The ongoing miniaturization of electronic devices has boosted the development of new post-silicon two-dimensional (2D) semiconductors, such as transition metal dichalcogenides, one of the most prominent materials being molybdenum disulfide (MoS₂). A major obstacle for the industrial production of MoS₂-based devices lies in the growth techniques. These must ensure the reliable fabrication of MoS₂ with tailored 2D properties to allow for the typical direct bandgap of 1.9 eV, while maintaining large-area growth and device compatibility. In this work, we used a versatile and industrially scalable MoS₂ growth method based on ionized jet deposition and annealing at 250 °C, through which a 3D stable and scalable material exhibiting excellent electronic and optical properties of 2D MoS₂ is synthesized. The thickness-related limit, i.e., the desired optical and electronic properties being limited to 2D single/few-layered MoS₂, was overcome in the thin film through the formation of encapsulated highly crystalline 2D MoS₂ nanosheets exhibiting a bandgap of 1.9 eV and sharp optical emission. The newly synthesized 2D-in-3D MoS₂ structure will facilitate device compatibility of 2D materials and confer superior optoelectronic device function.

High-quality Ga ₂ O ₃ films are obtained by spray pyrolysis from aqueous solutions through optimization of the solution composition and the spraying process parameters.

Layered materials like transition metal dichalcogenides (TMDCs) enable exciting new physics in their 2D limit. Combined with successful demonstrations of 2D transistors and devices, the need for high‐quality large‐scale monolayers increases. In this light, scalable gold‐mediated exfoliations attract broad attention to supersede the traditional scotch tape method as a means for high‐quality materials. Gold proved to be suitably adhesive for the exfoliation of several 2D materials, including TMDCs. Previously reported methods rely on a simple press and peel mechanism. However, herein, a gold‐mediated exfoliation enabled by low‐temperature annealing is presented for the first time. This simple modification potentially increases the range of external conditions under which gold‐mediated exfoliations operate in a robust manner. The exfoliation achieves scaling with parent crystal areas, rendering it on par with previously reported methods. On top of that, a unique gold‐mediated transfer concept is introduced, where gold is repurposed as a metallic (polymer‐free) transfer membrane. The transfer allows the deterministic and clean relocation of the exfoliated monolayers onto technologically relevant substrates like SiO₂/Si. The process is benchmarked using MoS₂ as the prototypical TMDC and monolayer areas up to ≈80 mm² are successfully exfoliated and transferred.