Fluorination process of carbon materials can be understood the F atom directly contact with C atom through changing the C structure form sp2 to sp3 structure. The different carbon sources, such as one-dimensional carbon dots, two-dimensional graphene materials, three-dimensional porous carbon, carbon nanotubes, and fullerene, exhibit the different carbon structures, influencing the F atom position and the type of C–F bonds at the C structure. The various treatment processes and fluorine (F) sources directly affect the carbon–fluorine bond types and the fluorine-to-carbon (F/C) ratio. These factors ultimately determine the physicochemical properties and the potential applications of the resulting carbon materials. In this chapter, we will systematically discuss and summarize the preparation methods of carbon fluorides. We also introduce the essential influencing factors for the final carbon fluorides under the prepared processes, and the resulted product properties. The sources for obtained carbon materials can be classified into two categories, which is fluorination and exfoliation. The former can be described as the reaction of F atom with C atom to form carbon fluorides, which is the chemical synthesis process with the redox reaction. Fluorination is quite a complex process that is affected by the different methods, carbon sources, fluorinating agents, reaction temperatures, times, etc. according to the reaction mechanism, fluorination can be divided into direct fluorination, controlled fluorination, catalytic fluorination, plasma fluorination, solvothermal fluorination, mechanochemical fluorination, and electrochemical fluorination etc. However, exfoliation is the physical separation of massive fluorinated carbon materials into the thin and small products, including sonochemical exfoliation, modified Hummer’s exfoliation, and thermal exfoliation. In this section we outline the relevant research on the preparation of fluorinated carbon and provide a reliable reference for fluorination mechanism and structure of CFx materials.