Abstract
Gold–nickel nanoparticles (NPs) of 3–4 nm diameter embedded in silica nanospheres of around 15 nm have been prepared by using [Au(en)2Cl3] and [Ni(NH3)6Cl2] as precursors in a NP‐5/cyclohexane reversed‐micelle system, and by in situ reduction in an aqueous solution of NaBH4/NH3BH3. Compared with monometallic Au@SiO2 and Ni@SiO2, the as‐synthesized Au–Ni@SiO2 catalyst shows higher catalytic activity and better durability in the hydrolysis of ammonia borane, generating a nearly stoichiometric amount of hydrogen. During the generation of H2, the synergy effect between gold and nickel is apparent: The nickel species stabilizes the gold NPs and the existence of gold helps to improve the catalytic activity and durability of the nickel NPs.

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