hydrogen evolution reaction (HER). [4] Among them, metal organic frameworks (MOFs) and their derivatives have attracted wide attention thanks to their unique and designable node-ligand structure, adjustable pore structure, programmable topology structure, and so on. [5] Recently, MOFs-derived electrocatalysts such as carbon-based materials, metal (oxy)hydroxides, and multi-composition complexes have exhibited promising activity in fuel cells, refined electrosynthesis, and water splitting. [6] MOFs derived carbon-based materials through pyrolysis of MOFs contained single-atom catalysts (SACs), [7] metal nanoparticles loaded carbon materials (M-NPs/C), carbon coating metal oxides, carbide, sulfide, or phosphide materials (MO x /C, MC x /C, MS x /C, and MP x /C). [8] Researchers have developed various strategies for synthesizing MOFs-derived SACs such as Ru-SACs, Ni-SACs, Pt-SACs and Co-SACs, and investigating their activity toward water splitting. [9] Even more, dual-metal SACs and single atom/cluster materials were reported subsequently via ration atomic-scale engineering in MOFs precursor. John Wang et al. proposed a cage-confinement pyrolysis approach of zeolitic imidazolate frameworks (ZIFs) confining molybdenum-based polyoxometalate precursor to synthesize size-controlled Mo-based carbon materials, including Mo-SACs, MoC/C, or Mo-NPs/C. [10] Under different pyrolysis experimental parameters, Mo species showed diverse aggregation behavior, from single atoms to nanoclusters and nanoparticles. Meanwhile, the production of MO x /C, MS x /C or MP x /C is dependent on the addition of another nonmetal source during the pyrolysis process, such as oxygen gas, sulfur powder, and NaH 2 PO 4 , respectively. [11] During the aforementioned oxidation, sulfuration, or phosphorization process, hierarchical pore structure, and hollow structure could be constructed artificially to satisfy mass transport and facilitate proton-electron coupling reaction.In decades, hydrolysis reaction of MOFs was proposed, where MOFs played the role of sacrificial templates. Chen et al. first reported hydrolysis factors (e.g., pH and cation ratio) and synthesized serial MOFs-derived metal hydroxides (M x (OH) y ) dodecahedron. [12] MOFs-derived M x (OH) y via hydrolysis reaction, in particular, typically expose more active sites owing to the generation of cross-scale pores during topological Metal organic frameworks (MOFs) and corresponding derivatives have attracted wide attention. As electrocatalysts, these derivatives (metal, metal compound, and associated composites) have a wide range of application in water-splitting devices, fuel cells, and other hydrogen-related technologies. However, with the exception of pyrolysis, limited studies have documented generated metal nanoparticles from MOFs hydrolysis reactions. Herein, NiRu dual-phase alloy nanoparticles are synthesized via in situ MOFs hydrolysis mediating solvothermal reduction reaction. The hcp-phase NiRu alloys can be rationally tuned by modulating experimental parameters of feedin...
