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Structure de chaines et particules dans les nanocomposites polymères

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Polymer nanocomposites are materials made of nanoparticles incorporated in a polymer matrix, where the filler particles are usually added to enhance mechanical properties, e.g. of car tire materials [1]. Material performance depends to a great extent on the structure of the filler, i.e. its dispersion state in the polymer matrix, as well as on the physical characteristics (mass, crosslinking, grafting, etc.) and the resulting conformation of the polymer chains. In this talk, we will first discuss how structural information can be extracted from small-angle neutron scattering [2], in particular using deuteration and zero average contrast. We will then present some recent results on chain structure in model nanocomposites [3], with special emphasis on difficulties encountered with contrast-matching in nanocomposites. As an outlook, the audience is invited to participate in a dream of a world where large quantities of deuterated polymer of any kind are available. [1] G. P. Baeza, A. C. Genix, C. Degrandcourt, L. Petitjean, J. Gummel, M. Couty and J. Oberdisse, Macromolecules 2013, 46, 317-329.[2] A.-C. Genix and J. Oberdisse, Structure and dynamics of polymer nanocomposites studied by X-ray and neutron scattering techniques. Current Opinion in Colloid & Interface Science 2015, 20, 293-303.[3] A. Banc, A.-C. Genix, C. Dupas, M. Sztucki, R. Schweins, M.-S. Appavou, J. Oberdisse, Macromolecules 2015, 48, 6596−6605, ILL Highlight.

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Polymer nanocomposites are mixtures of nanoparticles and polymer chains, where the filler particles are usually added to enhance mechanical properties, e.g. of car tire materials. Performance depends to a great extent on the structure of the filler, i.e. its dispersion state in the polymer matrix, which itself depends on mixing protocols, but also on the thermodynamics of the system. The latter can be tuned by performing either chemical surface modifications of the nanoparticles, or by playing with the mass and/or grafting properties of the polymer chains. In this talk, some straightforward ways to obtain information from small-angle scattering on the structure of nanocomposites will be presented [1].In particular, we will review recent results on nanocomposites close to industrial applications, including what is probably one of the first quantitative analyses of such disordered structures by a combination of SAXS, TEM and numerical simulations [2]. The study led to the identification of a unique structure-determining parameter [3]. The generalization of the above-mentioned approach – the correlation hole analysis – will furthermore be illustrated by structural studies by small angle scattering of well-defined model systems, showing the influence of chain mass [4] or surface grafting of small molecules [5]. Finally, a quick outlook on why contrast-matching with SANS in nanocomposites often fails to highlight chain structure will be proposed [6].[1] A.-C. Genix and J. Oberdisse, Structure and dynamics of polymer nanocomposites studied by X-ray and neutron scattering techniques. Current Opinion in Colloid & Interface Science 2015, 20, 293-303.[2] G. P. Baeza, A. C. Genix, C. Degrandcourt, L. Petitjean, J. Gummel, M. Couty and J. Oberdisse, Macromolecules 2013, 46, 317-329.[3] G. P. Baeza, A.-C. Genix, C. Degrandcourt, J. Gummel, A. Mujtaba, K. Saalwächter, T. Thurn-Albrecht, M. Couty, and J. Oberdisse, ACS MacroLetters 2014, 3 (5), 448–452[4] A. Banc, A. C. Genix, M. Chirat, C. Dupas, S. Caillol, M. Sztucki and J. Oberdisse, Macromolecules 2014, 47, 3219–3230.[5] C. Schmitt Pauly, A.-C. Genix, J. G. Alauzun, M. Sztucki, P. H. Mutin and J. Oberdisse, Polymer 2016, 97 138-146.[6] A. Banc, A.-C. Genix, C. Dupas, M. Sztucki, R. Schweins, M.-S. Appavou, J. Oberdisse, Macromolecules 2015, 48, 6596−6605.

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Résumé:

Polymer nanocomposites are mixtures of nanoparticles and polymer chains, where the filler particles are usually added to enhance mechanical properties, e.g. of car tire materials. Performance depends to a great extent on the structure of the filler, i.e. its dispersion state in the polymer matrix, which itself depends on mixing protocols, but also on the thermodynamics of the system. The latter can be tuned by performing either chemical surface modifications of the nanoparticles, or by playing with the mass and/or grafting properties of the polymer chains. In this talk, some straightforward ways to obtain information from small-angle scattering on the structure of nanocomposites will be presented [1]. In particular, we will review recent results on nanocomposites close to industrial applications, including what is probably one of the first quantitative analyses of such disordered structures by a combination of SAXS, TEM and numerical simulations [2]. This analysis will then be applied to the impact of small molecules on such structures [3]. Concerning chain structure, a quick outlook on why contrast-matching with SANS in nanocomposites often fails will be proposed [4]. REFERENCES1.A.-C. Genix and J. Oberdisse, Structure and dynamics of polymer nanocomposites studied by X-ray and neutron scattering techniques. Current Opinion in Colloid & Interface Science 2015, 20, 293-303 (2015).2. G. P. Baeza, A. C. Genix, C. Degrandcourt, L. Petitjean, J. Gummel, M. Couty and J. Oberdisse, Multiscale Filler Structure in Simplified Industrial Nanocomposite Silica/SBR Systems Studied by SAXS and TEM, Macromolecules, 46, 317-329 (2013).3. D. Musino, A.-C. Genix, C. Fayolle, A. Papon, L. Guy, N. Meissner, P. Weda, T. Bizien, T. Chaussée, J. Oberdisse, Synergistic effect of small molecules on large-scale structure of simplified industrial nanocomposites, submitted.4. A. Banc, A.-C. Genix, C. Dupas, M. Sztucki, R. Schweins, M.-S. Appavou, J. Oberdisse, Origin of small-angle scattering from contrast-matched nanoparticles: A study of chain and filler structure in polymer nanocomposites, Macromolecules, 48, 6596−6605 (2015).

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In recent years, materials with enhanced mechanical properties have attracted both fundamental and industrial interest. The present study concerns nanocomposites (NCs) made by dispersion of silica nanoparticles in a soft polymer matrix of styrene/butadiene (SB), which is commonly used in car tires. We work on both a simplified industrial system (solid mixing with millimetric silica pellets) and we developed a model system (solvent casting with surface-modified colloidal silica). The NC characteristics may be tuned by the grafting of silane coating agents (SCAs) which differ in the length of their alkyl groups (different hydrophobicity). These agents may influence filler dispersion via different polymer/filler and filler/filler interactions. The investigation of NC materials is essential for many industrial applications, in particular for the improvement of tire performances from an energetical and climatical point of view.

Ref HAL: hal-01653297_v1
DOI: 10.1039/c7sm01640a
WoS: WOS:000415352100017
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13 Citations
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Quantitative characterization of the average structure of dense nanoparticle assemblies and aggregates is a common problem in nanoscience. Small-angle scattering is a suitable technique, but it is usually limited to not too big assemblies due to the limited experimental range, low concentrations to avoid interactions, and monodispersity to keep calculations tractable. In the present paper, a straightforward analysis of the generally available scattered intensity – even for large assemblies, at high concentrations – is detailed, providing information on the local volume fraction of polydisperse particles with hard sphere interactions. It is based on the identical local structure of infinite homogeneous nanoparticle assemblies and their subsets forming finite-sized clusters. The approach is extended to polydispersity, using Monte-Carlo simulations of hard and moderately sticky hard spheres. As a result, a simple relationship between the observed structure factor minimum – termed the correlation hole – and the average local volume fraction  on the scale of neighboring particles is proposed and validated through independent aggregate simulations. The relationship shall be useful as an efficient tool for the structural analysis of arbitrary aggregated colloidal systems.

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Ref Arxiv: 1811.06903
DOI: 10.1039/c7sm00596b
WoS: WOS:000411436600003
Ref. & Cit.: NASA ADS
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5 Citations
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Vegetable oil based hybrid films were developed thanks to a novel solvent- and heating- free method at the air-water interface using silylated castor oil cross-linked via a sol-gel reaction. To understand the mechanism of the hybrid film formation, the reaction kinetics was studied in detail by using complementary techniques: rheology, thermogravimetric analysis, and infrared spectroscopy. The mechanical properties of the final films were investigated by nano-indentation, whereas their structure was studied using a combination of wide-angle X-ray scattering, electron diffraction, and atomic force microscopy. We found that solid and transparent films form in 24 hours and, by changing the silica precursor to castor oil ratio, their mechanical properties are tunable in the MPa-range by about a factor of twenty. In addition to that, a possible optimization of the cross-linking reaction with different catalysts was explored and finally, cytotoxicity tests were performed on fibroblasts proving the absence of film toxicity. The results of this work pave the way to a straightforward synthesis of castor-oil films with tunable mechanical properties: hybrid films cross-linked at the air-water interface combine an easy and cheap spreading protocol with the features of their thermal history optimized for possible future micro/nano drug loading, thus representing excellent candidates for the replacement of non-environment friendly petroleum-based materials.