Hot-spots during the calcination of MCM-41: a SAXS comparative analysis of a soft mesophase

Lidia López Pérez, M.J. Ortiz-Iniesta, Hero Jan Heeres, Ignacio Melián-Cabrera*

*Corresponding author for this work

Research output: Contribution to journalArticle

Abstract

The phenomenon of microscopic hot-spots, during the calcination of MCM-41, was investigated by quantifying the magnitude of the temperature increase during the calcination of a soft MCM-41 mesophase using a SAXS comparative study. This was performed by thermally treating a soft material that was detemplated via Fenton chemistry followed by equilibrating and drying in a low-surface-tension solvent (n-butanol or N,N-dimethylformamide); these samples have limited structural shrinkage. The resulting samples were thermally treated at increasing temperatures, and the structural shrinkage was compared with that of the directly calcined material. By comparing the structural shrinkage, it was found that the microscopic temperature increase would fall between 190 and 250 C, as deduced from N,N-dimethyl-formamide and n-butanol. The order of magnitude of the temperature increase appears to be consistent with the well-known glow effect. It is, however, substantially higher than the experimentally determined macroscopic temperature increase. Several aspects are discussed to interpret this difference.

Original languageEnglish
Pages (from-to)51-54
Number of pages4
JournalMaterials Letters
Volume118
Early online date1 Dec 2013
DOIs
Publication statusPublished - 1 Mar 2014

Keywords

  • Calcination
  • Glow effect
  • Hot-spots
  • MCM-41
  • Structural shrinkage
  • Surfactant-templated mesoporous materials

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