Abstract
AbstractThe glass transition is relevant for performance definition in rubber products. For extrapolation to high‐frequency behavior, time–temperature superposition is usually assumed, although most complex rubber compounds might be outside of its area of validity. Fast differential scanning calorimetry (FDSC) with cooling rates up to 1500 K/s and broadband dielectric spectroscopy (BDS) with frequencies up to 20 MHz are applied here to directly access both kinetics and dynamics of glass formation in a wide frequency range. For the first‐time, the relation between the thermal vitrification and the dielectric relaxation is studied on vulcanized styrene‐butadiene rubber, showing that both cooling rate and frequency dependence of its glass transition can be described by one single Vogel‐Fulcher‐Tammann‐Hesse equation. The results indicate the validity of the Frenkel‐Kobeko‐Reiner equation. Another focus is the sample preparation of vulcanized elastomers for FDSC and BDS as well as the temperature calibration below 0°C.
Highlights
The analysis of the kinetics of the glass transition of elastomers is important for studying the influence of the molecular structure,[1,2] the network system,[3] and the polymer filler interaction[4,5] on the vitrification
The glass transition is usually measured with conventional differential scanning calorimetry (DSC)
The dynamics of the glass transition are widely studied by conventional dynamic mechanical analysis (DMA) typically up to frequencies of 100 Hz
Summary
The analysis of the kinetics of the glass transition of elastomers is important for studying the influence of the molecular structure,[1,2] the network system,[3] and the polymer filler interaction[4,5] on the vitrification. There are many reports of FDSC measurements of the cooling rate dependence of vitrification on polymers with a high-glass transition temperature (thermoplastics).[21,24,25,26] To the best of our knowledge, FDSC measurements on vulcanized rubbers have not been previously published.
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