Two‐dimensional (2D) transition metal dichalcogenides (TMDs) nanostructures have been widely applied in environmental and biological analysis, biomedicine, electronic devices, and hydrogen evolution catalysis. Meanwhile, this excitement in 2D TMDs has spilled over to their counterparts of different dimensionalities like one‐dimensional (1D) and zero‐dimensional (0D) TMDs nanostructures. Eventual physical and chemical properties of TMDs nanostructures still remain to be highly dependent on their dimensionalities and size scale, and recently creatively exploring these physical and chemical properties is extremely impactful for the sensing field of TMD nanomaterials. Herein, we review a wide range of sensing applications based on not only graphene‐like 2D TMDs nanostructures but also the rapidly emerging subclasses of 1D, and 0D TMDs nanostructures. Their unique and interesting structures, excellent properties, and valid preparation methods are also included and the analytical objectives, ranging from heavy metal ions to small molecules, from DNA to proteins, from liquids to even vapors, can be met with extremely high selectivity and sensitivity. We have also analyzed our current understanding of 0D and 1D TMDs nanostructures and learning from graphene with the goal of contributing fresh ideas to the overall development of more advanced future TMDs based sensors.

Silver nanoclusters capped by hyperbranched polyethylenimine (PEI) have been developed as a highly sensitive fluorescent and colorimetric pH sensor. The probe responds rapidly to pH fluctuations and has such absorption characteristics that the color changes from the colorless or a nearly colorless state to a colored state with increasing acidity, so PEI-capped Ag nanoclusters could be used as a color indicator for colorimetric pH detection. Quantitatively, the fluorescence intensity of PEI-capped Ag nanoclusters exhibits a linear fashion over the pH range of 5.02-7.96 and increases by around 10-fold approximately with greater fluorescence at higher pH values. The repulsion development and conformational change of PEI with decreasing pH induce the aggregation of Ag nanoclusters, leading to an obvious color change and fluorescence quenching of Ag nanoclusters at low pH values. As expected, the pH probe is also sensitive to the different buffer solutions, except for those containing some anions that could react with Ag nanoclusters. Besides, the ionic strength of the buffers has a little influence on the pH-responsive behavior. Our pH sensor with nanoscaled physical dimensions would be a promising candidate in the applications in biological, medical, and pharmaceutical fields.

Electrochemically induced Fenton (electro-Fenton) reaction was used for efficient and controllable preparation of hydroxyl radicals, leading to the generation of luminescent quantum dots through etching of as-exfoliated MoS2 nanosheets. Morphologic changes of MoS2 nanosheets during the electro-Fenton reaction were monitored using transmission electron microscopy, showing that etching of MoS2 nanosheets induced by hydroxyl radicals resulted in rapid homogeneous fracturing of the sheets into small dots via a transition of nanoporous morphology. The as-generated dots with vertical dimensional thickness of ca. 0.7 nm and plane size of ca. 5 nm were demonstrated to be MoS2 quantum dots (MoS2-QDs), and their photoluminescence properties were explored based on quantum confinement, edge effect, and intrinsic characteristics. Moreover, the degree of etching and the concomitant porosity of MoS2 nanosheets could be conveniently tuned via the electro-Fenton reaction time, resulting in a new morphology of nanoporous MoS2 nanosheets, with potential new applications in various significant areas.

Ag nanoclusters functioned by hyperbranched polyethyleneimine have been developed as a new fluorescent and colorimetric platform for sensitive and selective recognition of halide ions (e.g., Cl(-), Br(-), and I(-)). The recognition mechanism is based on the unique reactions between halide ions and the silver atoms. In particular, halide-induced oxidative etching and aggregation can produce a strong fluorescence quenching of Ag nanoclusters. This sensing system exhibits a remarkably high selectivity toward halide ions over most of anions and cations and shows good linear ranges and lower detection limits: the linear ranges are 0.5-80 μM for Cl(-), 0.1-14 μM for Br(-), and 0.05-6 μM for I(-), respectively; the limits of detection for Cl(-), Br(-), and I(-), at a signal-to-noise ratio of 3, are estimated to be 200, 65, and 40 nM, respectively. Specifically, Br(-) and I(-) could be recognized selectively in the coexistence with Cl(-) under the condition of higher ionic strength, which is a significant advantage in the detection of Br(-) and I(-) in real samples. In addition, the recognition of halide could be performed by the colorimetric method, which is also attractive and promising because of its simplicity, rapidity, reliability, and low cost. Furthermore, this sensing system has been applied successfully to the detection of Cl(-) in real water samples.

Yellow, green, and blue photoluminescent polymer carbon dots were prepared by a hydrothermal method and the multicolor photoluminescence mechanism was discussed.

Size‐dependent optical absorption of semiconductive (2H) layered molybdenum disulfide (MoS2), exhibiting great discrimination abilities to single‐ and double‐stranded DNA (ssDNA) and (dsDNA), is studied. In the presence of high concentration of salt, layered MoS2 trends to aggregate rapidly, leading to the increases of sizes in both vertical and lateral dimensions of the nanosheets, which results from the interplay between van der Waals attraction and electrical double‐layer repulsion. Meanwhile, the aggregation behavior of layered MoS2 is remarkably inhibited by the synergistic effects of DNA oligonucleotides. ssDNA can adsorb on the surface of layered MoS2, resulting in a great dispersion, even in the presence of high concentration of salt, while the dispersion behavior is weakened when ssDNA is replaced by dsDNA. Whereas compared to graphene with zero bandgap energy, layered MoS2, with semiconductive properties, exhibits great characteristic optical absorption in visible wavelength region devoted to exploring the aggregation behavior of layered MoS2. Therefore, DNA oligonucleotides induced size control of layered MoS2, contributing to the regular change of its characteristic absorption in visible region, is considered a label‐free bioassay for the detection of single‐nucleotide polymorphism. Due to its easy operation and high specificity, it is expected that the proposed assay holds great promise for further applications.

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