Cellulose‐based reduced graphene oxide materials (r‐nGO) were fabricated and anchored onto polyvinyl alcohol stabilized gold nanoparticles. Their potential in applications in the electrocatalytic reduction of CO2 (ER‐CO2) is demonstrated. The nGO was synthesized by microwave‐assisted cellulose carbonization followed by two different reduction methods, that is, with super‐heated water (i) or caffeic acid (ii). These materials, denoted as r‐nGO (i) r‐nGO‐CA (ii), were utilized to immobilize colloidal gold nanoparticles (Au NPs) in an aqueous environment. The two r‐nGO‐supported Au NP materials were deposited on glassy carbon electrode surfaces and studied as catalysts for ER‐CO2. ER‐CO2 was investigated at room temperature and pressure (RTP) using ionic liquids (RTILs) or an aprotic solvent acetonitrile (ACN). Tetrabutylammonium hexafluoroborate (TBAPF6) was used as an electrolyte salt in the case of ACN. The current response resulting from ER‐CO2 was measured under cyclic voltammetric conditions using a one‐compartment three‐electrode cell. Results showed that, r‐nGO‐supported gold nanoparticles catalyze ER‐CO2 and they significantly reduce the overpotential of CO2 reduction from −1.9 V to −1.6 V vs. Ag/AgCl. Moreover, of all the materials studied, Au/r‐nGO was superior in reducing CO2 in both RTILs and TBAPF6/ACN. These outcomes serve as grounds for the further development of electrocatalysts from bio‐based reduced graphene oxides.

In the present work, solution‐phase synthesis was employed to prepare two sets of catalysts with different transition metals as active sites. One set contained Au or Pd supported on TiO2 (Au−TiO2, Pd−TiO2), whereas the other set contained layered double hydroxides (NiFe‐LDH and CuFe‐LDH). The electrocatalytic performance of these composite materials was investigated by cyclic voltammetry (CV) using a model compound 4‐nitrophenol (4‐NP). Composite materials were characterized by various analytical techniques to gain insight into the catalysts active sites. The morphology and structure of the prepared samples were investigated by X‐ray diffraction, attenuated total reflectance Fourier transform infrared, X‐ray photoelectron spectroscopy, transmission scanning electron microscope, and field emission scanning electron microscope. Metal nanoparticles loading on TiO2 was measured by inductively coupled plasma – optical emission spectrometry. CV measurements were performed in acetonitrile solution containing 0.1 m tetrabutylammonium hexafluorophosphate (TBAPF6) and 1 mm 4‐NP. Among all dioxides (Au−TiO2, Pd−TiO2) and hydroxides (NiFe‐LDH and CuFe‐LDH) studied, Pd−TiO2 shows the lowest onset potential (−0.32 V vs. Ag/AgCl) for the electrocatalytic reduction of 4‐NP. This is the first comparative study of such materials for 4‐NP electrocatalysis in aprotic solvent, thus demonstrating the suitability of dioxide and hydroxide based materials as electrocatalysts.