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In a Na2CO3 aqueous solution, PAH becomes colloidal particles of R-NHCOO- and R-NH3 + within a certain pH range. Under such a condition, if microbubbles are present in the solution, the colloidal particles adsorb to the microbubble surface, stabilizing the microbubbles. When PSS is added to the solution sequentially, a bilayer of PAH/PSS can be formed around microbubbles. We successfully fabricated hollow PAH/PSS microcapsules by this method and elucidated the conditions required for the formation of colloidal particles of PAH and a bilayer of PAH/PSS. 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