| Summary: | Reduced graphene oxide (rGO) was prepared by chemical reduction of graphene oxide (GO) (with a modified Hummers method) in aqueous solutions of hydrazine (N<sub>2</sub>H<sub>4</sub>), formaldehyde (CH<sub>2</sub>O), formic acid (HCO<sub>2</sub>H) accompanied by a microwave treatment at 250 °C (MWT) by a high pressure microwave reactor (HPMWR) at 55 bar. The substrates and received products were investigated by TEM, XRD, Raman and IR spectroscopies, XPS, XAES and REELS. MWT assisted reduction using different agents resulted in rGOs of a large number of vacancy defects, smaller than at GO surface C sp<sup>3</sup> defects, oxygen groups and interstitial water, interlayer distance and diameter of stacking nanostructures (flakes). The average number of flake layers obtained from XRD and REELS was consistent, being the smallest for CH<sub>2</sub>O and then increasing for HCO<sub>2</sub>H and N<sub>2</sub>H<sub>4</sub>. The number of layers in rGOs increases with decreasing content of vacancy, C sp<sup>3</sup> defects, oxygen groups, water and flake diameter. MWT conditions facilitate formation of vacancies and additional hydroxyl, carbonyl and carboxyl groups at these vacancies, provide no remarkable modification of flake diameter, what results in more competitive penetration of reducing agent between the interstitial sites than via vacancies. MWT reduction of GO using a weak reducing agent (CH<sub>2</sub>O) provided rGO of 8 layers thickness.
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