Cost-effective metal-based nanostructured hybrids have been widely dedicated to potential energy storage and conversion applications.H erein, we develop af acile methodology for the synthesis of precise carbon-confined hybrid nanostructures by stereoselective assembly accompanied by catalytic pyrolysis.P olyacrylonitrile fiber films favors not only metal-polymer coordination, but also oriented assembly to ensure the well-defined nanostructure of the carbon hybrids. During chemical vapor deposition (CVD), cobalt-nanoparticle-catalyzed growth of carbon-nanotube branches driven by organic molecules (e.g. melamine) delivers hierarchical carbon hybrids.T he resulting carbon hybrids exhibit outstanding electrochemical performance for metal-ion batteries,for example,ahigh specific capacity of 680 mAh g À1 after 320 cycles (Li-storage) and 220 mAh g À1 after 500 cycles (Na-storage) without decay.Over the past few decades,i ntensive efforts have been devoted to developing cost-effective methodologies to fabricate advanced nanostructured materials for various energystorage and conversion applications. [1] Specifically,constructing carbon-based hybrid nanomaterials has provided an opportunity to enable synergic effects between the individual components.Considerable progress has been achieved in the rational design of carbon hybrids towards energy-related electrochemical devices,for example,rechargeable metal-ion batteries,s upercapacitors,m etal-air batteries,a nd water splitting devices. [2] However, designing and tailoring the functional building blocks for hybrid structures with high reactivity,g ood electrical conductivity and excellent structural stability remains af ormidable challenge.R ecently, electrospinning has emerged as an effective technique allowing for the controlled formation of multichannel carbon-fiber networks with tunable porosity,assemblies and architectures.

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Cost‐effective metal‐based nanostructured hybrids have been widely dedicated to potential energy storage and conversion applications. Herein, we develop a facile methodology for the synthesis of precise carbon‐confined hybrid nanostructures by stereoselective assembly accompanied by catalytic pyrolysis. Polyacrylonitrile fiber films favors not only metal‐polymer coordination, but also oriented assembly to ensure the well‐defined nanostructure of the carbon hybrids. During chemical vapor deposition (CVD), cobalt‐nanoparticle‐catalyzed growth of carbon‐nanotube branches driven by organic molecules (e.g. melamine) delivers hierarchical carbon hybrids. The resulting carbon hybrids exhibit outstanding electrochemical performance for metal‐ion batteries, for example, a high specific capacity of 680 mAh g−1 after 320 cycles (Li‐storage) and 220 mAh g−1 after 500 cycles (Na‐storage) without decay.

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Lithium-metal batteries (LMBs) have attracted great attention because of their high theoretical capacity and low electrochemical potential. However, uncontrollable Li dendrite growth and significant volume expansion result in safety issues that largely limit their practical applications. Herein, we explore a microwave-assisted strategy for the rapid synthesis of vertically aligned metal hybrids on Cu foil (VAMH@CF). Such an elaborate architecture of VAMH provides a lithiophilic buffer layer after prelithiation, offering vast nucleation sites/seeds for Li deposition (Li@VAMH@CF) and lower nucleation overpotential. Consequently, Li@VAMH@CF exhibits an outstanding cyclability with a long lifespan (up to 5500 cycles) and a low voltage hysteresis (28 mV) in a symmetrical cell at 3 mA cm–2. LiFePO4||Li@VAMH@CF full cells deliver a reversible capacity of about 140 mAh g–1 for 200 cycles, further demonstrating opportunities of the microwave-involved strategy for optimizing Li-metal anodes.