Skip to main content
Log in

TEM observation of silane coupling agent in silica-filled rubber tyre compound

  • Original Paper
  • Published:
Journal of Rubber Research Aims and scope Submit manuscript

Abstract

The microdispersion of silica in filled elastomer vulcanisates was evaluated by transmission electron microscopy (TEM)—network visualisation analysis. In this study, the silica is modified with a wide range of coupling and non-coupling silanes. The silica-filled elastomer samples were microtomed using a glass knife. The resulting TEM micrographs were interpreted and characterised based on aggregates with a cross-sectional area larger than 100 nm2. The study showed that silica surface modification has reduced the silica aggregate size by approximately 30–40% compared to an untreated silica-filled elastomer vulcanisate. The TEM micrographs showed evidence of coupling between silica and the elastomer phase and demonstrated a good estimation of silica microdispersion in the elastomer phase. This study has shown that the presence of different surface functionalities has an effect on the silica microdispersion.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10
Fig. 11

Similar content being viewed by others

References

  1. Wang MJ (1998) Effect of polymer–filler and filler–filler interaction on dynamic properties of filled vulcanisates. Rubb Chem Technol 71:520–589

    Article  Google Scholar 

  2. Li YB, Wang MJ, Zhang T, Zhang F, Fu X (1994) Study on dispersion morphology of silica in rubber. Rubb Chem Technol 67:693–699

    Article  Google Scholar 

  3. Julve D, Menendez M, Perez J, Ramos J (2011) Microdispersion of silica in tire tread compounds above the percolation threshold by TEM image measurements. Rubb Chem Technol 84:74–87

    Article  Google Scholar 

  4. Le HH, Ilisch S, Radusch HJ (2009) Characterisation of the effect of the filler dispersion on the stress relaxation behaviour of carbon black filled rubber composites. Polymer 50:2294–2303

    Article  Google Scholar 

  5. Le HH, Tiwari M, Ilish S, Radusch HJ (2005) Effect of molecular structure on carbon black dispersion in rubber compounds. Kaut Gumm Kunst 58(11):575–580

    Google Scholar 

  6. ASTM D2663-14 (2014) Standard test methods for carbon black—dispersion in rubber. ASTM International, West Conshohocken

    Google Scholar 

  7. Otto S, Randl O, Goncalves O, Cantaloube B (2005) New reference value for the description of filler dispersion with the dispergrader 1000 NT. Kaut Gumm Kunst 58:390–393

    Google Scholar 

  8. ASTM D7723-17 (2018) Standard Test method for rubber property-macro-dispersion fillers in compounds. ASTM International, West Conshohocken

  9. Putman MC, Putman JB (2007) High resolution reflected light microscopy to determine filler micro-dispersion. Paper 103 Presented at Fall Technical Meeting of the Rubber Division of American Chemical Society, October 17, Cleveland, Ohio

  10. Bielinski D, Slusarski L, Dobrowolski O, Dryzek E (2004) Studies of filler agglomeration by atomic force microscopy and positron annihilation spectroscopy. Part 1: silica filled compounds. Kaut Gumm Kunst 11:579–586

    Google Scholar 

  11. Wang CC, Wu SH, Donnet JB, Wang TK (2006) Microdispersion of carbon blacks in rubber. Kaut Gumm Kunst 59:466–472

    Google Scholar 

  12. Chapman AV, Cook S, Davies RT, Patel J, Clark JL (2009) Microdispersion of silica in tire tread compounds based on epoxidized natural rubber. Paper 73 Presented at the Fall Technical Meeting of the Rubber Division of the American Chemical Society, 12–15 October 2009, Pittsburg

  13. Sarkawi SS, Dierkes WK, Noordermeer JMW (2014) Elucidation of filler-to-filler and filler-to-rubber interactions in silica-reinforced natural rubber by TEM network. Eur Polym J 54:118–127

    Article  Google Scholar 

  14. Sarkawi SS, Kaewsakul W, Sahakaro K, Dierkes WK, Noordermeer JMW (2015) A Review on reinforcement of natural rubber by silica fillers for use in low-rolling resistance tyres. J Rubb Res 18(4):203–233

    Google Scholar 

  15. Sarkawi SS, Dierkes WK, Noordermeer JMW (2015) Morphology of silica-reinforced natural rubber: the effect of silane coupling agent. Rubb Chem Technol 88(3):359–372

    Article  Google Scholar 

  16. Sarkawi SS, Dierkes WK, Noordermeer JMW (2014) Effect of a silane coupling agent on the morphology of silica reinforced natural rubber. Kaut Gumm Kunst 3:29–33

    Google Scholar 

  17. Ngeow YW, Chapman AV, Heng JYY, Williams DR (2016) Characterization of silica modified with silanes using thermogravimetric analysis combined with infrared detection. Paper 67 presented at the Fall 190th Technical Meeting of the Rubber Division of the American Chemical Society, Pittsburgh, PA

  18. Ngeow YW, Chapman AV, Heng JYY, Williams DR (2018) Characterization of silica modified with silanes by using thermogravimetric analysis combined with infrared detection. Rubb Chem Technol. https://doi.org/10.5254/rct.18.82626

    Google Scholar 

  19. Martin P, Brown P, Chapman AV, Cook S (2015) Silica-reinforced epoxidised natural rubber tire treads—performance and durability. Rubb Chem Technol 88:390–411

    Article  Google Scholar 

  20. Castellano M, Conzatti L, Turturro A, Costa G, Busca G (2007) Influence of the silane modifiers on the surface thermodynamic characteristics and dispersion of the silica into elastomer compounds. J Phys Chem B 111:4495–4502

    Article  Google Scholar 

  21. Ladouce-Stelandre L, Bomal Y, Flandin L, Labarre D (2003) Dynamic mechanical properties of precipitated silica filled rubber: influence of morphology and coupling agent. Rubb Chem Technol 76:145–159

    Article  Google Scholar 

  22. Ladouce-Stelandre L, Bomal Y, Flandin L, Labarre D (2000) Dynamic mechanical properties of precipitated silica filled rubber: influence of morphology and coupling agent. Paper 33 presented at the Spring Technical Meeting of the Rubber Division of the American Chemical Society, Dallas

  23. Hidehiko D, Shin H (2007) Locating a silane coupling agent in silica-filled rubber composites by EFTEM. Langmuir 23:12344–12349

    Article  Google Scholar 

  24. Ngeow YW, Heng JYY, Williams DR, Chapman AV (2016) Investigating the effect of silica modification on rubber vulcanisates. In: International rubber conference, Kitakyushu

  25. Blume A (2011) Kinetics of the silica–silane reaction. Kaut Gumm Kunst 64:38–43

    Google Scholar 

  26. Lin CJ, Hergenrother WL, Hilton AS (2002) Mooney viscosity stability and polymer filler interactions in silica filled rubbers. Rubb Chem Technol 75:215–245

    Article  Google Scholar 

  27. Robertson CG, Lin CJ, Bogoslovov RB, Rackaitis M, Sadhukhan P, Quinn JD, Roland CM (2011) Flocculation, reinforcement, and glass transition effects in silica-filled styrene-butadiene rubber. Rubb. Chem. Technol. 84:507–519

    Article  Google Scholar 

  28. Lin CJ, Hergenrother WL, Alexanian E, Bohm GGA (2002) On the filler flocculation in silica-filled rubbers Part I. quantifying and tracking the filler flocculation and polymer–filler interactions in the unvulcanized rubber compounds. Rubb Chem Technol 75:865–890

    Article  Google Scholar 

  29. Scurati A, Lin CJ (2006) The hysteresis temperature and strain dependences in filled rubbers. Rubb Chem Technol 79:170–197

    Article  Google Scholar 

  30. Mahtabani A, Alimardani M, Razzaghi-Kashani M (2017) Further evidence of filler–filler mechanical engagement in rubber compounds filled with silica treated by long chain silane. Rubb Chem Technol 90:508–520

    Article  Google Scholar 

  31. Sato M, Dierkes WK, Blume A (2017) Silane-polymer reaction: investigation of the silane–polymer reaction in a model system. Tire Technol Int 2017:66–70

    Google Scholar 

  32. Sato M (2018) Reinforcing mechanisms of silica/sulfide-silane vs. mercapto-silane filled tire tread compounds. PhD Thesis, The Netherlands: University of Twente

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Y. W. Ngeow.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Ngeow, Y.W., Heng, J.Y.Y., Williams, D.R. et al. TEM observation of silane coupling agent in silica-filled rubber tyre compound. J Rubber Res 22, 1–12 (2019). https://doi.org/10.1007/s42464-019-00005-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s42464-019-00005-y

Keywords

Navigation