On the hydrothermal stability of MCM-41. Evidence of capillary tension-induced effects

Lidia López Pérez, Ernst R.H. van Eck, Ignacio Melián-Cabrera*

*Corresponding author for this work

Research output: Contribution to journalArticle

Abstract

MCM-41's limited hydrothermal stability has been often related to the hydrolysis of Si-O-Si bonds due to the low degree of condensation, its thin walls or a combination of them. In this work, evidence for an additional factor is provided; a physical effect that occurs during the drying of the hydrothermally treated calcined material due to the intense capillary stress exerted in water. Depending on both physical (i.e. mechanical) and chemical (i.e. hydrolysis) resistances, the structure undergoes differently. Three MCM-41 samples with different degree of condensation were investigated. The most remarkable results are found with un-aged TEOS based material, which gets fully disordered and shrunk for all applied hydrothermal temperatures in water. Comparison between water and a low-surface-tension-solvent drying revealed that capillarity is responsible for the loss of ordering (and shrinkage) at moderate hydrothermal temperatures. The material's structure is hexagonal and shrinkage-free under the low-surface-tension-solvent route. At a high hydrothermal temperature, hydrolysis is extensive and responsible for the loss of ordering. The other remarkable finding regards the aged MCM-41 mesostructure that maintains the hexagonal features at all applied temperatures in water, and it is more stable against capillarity at high temperature. The Na-metasilicate based material is mechanically very stable and gets disordered at high temperature due to hydrolysis.

Original languageEnglish
Pages (from-to)88-98
Number of pages11
JournalMicroporous and Mesoporous Materials
Volume220
Early online date1 Sep 2015
DOIs
Publication statusPublished - 15 Jan 2016

Fingerprint

Multicarrier modulation
hydrolysis
Hydrolysis
shrinkage
water
drying
interfacial tension
Water
condensation
Capillarity
thin walls
Temperature
temperature
Surface tension
Condensation
Drying
routes
MCM-41

Bibliographical note

© 2015, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/

Keywords

  • capillary stress
  • hydrolysis
  • hydrothermal stability
  • MCM-41
  • mesoporous materials

Cite this

López Pérez, Lidia ; van Eck, Ernst R.H. ; Melián-Cabrera, Ignacio. / On the hydrothermal stability of MCM-41. Evidence of capillary tension-induced effects. In: Microporous and Mesoporous Materials. 2016 ; Vol. 220. pp. 88-98.
@article{f1ac3843030d433e822ad004703f0ddd,
title = "On the hydrothermal stability of MCM-41. Evidence of capillary tension-induced effects",
abstract = "MCM-41's limited hydrothermal stability has been often related to the hydrolysis of Si-O-Si bonds due to the low degree of condensation, its thin walls or a combination of them. In this work, evidence for an additional factor is provided; a physical effect that occurs during the drying of the hydrothermally treated calcined material due to the intense capillary stress exerted in water. Depending on both physical (i.e. mechanical) and chemical (i.e. hydrolysis) resistances, the structure undergoes differently. Three MCM-41 samples with different degree of condensation were investigated. The most remarkable results are found with un-aged TEOS based material, which gets fully disordered and shrunk for all applied hydrothermal temperatures in water. Comparison between water and a low-surface-tension-solvent drying revealed that capillarity is responsible for the loss of ordering (and shrinkage) at moderate hydrothermal temperatures. The material's structure is hexagonal and shrinkage-free under the low-surface-tension-solvent route. At a high hydrothermal temperature, hydrolysis is extensive and responsible for the loss of ordering. The other remarkable finding regards the aged MCM-41 mesostructure that maintains the hexagonal features at all applied temperatures in water, and it is more stable against capillarity at high temperature. The Na-metasilicate based material is mechanically very stable and gets disordered at high temperature due to hydrolysis.",
keywords = "capillary stress, hydrolysis, hydrothermal stability, MCM-41, mesoporous materials",
author = "{L{\'o}pez P{\'e}rez}, Lidia and {van Eck}, {Ernst R.H.} and Ignacio Meli{\'a}n-Cabrera",
note = "{\circledC} 2015, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/",
year = "2016",
month = "1",
day = "15",
doi = "10.1016/j.micromeso.2015.08.024",
language = "English",
volume = "220",
pages = "88--98",
journal = "Microporous and Mesoporous Materials",
issn = "1387-1811",
publisher = "Elsevier",

}

On the hydrothermal stability of MCM-41. Evidence of capillary tension-induced effects. / López Pérez, Lidia; van Eck, Ernst R.H.; Melián-Cabrera, Ignacio.

In: Microporous and Mesoporous Materials, Vol. 220, 15.01.2016, p. 88-98.

Research output: Contribution to journalArticle

TY - JOUR

T1 - On the hydrothermal stability of MCM-41. Evidence of capillary tension-induced effects

AU - López Pérez, Lidia

AU - van Eck, Ernst R.H.

AU - Melián-Cabrera, Ignacio

N1 - © 2015, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/

PY - 2016/1/15

Y1 - 2016/1/15

N2 - MCM-41's limited hydrothermal stability has been often related to the hydrolysis of Si-O-Si bonds due to the low degree of condensation, its thin walls or a combination of them. In this work, evidence for an additional factor is provided; a physical effect that occurs during the drying of the hydrothermally treated calcined material due to the intense capillary stress exerted in water. Depending on both physical (i.e. mechanical) and chemical (i.e. hydrolysis) resistances, the structure undergoes differently. Three MCM-41 samples with different degree of condensation were investigated. The most remarkable results are found with un-aged TEOS based material, which gets fully disordered and shrunk for all applied hydrothermal temperatures in water. Comparison between water and a low-surface-tension-solvent drying revealed that capillarity is responsible for the loss of ordering (and shrinkage) at moderate hydrothermal temperatures. The material's structure is hexagonal and shrinkage-free under the low-surface-tension-solvent route. At a high hydrothermal temperature, hydrolysis is extensive and responsible for the loss of ordering. The other remarkable finding regards the aged MCM-41 mesostructure that maintains the hexagonal features at all applied temperatures in water, and it is more stable against capillarity at high temperature. The Na-metasilicate based material is mechanically very stable and gets disordered at high temperature due to hydrolysis.

AB - MCM-41's limited hydrothermal stability has been often related to the hydrolysis of Si-O-Si bonds due to the low degree of condensation, its thin walls or a combination of them. In this work, evidence for an additional factor is provided; a physical effect that occurs during the drying of the hydrothermally treated calcined material due to the intense capillary stress exerted in water. Depending on both physical (i.e. mechanical) and chemical (i.e. hydrolysis) resistances, the structure undergoes differently. Three MCM-41 samples with different degree of condensation were investigated. The most remarkable results are found with un-aged TEOS based material, which gets fully disordered and shrunk for all applied hydrothermal temperatures in water. Comparison between water and a low-surface-tension-solvent drying revealed that capillarity is responsible for the loss of ordering (and shrinkage) at moderate hydrothermal temperatures. The material's structure is hexagonal and shrinkage-free under the low-surface-tension-solvent route. At a high hydrothermal temperature, hydrolysis is extensive and responsible for the loss of ordering. The other remarkable finding regards the aged MCM-41 mesostructure that maintains the hexagonal features at all applied temperatures in water, and it is more stable against capillarity at high temperature. The Na-metasilicate based material is mechanically very stable and gets disordered at high temperature due to hydrolysis.

KW - capillary stress

KW - hydrolysis

KW - hydrothermal stability

KW - MCM-41

KW - mesoporous materials

UR - http://www.scopus.com/inward/record.url?scp=84941353814&partnerID=8YFLogxK

U2 - 10.1016/j.micromeso.2015.08.024

DO - 10.1016/j.micromeso.2015.08.024

M3 - Article

AN - SCOPUS:84941353814

VL - 220

SP - 88

EP - 98

JO - Microporous and Mesoporous Materials

JF - Microporous and Mesoporous Materials

SN - 1387-1811

ER -