Abstract
The paper presents the morphological, structural and compositional properties of the sonochemically prepared ZnO-1.4wt% Graphene (Z-G) nanocomposites as a function of pH value of suspension varying from 8.5 to 14 and thermal annealing at 450°C in nitrogen or air ambient. The SEM analysis of the Z-G hybrids dried at 150°C in air has shown a nano-flower like nanostructure for a pH value of 14. The XRD analysis of dried Z-G hybrids revealed a crystallite size increase from 3.5 nm to 18.4 nm with pH increase, and this result was explained in terms of colloids zeta potential evolution with pH value. The Raman and EDS spectroscopy have shown a split of the G band (1575 cm−1) of graphene into two bands (1575 cm−1 and 1605 cm−1), an increased height of D (1323 cm−1) band, and an additional amount of carbon due to CO2 absorption from the air, respectively. The carbon incorporation increased with the decrease of pH, and was associated with a hydrozincite phase, Zn5(CO3)2(OH)6. The formation of dried Z-G nanocomposite was clearly demonstrated only at a pH value equal to 14, where two ZnO Raman active bands at 314.9 cm−1 and 428.2 cm−1 appeared. This result may indicate the sensitivity of the Raman spectroscopy to the nanoflower-like nanostructure of dried Z-G hybrids prepared at pH=14. The thermal treatment of Z-G hybrids in N2at 450°C has increased the number of ZnO Raman bands as a function of pH value, it has decreased the amount of additional carbon by conversion of hydrozincite to ZnO and preserved the graphene profile. The thermal treatment in air at 450°C has increased the crystalline symmetry and stoichiometry of the ZnO as revealed by high and narrow Raman band from 99 cm−1 specific to Zn optical phonons, but it has severely affected the graphene profile in the Z-G hybrid, due to combustion of graphene in oxygen from the ambient.
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