Rational construction of sulfur electrodes is essential in pursuit of practically viable lithium–sulfur (Li–S) batteries. Herein, bimetallic NiCo‐layered double hydroxide (NiCo‐LDH) with a unique hierarchical micro‐nano architecture is developed as an advanced sulfur reservoir for Li–S batteries. Compared with the monometallic Co‐layered double hydroxide (Co‐LDH) counterpart, the bimetallic configuration realizes much enriched, miniaturized, and vertically aligned LDH nanosheets assembled in hollow polyhedral nanoarchitecture, which geometrically benefits the interface exposure for host–guest interactions. Beyond that, the introduction of secondary metal intensifies the chemical interactions between layered double hydroxide (LDH) and sulfur species, which implements strong sulfur immobilization and catalyzation for rapid and durable sulfur electrochemistry. Furthermore, the favorable NiCo‐LDH is architecturally upgraded into closely packed micro‐nano clusters with facilitated long‐range electron/ion conduction and robust structural integrity. Due to these attributes, the corresponding Li–S cells realize excellent cyclability over 800 cycles with a minimum capacity fading of 0.04% per cycle and good rate capability up to 2 C. Moreover, highly reversible areal capacity of 4.3 mAh cm⁻² can be achieved under a raised sulfur loading of 5.5 mg cm⁻². This work provides not only an effective architectural design but also a deepened understanding on bimetallic LDH sulfur reservoir for high‐performance Li–S batteries.

The integration of Li–A/T-Nb₂O₅ and S–A/T-Nb₂O₅ electrodes realized an excellent rate capability and cyclability.

As lithium-ion battery (LIB) anode materials, porous carbons with high specific surface area are highly required because they can well accommodate huge volume expansion/contraction during cycling. In this work, hierarchically porous carbon (HPC) with high specific surface area (~1714.83 m² g⁻¹) is synthesized from biomass reed flowers. The material presents good cycling stability as an LIB anode, delivering an excellent reversible capacity of 581.2 mAh g⁻¹ after cycling for 100 cycles at a current density of 100 mA g⁻¹, and still remains a reversible capacity of 298.5 mAh g⁻¹ after cycling for 1000 cycles even at 1000 mA g⁻¹. The good electrochemical performance can be ascribed to the high specific surface area of the HPC network, which provides rich and fast paths for electron and ion transfer and provides large contact area and mutual interactions between the electrolyte and active materials. The work proposes a new route for the preparation of low cost carbon-based anodes and may promote the development of other porous carbon materials derived from various biomass carbon sources.

The practical application of lithium/sulfur (Li/S) batteries is hindered by the migration of soluble polysulfides (Li2Sn, 4 ≤ n ≤ 8) from cathode to anode, leading to poor electrochemical stability of the cell. To address this issue, in the present study, a TiO2/porous carbon (TiO2/PC) composite-coated Celgard 2400 separator was successfully fabricated and used as a polysulfide barrier for the Li/S battery. In TiO2/PC, the highly conductive PC with three-dimensional ordered porous structure physically constrains polysulfides and at the same time serves as an additional upper current collector. On the other hand, the TiO2 on the surface of PC chemically adsorbed polysulfides during the charge/discharge process. Due to the physical and chemical adsorption properties of TiO2/PC composite coating layer, an initial discharge capacity of 926 mAh g−1 at 0.1 C and a low fading rate (75% retention after 150 cycles) were achieved. Moreover, in the rate capability test, the discharge capacity for the TiO2/PC-modified Li/S battery was recovered to 728 mAh g−1 at 0.1 C after high-rate cycling and remained ~ 88% of the initial reversible capacity.