Polyhedral oligomeric silsesquioxane (POSS) is a family of organic/inorganic hybrid materials with specific molecular symmetry, and shows great potential in the structural design of nanomaterials. Here, a “bottom‐up” strategy is designed to fabricate 3D interconnected Si/SiOx/C nanorings (NRs) via AlCl3‐assisted aluminothermic reduction using dodecaphenyl cage silsesquioxane (T12‐Ph) as the building block. In this process, AlCl3 acts as both a liquid medium for reduction, and significantly as the catalyst to the cross‐linking of phenyl groups in T12‐Ph. The obtained Si/SiOx/C NRs exhibits uniform diameter of ≈165 nm and well distribution of C and Si elements. The unique ring‐like structure of Si/SiOx/C NRs makes it have great application potential in the field of lithium ion batteries. Notably, Si/SiOx/C NRs exhibits superior high‐rate capacity and good cycle stability when used as anode for LIBs. More excitingly, Si/SiOx/C NRs can deliver a high reversible capacity of 517.9 mA h g−1 at ultra‐low temperature of −70 °C, and the capacity retention as high as ≈50% of that at 25 °C. This work not only broadens structural design of carbon‐based nanomaterials but also provides more possibilities for the application of POSS.
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