Abstract
Despite the large use of differential scanning calorimetry (DSC) technique in advanced polymer materials characterization, the new methodology called DSC in high heating rates was developed. The heating rate during conventional DSC experiments varying from 10 to 20oC.min -1 , sample mass from 10 to 15mg and standard aluminum sample pan weighting, approximately, 27mg. In order to contribute to a better comprehension of DSC behavior in different heating rates, this work correlates as high heating rate infl uences to the thermal events in DSC experiments. Samples of metallic standard (In, Pb, Sn and Zn) with masses varying from 0.570mg to 20.9mg were analyzed in multiples sample heating rate from 4 to 324°C. min -1 . In order to make properly all those experiments, a precise and careful temperature and enthalpy calibrations were performed and deeply discussed. Thus, this work shows a DSC methodology able to generate good and reliable results on experiments under any researcher choice heating rates to characterize the advanced materials used, for example, for aerospace industry. Also it helps the DSC users to fi nd in their available instruments, already installed, a better and more accurate DSC test results, improving in just one shot the analysis sensitivity and resolution. Polypropylene melting and enthalpy thermal events are also studied using both the conventional DSC method and high heating rate method.
Highlights
In recent years, the fast development in science and technology of materials has improved the production of new products for the aerospace industry
The most commonly technique used in characterization of polymeric matrices is the thermal analyses, the differential scanning calorimetry (DSC)
A proper temperature calibration for high heating rates experiments consists of performing a conventional DSC calibration in an extended temperature range, utilizing primary metallic standards, which have a precise and clear thermal transition in the temperature range of interest
Summary
The fast development in science and technology of materials has improved the production of new products for the aerospace industry. Among them the advance in polymeric composites are an example of recognized success. It is necessary there are techniques to be able to characterize these new polymeric materials in the adequate way. The most commonly technique used in characterization of polymeric matrices is the thermal analyses, the differential scanning calorimetry (DSC). DSC is a thermal analysis technique that measures the difference in energy provided to a sample and a reference material in function of a controlled temperature programming. This technique keeps constant the heat supplied to the sample and reference. The record of the DSC curve is expressed in terms of heat flow versus temperature or time (Vasconcelos, 2010)
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