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A new class of core–shell adsorbents has been created by electrospun metal–organic framework (MOF) particles embedded in polymer nanofibers, which have provided many unique properties compared to the existing MOF coating technologies. For the first time, we demonstrate the improved adsorption selectivity of CO₂over N₂using electrospun polymer/ZIF‐8 adsorbents in experiments. Furthermore, an analytical model based on the assumption that the diffusivity in core is 10 times higher than that in shell is developed to describe the theory of improved selectivity for core–shell adsorbents that is validated against a more accurate finite element model developed in COMSOL. Our model shows three regimes including exclusive shell uptake, linear core uptake, and asymptotic core uptake. These regimes are related to material properties and uptake times, which could be used as design criteria to balance core stability, maximum selectivity, and maximum uptake. An advanced HAADF STEM tomography (MovieS1) shows that the shell thickness in the case of polymer/ZIF‐8 is on the order of 10 nm, allowing the regime of maximum selectivity to be realized. Kinetically limited adsorption tests at 45°C demonstrate that these composite fibers can perform in a regime of selectivity and uptake for the separation of CO₂and N₂that is unobtainable by either the MOF or fiber independently, showing a great potential for postcombustion CO₂capture.

Mixed‐matrix membranes (MMMs) have been studied widely in the field of gas separation due to their potential to overcome performance barriers found in traditional polymeric membranes. Most polymeric membranes exhibit a trade‐off between permeation and selectivity, which has limited their development in many challenging separation applications. One solution to this issue utilizes the introduction of fillers into the polymer matrix to produce MMMs. Out of the many different fillers, metal–organic frameworks stand out as a promising candidate due to their highly tunable structure, molecular sieving effect, and superior compatibility with the polymer matrix. This review will provide an in‐depth look into the basic mechanisms of MMMs for gas separation and different approaches to model the permeation of gases through the membrane. In addition, challenges facing the field and recent research trends for MMMs will be discussed as well as their many applications for different gas separations. Finally, some insight on the future direction for MMMs will be covered, focusing on many intriguing opportunities and challenges that must be further explored to advance this technology.