Nonuniformity in Cross-Linked Natural Rubber as Revealed by Contrast-Variation Small-Angle Neutron Scattering

Suzuki, Toshiharu; Osaka, Noboru; Endo, Hitoshi; Shibayama, Mitsuhiro; Ikeda, Yuko; Asai, H.; Higashitani, Norihito; Kokubo, Yota; Kohjiya, Shinzo

doi:10.1021/ma9019416

Cited by 49 publications

(28 citation statements)

References 47 publications

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“…The DCP crosslinked HNBR showed the strong upturn in the low q region and the intensity increased as the amount of DCP increased [Figure 7(a)]. This strong upturn in the crosslinked rubber originates from the spatially heterogeneous network structure induced during the crosslinking reaction 6, 8, 37, 38. Therefore, a large spatial heterogeneity exists in the DCP crosslinked HNBR and it increases as the amount of DCP increases.…”

Section: Resultsmentioning

confidence: 99%

“…The scattering profiles were then analyzed by fits using the Debye‐Bueche equation6, 8: where Ξ is the characteristic size of the heterogeneous network structure originating from the density difference between the densely crosslinked region and the loosely crosslinked one *. In Figure 8 is shown the Ξ as a function of the amount of the crosslinker.…”

Section: Resultsmentioning

confidence: 99%

“…By crosslinking the rubber, the stable and three‐dimensional network structure is formed. The network structure can be changed by using different crosslinking agents 1–8. The mechanical properties of the crosslinked rubbers depend on the network structure; i.e., the elastic modulus and the recovery deformation behavior are improved due to the enhanced entropic elasticity by network structure 9–14…”

Section: Introductionmentioning

confidence: 99%

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Mechanical properties and network structure of phenol resin crosslinked hydrogenated acrylonitrile‐butadiene rubber

Osaka

Kato

Saito

2013

J of Applied Polymer Sci

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The tough and stretchable crosslinked hydrogenated acrylonitrile-butadiene rubber (HNBR) could be prepared by resol type phenol resin as a crosslinker. The mechanical properties and the network structure of the phenol resin crosslinked HNBR were investigated by comparing with those of the peroxide crosslinked HNBR having the higher crosslink density and the heterogeneous network structure. The elastic modulus and the strain at break of the phenol resin crosslinked HNBR were much higher than those of the peroxide one. The residual strain was below 20 % after stretching up to 650 % and then releasing from the cramps. Since the crosslink density is low, the high elastic modulus and the good recovery deformation are attributed to the stiffness and rigidity of the crosslink junctions obtained by phenol resin. Small-angle X-ray scattering measurements revealed that the network structure is spatially homogeneous and the results of the wide angle X-ray diffraction indicate that the strain-induced crystallization is suppressed, which enable the longer elongation.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Mechanical properties and network structure of phenol resin crosslinked hydrogenated acrylonitrile‐butadiene rubber

Osaka

Kato

Saito

2013

J of Applied Polymer Sci

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“…In addition, for multicomponent systems, contrast variation 1 permits for instance to selectively extinguish the signal of one of the component allowing one to selectively probe specific objects in multicomponent samples, e.g. the shell or the core of core-shell particles 2 , the nanoparticles and polymers in nanocomposites gels 3 , or the network heterogeneities in natural rubber 4 . Contrast variation has also been proven as a powerful technique to study biological structures in dilute regime 5 , including protein-protein, proteinribosome, and protein-DNA complexes 5,6 or larger complexes as caseins 7 .…”

Section: Introductionmentioning

confidence: 99%

Small angle neutron scattering contrast variation reveals heterogeneities of interactions in protein gels

Banc

Charbonneau²,

Dahesh

et al. 2016

Soft Matter

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“…I have not mentioned the analysis of the network structure of rubber by scattering methods, but this is an important subject in rubber-filler systems. [78][79][80] In particular, the inhomogeneity of the network at the micron scale should be clarified.…”

Section: Resultsmentioning

confidence: 99%

Analysis of structures of rubber-filler systems with combined scattering methods

Takenaka

2012

Polym J

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This review presents an analysis of the hierarchical structures formed in rubber-filler systems by using combined scattering methods. The combined scattering methods utilize various scattering methods and are powerful tools for the quantitative characterization of hierarchical structures over a wide range of length scales, ranging from nanometers to micrometers. Scattering theories for the analysis of the experimental scattering functions and their applications are described. Polymer Journal (2013) 45, 10-19; doi:10.1038/pj.2012.187; published online 21 November 2012Keywords: combined scattering methods; hierarchical structure; rubber-filler systems INTRODUCTION Rubber-filler systems have been widely used in industrial applications, such as for tires and belts so on. 1-6 The use of fillers in rubber compounds reinforces the rubber material and improves the barrier properties. There are several important factors for controlling the efficiency of rubber reinforcement by fillers. The dispersion of filler particles in the rubber matrix is one of the most important factors in this process. Typically, following the use of conventional compounding processes, the fillers are not dispersed homogeneously and form hierarchical structures within the rubber matrices. For example, in rubber-carbon black (CB) systems, the CB primary particles are not distributed independently but coalesce into aggregates, which are indestructible units of CB, during conventional compounding processes. 2 The aggregates of CB, which are called aggregates or agglomerates, can also lead to the formation of hierarchical structures, which consist of higher levels of ordered structure. 2 It is believed that the hierarchical structures affect the efficiency of filler reinforcement. Other rubber-filler systems also form hierarchical structures; furthermore, the characteristic lengths and morphologies of each level of ordered structure, such as agglomerates, vary with the specific combination of rubber and filler used in the system in addition to the compounding processes. To analyze the hierarchical structure, scattering techniques are one of useful techniques. In scattering experiments, we investigated the angular dependence of the scattered intensities induced by the incident beam hitting samples. Although the interpretation of the scattering intensities is complicated, nonetheless, scattering techniques are suitable for obtaining the statistical features of rubber-filler systems. However, the length scales of the hierarchical structures can extend from nanometers to micrometers, which prevents the characterization

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Nonuniformity in Cross-Linked Natural Rubber as Revealed by Contrast-Variation Small-Angle Neutron Scattering

Cited by 49 publications

References 47 publications

Mechanical properties and network structure of phenol resin crosslinked hydrogenated acrylonitrile‐butadiene rubber

Mechanical properties and network structure of phenol resin crosslinked hydrogenated acrylonitrile‐butadiene rubber

Small angle neutron scattering contrast variation reveals heterogeneities of interactions in protein gels

Analysis of structures of rubber-filler systems with combined scattering methods

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