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A type of single helical carbon microsprings (SHCMSs) was synthesized by catalytic chemical vapor deposition. The as-prepared SHCMSs were characterized by a number of techniques such as scanning and transmission electron microscopy, x-ray powder diffraction, and x-ray photoelectron spectroscopy. Experimental results indicate that during the synthesis both morphology change and crystalline phase transformation occur for cobalt catalytic particles and certain chemical bonding form between cobalt and sulfur atoms. Based on the data from this study, a possible growth mechanism of SHCMSs was discussed.