2D layered materials have sparked great interest from the perspective of basic physics and applied science in the past few years. Extraordinarily, many novel stacked structures that bring versatile properties and applications can be artificially assembled, as exemplified by vertical van der Waals (vdW) heterostructures, twisted multilayer 2D materials, hybrid dimensional structures, etc. Compared with the ordinary synthesis process, the stacking technique is a powerful strategy to achieve high‐quality and freely controlled 2D material stacked structures with atomic accuracy. This review highlights the most advanced stacking techniques involving the preparation, transfer, and stacking of high‐quality single crystal 2D materials. Apart from the 2D–2D stacked structures, 2D–0D, 2D–1D, and 2D–3D structures offer a prospective platform for the increasing application of 2D materials. The assembly strategy and physical properties of these stacked structures strongly depend on the factors in the stacking process, including the surface quality, angle control, and sample size. In addition, comparative analysis tables on the techniques involved are also available. The summary of these strategies and techniques will hopefully provide a valuable reference for relevant work.

A “double-locked” and enzyme-activated molecular fluorescent probe for accurate bioimaging and hepatopathy differentiation.

A pH activated photodynamic/photothermal sensitizer applicable to tumor ablation.

The substrate effect is an important issue in the properties of two-dimensional transition metal dichalcogenides (2D TMDs). Quantitatively determining the dependence of the photoluminescence (PL) emission properties and the excitonic behavior of single-layer 2D materials in a specific dielectric environment would provide helpful guidance for the rational design of substrates for high performance 2D TMD PL emission devices. Here, using a WSe2 monolayer on different substrates as a model system, it is demonstrated that the PL emission intensities can drastically change depending on the substrate effect. From the analysis of the excitonic behavior, the results reveal that the spectral weight between the neutral and charged excitons in the PL spectra is significantly modified by the substrate types, and the weight factor is dependent on the laser excitation density. The charged exciton binding energy is obviously negatively related to the substrate dielectric constant. Furthermore, the change trends of the binding energy of the monolayer WSe2 on different substrates are basically the same for the increase of the excitation density. These results suggest that the choice of the substrate plays a significant role in the modulation of the PL properties and exciton states of atomically thin WSe2; hence, substrate engineering should be carefully considered in the design of future 2D devices.