Cavity formation in silica-filled rubber compounds observed during deformation by ultra small-angle x-ray scattering

Research output: Contribution to journalArticleResearchpeer review

Authors

  • Ilya Yakovlev
  • Michael Sztucki
  • Frank Fleck
  • Hossein Ali Karimi-Varzaneh
  • Jorge Lacayo-Pineda
  • Christoph Vatterott
  • Ulrich Giese

Research Organisations

External Research Organisations

  • European Synchrotron Radiation Facility
  • Continental AG
  • German Institute of Rubber Technology (DIK e.V.)
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Details

Original languageEnglish
Article numbere56403
JournalJournal of applied polymer science
Volume142
Issue number4
Early online date30 Oct 2024
Publication statusPublished - 14 Dec 2024

Abstract

When silica-filled rubber compounds are deformed, structural modifications in the material's bulk lead to irreversible damage, the most significant of which is cavitation appearing within the interfaces of interconnected polymer and filler networks. This work introduces a new method to analyze cavitation in industrial-grade rubbers based on ultra small-angle x-ray scattering. This method employs a specially designed multi-sample stretching device for high-throughput measurements with statistical relevance. The proposed data reduction approach allows for early detection and quantification of cavitation while providing at the same time information on the hierarchical filler structures at length scales ranging from the primary particle size to large silica agglomerates over four orders of magnitude. To validate the method, the scattering of SSBR rubber compounds filled with highly dispersible silica at different ratios was measured under quasi-static strain. The strain was applied in incremental steps up to a maximum achievable elongation or breakage of the sample. From the measurements performed in multiple repetitions, it was found that the minimum strain necessary for cavity formation and the size evolution of the cavities with increasing strain are comparable between these samples. The sample with the highest polymer content showed the lowest rate of cavity formation and higher durability of silica structures. The structural stability of the compounds was determined by the evolution of the filler hierarchical structures, obtained by fitting data across the available strain range.

Keywords

    cavitation, filled rubber compounds, in situ straining, ultra small-angle x-ray scattering (USAXS)

ASJC Scopus subject areas

Cite this

Cavity formation in silica-filled rubber compounds observed during deformation by ultra small-angle x-ray scattering. / Yakovlev, Ilya; Sztucki, Michael; Fleck, Frank et al.
In: Journal of applied polymer science, Vol. 142, No. 4, e56403, 14.12.2024.

Research output: Contribution to journalArticleResearchpeer review

Yakovlev I, Sztucki M, Fleck F, Karimi-Varzaneh HA, Lacayo-Pineda J, Vatterott C et al. Cavity formation in silica-filled rubber compounds observed during deformation by ultra small-angle x-ray scattering. Journal of applied polymer science. 2024 Dec 14;142(4):e56403. Epub 2024 Oct 30. doi: 10.48550/arXiv.2407.08541, 10.1002/app.56403
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abstract = "When silica-filled rubber compounds are deformed, structural modifications in the material's bulk lead to irreversible damage, the most significant of which is cavitation appearing within the interfaces of interconnected polymer and filler networks. This work introduces a new method to analyze cavitation in industrial-grade rubbers based on ultra small-angle x-ray scattering. This method employs a specially designed multi-sample stretching device for high-throughput measurements with statistical relevance. The proposed data reduction approach allows for early detection and quantification of cavitation while providing at the same time information on the hierarchical filler structures at length scales ranging from the primary particle size to large silica agglomerates over four orders of magnitude. To validate the method, the scattering of SSBR rubber compounds filled with highly dispersible silica at different ratios was measured under quasi-static strain. The strain was applied in incremental steps up to a maximum achievable elongation or breakage of the sample. From the measurements performed in multiple repetitions, it was found that the minimum strain necessary for cavity formation and the size evolution of the cavities with increasing strain are comparable between these samples. The sample with the highest polymer content showed the lowest rate of cavity formation and higher durability of silica structures. The structural stability of the compounds was determined by the evolution of the filler hierarchical structures, obtained by fitting data across the available strain range.",
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AU - Fleck, Frank

AU - Karimi-Varzaneh, Hossein Ali

AU - Lacayo-Pineda, Jorge

AU - Vatterott, Christoph

AU - Giese, Ulrich

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