The dynamic viscoelasticities of unsupported phenolic-epoxy resin films were studied by using the forced vibration technique of longitudinal deformation.
Epikote # 1009 and a resole-type phenolic resin were mixed at the solids weight ratio of 1/1, precondensed, applied on tin plates by a roller coater and baked at 180°and 210°C for 10 min., which were then kept immersed in mercury to obtain film of about 4.8×52.5×0.0455 mm. The angular frequencies employed ranged from 31.4 to 596 sec
-1, and the temperatures from 82° to 178°C.
The dynamic Young's moduli, E′ (ω), of all the samples increased with increase in angular frequency, and the maxima of loss tangent, tan δ, appeared at the frequencies and temperatures which corresponded to the inflection points of the E′ (ω) curves. These viscoelastic properties resembled those of thermoplastic materials in the glass transition region.
According to the phenomenological theory of linear viscoelasticity, the curves for the dynamic Young's modulus plotted against the angular frequency and those for the loss tangent plotted against the angular frequency can be shifted along the logarithm of frequency axis to form a composite curve of E′ (ω) and that of tan δ. The shift factors, aT, obtained from the dynamic Young's modulus and the loss tangent agreed with one another for both the systems, which suggested that the time-temperature superposition law was applicable to the phenolic-epoxy systems studied.
The activation energy, ΔH, of the shift factor increased as the temperature was lowered, reaching a maximum at a temperature near the glass transition and then decreasing with further decrease in temperature. The glass transition temperatures, at which each activation energy showed a maximum, were 110°C for the system cured at 180°C, and 123°C for the system cured at 210°C. The glass transition temperature increased with the increase in curing temperature, reflecting the increase in crosslinking density.
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