Summary: | We demonstrate an accessible and effective technique for exfoliating graphite foil and graphite powder into graphene in a water solution of inorganic salt. In our research, we report an electrochemical cathodic exfoliation in an aqueous solution of Na<sub>2</sub>SO<sub>4</sub>. After electro-exfoliation, the resulting graphene was premixed with furfuryl alcohol (FA) and an inorganic template (CaCO<sub>3</sub> and Na<sub>2</sub>CO<sub>3</sub>). Once FA was polymerized to poly(furfuryl alcohol) (PFA), the mixture was carbonized. Carbon bridges originating in thermally-decomposed PFA joined exfoliated graphene flakes and stabilized the whole sponge-type structure after the nano-template was removed. Gases evolved at the graphite electrode (cathode) played an important role in the process of graphene-flake splitting and accelerated the change of graphite into graphene flakes. Starting graphite materials and graphene sponges were characterized using Raman spectroscopy, SEM, high-resolution transmission electron microscopy (HRTEM), elemental analysis, and low-temperature adsorption of nitrogen to determine their structure, morphology, and chemical composition. The discovered manufacturing protocol had a positive influence on the specific surface area and porosity of the sponges. The SEM and HRTEM studies confirmed a high separation degree of graphite and different agglomeration pathways. Raman spectra were analyzed with particular focus on the intensities of I<sub>D</sub> and I<sub>G</sub> peaks; the graphene-type nature of the sponges was confirmed.
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