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Seaweed from macroalgae and cellulose from nonwood materials have gained attention in various fields. This study explores how seaweed and cellulose nanofibers (CNF) interact to form 3D networks in composite bioaerogels. The ratio of CNF and seaweed was varied to see how it affects the aerogel's inside and its properties. The observations show that the biocomposite aerogel is more rigid and shrinks less than using a single biopolymer. The CNF aerogel has a fine, thin network structure, and the seaweed aerogel has a thin sheet structure. The biocomposite aerogel combines both a fine network and a thin sheet structure. The composite aerogel's mechanical properties are significantly influenced by seaweed composition. The introduction of CNF increases elasticity, while seaweed enhances firmness. Generated computer modelling revealed that the abundant hydroxyl groups in CNF facilitated the formation of intermolecular bonds with seaweed. The bonding led to increased adhesion and entanglement between biopolymers, consequently enhancing elasticity and establishing a stable intermolecular interaction. The 3D X-ray imaging model shows that the skeletal framework primarily consists of seaweed biopolymer, with CNF serving to reinforce this structure thus enhancing the mechanical properties and robustness of the composite bioaerogels. [ABSTRACT FROM AUTHOR]

A sustainable and environmentally conscious approach was employed to create a cellulose nanofiber (CNF) bioaerogel. This modified technique was used for its affordability and eco‐friendly nature, involved the use of reduced concentrations of NaOH solution (ranging from 0 to 0.5 M) to disperse the CNFs. The process included mixing, freezing, neutralizing, and freeze‐drying, ultimately resulting in well‐structured 3D bioaerogels. The concentration of NaOH had a significant impact on the properties of the bioaerogels. The density of the aerogels increases with higher concentration of NaOH. All treated aerogels exhibited impressive water resistance and maintained their structural integrity when exposed to water, indicating promising practical applications. This enhanced structural integrity is attributed to CNF chain rearrangement, facilitated by CNF swelling, dissolution in NaOH, and homogenization. FTIR and XRD analyses provided insight into the transition from cellulose I to cellulose‐II in the bioaerogel structure. These findings contribute to the development of eco‐friendly bioaerogels for environmentally conscious applications. Further research is needed to gain a deeper understanding of the process and to optimize conditions for specific bioaerogel properties. [ABSTRACT FROM AUTHOR]