The graphene was produced in 2 to 5 s with a sound of a bomb. Fifty milliliters of 3.5 wt% aqueous PDDA (Sigma-Aldrich) and 100 mg of graphene prepared by the method as mentioned were put into a 100-mL flask and then heated at 90°C for 4 h with a flux apparatus. About 0.45 mmol Ni(NO3)2 · 2.5H2O was added into the above mentioned PDDA-G solution, followed by the addition of hydrazine hydrate of about 20 mmol. Then, the mixed solution was transferred into a Teflon-lined autoclave and heated at 90°C for 24 h.
The mixture was centrifuged and washed for three times prior to drying at 90°C to produce the Ni-NiO nanoparticles on the PDDA-modified graphene (Ni-NiO/PDDA-G). The crystalline structure of Ni-NiO/PDDA-G was examined by X-ray diffraction (XRD) using a Bruker D8 diffractometer (Bruker AXS, Karlsruhe, Germany) equipped with CuKα X-ray source. The chemical environments
of Ni-NiO/PDDA-G NVP-HSP990 purchase were analyzed by electron spectroscopy for chemical analysis/X-ray photoelectron spectroscopy (ESCA/XPS) using a Thermo VG ESCAlab 250 (Thermo Fisher Scientific, Waltham, MA, USA) equipped with a dual-anode (MgKα/AlKα) Thiazovivin mouse X-ray source. The microstructures of Ni-NiO/PDDA-G were investigated with the high-resolution microstructural images produced using the JOEL FEM 2100F (JEOL Ltd., Akishima, Tokyo, Japan) equipped with an Oxford energy-dispersive X-ray spectroscope (EDS) for element analysis. Thermal gravimetric analysis (TGA) for nanoparticle loading was carried out using a selleckchem PerkinElmer Pyris 1 instrument (PerkinElmer, Waltham, MA, USA) and by applying a heating rate of 10°C/min from room temperature
to 800°C in an oxygen-purged environment. The ORR study was examined using an Autolab potentiostat/galvanostat PGSTAT30 (Eco Chemie BV, Utrecht, The Netherlands). The reference electrode is Ag/AgCl (ALS Co. Ltd., Tokyo, Japan), and the counter electrode is a 0.5 mm × 10 cm platinum wire. The working electrode is the glassy carbon whose surface is deposited 5.24 μg/cm2 of Ni-NiO/PDDA-G. Cyclic voltammetry was used to investigate the 0.5 M aqueous H2SO4 and O2-saturated 0.5 M aqueous H2SO4 with a scanning rate of 50 mV/s. BCKDHB The electrochemical impedance spectroscopy (EIS) is also used as a test with an amplitude of 10 mV from 1 to 100 mHz. Results and discussion The crystallization of Ni-NiO/PDDA-G was examined by XRD as shown in Figure 1. The peaks of the (002) plane in the PDDA-modified graphene was shifted from 20.5° to 22°, which revealed the change in the layer-to-layer distance of graphene due to incorporation of PDDA . The hydrothermal method for synthesis of the Ni-NiO alloy nanoparticles was one-pot synthesis with a mixture of PDDA-G, Ni precursors, and hydrazine hydrates at 90°C for 24 h. The XRD result of Ni-NiO/PDDA-G indicated peaks assigned as Ni (111), Ni (200), Ni (012), Ni (222), NiO (111), NiO (012) and NiO (220), respectively [26, 27].