings of 35 Å, 37 Å and 38 Å have been identified.</p>}},
  author       = {{Edler, K. J. and Dougherty, J. and Durand, R. and Iton, L. and Kirton, G. and Lockhart, G. and Wang, Z. and Withers, R. and White, J. W.}},
  issn         = {{0927-7757}},
  keywords     = {{Characterisation; Mesoporous molecular sieve; Synthesis}},
  language     = {{eng}},
  month        = {{09}},
  number       = {{C}},
  pages        = {{213--230}},
  publisher    = {{Elsevier}},
  series       = {{Colloids and Surfaces A: Physicochemical and Engineering Aspects}},
  title        = {{Small angle X-ray scattering from MCM-41 and its synthesis gels : optimisation of the synthesis parameters}},
  url          = {{http://dx.doi.org/10.1016/0927-7757(95)03241-5}},
  doi          = {{10.1016/0927-7757(95)03241-5}},
  volume       = {{102}},
  year         = {{1995}},
}