Oxo-Functionalized Graphene: A Versatile Precursor for Alkylated Graphene Sheets by Reductive Functionalization.

Controlled covalent functionalization of graphene remains a challenging task owing to the heterogeneous nature of materials. Functionalization approaches for graphene either lack in quantifying the degree of functionalization or they do not discriminate between covalent and non-covalent functionalization. Here, graphite is oxidized and exfoliated in a three-step procedure and subsequently reduced and functionalized by hexylation. Although Raman spectroscopy is powerful to determine the degree of in-plane lattice defects (θLD ) and functionalization (θFD ), the method fails at detecting introduced hexyl groups at a concentration of about 0.03 %, next to the pre-existing in-plane lattice defects of 0.7 %. However, sensitive thermogravimetric analysis coupled with gas chromatography and mass spectrometry (TGA-GC/MS) can prove the hexylation reaction. The efficiency of functionalization is comparable to reductive functionalization of pristine chemical vapor deposition (CVD)-graphene and bulk graphite.