Mesoporous carbon hollow spheres (MCHS) have wide applications, including catalysis, absorption, and energy storage/conversion. Herein, we report a one-pot, surfactant-free synthesis of MCHS using three molecules: resorcinol, formaldehyde, and tetrapropyl orthosilicate. The co-condensation process between the in situ generated silica primary particles and the polymer oligomers is regulated, leading to monodispersed MCHS with adjustable pore sizes from micropores to 13.9 nm. The resultant MCHS shows excellent performance for electrochemical double-layer capacitors with high capacitance (310 F g(-1) at 1 A g(-1)), excellent rate capability (157 F g(-1) at 50 A g(-1)), and outstanding cycling stability (98.6% capacity retention after 10 000 cycles at 10 A g(-1)). Our one-pot synthesis strategy is versatile and can be extended to fabricate metal oxide@mesoporous carbon yolk-shell structures in the absence of surfactant, paving the way toward designed synthesis of nanostructured mesoporous carbon composites for various applications.

High‐capacity lithium‐ion battery anode materials, such as transition metal oxides, Sn and Si, suffer from large volume expansion during lithiation, which causes capacity decay. Introducing sufficient void space to accommodate the volume change is essential to achieve prolonged cycling stability. However, excessive void space may significantly compromise the volumetric energy density. Herein, a method to control the void size in iron oxide@carbon (FeOx@C) yolk–shell structures is developed and the relationship between the void space and electrochemical performance is demonstrated. With an optimized void size, the FeOx@C yolk–shell structure exhibits the best cycling performance. A high reversible capacity of ≈810 mA h g−1 is obtained at 0.2 C, maintaining 790 mA h g−1 after 100 cycles. This contrasts with FeOx@C materials having either smaller or larger void sizes, in which significant capacity fading is observed during cycling. This contribution provides an effective approach to alleviate the volume expansion problem, which can be generally applied to other anode materials to improve their performance in LIBs.

A new type of monodispersed mesoporous silica nanoparticles with a core-cone structure (MSN-CC) has been synthesized. The large cone-shaped pores are formed by silica lamellae closely packed encircling a spherical core, showing a structure similar to the flower dahlia. MSN-CC has a large pore size of 45 nm and a high pore volume of 2.59 cm(3) g(-1). MSN-CC demonstrates a high loading capacity of large proteins and successfully delivers active β-galactosidase into cells, showing their potential as efficient nanocarriers for the cellular delivery of proteins with large molecular weights.

A yolk–shell Sn@C nanobox composite with controllable structures has been synthesized using a facile approach. The void space is engineered to fit the volume expansion of Sn during cycling. It is demonstrated that the shell thickness of carbon nanobox has substantial influence on both nanostructures and the electrochemical performance. With an optimized shell thickness, a high reversible capacity of 810 mA h g−1 can be maintained after 500 cycles, corresponding to 90% retention of the second discharge capacity. For Sn@C materials with either thinner or thicker carbon shells, significant capacity decay or a decreased specific capacity are observed during cycling. The present study sheds light on the rational design of nanostructured electrode materials with enhanced electrochemical performance for next‐generation lithium ion batteries.

An aluminum–selenium battery powered by the reversible redox reaction of Se/Se2Cl2 has been developed for the first time.