Preparation and Characterization of Varying Carbon Black Particle Sizes on Poly(Epichlorohydrin) Elastomer: II. Effect of Damping and Temperature Scanning Stress Relaxation Properties

Year 2025, Volume: 8 Issue: 2, 175 - 184

Davut Aksüt

Abstract

This study investigates the influence of carbon black (CB) particle size on the curing behavior, damping characteristics, and temperature scanning stress relaxation (TSSR) properties of poly(epichlorohydrin) (H55) elastomers. Curing analysis using a moving die rheometer (MDR) at 200 °C revealed that the addition of CB significantly reduces the scorch time (ts2) from 5.05 min (unfilled H55) to 0.83 min for H55-N330, as well as the optimum cure time (t90) from 8.85 min to 2.21 min. The ΔTorque values increased nearly threefold from 2.73 dNm (H55) to 7.87 dNm (H55-N330), indicating a substantial rise in crosslink density. Cyclic compression tests demonstrated enhanced hysteresis behavior and energy dissipation with CB reinforcement. The highest relative hysteresis loss (tan δ) was observed in CB-filled blends, with a notable decline for the smallest particle size (N550), indicating a stronger filler-matrix interaction and reduced internal friction. TSSR results showed that initial stress (σs) increased from 0.15 MPa (H55) to 0.85 MPa (H55-N330), and crosslink density (v) rose from 20.9 mol/m³ to 77.3 mol/m³ (H55-N550). Furthermore, the relaxation rate was inversely related to particle size, with the smallest particles (N220) yielding the fastest relaxation and lowest TSSR index (RI = 0.54). These findings provide valuable insights for optimizing filler characteristics to enhance mechanical damping and stress relaxation in high-performance elastomer applications.

Keywords

polyepichlorohydrin, Carbon Black, Damping properties, Temperature Scanning Stress Relaxation, cyclic loading

Thanks

Dr. Davut Aksüt would like to thank Dr. Murat Şen for his helpful discussions.

References

• Aksüt, D. (2025). Preparation and Characterization of Varying Carbon Black Particle Sizes on Poly(Epichlorohydrin) Elastomer: I. Improving of Curing Kinetics and Mechanical Properties. Journal of the Turkish Chemical Society Section B: Chemical Engineering, 8(1), 123-136. https://doi.org/10.58692/jotcsb.1633684
• Al-Nesrawy, S., Al-Maamori, M. H., & Jappor, H. (2016). Effect of temperature on rheological properties of sbr compounds reinforced by some industrial scraps as a filler. International Journal of Chemical Sciences. 2016. 14-1285. https://www.researchgate.net/publication/308983634_Effect_of_temperature_on_rheological_properties_of_sbr_compounds_reinforced_by_some_industrial_scraps_as_a_filler
• Babapour, A., Şen, M. (2024), ” Effect of silica type. content. and silanization on the curing. mechanical and energy dissipation properties of poly (epichlorohydrin-co-ethylene oxide-co-allyl glycidyl ether) elastomers”. European Polymer Journal, 206 (2024) 112774. https://doi.org/10.1016/j.eurpolymj.2024.112774
• Balasooriya, W., Schrittesser, B., Pinter, G., Schwarz, T., & Conzatti, L. (2019). The Effect of the Surface Area of Carbon Black Grades on HNBR in Harsh Environments. Polymers, 11(1), 61. https://doi.org/10.3390/polym11010061
• Barbe. A., Bökamp. K., Kummerlöwe. C., Sollmann. H., Vennemann. N., & Vinzelberg. S. (2005). Investigation of modified SEBS-based thermoplastic elastomers by temperature scanning stress relaxation measurements. Polymer Engineering & Science. 45(11). 1498–1507.. https://doi.org/10.1002/pen.20427
• Burgaz, E., & Goksuzoglu, M. (2020). Effects of magnetic particles and carbon black on structure and properties of magnetorheological elastomers. Polymer Testing. DOI:10.1016/j.polymertesting.2019.106233
• Chatterjee, T., N. Vennemann, K. Naskar,(2017).“Temperature scanning stress relaxation measurements: a unique perspective for evaluation of the thermomechanical behavior of shape memory polymer blends, J. Appl. Polym. Sci. 135 45680, https://doi.org/10.1002/app.45680.
• Diani, J., B. Fayolle, P. Gilormini, A review on the Mullins effect, European Polymer Journal, 45 601–612, 2009. https://doi.org/10.1016/j.eurpolymj.2008.11.017.
• Fan, L., Wang, G., Wang, W., Lu, H., Yang, F., & Zhang, Y. (2019). Size effect of carbon black on the structure and mechanical properties of magnetorheological elastomers. Journal of Materials Science. DOI:10.1007/s10853-018-2898-8
• Gent, A.N. (1974). Energy dissipation in stretching filled rubbers. Journal of Applied Polymer Science, 18: 1397–1406. https://doi.org/10.1002/app.1974.070180510
• Ismail, H., R Nordin, A.M Noor,“ Cure characteristics, tensile properties and swelling behavior of recycled rubber powder-filled natural rubber compounds, “Polymer Testing, Volume 21, Issue 5, 2002, Pages 565–569. https://doi.org/10.1016/S0142-9418(01)00125–8.
• Ismaıl, H., P. K. Freakley And E. Sheng, (1994),The Effect of Carbon Black Partıcle Sıze on Multifunctional Additive-Carbon Black Interaction”,Eur. Polym. J. Vol. 31, No. II, pp. 1049-1056, 1995.
• Katbab, A. A., Nazockdast, H., & Karrabi, M. (2000). Carbon black‐reinforced dynamically cured EPDM/PP thermoplastic elastomers: Morphology, rheology, and dynamic mechanical properties. Journal of Applied Polymer Science. DOI:10.1002/(SICI)1097-4628(20000228)75:9%3C1127::AID-APP5%3E3.0.CO;2-2
• Kato, A., Ikeda, Y., Kohjiya, S., 2018. Reinforcement mechanism of carbon black (CB) in natural rubber vulcanizates: relationship between CB aggregate and network structure and viscoelastic properties. Polymer-Plastics Technol. Eng. 57 (14), 1418e1429. https://doi.org/10.1080/03602559.2017.1381257.
• Lu, S., & Chung, D. D. L. (2013). Viscoelastic behavior of carbon black and its relationship with the aggregate size. Carbon. DOI:10.1016/j.carbon.2013.03.007
• Meier, J. G., & Klüppel, M. (2008). Carbon black networking in elastomers monitored by dynamic mechanical and dielectric spectroscopy. Macromolecular Materials and Engineering. DOI:10.1002/mame.200700228
• Mujtaba, A. (2014). Viscoelasticity of filled elastomers. Halle University. https://opendata.uni-halle.de/bitstream/1981185920/8048/1/Doktorarbeit_Anas%20Mujtaba2014.pdf
• Mullins, L. (1969). Softening of rubber by displacement. Rubber Chemistry and Technology, 42(2), 339–362. DOI:10.5254/1.3539210
• Norbert, V. (2012). Characterization of Thermoplastic Elastomers by Means of Temperature Scanning Stress Relaxation Measurements. InTech. doi: 10.5772/35976
• Persson, A. M. M. R., Andreassen, E. (2022). Cyclic compression testing of three elastomer types—a thermoplastic vulcanizate elastomer, a Liquid silicone rubber, and two ethylene-propylene-diene rubbers. Polymers, 14, 1316. https://doi.org/10.3390/polym14071316
• Plagge, J., Andrej Lang,(2021).”Filler-polymer interaction investigated using graphitized carbon blacks: Another attempt to explain reinforcement”, Polymer, Volume 218, 2021,123513. https://doi.org/10.1016/j.polymer.2021.123513.
• Pöschl, M., Vašina, M., Zádrapa, P., Měřínská, D., & Žaludek, M. (2020). Study of Carbon Black Types in SBR Rubber: Mechanical and Vibration Damping Properties. Materials, 13(10), 2394. https://doi.org/10.3390/ma13102394
• Reyes, S. (2024). Numerical and Experimental Analysis of Earthquake Protection Systems Based on Elastomeric Spheres. https://doi.org/10.3929/ethz-b-000699146
• Reyes, S., Lopez, E. L., & Vassiliou, M. F. (2024). Modeling of a thermoplastic-polyurethane and its potential for energy dissipation devices. 18th World Conference on Earthquake Engineering. https://doi.org/10.3929/ethz-b-000698028
• Sirisinha, C., & Prayoonchatphan, N. (2001). Study of carbon black distribution in BR/NBR blends based on damping properties. Journal of Applied Polymer Science. DOI:10.1002/app.1773
• Vašina, M., Pöschl, M., Zádrapa, P., & Měřínská, D. (2020). Study of carbon black types in SBR rubber: mechanical and vibration damping properties. Materials. DOI:10.3390/ma13102394