We employ a microcalorimeter device to study the thermal decomposition of organic energetic materials at very high heating rates. The compact size of this device enables rapid heating rates and sensitive detection of thermal loads from very small samples. Calibration for the device was done by heating 3 samples with known thermal properties, Sn, KNO3, and KClO4 at the desired heating rates to determine the temperature profile for each rate. The samples: 5-amino-1H-tetrazole, 5-amino-1-methyl-1H-tetrazolium dinitramide, 1,5-diamino-4-methyl-1H-tetrazolium dinitramide, and 1,5-diamino-4-methyl-1H-tetrazolium azide, were all tested at four heating rates ranging from ~1,300-29,000 oC/s. These heating rates are orders of magnitude greater than those used in traditional DSC experiments, and the unique thermal signatures can be compared in the different heating regimes. Comparison at high and low heating rates shows that the activation energies at these vey high heating rates are significantly lower than those observed in traditional DSC ( low heating rate) measurements.
Citation: Thermochimica ACTA
Pub Type: Journals
explosives, energetic materials, calorimetry, microcalorimeter, nanocalorimeter, microhotplate, microheater, mems, microelectromechanical systems, differential scanning calorimeter