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Abstract: Ternary intercalation compounds of carbon fiber (ICCF) were successfully synthesized by soaking pitch-based carbon fibers in solvents such as 1,2-dimethoxyethane (DME) or tetrahydrofuran (THF) containing dissolved alkali metals (lithium, sodium, or potassium). ICCF with stage-1 and random stage was synthesized in alkali metal–DME and potassium–THF systems using different types of carbon fibers. However, ICCF with stage-1 could not be synthesized in lithium– or sodium–THF systems using carbon fibers with a low graphitization degree. Furthermore, the influence of the graphitization degree in the synthesis of ICCF was discussed. The graphitization degree of the host carbon fiber, in addition to the dimensions and steric structure of the intercalated complex affected the formation of TICCF. [Copyright &y& Elsevier]