Influence of the silica content in SPEEK-silica membranes prepared from the sol-gel process of polyethoxysiloxane: Morphology and proton mobility

Irene Colicchio, Dan E. Demco, Maria Baias, Helmut Keul, Martin Moeller

Research output: Contribution to journalArticle

Abstract

Sulfonated poly(ether ether ketone) (SPEEK)-silica membranes with increasing silica content are presented. The silica is generated in situ via the water free sol-gel process of polyethoxysiloxane (PEOS), a liquid hyperbranched inorganic polymer of low viscosity. The conversion of PEOS into silica during membrane formation induces changes in the hydrophobic-hydrophilic phase separation of the pure ionomer, influencing morphology and proton mobility. The hybrid membranes are studied regarding their morphology (transmission electron microscopy) and their proton mobility at bulk (impedance spectroscopy) and molecular level (1H wide-line NMR, and self-diffusion). Water self-diffusion by stimulated-echo edited spectra shows two components corresponding to fast and slow diffusion. This can be correlated with the water diffusion in the ionic clusters (more hydrophobic) and in the channels (more hydrophilic). The apparent diffusion coefficients depend on the temperature and on the silica content. At 90% RH, the bulk proton conductivity of the composite membranes is higher than the pure ionomer. Starting from 80 °C, the proton conductivity of the SPEEK-silica membranes is independent from the silica content. The samples prepared with low PEOS content (10 and 20 wt.%) are more stable upon successive heating/cooling measuring cycles, showing less dependency on membrane hydration than the pure SPEEK.

Original languageEnglish (US)
Pages (from-to)125-135
Number of pages11
JournalJournal of Membrane Science
Volume337
Issue number1-2
DOIs
StatePublished - Jul 15 2009

Fingerprint

Polyether ether ketones
Polymethyl Methacrylate
sol-gel processes
Ketones
ketones
Silicon Dioxide
Ether
Sol-gel process
Protons
ethers
Gels
Silica
silicon dioxide
membranes
Membranes
protons
Proton conductivity
Ionomers
Water
water

Keywords

  • H NMR
  • Hybrid membranes
  • Morphology
  • Proton conductivity
  • Water self-diffusion

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Materials Science(all)
  • Biochemistry
  • Filtration and Separation

Cite this

Influence of the silica content in SPEEK-silica membranes prepared from the sol-gel process of polyethoxysiloxane : Morphology and proton mobility. / Colicchio, Irene; Demco, Dan E.; Baias, Maria; Keul, Helmut; Moeller, Martin.

In: Journal of Membrane Science, Vol. 337, No. 1-2, 15.07.2009, p. 125-135.

Research output: Contribution to journalArticle

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AB - Sulfonated poly(ether ether ketone) (SPEEK)-silica membranes with increasing silica content are presented. The silica is generated in situ via the water free sol-gel process of polyethoxysiloxane (PEOS), a liquid hyperbranched inorganic polymer of low viscosity. The conversion of PEOS into silica during membrane formation induces changes in the hydrophobic-hydrophilic phase separation of the pure ionomer, influencing morphology and proton mobility. The hybrid membranes are studied regarding their morphology (transmission electron microscopy) and their proton mobility at bulk (impedance spectroscopy) and molecular level (1H wide-line NMR, and self-diffusion). Water self-diffusion by stimulated-echo edited spectra shows two components corresponding to fast and slow diffusion. This can be correlated with the water diffusion in the ionic clusters (more hydrophobic) and in the channels (more hydrophilic). The apparent diffusion coefficients depend on the temperature and on the silica content. At 90% RH, the bulk proton conductivity of the composite membranes is higher than the pure ionomer. Starting from 80 °C, the proton conductivity of the SPEEK-silica membranes is independent from the silica content. The samples prepared with low PEOS content (10 and 20 wt.%) are more stable upon successive heating/cooling measuring cycles, showing less dependency on membrane hydration than the pure SPEEK.

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