Because of their good performance in diffusion‐limited processes, ordered macro‐microporous single‐crystalline metal‐organic frameworks (MOFs) have potential for use in various fields. However, there are still very few reports of the synthesis of such MOFs. A general synthesis methodology for ordered macro‐microporous single‐crystalline MOFs is highly desired. Here, a novel strategy is reported for synthesizing single‐crystalline ordered macro‐microporous MOFs by monodentate‐ligand‐induced in situ crystallization within a 3D ordered hard template in a double‐solvent system. A space‐confined growth model is proposed to clarify the shaping effect of the template; the role of the monodentate ligand is also analyzed. Moreover, a carbon material derived from the macro‐microporous MOF inherits the ordered interconnected macroporous structure. The improved diffusion and lower resistance, as well as the structural robustness, endow the derivative carbon material with superior rate performance and excellent cycling stability when prepared as electrodes for a supercapacitor. It is anticipated that the method will provide new paths to the synthesis of such macro‐microporous materials for applications in energy‐related fields and beyond.

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The design and self-assembly of graphene oxide (GO)-based composite membranes have attracted enormous attention due to their wide application in nanomaterial and environmental fields. In this work, we have successfully developed a strategy to fabricate new composite membranes based on poly(vinyl alcohol)/poly(acrylic acid)/carboxyl-functionalized graphene oxide modified with silver nanoparticles (PVA/PAA/GO-COOH@AgNPs), which were prepared via thermal treatment and the electrospinning technique. Due to the strong π-π forces and strong electrostatic interactions of GO–COOH sheets, the prepared composite membranes and their lager surface areas were modified by scores of AgNPs, which demonstrated that a high-efficiency photocatalyst removed the organic dyes from the aqueous solutions. The prepared PVA/PAA/GO-COOH@AgNPs nanocomposite membranes showed a remarkable photocatalytic capacity in the catalytic degradation of the methylene blue dye solutions. Most importantly, the whole process was easy, mild, and eco-friendly. Additionally, the as-prepared membranes could be repeatedly used after the catalytic reaction.

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