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Chabazite (CHA) zeolite membranes with an intermediate layer of various thicknesses were prepared using planetary-milled seeds with an average particle diameter of 300, 250, 200, 140, and 120 nm. The 120 nm seed sample also contained several smaller particles with a diameter of 20 nm. Such small seeds deeply penetrated into the pore channels of the α-alumina support during the vacuum-assisted infiltration process. During the secondary growth, the penetrated seeds formed a thick intermediate layer exiting between the zeolite layer and support. A decrease in seed size increased the penetration depth of seeds and the thickness of the intermediate layer, while the thickness of seed coating and zeolite layers was decreased. CHA zeolite membranes with a thin top zeoliate layer and a thick intermediate layer showed an excellent water/ethanol separation factor (>10,000) for 90 wt.% ethanol at 70 ℃ with a total flux of 1.5 kg m−2 h−1. There was no observation of thermal cracks/defects on the zeolite separation layer. The thick intermediate layer effectively suppressed the formation of thermal cracks during heating, since the tensile stress induced in the zeolite layer was well compensated by the compressive stress on the support. Therefore, it was successfully proven that controlling the microstructure of top surface and intermediate layers is an effective approach to improve the thermal stability of the CHA zeolite membrane.

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Two-dimensional (2D) zeolite nanosheets are important for the synthesis of high flux zeolite membranes due to their lateral size in a preferred orientation. A way to obtain 2D zeolite nanosheets is to exfoliate interlocked structures generated during the hydrothermal synthesis. The mechanical and polymer assisted exfoliation process leads to mechanical damage in nanosheets and short lateral size. In the present study, polyvinylpyrrolidone (PVP) was introduced as an exfoliation agent and dispersant, so that multilamellar interlocked silicalite-1 zeolite nanosheets successfully exfoliated into a large lateral size (individual nanosheets 500~1200 nm). The good exfoliation behavior was due to the strong penetration of PVP into multilamellar nanosheets. Sonication assisted by mild milling helps PVP molecules to penetrate through the lamellar structure, contributing to the expansion of the distance between adjacent layers and thus decreasing the interactions between each layer. In addition, the stability of exfoliated nanosheets was evaluated with a series of organic solvents. The exfoliated nanosheets were well dispersed in n-butanol and stable for 30 days. Therefore, the PVP-assisted solution-based exfoliation process provides high aspect ratio MFI zeolite nanosheets in organic solvents for a long period.