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Large‐scale synthesis of van der Waals (vdW) metal–organic framework (MOF) nanosheets with controlled crystallinity and interlayer coupling strength is one of the bottlenecks in 2D materials that has limited its successful transition to large‐scale applications. Here, scalable synthesis of mBDC (m = Zn and Cu) 2D MOFs at large scales through a biphase method is demonstrated. The results show replacing water molecules with pyridine eliminates hydrogen bond formation at metal cluster sites. This prohibits tight coupling across adjacent MOF layers and sustains controllable 2D vdW MOF growth. It is further shown that control over the growth speed, crystallinity, and thickness can be achieved by addition of a controlled amount of triethylamine and formic acid to achieve highly crystalline vdW MOF nanosheets with extraordinarily high aspect ratio. The described synthesis route can easily be scaled up for large‐scale production either by deposition onto desired substrates or in crystalline layered powder form. Owing to its large lateral size, vdW nature, and high crystallinity, it is possible to perform atomic force microscopy, Kelvin probe force microscopy, and Raman measurements on the 2D MOFs. The results not only establish their vibrational properties and layer‐dependent responses but also show striking differences from other 2D inorganic materials.

Direct air capture (DAC) of CO₂is an emerging technology in the battle against climate change. Many sorbent materials and different technologies such as moisture swing sorption have been explored for this application. However, developing efficient scaffolds to adopt promising sorbents with fast kinetics is challenging, and very limited effort has been reported to address this critical issue. In this work, the availability and kinetic uptake of CO₂in sorbents embedded in various matrices are studied. Three scaffolds including a commercially available industrial film containing ion‐exchange resin (IER), IER particles embedded in dense electrospun fibers, and IER particles embedded in porous electrospun fibers are compared, in which a solvothermal polymer additive removal technique is used to create porosity in porous fibers. A frequency response technique is developed to measure the uptake capacity, sorbent availability, and kinetic uptake rate. The porous fiber has 90% IER availability, while the dense fibers have 50% particle accessibility. The sorption half time for both electrospun fiber samples is 10 ± 3 min. Our experimental results demonstrate that electrospinning polymer/sorbent composites is a promising technology to facilitate the handleability of sorbent particles and to improve the sorption kinetics, in which the IER embedded in porous electrospun fibers shows the highest cycle capacity with an uptake rate of 1.4 mol CO₂per gram‐hour. © 2018 American Institute of Chemical EngineersAIChE J, 65: 214–220, 2019