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A series of novel crosslinked polyphosphazene-aromatic ether organic–inorganic hybrid microspheres with different structures were prepared via precipitation polycondensation between hexachlorocyclotriphosphazene (HCCP) and bisphenol monomers. The bisphenol monomers have different numbers of –CF₃ in the side group, which correspond to distinct oligomeric species-absorbing mechanisms. The wetting behavior of the microsphere surface was evaluated using a water contact angle (CA) measurement, which increased with the increase in the content of –CF₃ in polyphosphazene. We also investigated the effects of HCCP concentration and ultrasonic power on the morphology of the microspheres.