For the first time, few-layer Ti3C2T x (FL-Ti3C2T x ) supporting highly dispersed nano-Ni particles with an interconnected and interlaced structure was elaborated through a self-assembly reduction process. FL-Ti3C2T x not only acts as a supporting material but also self-assembles with Ni2+ ions through the electrostatic interaction, assisting in the reduction of nano-Ni. After ball milling with MgH2, Ni30/FL-Ti3C2T x (few-layer Ti3C2T x supported 30 wt % nano-Ni via self-assembly reduction) shows superior catalytic activity for MgH2. For example, MgH2-5 wt % Ni30/FL-Ti3C2T x can release approximately 5.83 wt % hydrogen within 1800 s at 250 °C and absorb 5 wt % hydrogen within 1700 s at 100 °C. The combined effects of finely dispersed nano-Ni in situ-grown on FL-Ti3C2T x , large specific area of FL-Ti3C2T x , multiple-valence Ti (Ti4+, Ti3+, Ti2+, and Ti0) derived from FL-Ti3C2T x , and the electronic interaction between Ni and FL-Ti3C2T x can explain the superb hydrogen storage performance. Our results will attract more attention to the elaboration of the metal/FL-Ti3C2T x composite via self-assembly reduction and provide a guideline to design high-efficiency composite catalysts with MXene in hydrogen storage fields.

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In this work, Magnesium nanoparticles with Pd decoration, ranging from 40 to 70 nm, were successfully coprecipitated from tetrahydrofuran (THF) solution, assigned as the Mg-Pd nanocomposite. The Mg-Pd nanocomposite exhibits superior hydrogen storage properties. For the hydrogenated Mg-Pd nanocomposite at 150 • C, the onset dehydrogenation temperature is significantly reduced to 216.8 • C, with a lower apparent activation energy for dehydrogenation of 93.8 kJ/mol H 2 . High-content γ-MgH 2 formed during the hydrogenation process, along with PH 0.706 , contributes to the enhancing of desorption kinetics. The Mg-Pd nanocomposite can take up 3.0 wt% hydrogen in 2 h at a temperature as low as 50 • C. During lower hydrogenation temperatures, Pd can dissociate hydrogen and create a hydrogen diffusion pathway for the Mg nanoparticles, leading to the decrease of the hydrogenation apparent activation energy (44.3 kJ/mol H 2 ). In addition, the Mg-Pd alloy formed during the hydrogenation/dehydrogenation process can play an active role in the reversible metal hydride transformation, destabilizing the MgH 2 .