PVDF-HFP/silica-SH nanocomposite synthesis for PEMFC membranes through simultaneous one-step sol–gel reaction and reactive extrusion

Seck, Serigne Massamba; Magana, Sylvain; Prébé, Arnaud; Niepceron, Frédérick; Bounor‐Legaré, Véronique; Bigarré, J.; Buvat, Pierrick; Gérard, Jean‐François

doi:10.1016/j.matchemphys.2015.07.014

Cited by 19 publications

(6 citation statements)

References 47 publications

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“…The synthesis involves the copolymerisation of VDF and PMVE from hydrophilic poly(N,N-dimethylacrylamide) macroRAFT agents (Scheme 6.10) [66]. Interestingly, such PVDF-based fluorinated copolymers have successfully been employed as compatibilisers for the preparation of poly(VDF-co-HFP) copolymer/functional silica nanocomposites, for use as novel proton exchange membrane fuel cells, by reactive extrusion [68]. The synthesis of these composites involved the in situ generation of the inorganic phase (via sol-gel chemistry from mercaptopropylethoxysilane).…”

Section: Functional Polymers By Reversible Deactivation Radical Polymmentioning

confidence: 99%

6. Recent advances in the reversible deactivation radical (co)polymerization of fluorinated alkenes/acrylates/ methacrylates/styrenes

Banerjee¹,

Chakrabarty²,

Singha³

et al. 2019

Reversible Deactivation Radical Polymerization

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HAL is a multi-disciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L'archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d'enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.Recent advances in the reversible deactivation radical (co)polymerization of fluorinated alkenes/acrylates/ methacrylates/styrenes

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Section: Functional Polymers By Reversible Deactivation Radical Polymmentioning

confidence: 99%

6. Recent advances in the reversible deactivation radical (co)polymerization of fluorinated alkenes/acrylates/ methacrylates/styrenes

Banerjee¹,

Chakrabarty²,

Singha³

et al. 2019

Reversible Deactivation Radical Polymerization

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“…Therefore, an alternative strategy, which relies on the incorporation of inorganic phases via in situ sol–gel processing, have been proposed. [ 15,20,21 ] This approach permits fabrication of hybrid membranes with a homogeneous distribution of inorganic phase across the host polymer matrix.…”

Section: Introductionmentioning

confidence: 99%

Proton Conductive Membranes from Covalently Cross‐Linked Poly(Acrylate)/Silica Interpenetrating Networks

Zhyhailo

Horechyy

Meier‐Haack

et al. 2021

Macro Materials & Eng

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The preparation of hybrid proton conductive membranes that comprise of covalently linked interpenetrating polymer and inorganic networks is reported. The hybrid membranes are synthesized via simultaneous photo‐initiated polymerization and sol–gel processing. The simultaneous processing permeates fabrication of the membranes that comprises covalently cross‐linked polymeric and inorganic networks. The membranes are characterized by attenuated total reflectance‐Fourier transform infrared spectroscopy, scaning electron microsopy, thermogravimetric analysis, differential scanning calorimetry, in order to confirm their chemical composition, structure, and morphology. An addition of 3‐methacryloxypropyl trimethoxysilane into the sol–gel composition allows the formation of covalent linkages between polymeric and inorganic networks, which facilitates a uniform distribution of the molecular components across the fabricated membranes. The incorporation of the silica network leads to an increase in water retention and proton conductivity of hybrid membranes as compared to their purely polymeric analogues.

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“…The objective of this study deals with the processing of new protonconducting membranes by reactive extrusion of conventional non-functional fluoropolymers with a functional trialkoxysilane (able to undergo oxidization modification to display sulfonic acid group) in the presence of a compatibilizing agent. Our previous work [50,51] demonstrated the possibility to prepare new fluoropolymers/functional silica basednanocomposites for fuel cell membrane application by combining reactive extrusion and in situ formation of the inorganic phase by the sol-gel chemistry. Original membranes were synthetized by extrusion without any solvent.…”

Section: Introductionmentioning

confidence: 99%

“…In order to investigate the proof of concept, i.e. the design by an extrusion process of such membranes, two preliminary experiments (results not shown here and based on our previous[50,51]) were conducted with either i) 8 wt% of poly(VDF-co-MAF) copolymer (denoted as PVDF-co-MAF 6) for a system with 15wt % of inorganic phase or with ii) 5 wt% of PVDF-co-MAF 6 and 20 wt% of generated equivalent SiO 2 . The interfacial agent was introduced for all the systems at step b during the addition of the precursor solution in the molten poly(VDF-co-HFP) matrix.…”

mentioning

confidence: 99%

“…Our first work[50], dedicated to a proof-of-concept to design PVDF/functionalized silica for PEMFC, evidenced that a pre-hydrolysis step was necessary for a proper in situ generation of the functionalized silica according to the reactive processing conditions. Hence, a water/alkoxy ratio (R 0 ) of 0.5 was required for a high sol-gel condensation reaction yield.…”

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confidence: 99%

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New fluorinated polymer- based nanocomposites via combination of sol -gel chemistry and reactive extrusion for polymer electrolyte membranes fuel cells (PEMFCs)

Seck

Magana

Prébé

et al. 2020

Materials Chemistry and Physics

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Proton exchange membranes designed via reactive extrusion from the in situ generation of functional silica-like particles in a new poly(vinylidene fluoride-co-hexafluoropropylene (poly(VDF-co-HFP)) copolymer are presented. These sulfonic acid-functionalized polysiloxane-based fillers were synthesized via sol-gel chemistry from 3mercaptopropyltri(ethoxy)silane and polydimethoxysiloxane in the molten PVDF-co-HFP polymer. To process such nanocomposites materials, the reactive extrusion parameters were selected to (i) reach silanol condensation extents in the processing conditions of a conventional poly(VDF-co-HFP) copolymer and (ii) obtain a surface functionalization high enough with respect to reach a suitable protonic conductivity value of the nanocomposites films. Nevertheless, the enhancement of the proton conductivity being deeply associated with the morphologies of the nanocomposites materials (i.e. the dispersed functional silica phase need to display the larger interface area with the polymer matrix), an interfacial agent was synthesized. This compatibilizer was either poly(VDF-co-α-trifluoromethacrylic acid) or poly(VDF-co-MAF) copolymers or a poly(VDF-co-HFP) copolymer grafted with maleic anhydride, denoted poly(VDF-co-HFP)-g-MA. In a second step, to obtain the required sulfonic acid-functionalized silica dispersed phase from the presence of the mercaptan functions, the resulting films were oxidized. Electrochemical properties were evaluated: for a theoretical ionic exchange capacity (IEC) of 2 meq.g-1 , while experimental IEC ranged between 1.0 and 1.3 meq.g-1. The proton conductivity was found to reach 78 mS.cm-1 at room temperature for 100% of relative humidity. Interestingly, these values are higher than those of the same membranes processed without any compatibilizer (54 mS.cm-1) and to that of Nafion ® NR112 (52 mS.cm-1). This approach also allows limiting the swelling (or water uptake) of proton conductive membranes below 15wt% while it reachs 30 wt% for Nafion ® NR112 in similar conditions.

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PVDF-HFP/silica-SH nanocomposite synthesis for PEMFC membranes through simultaneous one-step sol–gel reaction and reactive extrusion

Cited by 19 publications

References 47 publications

6. Recent advances in the reversible deactivation radical (co)polymerization of fluorinated alkenes/acrylates/ methacrylates/styrenes

6. Recent advances in the reversible deactivation radical (co)polymerization of fluorinated alkenes/acrylates/ methacrylates/styrenes

Proton Conductive Membranes from Covalently Cross‐Linked Poly(Acrylate)/Silica Interpenetrating Networks

New fluorinated polymer- based nanocomposites via combination of sol -gel chemistry and reactive extrusion for polymer electrolyte membranes fuel cells (PEMFCs)

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