Synthesis and Characterization of EG/Au Composites via Thermal Exfoliation of Graphite Intercalation Compounds with Tetrachloroauric Acid

This study demonstrates a novel route to synthesize gold-decorated exfoliated graphite (EG) through graphite intercalation compounds (GICs) with tetrachloroauric acid (HAuCl₄). We aimed to develop a scalable method for producing EG/Au composites with controlled nanoparticle morphology by investigating the effects of precursor chemistry and thermal expansion conditions. II-stage GIC-HAuCl₄ (average gross-composition: C₂₃HAuCl₄; intercalate layer thickness d_i = 6.85 Å) was prepared via an exchange reaction of HAuCl₄ with graphite nitrate. Interaction of this GIC with liquid methylamine yielded an occlusive complex, where methylamine-bound HAuCl₄ occupies both interlayer and intercrystalline spaces in the graphite matrix. Methylamine treatment of GIC reduces the onset temperature of exfoliation by ≈100 °C and enhances the expansion efficiency, yielding EG with a low bulk density range of 4-6 g/L when processed at 900 °C in air or nitrogen. Thermal exfoliation of these GICs yielded EG decorated with gold nanoparticles, exhibiting a broad size distribution from a few nanometers to several hundred nanometers, as confirmed by electron microscopy. An X-ray diffraction analysis identified the coexistence of crystalline gold and hexagonal graphite phases, with no detectable impurity phases.