This work presents a simple procedure for the preparation of 2D carbon flakes by a catalyst-free redox reaction in the range of 400–600 °C at atmospheric pressure. Tetrachloromethane (CCl4) was reduced by aluminium flakes (Al), which also serve as a template for carbon flakes, for either 60 min or 120 min. Gaseous aluminium chloride (AlCl3) was released from the synthesis. According to BET analysis, the prepared carbon flakes exhibit a mesoporous structure with surface area in the range of 300–500 m2 g−1. The 2D morphology and amorphous character was confirmed by XRD, Raman spectra and TEM analyses. In addition, SEM and TEM images revealed the carbon flakes are composed from carbon layers which can be also folded. A mechanism of their formation was also proposed. At higher reaction temperature, e.g., 700 °C, 1D carbon nanostructures with worm-like morphology was obtained.