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Carbon molecular sieve membranes (CMSM) were prepared from the pyrolysis of polyimide films within a temperature range of 600°C‐800°C under nitrogen stream. The membrane samples were characterized and tested for the permeation of He, CH4, CO2, and N2 at different pressures and temperatures, respectively. The CMSM700 membrane (pyrolyzed at 700°C) showed an ideal selectivity of ~ 11 for N2/CH4 with...