Effect of Microwave Treatment in a High Pressure Microwave Reactor on Graphene Oxide Reduction Process-TEM, XRD, Raman, IR and Surface Electron Spectroscopic Studies

Reduced graphene oxide (rGO) was prepared by chemical reduction of graphene oxide (GO) (with a modified Hummers method) in aqueous solutions of hydrazine (N2H4), formaldehyde (CH2O), formic acid (HCO2H) accompanied by a microwave treatment at 250 degrees 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(3) 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 CH2O and then increasing for HCO2H and N2H4. The number of layers in rGOs increases with decreasing content of vacancy, C sp(3) 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 (CH2O) provided rGO of 8 layers thickness.

Automated summary

The reduction of graphene oxide to reduced graphene oxide (rGO) using different reducing agents and microwave treatment resulted in the formation of vacancy defects, surface C sp(3) defects, oxygen groups, and interstitial water in the nanostructures. The number of layers in rGO increased as the content of defects, oxygen groups, and water decreased, with microwave treatment facilitating the formation of vacancies and additional functional groups.