Abstract: | Ternary nanocomposites (NCs) containing copper oxide (CuO)/poly(methyl methacrylate)/various carbon‐based nanofillers have been successfully prepared as thin films by an ex situ method as a selective Hg+2 sensor. The structural, morphological, and electrochemical properties of the NCs were identified by all common characterization tools. The FT‐IR curves of these NCs proved the efficiency of CuO mixed with single‐walled CNTs (CuO/SWCNTs), multi‐walled CNTs (CuO/MWCNTs), or graphene (CuO/G) nanoparticles in the PMMA polymer matrix. The mixed nanofillers significantly improved the properties of the PMMA film. The thermal characteristics of the pure PMMA polymer matrix were highly developed by adding nanofillers in the form of NCs. The maximum composite degradation temperature (CDTmax) values were comparable for all the NCs and were in the range of 345 to 406°C. For fabrication, the CuO‐PMMA‐SWCNT, CuO‐PMMA‐MWCNT, and CuO‐PMMA‐GNCs were coated onto a glassy carbon electrode (GCE) to form a tiny layer with orderly thickness using a conductive 5% Nafion chemical binder. During the electrochemical investigation, it was found that CuO‐PMMA‐SWCNT had the maximum response toward Hg2+ ions compared to the other nanofillers in a buffer medium (phosphate type). To calibrate the Hg2+ ionic sensor, the data were plotted against Hg2+ ion concentration and the proposed sensor showed linearity over a wide range of concentrations (0.1‐0.01 mM), which is called the linear dynamic range (LDR). The analytical parameters, such as sensitivity (1.70 × 102 μAμM‐1 cm?2), detection limit (55.76 ± 2.79 pM), and limit of quantification (185.87 pM) were calculated from the calibration curve. Moreover, it showed good reproducibility, fast response time, good linearity, large LDR, and good stability. The CuO‐PMMA‐SWCNT NC‐modified GCE offers a new route to fabricate novel heavy metal ionic sensors, which might be used in green environment and health development applications. |