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One-Step Hydrophobic Silica Nanoparticle Synthesis at the Air/Water Interface

A template-free, single-precursor method is presented for constructing hydrophobic silica nanoparticles (NPs) without organic solvent in a Langmuir trough divided into two isolated interfaces connected by a mildly acidic subphase. A water-insoluble trimethoxysilane with an n-propyl side group (nPM) spread at one interface is solubilized upon hydrolysis and diffuses through the subphase to the clean air/water interface where a wire probe tensiometer measures the interfacial sol–gel reaction. Adsorption and assembly of hydrolyzed nPM at the air/water interface is reflected by a steady increase in surface pressure followed by a plateau. Transferred films characterized with FTIR, XRD, SEM, AFM, and water contact angle confirm self-assembly of hydrolyzed nPM into an ∼1 nm thin film at the air/water interface that undergoes polycondensation into sub-10 nm “seed” particles, which further assemble into amorphous, ∼150 nm hydrophobic NPs. Films transferred through the Langmuir–Schaefer method yield modestly hydrop...