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Water-stable MIL-101 microcrystals adhere well to polysulfone (PSF) and yield a very robust mixed-matrix MIL-101-PSF membrane for the O2/N2 separation with a selectivity of 5–6 and an unsurpassed O2 permeability increase by a factor of four to above 6 barrer for MIL-101 loadings of 24%.