AbstractThe fluorescent nanomaterial carbon dots (CDs) have attracted tremendous attention in the recent times because of their unique physico‐chemical characteristics. Highly fluorescent CDs were prepared through a simple and nontoxic one‐step hydrothermal carbonization of polyvinylpyrrolidone (PVP). The as‐synthesised CDs, without any pre‐treatments or post‐treatments, show high stability over a broad pH range and have an excellent potential in chemical sensing applications. The as‐prepared CDs have been demonstrated to be an excellent nano probe for Fe3+ ions sensing in aqueous media based on the fluorescence quenching with high sensitivity (lower limit of detection ∼ 1 μM) and selectivity towards Fe3+ ions. “Turn off” fluorescence arises due to the formation of CDs‐Fe3+ nanocomposite complex in the solution. The nanocomposite complex forms by the attachment of Fe3+ ions to the surface emissive site of the CDs, resulting in an obvious fluorescence quenching. Here, CDs itself act as a promising nano carrier for loading of Fe3+ ions to form the CDs‐Fe3+ nanocomposite complex in the solution. In addition to all, in this study we are intensely focused to explore the application of CDs‐Fe3+ nanocomposite complex. We have used the CDs‐Fe3+ nanocomposite complex as a novel sensor probe for the detection of F‐ ions in aqueous media based on “Turn on” fluorescence mechanism. “Turn on” fluorescence occurs due to the formation of thermodynamically highly stable [FeF6]3‐ complex and bare CDs in the solution. The developed sensor has high sensitivity (lower limit of detection ∼ 1 μM) and selectivity towards F‐ ions over a wide‐ranging other competing anions. Finally, we successfully demonstrate the real life application of the developed sensor by estimating the trace F‐ ions in the real world drinking water samples.