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

K. J. Edler, J. Dougherty, R. Durand, L. Iton, G. Kirton, G. Lockhart, Z. Wang, R. Withers, J. W. White

Research output: Contribution to journalArticle

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 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.

Original languageEnglish
Pages (from-to)213-230
Number of pages18
JournalColloids and Surfaces A: Physicochemical and Engineering Aspects
Volume102
Issue numberC
DOIs
Publication statusPublished - 13 Sep 1995

Keywords

  • Characterisation
  • Mesoporous molecular sieve
  • Synthesis

ASJC Scopus subject areas

  • Surfaces and Interfaces
  • Physical and Theoretical Chemistry
  • Colloid and Surface Chemistry

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