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Nanofiller Dispersion in Rubber as Revealed by 3D-TEM

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Reinforcement of Rubber

Abstract

Firstly, it was found that visualization of three-dimensional structure of rubber vulcanizate by 3D-TEM observation necessitated a removal of rubber-soluble zinc compounds, which was derived from ZnO annexed as a vulcanization reagent. The Zn compounds deteriorated the resolution to give enough good resolution for 3-dimensional image construction. Secondly, an experimental method how to remove them on silica-loaded natural rubber vulcanizates was reported. Lastly, the nearest distance (dp) between the silica aggregates in the high-loading region was found 1.3 nm. It was suggested that this dp corresponds to the thickness of the silica/NR interaction layer, i.e., more or less intrinsic bound rubber on particulate silica surface, and the silica network structure in the rubber matrix was clearly visualized. Furthermore, in the case of carbon black (CB), dp in the high loading region was found 3 nm, and the CB network was also visualized. CB network formation was explained by the gelation theory: in the region of CB loading ≦ 20 phr pregel states, and the transition to gel state occurred in the region of CB loading  > 20 phr.

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1 Electronic Supplementary Material

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Video 4.1a: Movie for Fig. 4.4a 3D-TEM image of NR-mix-V. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file1 (AVI 1854 kb)

Video 4.1b: Movie for Fig. 4.4b 3D-TEM image of NR-insitu=V. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file2 (AVI 1858 kb)

Video 4.2a: Movie for Fig. 4.5a NR-mix-V. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file3 (AVI 75265 kb)

Video 4.2b: Movie for Fig. 4.5b NR-insitu-V. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file4 (AVI 75265 kb)

Video 4.3a: Movie for Fig. 4.7a RX10. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

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Video 4.3b: Movie for Fig. 4.7b RX30. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file6 (MPG 28083 kb)

Video 4.3c: Movie for Fig. 4.7c RX80. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

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Video 4.3d: Movie for Fig. 4.7d 10VN. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

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Video 4.3e: Movie for Fig. 4.7e 30VN. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file9 (AVI 1858 kb)

Video 4.3f: Movie for Fig. 4.7f 80VN. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file10 (AVI 1853 kb)

Video 4.4a: Movie for Fig. 4.11a NR-P-10RX. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file11 (AVI 75265 kb)

Video 4.4b: Movie for Fig. 4.11b NR-P-30RX. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file12 (AVI 75265 kb)

Video 4.4c: Movie for Fig. 4.11c NR-P-80RX. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file13 (AVI 75265 kb)

Video 4.4d: Movie for Fig. 4.11d NR-P-10VN. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file14 (AVI 75265 kb)

Video 4.4e: Movie for Fig. 4.11e NR-P-30VN. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file15 (AVI 75265 kb)

Video 4.4f: Movie for Fig. 4.11f NR-P-80VN. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file16 (AVI 75265 kb)

Video 4.5a: Movie for Fig. 4.14a CB-10. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file17 (AVI 1862 kb)

Video 4.5b: Movie for Fig. 4.14b CB-20. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file18 (AVI 1869 kb)

Video 4.5c: Movie for Fig. 4.14c CB-40. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file19 (AVI 1857 kb)

Video 4.5d: Movie for Fig. 4.14d CB-80. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file20 (AVI 1876 kb)

Video 4.6a: Movie for Fig. 4.15a CB-10. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file21 (AVI 75265 kb)

Video 4.6b: Movie for Fig. 4.15b CB-20. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file22 (AVI 75265 kb)

Video 4.6c: Movie for Fig. 4.15c CB-40C. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file23 (AVI 75265 kb)

Video 4.6d: Movie for Fig. 4.15d CB-80. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file24 (AVI 75265 kb)

Video 4.7a: Movie for Fig. 4.18a CB-10. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file25 (AVI 75265 kb)

Video 4.7b: Movie for Fig. 4.18b CB-20. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file26 (AVI 75265 kb)

Video 4.7c: Movie for Fig. 4.18c CB-40. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file27 (AVI 75265 kb)

Video 4.7d: Movie for Fig. 4.18d CB-80. © NISSAN ARC, LTD. ALL RIGHTS RESERVED

Supplementary file28 (AVI 75265 kb)

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Kohjiya, S., Kato, A., Ikeda, Y. (2020). Nanofiller Dispersion in Rubber as Revealed by 3D-TEM. In: Reinforcement of Rubber. Springer Series on Polymer and Composite Materials. Springer, Singapore. https://doi.org/10.1007/978-981-15-3789-9_4

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