• thermal properties;
  • microstructure;
  • fibers


The thermal properties of Bombyx mori silk fibers subjected to heat treatment were examined by thermogravimetry, differential thermal analysis, Fourier transform infrared absorption spectrometry (TG-DTA-FTIR) and scanning electron microscopy (SEM). The color, size, and shape of B. mori cocoon shells were observed as they were heated from 25 to 550°C. Only 1% of the original cocoon shell weight remains as cocoon ash after treatment at 550°C. Inorganic components, such as calcium, potassium, sulfur, magnesium, etc., were detected in the cocoon ash by energy dispersion fluorescent X-ray spectrometry. A sharp decrease in weight was observed in the TG data beginning around 280°C, and an endothermic peak appeared at 308°C, as evidenced by the DTA curves. The IR bands observed at 2380 cm−1 ([BOND]OH stretching), 1760 cm−1 (C[DOUBLE BOND]O stretching), 1503 (N[BOND]H stretching), 1085 cm−1 (C[BOND]N stretching) and 965 cm−1 ([BOND]NH2 stretching) become stronger as an exothermic reaction beginning at 280°C takes place. This is probably due to cleavage of the main chain and the accompanying decomposition of the silk fibers. Similarly, a SEM micrograph of silk fibers treated at 300°C shows a microtubule in the middle of the silk fibers of about 25-μm diameter. This suggests that the thermal reactions starts in the middle of the silk fiber and forms a microtubule. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 1817–1820, 2002