Abstract
Thermal cycling of an epoxy coating on silicon through the glass transition temperature (T g) revealed a large stress hysteresis on the first thermal cycle through T g and a change in the stress–temperature slope at T g resulting from the change in the epoxy elastic properties due to the glass transition. This stress hysteresis was not observed on subsequent thermal cycles through T g. However, after the coating was annealed (aged) below T g (for hours or longer)—during which the stress relaxed exponentially with time—the stress hysteresis returned. The magnitude of stress hysteresis, on cycling through T g, was found to correlate to the magnitude of long-time relaxation that occurred during annealing at temperatures below T g.
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The author (JT) acknowledges Awirut Maglai for assistance with sample preparation and Bob Matz for helpful discussions.
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Appendix A: Non-linear deformation analysis
Appendix A: Non-linear deformation analysis
The use of Eq. 1 requires that the strains and rotations in the system be infinitesimally small. This requirement was examined using the analysis of Freund et al. [27], who showed that non-linear deformation effects can be avoided if the dimensionless parameters S or K are less than 0.3–0.4 or 0.2, respectively:
and
where ε m is the imposed thermal mismatch strain, R is the sample radius (50 mm), E f is the film Young’s Modulus, and ν is the film Poisson’s Ratio. Since the film mechanical properties are not known, the parameter K was evaluated using the largest change in curvature observed over the course of the experiment, Δκ = 0.02 m−1, to be K = 0.016. As K < 0.2, non-linear deformations were not considered.
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Thurn, J., Hermel-Davidock, T. Thermal stress hysteresis and stress relaxation in an epoxy film. J Mater Sci 42, 5686–5691 (2007). https://doi.org/10.1007/s10853-006-0654-y
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DOI: https://doi.org/10.1007/s10853-006-0654-y