The evolution of high-performance and stable electrode materials for supercapacitors plays a vital role in the next generation of energy storage devices. In this work we present a simple method for preparing Bi(nanoparticles)/CNx(nanosheets) nanocomposites as electrode materials for supercapacitors, which were synthesized by thermally treating bismuth citrate and urea at 550-700 °C under an Ar atmosphere. According to physicochemical studies (XRD, SEM, TG-DTA, XPS, FTIR, and BET), a "smeared" bismuth formation or the formation of nanoparticles on the CNx surface of interwoven 2D-nanosheets at different calcination temperatures was observed.
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