A simple temperature-assisted solution interaction technique was used to functionalize and reduce graphene oxide (GO) using tetraethylenepentamine (TEPA) with less chemicals, low temperature, and without using other reducing agents. GO nanosheets, produced using a modified Hummers’ method, were functionalized using two different GO:TEPA ratios (1:5 and 1:10). The reduction of GO was evaluated and confirmed by different spectroscopic and microscopic techniques. The FTIR and XPS spectra revealed that most of the oxygenated groups of GO were reduced. The emergence of amide groups in the XPS survey of the rGO-TEPA samples confirmed the successful reaction of TEPA with the carboxyl groups on the edges of GO. The replacement of the oxygenated groups increased the carbon/oxygen (C/O) ratio of GO by approximately 60%, suggesting a good reduction degree. It was found that the I2D/ID+D′ ratio and the relative intensity of the D′′ band clearly increased after the reduction reaction, suggesting that these bands are good estimators for the reduction degree of GO. The morphological structure of GO was also affected by the reaction with TEPA, which was confirmed by SEM and TEM images. The TEM images showed that the transparent GO sheets became denser and opaque after functionalization with TEPA, indicating an increase in the stacking level of the GO sheets. This was further confirmed by the XRD analysis, which showed a clear decrease in the d-spacing, caused by the removal of oxygenated groups during the reduction reaction.
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