LAUSR

Abstract Recently, 2D niobium carbide MXene has drawn vast attention due to its merits of large surface area, good metallic conductivity, and tunable band gap, making it desirable for various applications. However, the usage of highly toxic fluoride‐containing etchant and quite long etching time in the conventional synthesis route has greatly hindered further exploration of MXene, especially restricting its biomedical application. Herein, novel fluoride‐free Nb2CTx nanosheets are prepared by a facile strategy of electrochemical etching (E‐etching) exfoliation. Taking advantage of rapid aluminum clearance, excellent chemical stability, and biocompatibility from the MXene by E‐etching, fluoride‐free Nb2CTx/acetylcholinesterase‐based biosensors are constructed for phosmet detection with the limit of detection down to 0.046 ng mL−1. The fabricated Nb2CTx‐based biosensor is superior to the counterpart from hydrofluoric acid‐etched Nb2CTx, indicating that fluoride‐free MXene can enhance the enzyme activity and electron transfer in the biosensor. The results prove that the fluorine‐free MXene shows promise for developing biosensors with high performance of ultrahigh sensitivity and selectivity. It is highly expected that the fluoride‐free MXene as a stable and biocompatible nanoplatform has great potential to be expanded to many other biomedical fields.