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Title: Physisorbed films in periodic mesoporous silica studied by in situ synchrotron small-angle diffraction

Abstract

Adsorption and capillary condensation of an organic fluid in a periodic mesoporous silica (SBA-15) are studied by in situ synchrotron diffraction. Powder diffraction patterns resulting from the two-dimensional hexagonal packing of the cylindrical pores of SBA-15 are collected as a function of vapor pressure during continuous adsorption and desorption of the fluid (perfluoropentane C{sub 5}F{sub 12}), using a specially designed sorption cell. Seven diffraction peaks with systematic changes of the intensity are resolved as the adsorbed film thickness increases along the adsorption isotherm. The integrated intensities of the diffraction peaks are analyzed with a structural model involving four levels of electron density (dense silica matrix, microporous corona around the pores, adsorbed film, and core space of the pores). The model provides quantitative information about the structure of the evacuated specimen, the filling of the corona, and the growing thickness of the liquid film with increasing pressure. A very good fit of the data by this model is found for relative pressures up to p/p{sub 0}{approx_equal}0.5, but the fit of the high-indexed diffraction peaks becomes poor close to the capillary condensation pressure (p/p{sub 0}{approx_equal}0.68). Tentatively, this fact may be attributed to a deviation of the liquid film structure from the simplemore » flat geometry close to the phase transformation, presumably caused by density fluctuations.« less

Authors:
; ;  [1]; ;  [2];  [3]
  1. Department of Biomaterials, Max Planck Institute of Colloids and Interfaces, D-14424 Potsdam (Germany)
  2. Stranski Laboratory of Physical and Theoretical Chemistry, Technical University Berlin, Strasse des 17. Juni 135, D-10623 Berlin (Germany)
  3. Hamburger Synchrotronstrahlungslabor (HASYLAB), Deutsches Elektronen-Synchrotron (DESY), Notkestrasse 85, D-22603 Hamburg (Germany)
Publication Date:
OSTI Identifier:
20788170
Resource Type:
Journal Article
Resource Relation:
Journal Name: Physical Review. B, Condensed Matter and Materials Physics; Journal Volume: 73; Journal Issue: 18; Other Information: DOI: 10.1103/PhysRevB.73.184109; (c) 2006 The American Physical Society; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; 36 MATERIALS SCIENCE; ADSORPTION; ADSORPTION ISOTHERMS; CAPILLARIES; DESORPTION; DIFFRACTION; ELECTRON DENSITY; FLUCTUATIONS; LIQUIDS; ORGANIC COMPOUNDS; PERIODICITY; PHASE TRANSFORMATIONS; SILICA; STRUCTURAL MODELS; THIN FILMS; VAPOR PRESSURE

Citation Formats

Zickler, Gerald A., Wagermaier, Wolfgang, Paris, Oskar, Jaehnert, Susanne, Findenegg, Gerhard H., and Funari, Sergio S. Physisorbed films in periodic mesoporous silica studied by in situ synchrotron small-angle diffraction. United States: N. p., 2006. Web. doi:10.1103/PHYSREVB.73.1.
Zickler, Gerald A., Wagermaier, Wolfgang, Paris, Oskar, Jaehnert, Susanne, Findenegg, Gerhard H., & Funari, Sergio S. Physisorbed films in periodic mesoporous silica studied by in situ synchrotron small-angle diffraction. United States. doi:10.1103/PHYSREVB.73.1.
Zickler, Gerald A., Wagermaier, Wolfgang, Paris, Oskar, Jaehnert, Susanne, Findenegg, Gerhard H., and Funari, Sergio S. Mon . "Physisorbed films in periodic mesoporous silica studied by in situ synchrotron small-angle diffraction". United States. doi:10.1103/PHYSREVB.73.1.
@article{osti_20788170,
title = {Physisorbed films in periodic mesoporous silica studied by in situ synchrotron small-angle diffraction},
author = {Zickler, Gerald A. and Wagermaier, Wolfgang and Paris, Oskar and Jaehnert, Susanne and Findenegg, Gerhard H. and Funari, Sergio S.},
abstractNote = {Adsorption and capillary condensation of an organic fluid in a periodic mesoporous silica (SBA-15) are studied by in situ synchrotron diffraction. Powder diffraction patterns resulting from the two-dimensional hexagonal packing of the cylindrical pores of SBA-15 are collected as a function of vapor pressure during continuous adsorption and desorption of the fluid (perfluoropentane C{sub 5}F{sub 12}), using a specially designed sorption cell. Seven diffraction peaks with systematic changes of the intensity are resolved as the adsorbed film thickness increases along the adsorption isotherm. The integrated intensities of the diffraction peaks are analyzed with a structural model involving four levels of electron density (dense silica matrix, microporous corona around the pores, adsorbed film, and core space of the pores). The model provides quantitative information about the structure of the evacuated specimen, the filling of the corona, and the growing thickness of the liquid film with increasing pressure. A very good fit of the data by this model is found for relative pressures up to p/p{sub 0}{approx_equal}0.5, but the fit of the high-indexed diffraction peaks becomes poor close to the capillary condensation pressure (p/p{sub 0}{approx_equal}0.68). Tentatively, this fact may be attributed to a deviation of the liquid film structure from the simple flat geometry close to the phase transformation, presumably caused by density fluctuations.},
doi = {10.1103/PHYSREVB.73.1},
journal = {Physical Review. B, Condensed Matter and Materials Physics},
number = 18,
volume = 73,
place = {United States},
year = {Mon May 01 00:00:00 EDT 2006},
month = {Mon May 01 00:00:00 EDT 2006}
}