Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid

Abstract

In this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH4)2S2O8, K2S2O8, and CrO3 with and without P2O5 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 CrO3 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 K2S2O8, while the use of (NH4)2S2O8 causes a slightly higher concentration of defects. It was also established that the additional use of P2O5 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 CrO3 stand out with the most significant changes in their surface morphology. Therefore, analysis suggests that GICs obtained using persulfate oxidizers and P2O5 could be a candidate to produce high-quality graphene or graphene oxide.

Keywords

• graphite intercalation compounds
• graphite bisulfate
• staging in graphite intercalation compounds
• structural characterization
• thermal treatment