Metal–organic frameworks (MOFs), which consist of central metal nodes and organic linkers, constitute a fast growing class of crystalline porous materials with excellent application potential. Herein, a series of Mn‐based multimetallic MOF (bimetallic and trimetallic MIL‐100) nano‐octahedra are prepared by a facile one‐pot synthetic strategy. The types and proportions of the incorporated elements can be tuned while retaining the original topological structure. The introduction of other metal ions is verified at the atomic level by combining X‐ray absorption fine structure experiments and theoretical calculations. Furthermore, these multimetallic Mn‐based MIL‐100 nano‐octahedra are utilized as sulfur hosts to prepare cathodes for Li–S batteries. The MnNi‐MIL‐100@S cathode exhibits the best Li–S battery performance among all reported MIL‐100@S composite cathode materials, with a reversible capacity of ≈708.8 mAh g−1 after 200 cycles. The synthetic strategy described herein is utilized to incorporate metal ions into the MOF architecture, of which the parent monometallic MOF nano‐octahedra cannot be prepared directly, thus rationally generating novel multimetallic MOFs. Importantly, the strategy also allows for the general synthesis and study of various micro‐/nanoscale MOFs in the energy storage field.

In this study, we propose a versatile method for synthesizing uniform three-dimensional (3D) metal carbides, nitrides, and carbonitrides (MXenes)/metal-organic frameworks (MOFs) composites (Ti 3 C 2 T X /Cu-BTC, Ti 3 C 2 T X / Fe,Co-PBA, Ti 3 C 2 T X /ZIF-8, and Ti 3 C 2 T X /ZIF-67) that combine the advantages of MOFs and MXenes to enhance stability and improve conductivity. Subsequently, 3D hollow Ti 3 C 2 T X /ZIF-67/CoV 2 O 6 composites with excellent electronand ion-transport properties derived from Ti 3 C 2 T X /ZIF-67 were synthesized. The specific capacitance of the Ti 3 C 2 T X / ZIF-67/CoV 2 O 6 electrode was 285.5 F g À 1 , which is much higher than that of the ZIF-67 and Ti 3 C 2 T X /ZIF-67 electrode. This study opens a new avenue for the design and synthesis of MXene/MOF composites and complex hollow structures with tailorable structures and compositions for various applications.

2D materials are ideal for constructing flexible electrochemical energy storage devices due to their great advantages of flexibility, thinness, and transparency. Here, a simple one‐step hydrothermal process is proposed for the synthesis of nickel–cobalt phosphate 2D nanosheets, and the structural influence on the pseudocapacitive performance of the obtained nickel–cobalt phosphate is investigated via electrochemical measurement. It is found that the ultrathin nickel–cobalt phosphate 2D nanosheets with an Ni/Co ratio of 4:5 show the best electrochemical performance for energy storage, and the maximum specific capacitance up to 1132.5 F g−1. More importantly, an aqueous and solid‐state flexible electrochemical energy storage device has been assembled. The aqueous device shows a high energy density of 32.5 Wh kg−1 at a power density of 0.6 kW kg−1, and the solid‐state device shows a high energy density of 35.8 Wh kg−1 at a power density of 0.7 kW kg−1. These excellent performances confirm that the nickel–cobalt phosphate 2D nanosheets are promising materials for applications in electrochemical energy storage devices.

Controlled synthesis for electrode materials and excellent electrochemical performances were introduced for advanced supercapacitors.

The controllable synthesis of metal-based nanoclusters for heterogeneous catalytic reactions has received considerable attention. Nevertheless, manufacturing these architectures, while avoiding aggregation and retaining surface activity, remains challenging. Herein, for the first time we designed NiCoFe-Prussian blue analogue (PBA) nanocages as a support for in situ dispersion and anchoring of polymetallic phosphide nanoparticles (pMP-NPs). Benefiting from the porous surfaces and the synergistic effects between pMP-NPs and the cyano groups in PBA, the NiCoFe-P-NP@NiCoFe-PBA nanocages exhibit a significantly enhanced catalytic activity for oxygen evolution reaction (OER) with an overpotential of 223 mV at 10 mA cm–2 and a Tafel slope of 78 mV dec–1, outperforming the NiCoFe-PBA nanocubes, NiCoFe-P nanocages, NiFe-P-NP@NiFe-PBA nanocubes, and CoFe-P-NP@CoFe-PBA nanoboxes. This work not only offers the synthesis strategy of in situ anchoring pMP-NPs on PBA nanocages but also provides a new insight into optimized Gibbs free energy of OER by regulating electron transfer from metallic phosphides to PBA substrate.