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Development of materials with excellent separation performances remains an ongoing challenge in methane/nitrogen (CH4/N2) separation science. Herein, a facile and effective method for enhancing CH4 uptake, binding, and CH4/N2 selectivity using the surface‐carbonized and stiffened zeolitic imidazolate framework‐8 (CSZ) via high‐vacuum‐resistance calcination (HVRC) was demonstrated. Such vacuum‐treated...