As an emerging 2D layered material, Bi2O2Se has shown great potential for applications in thermoelectric and electronics, due to its high carrier mobility, near‐ideal subthreshold swing, and high air‐stability. Although Bi2O2Se has a suitable band gap for infrared (IR) applications, its photoresponse properties have not been investigated. Here, high‐quality ultrathin Bi2O2Se sheets are synthesized via a low‐pressure chemical vapor deposition method. The thickness of 90% Bi2O2Se sheets is below 10 nm and lateral sizes mainly distribute in the range of 7–11 µm. In addition, it is found that triangular sheets largely lack “O” content, even only 0.2 for Bi2O0.2Se. The near‐IR photodetection performance of Bi2O2Se nanosheets is systematically studied by variable temperature measurements. The response time, responsivity, and detectivity can approach up to 2.8 ms, 6.5 A W−1, and 8.3 × 1011 Jones, respectively. Additionally, the critical performance parameters, including responsivity, rising time, and decay time, remain at almost the same level when the temperature is changed from 80 to 300 K. These phenomena are likely due to the fact that as‐grown ultrathin Bi2O2Se sheets have no surface trap states and shallow defect energy levels. The findings indicate ultrathin Bi2O2Se sheets have great potentials for future applications in ultrafast, flexible near‐IR optoelectronic devices.

2D materials, represented by transition metal dichalcogenides (TMDs), have attracted tremendous research interests in photoelectronic and electronic devices. However, for their relatively small bandgap (<2 eV), the application of traditional TMDs into solar-blind ultraviolet (UV) photodetection is restricted. Here, for the first time, NiPS 3 nanosheets are grown via chemical vapor deposition method. The nanosheets thinning to 3.2 nm with the lateral size of dozens of micrometers are acquired. Based on the various nanosheets, a linearity is found between the Raman intensity of specific A g modes and the thickness, providing a convenient method to determine their layer numbers. Furthermore, a UV photodetector is fabricated using few-layered 2D NiPS 3 nanosheets. It shows an ultrafast rise time shorter than 5 ms with an ultralow dark current less than 10 fA. Notably, this UV photodetector demonstrates a high detectivity of 1.22 × 10 12 Jones, outperforming some traditional widebandgap UV detectors. The wavelength-dependent photoresponsivity measurement allows the direct observation of an admirable cut-off wavelength at 360 nm, which indicates a superior spectral selectivity. The promising photodetector performance, accompanied with the controllable fabrication and transfer process of nanosheet, lays the foundation of applying 2D semiconductors for ultrafast UV light detection.

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