Chlor-alkali (CA) membranes as key materials to generate chlorine gas and sodium hydroxide are composed of sulfonic acid layer (S-layer) and carboxylic acid layer (C-layer) to provide fast sodium ion transport and slow hydroxide ion diffusion, respectively. Aciplex F, a representative CA membrane is made in a double layer form via thermal adhesion of both layers after each single layer film is independently fabricated. Unfortunately, the membrane fabrication induces delamination particularly in their interface as a result of hydroxide ion diffusion occurring during CA operation, leading to rapid increase in electrochemical overpotential. In this study, selective chemical conversion technique was developed to solve the delamination issue. Their effectiveness was proved by applying the same concept to a wide range of PFSA membrane.