An à la Carte Synthesis Approach for Chemically Linking Au, Pt, and Pd Nanoparticles to Few‐Layer 2H‐MoS ₂

Abstract The combination of 2D materials and metallic nanoparticles (NPs) enables the creation of hybrid systems with enhanced properties, such as improved light absorption via plasmon resonance or the introduction of active catalytic sites. However, effectively interfacing 2D materials with NPs remains challenging. This work presents a novel and efficient à la carte synthesis approach that enables the tailored chemical linkage of noble metal NPs—gold (Au), platinum (Pt), and palladium (Pd)— to ultrathin 2H‐MoS ₂ sheets using orthogonal maleimide‐based linkers. Specifically, alkyne‐, carboxylic acid‐, and phenyl bromide‐terminated maleimides are employed to anchor Au, Pt, and Pd NPs, respectively. This modular strategy allows precise control over the surface chemistry, leading to uniform decoration with sub‐2 nm NPs and robust attachment to the MoS ₂ substrate. This chemical linkage is expected to enhance the interaction between the MoS ₂ and the NPs while also improving the mechanical stability of the hybrid material. These combined effects make the system particularly promising for applications requiring both strong interfacial coupling and durability, such as electrocatalysis, sensing, and flexible electronic devices.