Atmosphere‐Induced Strategy of Mo‐Promoted Ni Encapsulated in Silicalite‐1 for Dry Reforming of Methane

ABSTRACT Dry reforming of methane (DRM) offers a promising route to convert greenhouse gases into syngas, although fabricating Ni‐based catalysts with long‐term stability during reaction conditions remains challenging. Unlike the conventional H 2 pretreatment typically required for activating Ni‐based catalysts prior to DRM, we herein reported a one‐pot hydrothermal encapsulation strategy to directly synthesize Ni‐Mo bimetallic catalysts confined within silicalite‐1 (Ni x Mo@S‐1) under CH 4 /CO 2 atmosphere for catalyst activation. In contrast to the conventional impregnation Ni 5 Mo/S‐1 catalyst, this structural encapsulation approach effectively improved nickel dispersion and enhanced catalytic performance. XRD and TEM revealed that the encapsulated Ni 5 Mo@S‐1 exhibited ultra‐small nanoparticle size (∼2.3 nm) and Mo promoted high dispersion of Ni nanoparticles. Furthermore, XPS and XANES confirmed that Ni 5 Mo@S‐1 facilitated the direct reduction of NiO to metallic Ni under CH 4 /CO 2 atmosphere, thereby inducing active Ni 0 sites and Ni‐O‐Si bond formation with reinforced metal‐support interaction.