In the Copper Acetate(WSDTY) polyol synthesis procedure, 15.2 mL of ethylene glycol solution containing 0.030 g [Cu(OAc)2(bpy)] was mixed with 3 mL of ethylene glycol solution con-taining 0.040 g NaOH. The mixture was heated in a MW reactor in a sealed glass tube for 30 min at 185°C (or 200 °C). Then, the formed particles were separated by centrifugation, washed with DI water and dried in a vacuum oven at 60 °C overnight. The product appeared red–brownish, a color known for lower oxides of Copper Acetate. The results for the sample obtained at 185 °C are reported in the main text, while the data concerning the sample produced at 200 °C are presented in the Supplementary material. It should be emphasized here that in polyol synthesis, ethylene glycol played a triple role, i.e., as the solvent, the reducing agent and the surfactant.
The reduction ability of ethyl-ene glycol is temperature-dependent and it was found that in the MW-assisted polyol syn-thesis, the reaction did not proceed at temperatures lower than 160 °C.In the borohydride method, a [Cu(OAc)2(bpy)] solution was prepared by dissolving 0.1015 g of the complex in 50 mL of ethanol. A sodium hydroxide solution was prepared by dissolving 0.0121 g NaOH in 10 mL of ethanol. Both solutions were stirred separately until full dissolution of the reagents and then combined under stirring. Then, a sodium borohydride solution was added. Prepared black colored suspension was kept under magnetic stirring for 40 min. Finally, the sample was washed with DI water and dried at 60 °C in a vacuum oven. Borohydrides are very strong reducing agents in alkaline, neutral and acidic media. However, without a protective inert gas atmosphere, copper could be oxidized during the synthesis.
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