Korea-Australia Rheology Journal, Vol.29, No.3, 157-162, August, 2017
Multi-step cure kinetic model of ultra-thin glass fiber epoxy prepreg exhibiting both autocatalytic and diffusion-controlled regimes under isothermal and dynamic-heating conditions
As packaging technologies are demanded that reduce the assembly area of substrate, thin composite laminate substrates require the utmost high performance in such material properties as the coefficient of thermal expansion (CTE), and stiffness. Accordingly, thermosetting resin systems, which consist of multiple fillers, monomers and/or catalysts in thermoset-based glass fiber prepregs, are extremely complicated and closely associated with rheological properties, which depend on the temperature cycles for cure. For the process control of these complex systems, it is usually required to obtain a reliable kinetic model that could be used for the complex thermal cycles, which usually includes both the isothermal and dynamic-heating segments. In this study, an ultra-thin prepreg with highly loaded silica beads and glass fibers in the epoxy/amine resin system was investigated as a model system by isothermal/dynamic heating experiments. The maximum degree of cure was obtained as a function of temperature. The curing kinetics of the model prepreg system exhibited a multi-step reaction and a limited conversion as a function of isothermal curing temperatures, which are often observed in epoxy cure system because of the rate-determining diffusion of polymer chain growth. The modified kinetic equation accurately described the isothermal behavior and the beginning of the dynamic-heating behavior by integrating the obtained maximum degree of cure into the kinetic model development.
Keywords:cure kinetics;epoxy prepreg;multi-step cure reaction;diffusion-controlled reaction;differential scanning calorimetry
- Fava RA, Polymer, 9, 137 (1968)
- Garschke C, Parlevliet PP, Weimer C, Fox BL, Polym. Test, 32, 150 (2013)
- Halley PJ, Mackay ME, Polym. Eng. Sci., 36(5), 593 (1996)
- Kim J, Moon TJ, Howell JR, J. Compos. Mater., 36, 2479 (2002)
- Kim YC, Min H, Yu J, Suhr J, Lee YK, Kim KJ, Kim SH, Nam JD, Thermochim. Acta, 644, 28 (2016)
- Kubota H, J. Appl. Polym. Sci., 19, 2279 (1975)
- Matsuoka S, Quan X, Bair HE, Boyle DJ, Macromolecules, 22, 4093 (1989)
- Nam JD, Seferis JC, J. Polym. Sci. B: Polym. Phys., 29, 601 (1991)
- Nam JD, Seferis JC, J. Polym. Sci. B: Polym. Phys., 30, 455 (1992)
- Ng H, Manas-zloczower I, Polym. Eng. Sci., 29, 1097 (1989)
- Park IK, Lee DS, Nam JD, J. Appl. Polym. Sci., 84(1), 144 (2002)
- Prime RB, Polym. Eng. Sci., 13, 365 (1973)
- Prime RB, Turi EA, 1981, Thermal characterization of polymeric materials, Turi, EA, Ed 1380.
- Shim HY, Shim JJ, Kang JA, Min HS, 2012, Thermosetting resin composition and prepreg and metal clad laminate using the same, US Patent US9278505 B2.
- Turi EA, 1981, Thermal Characterization of Polymeric Materials, Academic Press, Inc., New York.
- Vyazovkin S, Burnham AK, Criado JM, Perez-Maqueda LA, Popescu C, Sbirrazzuoli N, Thermochim. Acta, 520(1-2), 1 (2011)
- Yousefi A, Lafleur PG, Gauvin R, Polym. Compos., 18, 157 (1997)