The effect of annealing PVDF at temperatures above T g and below T m was investigated by differential scanning calorimetry (DSC), thermostimulated current spectroscopy (TSC) and solidstate NMR. This study evidences a progressive structural evolution, taking place during such annealing. Its characteristics (kinetics and its temperature dependence, lack of reversibility at lower temperature over extended periods of time, double organization corresponding to double annealing with unmodified kinetics) point to a mechanism of secondary crystallization as described by Marand et al. In addition to the formation of extra crystalline (hence rigid) material, this phenomenon is believed to generate increasing conformational constraints in the residual amorphous material. Accordingly, a progressive reduction of the molecular mobility was demonstrated by NMR during annealing.
This article is dedicated to the study of the thermal parameters of composite materials. A nonlinear least-squares criterion is used on experimental transfer functions to identify the thermal conductivity and the diffusivity of aluminum-polymer composite materials. The density measurements were achieved to deduce the specific heat and thereafter they were compared to values given by differential scanning calorimetry measurement. The thermal parameters of the composite material polypropylene/aluminum were investigated for the two different types of aluminum filler sizes. The experimental data were compared with several theoretical thermal conductivity prediction models. It was found that both the Agari and Bruggeman models provide a good estimation for thermal conductivity. The experimental values of both thermal conductivity and diffusivity have shown a better heat transport for the composite filled with large particles.
A periodic method is used to determine simultaneously both thermal conductivity and diffusivity of various polymer materials at room temperature. The sample is placed between two metallic plates and temperature modulation is applied on the front side of one of the metallic plates. The temperature at the front and rear sides of both plates is measured and the experimental transfer function is calculated. The theoretical thermal heat transfer function is calculated by the quadrupole method. Thermal conductivity and diffusivity are simultaneously identified from both real and imaginary parts of the experimental transfer function. The thermophysical parameters of several polymer samples (PTFE, PVDF and PA11) with different thicknesses (respectively, 5 mm, 2 mm and 300 µm) were studied and compared with values from the literature. The values identified for the thermal parameters are in good agreement with values from the literature for PTFE and PVDF samples; however, we show that the method reaches its limit for the thinner PA11 sample, owing to inadequacy of the thermal model.
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