In this work, uniform molybdenum disulfide (MoS2)/tungsten disulfide (WS2) quantum dots are synthesized by the combination of sonication and solvothermal treatment of bulk MoS2/WS2 at a mild temperature. The resulting products possess monolayer thickness with an average size about 3 nm. The highly exfoliated and defect‐rich structure renders these quantum dots plentiful active sites for the catalysis of hydrogen evolution reaction (HER). The MoS2 quantum dots exhibit a small HER overpotential of ≈120 mV and long‐term durability. Moreover, the strong fluorescence, good cell permeability, and low cytotoxicity make them promising and biocompatible probes for in vitro imaging. In addition, this work may provide an alternative facile approach to synthesize the quantum dots of transition metal dichalcogenides or other layered materials on a large scale.

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The trade‐off between the open‐circuit voltage (Voc) and short‐circuit current density (Jsc) has become the core of current organic photovoltaic research, and realizing the minimum energy offsets that can guarantee effective charge generation is strongly desired for high‐performance systems. Herein, a high‐performance ternary solar cell with a power conversion efficiency of over 18% using a large‐bandgap polymer donor, PM6, and a small‐bandgap alloy acceptor containing two structurally similar nonfullerene acceptors (Y6 and AQx‐3) is reported. This system can take full advantage of solar irradiation and forms a favorable morphology. By varying the ratio of the two acceptors, delicate regulation of the energy levels of the alloy acceptor is achieved, thereby affecting the charge dynamics in the devices. The optimal ternary device exhibits more efficient hole transfer and exciton separation than the PM6:AQx‐3‐based system and reduced energy loss compared with the PM6:Y6‐based system, contributing to better performance. Such a “two‐in‐one” alloy strategy, which synergizes two highly compatible acceptors, provides a promising path for boosting the photovoltaic performance of devices.