The self-assembly of sodium stearate and its homologs ( >C12) in hydrotalcite (LDH) interlayers was found to change reversibly between mono- and bilayer structures with a ratio changing continuously within a range of 70 °C and 5 °C in stoichiometric intercalations in aqueous dispersion. The bilayer structure was more stable than the monolayer, judging from the fact that bilayer aggregations were formed even in high temperatures with the addition of excess amounts of guest stearates over the anion exchange capacity (AEC). Hydrophobic interaction was determined to be the key factor for the formation of a bilayer assembly.
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