Filler–elastomer interaction in model filled rubbers, a 1H NMR study

Berriot, Julien; Lequeux, François; Monnerie, L.; Montès, H.; Long, Didier; Sotta, Paul

doi:10.1016/s0022-3093(02)01552-1

Cited by 170 publications

(187 citation statements)

References 16 publications

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“…(ii) Gaussian decay, 41 which is a common shape for dipolar-broadened lines in solids, but not the correct function when molecular motions are significant; (iii) Weibull distribution, 37,42 a very general empirical line shape; (iv) normal and log-normal distributions functions; 36 and (v) more complicated equations such as the relaxation function proposed by Cohen-Addad 43 or having different decay functions (not just different time constants) for the mobile and (presumed) immobilized fraction. [44][45][46] We demonstrate the problem with this approach by fitting FID curves reported by Kaufman et al 39 for BR with 50 phr SAF carbon black. The original authors fit the relaxation to two exponential functions.…”

Section: Nuclear Magnetic Resonancementioning

confidence: 90%

Glass Transition and Interfacial Segmental Dynamics in Polymer-Particle Composites

Robertson

Roland

2008

Rubber Chemistry and Technology

150

125

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We review the literature concerned with the effect of proximity to a filler surface on the local segmental mobility of polymer chains. This mobility is commonly assessed from either the glass transition temperature, Tg, or the segmental relaxation times measured by mechanical, dielectric, or NMR spectroscopy. Published studies report increases, decreases, or no change in Tg upon the addition of carbon black, silica, and other reinforcing fillers. Similarly, the segmental relaxation times have been found to increase or be invariant to the presence of nanometer-sized particles. Some of these discrepancies can be ascribed to ambiguous methods of data analysis; others likely reflect the variation in filler-polymer interaction among different systems. There are unequivocal examples of polymers that have segmental dynamics and glass transitions unaffected by nano-particle reinforcement. However, the general principles governing the behavior remain to be clarified, with further work, focusing on the micromechanics at the particle interface, required for resolution of this important aspect of rubber science and technology.

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Section: Nuclear Magnetic Resonancementioning

confidence: 90%

Glass Transition and Interfacial Segmental Dynamics in Polymer-Particle Composites

Robertson

Roland

2008

Rubber Chemistry and Technology

150

125

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“…Bare oxide fillers such as silica and alumina, displaying surface hydroxy groups, interact favorably with polymers capable of acting as hydrogen-bond acceptor, such as poly(dimethyl siloxane), PDMS, [8][9][10] poly(ethylene oxide), PEO, [11][12][13][14][15] poly(2-vinyl pyridine), P2VP, 16,17 or different acrylate polymers. 5,[18][19][20][21][22] The amount of dynamically modified polymer, and with this the nominal thickness of an assumed-to-be contiguous reduced-mobility layer, can be estimated on the basis of results from different techniques. Such results are often not compatible with each other even for virtually the same polymer-surface a) Electronic address: kay.saalwaechter@physik.uni-halle.de.…”

Section: Introductionmentioning

confidence: 99%

“…URL: www.physik.uni-halle.de/nmr system and the same method. [12][13][14] In this context DSC, 10,16,19 dielectric spectroscopy, 23,24 NMR spectroscopy, 13,18,20,21 and static 22 as well as dynamic 9,11,12,14,15 neutron scattering techniques have been used. Apart from purely structural (=density) information obtained by static scattering, 22 most other techniques are sensitive to dynamic properties.…”

Section: Introductionmentioning

confidence: 99%

“…For example, the notion of a "glassy layer" has emerged 1,4,13,18,20 but is subject to ambiguity as this implies literally that the reduced-mobility components are below their T g , i.e., have a cooperative segmental relaxation time (τ α ) of at least 100 s at the temperature of measurement, and may exhibit only rather localized faster motions ( β and higher relaxations). Therefore, conclusions based upon neutron-scattering observations at comparably high temperatures, stating the absence of a "glassy" layer 9 or even claiming "contradiction" 14 to earlier NMR results, 13 originate partially from the simplistic nomenclature and, specifically, a lack of a more detailed discussion of the layer properties in Ref.…”

Section: Introductionmentioning

confidence: 99%

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Reduced-mobility layers with high internal mobility in poly(ethylene oxide)–silica nanocomposites

Golitsyn

Schneider

Saalwächter

2017

The Journal of Chemical Physics

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A series of poly(ethylene oxide) nanocomposites with spherical silica was studied by proton NMR spectroscopy, identifying and characterizing reduced-mobility components arising from either roomtemperature lateral adsorption or possibly end-group mediated high-temperature bonding to the silica surface. The study complements earlier neutron-scattering results for some of the samples. The estimated thickness of a layer characterized by significant internal mobility resembling backbone rotation ranges from 2 nm for longer (20 k) chains adsorbed on 42 nm diameter particles to 0.5 nm and below for shorter (2 k) chains on 13 nm particles. In the latter case, even lower adsorbed amounts are found when hydroxy endgroups are replaced by methyl endgroups. Both heating and water addition do not lead to significant changes of the observables, in contrast to other systems such as acrylate polymers adsorbed to silica, where temperature-and solvent-induced softening associated with a glass transition temperature gradient was evidenced. We highlight the actual agreement and complementarity of NMR and neutron scattering results, with the earlier ambiguities mainly arising from different sensitivities to the component fractions and the details of their mobility.

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“…So far, serious attempts to investigate the reinforcing mechanism in polymer nanocomposites have been predominantly restricted to systems with amorphous matrices [1][2][3][4][5][6][7][8][9][10][11][12][13][14]. In these matrices above their T g , the chains can undergo segmental immobilization induced even by weak interactions on the large filler-matrix internal interface.…”

Section: Introductionmentioning

confidence: 99%

Effect of weakly interacting nanofiller on the morphology and viscoelastic response of polyolefins

Kalfus

Jančář

Kučera

2008

Polymer Engineering & Sci

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Effect of silica nanofiller on the deformation response and morphology of low-and high-density polyethylene (HDPE, LDPE) and isotactic polypropylene (PP) modified with fumed silica was investigated. The dynamicmechanical thermal spectroscopy, differential scanning calorimetry, optical microscopy, and density measurements were carried out to determine the temperature dependence of storage and loss moduli as well as nanocomposite morphology. It was demonstrated that the degree of matrix reinforcement is considerably affected by the extent of matrix crystallinity, especially, in the temperature range from (T m -1308C) to T m . Based on experimental evidence and literature review, it is proposed that this phenomenon may be attributed to the alpha-mechanical relaxation process occurring above matrix T g . As a result of adding silica into the melted matrix, mobility of chains in contact with silica particles became reduced. This caused substantial changes in morphology of these semicrystalline nanocomposites.

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Filler–elastomer interaction in model filled rubbers, a 1H NMR study

Cited by 170 publications

References 16 publications

Glass Transition and Interfacial Segmental Dynamics in Polymer-Particle Composites

Glass Transition and Interfacial Segmental Dynamics in Polymer-Particle Composites

Reduced-mobility layers with high internal mobility in poly(ethylene oxide)–silica nanocomposites

Effect of weakly interacting nanofiller on the morphology and viscoelastic response of polyolefins

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