The assembling properties of single‐chain ammonium amphiphiles containing benzylideneaniline and salicylideneaniline units as rigid segments in the formation of aqueous bilayers, cast multi‐bilayers, and surface monolayers were studied. Electron microscopy indicated that aggregate morphologies observed in water, such as vesicles and fibers, were dependent on the nature of the aromatic unit and the alkyl‐chain length of the component amphiphiles. The patterns of molecular assembly in bilayers were examined by absorption spectroscopy of aqueous bilayers and X‐ray diffraction of cast multi‐bilayer films. The patterns were virtually identical to those of the corresponding azobenzene bilayers, and commonly determined by combinations of alkyl‐chain lengths. This alkyl‐chain combination was crucial for formation of stable surface monolayers.
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