Carbon fiber from natural biopolymer Bombyx mori silk fibroin with iodine treatment

Carbon fibers were prepared from silk fibers after an iodine treatment and the carbon yield, fiber morphology, structure and mechanical properties were investigated. A single or multi-step carbonization process was used for the preparation. In the single step process, silk fibroin (SF) fibers were heated from 25 to 800 °C with a heating rate of 5 °C min−1 under Ar atmosphere. However, the carbon fiber obtained was partially melted and was too fragile to handle. For better performance, SF fibers were treated with iodine vapor at 100 °C for 12 h and untreated and iodinated SF fibers were heated from 25 to 800 °C by a multi-step carbonization process, which was defined based on the optimum thermal degradation rate of silk. In this multi-step process, the carbon fibers obtained from iodinated SF were structurally intact and stable in appearance, and the carbon yield achieved was ca. 36 wt.%, much higher than the value for untreated SF. X-ray diffraction, Raman spectroscopy and transmission electron microscopic observation revealed that the obtained carbon fibers from both untreated and iodinated SFs had a basically amorphous structure. The strength of carbon fibers prepared from iodinated SF using the multi-step carbonization was considerably increased compared to that of untreated SF. According to viscoelastic measurement, by heating above 280 °C the iodine introduced intermolecular cross-linking of the SF, and its melt flow was inhibited which produced a higher yield and better performance of the carbon fiber.