Characterization of proton‐conducting organic–inorganic polymeric materials by ASAXS

The distribution of ZrO2 and phosphotungstic acid (PTA) in a matrix of sulfonated polyether ketone was investigated by anomalous small-angle X-ray scattering (ASAXS). Scattering curves were obtained using X-ray energies near the Zr and W absorption edges, allowing the independent analysis of the distribution of ZrO2 and PTA in the sample. The interaction between both inorganic components improved their dispersion considerably when compared with films containing just one of the additives. The synergism was correlated to previous investigations concerning proton conductivity and permeability of the membranes developed for direct methanol fuel cell. © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 2981–2992, 2005

[1]  Helmut Schmidt,et al.  Investigation of Ion-Conducting Ormolytes: Structure-Property Relationships , 1994 .

[2]  G. Robertson,et al.  Synthesis and characterization of poly(aryl ether ketone) copolymers containing (hexafluoroisopropylidene)-diphenol moiety as proton exchange membrane materials , 2005 .

[3]  H.-G. Haubold,et al.  Nano structure of NAFION: a SAXS study , 2001 .

[4]  A. Włochowicz,et al.  The state of ion aggregation in ionomers based on copolymers of styrene and acrylic acid: 2. Small-angle X-ray scattering studies , 2000 .

[5]  Michael A. Hickner,et al.  Fabrication and characterization of heteropolyacid (H3PW12O40)/directly polymerized sulfonated poly(arylene ether sulfone) copolymer composite membranes for higher temperature fuel cell applications , 2003 .

[6]  I. Torriani,et al.  Hybrid materials derived from divinylbenzene and cyclic siloxane , 2004 .

[7]  H. Iijima,et al.  Small-Angle X-ray and Neutron Scattering from Dilute Solutions of Cesium Perfluorooctanoate. Micellar Growth along Two Dimensions , 1998 .

[8]  Suzana P. Nunes,et al.  Inorganic modification of proton conductive polymer membranes for direct methanol fuel cells , 2002 .

[9]  V. Silva,et al.  Membranes for direct methanol fuel cell based on modified heteropolyacids , 2004 .

[10]  Gérard Gebel,et al.  Gas transport mechanism in sulfonated polyimides . Consequences on gas selectivity , 2002 .

[11]  K. Mauritz,et al.  Surlyn®/titanate hybrid materials via polymer in situ sol–gel chemistry , 2003 .

[12]  G. Gebel,et al.  Sulfonated Polyimide Ionomers: A Structural Study , 2004 .

[13]  U. Schubert,et al.  Metal Complexes in Inorganic Matrixes. 18.1 Phosphanyl-Substituted Titanium and Zirconium Alkoxides for Tethering Metal Complexes on Titania or Zirconia and the X-ray Structure Analysis of Polymeric Zr(OPr)(O3SMe)3 , 1997 .

[14]  S. Cooper,et al.  Blends of metal acetates and polyurethanes containing pyridine groups II. SAXS and EXAFS studies , 1994 .

[15]  Keisuke Iwata,et al.  Physical properties and structure of organic-inorganic hybrid materials produced by sol-gel process , 1998 .

[16]  A. Craievich,et al.  Small-angle X-ray and nuclear-magnetic resonance study of siloxane-PMMA hybrids prepared by the sol-gel process , 2003 .

[17]  T. Okuhara,et al.  Effect of alkaline metal on microporosity of acidic alkaline salts of 12-tungstophosphoric acid , 2002 .

[18]  I. Torriani,et al.  Polycyclic silicone membranes. Synthesis, characterization and permeability evaluation , 2001 .

[19]  Horst Halling,et al.  JUSIFA—A new user‐dedicated ASAXS beamline for materials science , 1989 .

[20]  K. Richau,et al.  Reduction of Methanol Permeability in Polyetherketone-Heteropolyacid Membranes , 2003 .

[21]  G. Goerigk,et al.  Anomalous small-angle X-ray scattering characterization of composites based on sulfonated poly(ether ether ketone), zirconium phosphates, and zirconium oxide , 2004 .

[22]  G. Scherer,et al.  Acid functionalized poly(arylene ether)s for proton-conducting membranes , 2004 .

[23]  J. Putaux,et al.  Anisotropy of structure and transport properties in sulfonated polyimide membranes , 2003 .

[24]  S. Cooper,et al.  Anomalous small-angle x-ray scattering from nickel-neutralized ionomers. 2. Semicrystalline polymer matrixes , 1990 .

[25]  M. Guiver,et al.  Clustering in carboxylated polysulfone ionomers: A characterization by dynamic mechanical and small-angle X-ray scattering methods , 1999 .

[26]  N. M. José,et al.  Synthesis, characterization, and permeability evaluation of hybrid organic–inorganic films , 2004 .

[27]  K. Sanui,et al.  Proton-conducting polymer electrolyte membranes based on hydrocarbon polymers , 2000 .

[28]  Nádia Mamede José,et al.  Materiais híbridos orgânico-inorgânicos: preparação e algumas aplicações , 2005 .

[29]  Ronghuan He,et al.  Proton conductivity of phosphoric acid doped polybenzimidazole and its composites with inorganic proton conductors , 2003 .

[30]  T. Hashimoto,et al.  Effect of Volume Fraction on the Order−Disorder Transition in Low Molecular Weight Polystyrene-block-polyisoprene Copolymers. 2. Order−Disorder Transition Temperature Determined by Small-Angle X-ray Scattering , 1996 .

[31]  L. M. Toth,et al.  Structure and growth kinetics of zirconium hydrous polymers in organic solutions , 1999 .

[32]  O. Lyon,et al.  Anomalous small-angle X-ray scattering in materials science , 2003 .

[33]  D. Nguyen,et al.  Block ionomer micelles in solution. I: Characterization of ionic cores by small-angles X-ray scattering , 1994 .

[34]  Lauro T. Kubota,et al.  Electrochemical Properties of [Ru(edta)(H2O)]−Immobilized on a Zirconium(IV) Oxide-Coated Silica Gel Surface , 1996 .

[35]  P. Goudeau,et al.  Scattering of X-rays , 1995 .

[36]  G. Robertson,et al.  Synthesis and characterization of sulfonated poly(ether ether ketone) for proton exchange membranes , 2004 .

[37]  K. Mauritz,et al.  Surlyn®/silicate nanocomposite materials via a polymer in situ sol–gel process: Morphology , 2003 .

[38]  A. Włochowicz,et al.  The state of ion aggregation in ionomers based on copolymers of styrene and acrylic acid: 1. Small-angle X-ray scattering studies , 2000 .