Hybrid structures composed of exfoliated expanded graphite (EG) and iron oxide nanocrystals were produced by an ex situ process. The iron oxide nanoparticles coated with meso-2,3-dimercaptosuccinic acid (DMSA), or poly(acrylic acid) (PAA) were integrated onto the exfoliated EG flakes by mixing their aqueous suspensions at room temperature under the support of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and N-hydroxysuccinnimide (NHS). EG flakes both naked and functionalized with branched polyethylenimine (PEI) were employed. Complete integration of the two constituents was achieved and stability was maintained for more than 12 months. No preferential spatial distribution of anchoring sites for attachment of iron oxide nanoparticles was observed, regardless of whether the EG flakes were used naked or functionalized with PEI molecules. The structural and physicochemical characteristics of the exfoliated expanded graphite and its hybrid nanostructures were investigated by SEM, TEM, FTIR and Raman techniques.

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