reported as a new effi cient Fenton-like catalyst for yielding oxidative hydroxyl radicals (HO•) to degrade organic contaminants. [ 5 ] Other applications are rarely reported in the literature. In any case, it is commonly accepted that the performances are closely related with morphology, structure, specifi c area, and chemical stability of FeOCl nanomaterials, which strongly depends on the preparation strategies and experimental conditions. [ 6 ] For decades, however, almost all the reported FeOCl materials were obtained by one exclusive strategy, the chemical vapor transport (CVT), which utilizes FeCl 3 and Fe 2 O 3 mixed powders as precursor and requires a heating procedure at a temperature of 380 °C over days. [ 5,7 ] The CVT strategy is extremely time consuming and asobtained FeOCl materials possess single morphology of nanoplate with micrometer dimensions. Also, the fi nite experimental parameters make it diffi cult to effectively modulate the microstructure, morphology and composition, which limits its practical applications in fi elds of catalysis, energy storage, and conducting materials. Recently, we developed a new technique, laser ablation in liquid solution (LAL), to facilely synthesize the crystalline FeOCl nanosheets at ambient conditions. By laser ablating Au foil in surrounding FeCl 3 solutions for minutes, spherical Au nanoparticles (NPs) decorated FeOCl nanosheets could be synthesized in a one-pot procedure. Technical characterizations illustrate that the crystalline nanosheets possess (010) preferred orientations with microsized dimensions in the plane and tens of nanometers in thickness. The Au/FeOCl nanocomposites own good thermal stability and surface of which adsorbs abundant H 2 O molecularly and oxygen species chemically. The fabrication route is simple and much more effi cient compared to the traditional CVT method. Furthermore, the crystalline size and proportion of Au or FeOCl in the nanocomposites could be effectively modulated by simply changing FeCl 3 concentrations. We proposed that the localized liquid region, formed around the interface between LAL-induced plasma plume and surrounding liquid, provides the hydrolysis reaction platform for the formation of FeOCl nanosheets.