| Summary: | In this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, and CrO<sub>3</sub> with and without P<sub>2</sub>O<sub>5</sub> as a water-binding agent. Furthermore, the samples obtained were heat-treated at 800 °C. Specimens were characterized by optical microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The correlation between different characteristic parameters of the Raman analysis has shown that the use of CrO<sub>3</sub> results in a much higher structural disorder compared to the products obtained using persulfate oxidizers. Narrowing the correlation set revealed that minimal defect concentration can be reached by using K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, while the use of (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub> causes a slightly higher concentration of defects. It was also established that the additional use of P<sub>2</sub>O<sub>5</sub> can help to achieve more effective intercalation and has a positive effect on the formation of the stage I GIC phase. After heat treatment, the intercalated products mostly return to a graphite-like structure; however, the samples obtained with CrO<sub>3</sub> stand out with the most significant changes in their surface morphology. Therefore, analysis suggests that GICs obtained using persulfate oxidizers and P<sub>2</sub>O<sub>5</sub> could be a candidate to produce high-quality graphene or graphene oxide.
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