Abstract:A 2D/2D MXene/TiO2-MoS2 heterostructure was fabricated via wet etching. The structure was characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). And the electrochemical properties of the heterostructure were investigated as well. It is found that wet-etching yields few layer of 2D MXene nanosheets, which could provide a larger surface area for the growth of ultrathin 2D MoS2 nanosheets. The MoS2 nanosheets tend to grow vertically on the MXene nanosheets, thereby offering a greater surface area and more exposed active sites. Some MXene nanosheets are in-situ derived into TiO2 nanoparticles, forming a rich heterogeneous interface between MXene, TiO2 and MoS2. And these interfaces modulate the electronic structure of the heterostructure, effectively improving its charge transfer efficiency, thereby improving the catalytic activity and stability of the material. The 2D/2D MXene/TiO2-MoS2 heterostructure exhibits remarkable oxygen evolution reaction (OER) performance, with an overpotential of only 376 mV at a current density of 50 mA/cm2. After a 40 h constant voltage stability test, the voltage retention rate reaches 99.2%.