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The effects of sulfur on the size of iron catalyst particles and synthesized carbon nanotubes (CNTs) were investigated during the direct spinning of CNT fibers. CNT fibers containing mainly double-walled CNTs (DWCNTs) 5–10 nm in diameter were synthesized from acetone, ferrocene, and thiophene, whereas CNT fibers containing mainly single-walled CNTs (SWCNTs) 1–1.5 nm in diameter were obtained from methane, ferrocene, and sulfur. The differences in the products arose from the anti-agglomeration effects of the sulfur atoms, which were adsorbed onto the surfaces of the iron catalyst particles, as indicated by direct experimental evidence. A model for the interplay between sulfur atoms and the iron catalyst particles was proposed based on these results, and experimental confirmation of this model was sought by modulating the sulfur injection time into the reactor at different temperatures. This simple experimental modification was used to control the majority of CNTs in the CNT fibers synthesized from SWCNTs, through DWCNTs, and finally to multi-walled CNTs (MWCNTs), with corresponding IG/ID ratios that varied from 26.9 to 1.5.

Synthesis of high-quality carbon nanotube fibers by controlling the effects of sulfur on the catalyst agglomeration during the direct spinning process