Increasing hydrophilicity of hydrophobic membrane is one of the strategies to improve its antifouling performance. Herein we report a procedure of reactive‐vapor induced phase separation to prepare an N‐vinyl pyrrolidone (NVP) modified poly(vinylidene fluoride) (PVDF) membrane to improve its hydrophilicity. PVDF solution containing NVP monomer was cast in ammonia water vapor atmosphere to prepare the modified membrane. During the process, PVDF was dehydrofluorinated by the reactive vapor of ammonia water to generate double bond of FC═CH, and then NVP was grafted. The degree of grafting modification and the microstructure evolution of the membrane were studied by adjusting the amount of NVP addition. A possible mechanism of membrane formation from crystallization gelling to non‐crystallization gelling has been proposed to understand the morphology change from nodular sphere to bi‐continuous microstructure with fibril matrix. It has been found that rising the degree of modification has changed the polymorph of PVDF from β to α crystalline phase, as well as turned the hydrophobic PVDF membrane into hydrophilic. Moreover, the modified membrane displayed obvious reduction in bovine serum albumin adsorption, suggesting improvement in anti‐fouling performance. Therefore, our work provides an easy strategy to prepare hydrophilic PVDF membrane, which may have promising potential applications.
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