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This study introduces a cellulose nanofiber surfactant system, in which the surface is hydrophobically modified with different alkyl chain structures for the effective envelopment of solid lipid microparticles (SLMs). To endow bacterial cellulose nanofibers (BCNFs) with excellent ability to assemble at the lipid–water interface, alkyl chains with designated molecular structures, such as decane, didecane, and eicosane, are covalently grafted onto the BCNF surface. Interfacial tension and interfacial rheology measurements indicate that dialkyl chain‐grafted BCNFs (diC10BCNF) exhibit strong interfibrillar association at the interface. The formation of a dense and tough fibrillary membrane contributes significantly to the enveloping of the SLMs, regardless of the lipid type. Because the diC10BCNF‐enveloped SLMs exhibit a core molecular crystalline phase at the microscale, they can immobilize an oil‐soluble antioxidant while maintaining its long‐term storage stability. These findings show that the cellulose‐surfactant‐based SLM technology is applicable to the stabilization and formulation of readily denatured active ingredients. [ABSTRACT FROM AUTHOR]

[Display omitted] • Monodisperse macroemulsions were produced through electrostatic attraction-driven in situ interfacial coacervation. • Interfacial coacervation led to formation of a mechanically robust membrane, thus solidifying emulsion interfaces. • Our interfacial engineering technology will overcome the conventional challenge of stabilizing macroemulsions. Since macroemulsions tend to break down to lower free energy, they hardly retain their initial drop state. Therefore, studies are being conducted to overcome this based on advanced interface engineering techniques, but it is still challenging. Herein we hypothesize that the stability of giant droplets can be secured without chemical bonding through the interfacial coacervation of polyelectrolyte and associative nanoplatelets. We synthesized associative silica nanoplates (ASNPs) via polypeptide-templated silicification and consecutive wettability adjustment. To produce monodisperse macrodroplets, the inner fluid containing partially positively charged ASNPs and the outer fluid dissolving negatively charged polyacrylic acid (PAA) were coflowed through a capillary-based microfluidic channel. Dynamic interfacial tension and interfacial rheology measurements revealed that the migration of ASNPs and PAA from each phase to the interface led to the formation of a complex bilayered thin membrane with an enhanced interfacial modulus. In addition, we demonstrated that adjusting the surface properties of ASNPs by coupling a fluorochemical enabled the production of monodisperse fluorocarbon-in-oil-in-water double macroemulsions. These results highlighted the applicability of our microfluidics-based interfacial coacervation technology in the development of complex fluid products with visual differentiation and drug encapsulation. [ABSTRACT FROM AUTHOR]