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Synthesis of carbon fibers of cotton by chemical vapor deposition (CDV) method is the main focus of this study. Having ferocene as the catalyst, the study explored effects of synthesis process at different temperatures (750°C, 850°C and 950°C). Analysis of size, shape and structure were conducted using scanning electron microscope (SEM), transmission electron microscope (TEM) and Raman spectroscope. The result showed that average diameter of carbon fibers tended to increase according to temperature. In addition, it was found that surface of the fiber is bend and helical. Also, higher temperature affected graphitic of the fiber.