Bacterial biofilms attach to various surfaces and represent an important clinical and public health problem, as they are highly recalcitrant and are often associated with chronic, nonhealing diseases and healthcare-associated infections. Antibacterial agents are often not sufficient for their elimination and have to be combined with mechanical removal. Mechanical forces can be generated by actuating nonspherical (anisotropic) magnetically responsive nanoparticles in a rotating magnetic field. We have thus prepared anisotropic superparamagnetic nanochains in the size range of 0.5-1 μm by magnetically assembling several iron oxide nanoparticle clusters and coating them with a layer of silica with different shell morphologies: smooth, moderately rough, and highly rough. The silica surface was additionally functionalized with carboxylic groups to increase colloidal stability. The efficacy of the nanochains in biofilm removal was studied systematically with three different model nonpathogenic bacterial species Escherichia coli, Lactococcus lactis, and Pseudomonas fragi; two different magnetic field strengths; two stirring speeds; and two treatment durations. All bacterial species were engineered to express fluorescent proteins to enable quantification of biofilm removal by colony-forming unit count and fluorescence measurements. Nanochains removed >90% of Gram-negative E. coli and P. fragi with a stronger magnetic field, and <90% of Gram-positive L. lactis with a weaker magnetic field. Surface roughness of nanochains, duration, and stirring speed also affected removal, but the effect could not be generalized. In contrast to their effects on biofilms, the functionalized nanochains showed no toxicity to Caco-2 intestinal epithelial cells, regardless of whether magnetomechanical force was employed or not. In summary, we demonstrated that remotely controlled spatial movement of nanoparticles can generate sufficient mechanical forces to disperse attached biofilms while retaining safety in an epithelial cell model.

5-Fluorouracil (5-FU) is a chemotherapeutic drug that is widely used to treat gastrointestinal cancers (e.g., hepatocellular carcinoma). Unfortunately, its systemic toxicity limits its clinical utility; therefore, new means for its targeted delivery at the pathological site are highly sought after to enhance therapeutic efficacy. In this work, we describe a 5-FU covalent conjugate with the self-assembling, heterochiral tripeptide DLeu-Phe-Phe (lFF) via a redox-sensitive linker (5-FU-SS-lFF). The conjugate yields supramolecular hydrogels with rheological properties similar to those of lFF hydrogels and enables 5-FU release under reducing conditions, such as those present in the tumor microenvironment. We demonstrate the selectivity of the drug release under such conditions over a period of 24 h, with consequent significant cytotoxicity on cancer cells, as demonstrated on hepatocellular carcinoma spheroids. Overall, this study opens new opportunities for peptide-based supramolecular hydrogels as versatile and smart vehicles for the selective release of anticancer drugs under tumor-like reducing conditions.

The thorough understanding of the interactions between nanoparticles and lipid membranes has attracted major interest over the past few decades. This spans fundamental biophysics and biomechanics, as well as medical applications, where nanoparticles could serve as potential drug carriers. The influence of the lipid phase in these interactions has been studied to markedly less extent with respect to the nanoparticle size, shape and coating, as well as the presence of electric charge in either the nanoparticles or the membranes. Seeking to gain new insights into the lipid phase, we have systematically investigated the role of the liquid-disordered, the gel-ordered, as well as the seldom-studied ripple phases in modulating the interaction strength between nanoparticles and biomimetic membranes. Supported lipid vesicles and supported lipid bilayers of different composition and amount of electric charge, as well as spherical functionalized Au nanoparticles with and without charge have formed our experimental platform. The results, obtained by quartz crystal microbalance with dissipation monitoring and complemented by atomic force microscopy, reveal a strikingly different mechanistic picture of the interactions between the various lipid phases and types of nanoparticles. We demonstrate enhanced vesicle rupture in the case of stiffer membranes, consistent with recent theoretical studies, yet supported by limited existing experimental evidence. This work advances fundamental understanding of lipid-state-driven nanoparticle-membrane interactions. Such insight is essential, as dynamic changes in bilayer rigidity, composition, and surface charge determine how membranes and nanoparticles interact.

Microorganisms in biofilms are protected from environmental stressors and therefore exhibit strong resistance to conventional removal strategies, including chemical disinfectants and antibiotics. In this study, we systematically evaluated nanomaterial-based removal methods on Listeria innocua biofilms. Anisotropic magnetic particles, composed of iron oxide, and silver nanoparticles, known for their intrinsic antibacterial properties, were used to assess the potential of nanostructure-triggered biofilm disruption. We investigated how particle surface roughness and size affect biofilm removal under magnetic actuation, using both classical colony-forming unit quantification (viability assessment) and fluorescence-based detection via a reporter protein. The surface roughness and size of anisotropic magnetic particles only modestly affected biofilm disruption. Conversely, a synergistic effect was observed when anisotropic magnetic particles were grafted with silver nanoparticles. Furthermore, we used Enterococcus faecalis and Candida albicans biofilms and observed pronounced species-dependent variability of the silver-based treatments. Our results indicate that hybrid magneto-chemical strategies represent a promising and likely necessary approach for reliable and robust biofilm removal.

Supramolecular hydrogels based on heterochiral tripeptides are suited for biomedical applications, particularly as drug delivery platforms for small-molecule therapeutics that do not disrupt the self-assembly process. The chemotherapeutic drug 5-fluorouracil (5-FU) is widely used in the treatment of gastrointestinal cancers (i.e., hepatocellular carcinoma). However, its clinical utility is limited by systemic toxicity. Redox-triggered drug release, using disulfide linkers, represents a viable strategy to enhance therapeutic efficacy. Here, 5-FU is 2 covalently conjugated to heterochiral tripeptide DLeu–Phe–Phe (lFF) through a disulfidecontaining linker to afford a redox-responsive prodrug hydrogelator. The resulting 5-FU–SS–lFF conjugate retains its ability to form supramolecular hydrogels with viscoelastic properties comparable to those of native lFF hydrogels. Under reducing conditions, disulfide bonds are cleaved, enabling controlled release of 5-FU. Importantly, 5-FU–SS–lFF exhibits anticancer activity in hepatocellular carcinoma spheroids. This work advances heterochiral peptide-based supramolecular hydrogels as versatile and responsive platforms for controlled drug delivery.

The development of plasmon-enhanced TiO2 photocatalysts offers exciting opportunities for the use of visible light in environmental and energy-related applications. A key parameter that determines their performance is the size and distribution of the plasmonic metal nanoparticles (NPs), which strongly influence charge separation, light absorption and interfacial chemistry. In this work, we have systematically investigated the role of Au NPs size on the structural, electronic and photocatalytic properties of hydrothermally synthesized TiO2 nanorods (TNR). Au NPs with well-controlled diameters in the range of 10-50 nm were uniformly deposited on the TNR surfaces, which was confirmed by electron microscopy and elemental mapping. UV-Vis diffuse reflectance spectra confirmed the absorption of localized surface plasmon resonance (LSPR) in the visible region, with peak positions depending on both the size of the NPs and the presence of Na-citrate residues from the synthesis. Supplementary spectroscopic analyses showed that citrate residues altered the surface chemistry, impaired charge transfer and partially blocked active sites. Photoluminescence and time-correlated single photon counting measurements revealed that Au decoration effectively suppressed the recombination of electrons and holes and prolonged the lifetime of charge carriers, while electron paramagnetic resonance spectroscopy showed improved stabilization of Ti3+ centers and oxygen vacancies upon visible-light irradiation. Photocatalytic tests, evaluated by the generation of reactive oxygen species and the degradation of bisphenol A (BPA), showed that the activity increased with decreasing NPs size. The sample with the smallest Au NPs showed the highest reactivity and achieved a BPA degradation of similar to 40 within 4 h. Thus, it clearly outperformed both the larger Au-decorated TNR and the untreated TNR reference sample. Nevertheless, residual citrate limited the overall efficiency by hindering charge transport and surface reactivity. These findings provide a pathway for the rational design of more efficient plasmonic photocatalysts by controlling NP size and removing synthesis by-products.

A new nasal formulation combining xylometazoline, a well-established nasal decongestant, and hyaluronic acid (HA) at a 3 mg/ml concentration and low-molecular-weight has been developed as a topical product intended for use in viral acute rhinosinusitis, with the aim of relieving nasal congestion and supporting epithelial integrity. HA, a moisturizing component of respiratory secretions, has been shown to promote epithelial integrity, stimulate mucociliary clearance and support wound healing. As part of the drug development process, this study investigated the permeation and penetration properties of xylometazoline and HA in the new formulation using a human nasal epithelium in vitro model. Results were compared to those of a xylometazoline mono-formulation and a well-established fixed-dose combination of xylometazoline and dexpanthenol. Morphological, ultrastructural and physiological analyses were performed to test nasal cells tolerability on prolonged drug exposure (6 h). HA in this new nasal formulation seems to be a component that exerts its effect mainly on the mucosal surface, which is the favoured site of action for topical products. HA was not detected in the basolateral compartment, consistent with retention at the mucosal surface. The results of our preclinical study do not indicate that the safety profile of xylometazoline would be altered by the addition of HA (or dexpanthenol). The barrier integrity of the in vitro human nasal epithelium was preserved across all tested formulations. Nanoparticle endocytosis was absent. These findings, obtained in a healthy in vitro nasal epithelial model, provide a valuable foundation for subsequent evaluation of this formulation in human clinical studies.

This article provides comprehensive methodological guidance for implementing rotating magnetic nanochain-enhanced lateral flow immunoassays with volumetric magnetic detection. Rotating magnetic nanochains act as microscale stirrers that substantially enhance antibody-antigen binding kinetics through convective mixing, yet their integration into lateral flow platforms presents unique technical challenges requiring both computational optimization and specialized characterization. We describe complete workflows for: (i) computational fluid dynamics modeling using COMSOL Multiphysics to simulate nanochain rotation, fluid flow, and mass transport enhancement; (ii) electron microscopy characterization of magnetic nanochain morphology and size distributions; (iii) rotating magnetic field generator design and operation; and (iv) magnetic particle quantification measurement procedures for volumetric signal readout. Each section provides step-by-step instructions with sufficient detail to enable independent replication. The described methods enable development of lateral flow assays achieving sub-nanogram detection limits with rapid (6-minute) analysis times, addressing critical needs in point-of-care diagnostics. These methods complement our related research article in Biosensors and Bioelectronics by providing the technical foundation necessary for adoption and adaptation of this technology by other laboratories.•COMSOL Multiphysics workflow for modeling convective enhancement by rotating magnetic nanochains•Electron microscopy procedures for comprehensive nanochain characterization•Instrumentation methods for rotating field generation and volumetric magnetic particle quantification

Magnetoactive elastomers (MAEs) are smart composite materials suitable for various applications, such as artificial muscles, radiation absorbers, sensors, and grippers. As an alternative to classic soft-magnetic filler particles, we studied the incorporation of hard-magnetic strontium hexaferrite (HF) particles in a poly(dimethylsiloxane) (PDMS) matrix. In particular, we investigated the combined effects of the surface modification with dodecylbenzenesulfonic acid (DBSA), residual solvent, and crosslinking under a magnetic field on the MAEs’ microstructure, rheological behaviour, and magnetic properties. The HF particles’ surfaces were modified with DBSA in a nitric acid solution. The as-modified particles were dispersed in butanol and used as such or freeze-dried for the preparation of MAEs by manual mixing or ball milling. The crosslinking of the PDMS precursors in the presence of differently modified particles was followed by measuring the change in rheological properties over time. The DBSA modification increased particles’ surface area, reduced agglomeration, and improved filler–matrix compatibility compared to untreated HF fillers. In contrast, the residual 1-butanol promoted particle aggregation and hindered the crosslinking of the elastomer network. Magnetic characterization showed that crosslinking under a magnetic field induces magnetic anisotropy, with the strongest effect observed for the systems with freeze-dried DBSA-modified particles. These results demonstrate that the surface chemistry, residual solvent, and processing conditions collectively govern the filler distribution, network formation, and magnetic sensitivity of MAEs.

Electroporation outcomes are governed by the local electric field distribution and transmembrane voltage, both of which may be altered by nanoscale elements positioned near the cell membrane. In this study, we developed a two-dimensional finite-element electromagnetic model to investigate the effect of a membrane-proximal silica-coated superparamagnetic iron oxide nanoparticle cluster during a trapezoidal electroporation pulse. The model couples electric and magnetic field components with a membrane electroporation formulation based on Smoluchowski-type pore-density dynamics. Simulations were performed with and without a nanoparticle positioned 5 nm from the membrane, considering different cytosol and extracellular medium conductivities. The results show that the nanoparticle induces a highly localized perturbation of the electric field, whose magnitude depends on the sampling region and conductivity contrast. Transmembrane voltage is modestly and transiently modulated during pulse rise time, whereas the effect is limited during the pulse plateau. Pore-density analysis further indicates that the nanoparticle does not induce a generalized increase in electroporation-related parameters and may locally reduce pore density near the nanoparticle–membrane interface. Overall, the model identifies transient and conductivity-dependent nanoscale field redistribution caused by membrane-proximal silica-coated magnetic nanoparticles, while highlighting the need for three-dimensional modeling and experimental validation before inferring electroporation enhancement.

Introduction:High-intensity pulsed electromagnetic fields (HI-PEMF) can be used to trigger contactless permeabilization of the plasma membrane similar to electroporation (EP). The permeabilization efficiency and gene delivery by HI-PEMF in vitro are currently inferior to EP. It was suggested that the methodology can be improved with conductive gold nanoparticles (AuNPs), which are reported to amplify the induced electric field in close proximity to the cell membrane. Objectives:Therefore, in this work, we have studied different NPs, which varied in material/conductivity (gold and silica), size (10-50+ nm), shape (i.e., round and rods), concentration (50-200 µg/mL), and functionalization (pegylated or not), and combined them with HI-PEMF (6.7 T × 100 pulses, 1 Hz). Methods:The normal Chinese hamster ovary cell line (CHO) and the cancer human urinary bladder's transitional carcinoma cell line (T24) were used as a model. We have characterized cell membrane permeabilization using propidium iodide (PI) and the efficacy of gene delivery using pEGFP-N1. Results:Larger NPs and higher NP concentrations resulted in up to a 10% increase in membrane permeability. In contrast, semispherical and rod-shaped AuNPs did not further enhance permeabilization efficiency. Gene delivery efficiency increased from 3% in control samples to 6% in the presence of 50 nm AuNPs. Overall, CHO cells were more susceptible to HI-PEMF-induced effects than T24 cells. Conclusions:This study shows the potential to increase gene delivery efficacy by combining HI-PEMF treatment with conductive NPs. However, it was concluded that the HI-PEMF-induced effects are highly dependent on the cell line, NP type, and concentration and therefore require further investigation.

Biofilms are structured communities of bacteria embedded within an extracellular polymeric substance (EPS) matrix, which forms a protective barrier that restricts drug penetration and increases antibiotic tolerance, making their complete elimination particularly challenging. Here, we investigate a magneto-mechanical approach using rotating magnetic fields (RMFs) to deliver controlled mechanical stress to Enterococcus faecalis biofilms via anisotropic magnetic particles (AMPs). Microrods, nanochains, and nanorods with distinct sizes and magnetic properties were actuated under identical RMF conditions on implant-relevant titanium substrates. Micron-scale magnetic microrods generate sufficient magnetic torque to mechanically disrupt the EPS matrix and detach biofilm structures, significantly increasing suspended bacterial cells without marked bactericidal effects. In contrast, nanoscale AMPs do not induce biofilm detachment but cause membrane damage, increasing the proportion of injured cells. These findings demonstrate a size-dependent transition between microscale biofilm detachment and nanoscale membrane interactions, identifying particle size as the dominant parameter governing magneto-mechanical biofilm disruption.

This work reports the heterochiral tripeptide L-Phe-D-Phe-L-Phe, N-capped with vermellogen, as an ionizable pseudopeptide hydrogelator, and how the pH-responsiveness is transferred from the molecular to the nanoscale, and all the way up to the macroscale through self-assembly. In particular, the protonation of the vermellogen moiety is responsible for hydrogelation, while that of the peptide fine-tunes the matrix nanostructure and viscoelastic properties. Electron microscopy reveals the correlation of varying viscoelastic properties with the nanostructure of the hydrogel matrices. Self-assembly of the pseudopeptide undergoes a peculiar evolution from nanofibers to nanotubes. This process depends on the degree of C-terminal deprotonation, notably with the gradual increase in the internal diameter of the resulting nanotubes as the deprotonation progresses to completion. State-of-the-art characterization techniques confirm that the nanostructured gels are predominantly comprised of parallel β-sheets as primary self-assembling motifs, arranging vermellogen units in a clockwise helical pattern, which minimizes electrostatic repulsions. The evolution from nanofibers to nanotubes appears to be driven by a long-range hydrogen bonding interaction, involving the hydrazone group and the deprotonated C-terminus of adjacent β-sheets. The potential biomedical application of the gels is demonstrated through the controlled release of a model anticancer drug, and in vitro cytocompatibility assays.

Biofilms, structured communities of microbial cells embedded in extracellular polymeric substances, are notorious for their resilience against conventional antimicrobial treatments. They contribute significantly to chronic infections and industrial biofouling, necessitating innovative strategies for their eradication. Magnetic iron oxide nanoparticles have emerged as a promising tool in combating biofilms due to their biocompatibility and unique physicochemical properties, which enable magnetic delivery of antibacterial agents, magnetic hyperthermia, magneto-mechanical actuation including mechanical biofilm disruption, and reversible dynamic magnetic assembly into hierarchical structures. This review describes developing stages of magnetic nanoscale weapons against biofilms ranging from individual iron oxide nanoparticles to complex hierarchical nanoparticle assemblies in the form of magnetic robots and their swarms. A vast array of possible antibiofilm and antibacterial functionalities originating from iron ions, individual iron oxide nanoparticles, spherical nanoparticle assemblies, magnetic robots, and swarms of robots are presented. Magnetic nanotools offer significant improvements and advantages over conventional methods for biofilm eradication, yet their successful future applications depend on addressing and overcoming critical material, biological, and engineering challenges.

Temperature sensing at the micro- and nanoscale remains a significant challenge due to the limitations of conventional techniques in spatial resolution and invasiveness. Here, we report the development of luminescent, temperature-sensitive coatings and nanoparticles based on a newly synthesized europium (Eu) complex integrated into a composite poly(methyl methacrylate)-siloxane-silica (PMMA-siloxane silica) matrix. The Eu complex, identified as the most promising candidate among three lanthanide complexes, was functionalized with silyl ethers via copper-catalyzed azide-alkyne cycloaddition and successfully incorporated into thin PMMA-siloxane silica films on glass surfaces and within silica nanoparticles. These materials exhibited strong thermal responsiveness, chemical stability, and suitability for high-resolution temperature sensing. Furthermore, Eu-loaded silica nanoparticles showed a distinct fluorescent signal and multiplexing capability in live-cell confocal microscopy and were internalized by lung epithelial cells (LA-4 cell line), highlighting their potential as bioimaging probes for localized intracellular temperature sensing. Although some photobleaching was observed under prolonged excitation, the materials demonstrated sufficient chemical and mechanical stability, making them promising for luminescent temperature sensing and live-cell imaging. These results establish the developed Eubased hybrid materials as robust, non-invasive luminescent probes for high-resolution thermal sensing and cellular imaging.

ε-Fe2O3 exhibits the highest room-temperature coercivity among metal oxides, making it a highly attractive candidate for the development of next-generation ultra-hard permanent magnets without the use of expensive rare-earth elements. However, producing ε-Fe2O3 in a controlled and scalable way is difficult because it is thermodynamically unstable, forms only within a narrow particle size range and the nanoparticles easily grow and phase transform into other iron oxide phases. Here, we present a simple, scalable and robust method for synthesizing high-coercivity ε-Fe2O3 nanoparticles based on pH-controlled tetraethyl orthosilicate (TEOS) condensation during a combined sol-gel and hydrolysis process. By adjusting the reaction pH, the hydrolysis of FeCl3 and the condensation of TEOS are controlled, allowing akaganeite (β-FeOOH) nanorods to form in situ and become confined within the growing amorphous silica matrix. This one-step confinement strategy suppresses aggregation, controls particle size, stabilizes the precursor phase and directs its phase transformation toward ε-Fe2O3 during thermal treatment. It advances the scalable production of ε-Fe2O3 nanostructures for magnetic storage, electromagnetic shielding and permanent magnets. The incorporation of Ba2+ ions provides an effective means of tuning the magnetic properties, resulting in an enhancement of coercivity. Magnetic measurements reveal room-temperature coercivity values of up to ≈18 kOe, with a clear dependence on Ba2+ concentration. The thermal stability of ε-Fe2O3 nanoparticles was investigated by measuring the magnetic hysteresis loops of the post-heatedε-Fe2O3/SiO2 samples at 900 °C and 950 °C. We found that the ε-iron oxide remained highly thermally stable and retained a high magnetic coercivity of about 15 kOe.

Industrial water pollution caused by persistent organic contaminants remains a major environmental concern, necessitating the development of efficient and advanced photocatalytic materials. In this study, we present a novel photocatalytic system based on ultrathin ZnO coatings deposited on microstructured gamma-Fe2O3 films by atomic layer deposition (ALD). The microstructured gamma-Fe2O3 films were prepared by the drop-casting of gamma-Fe2O3-SiO2 core-shell structures with controlled shape, size and silica shell thickness. Our results demonstrate that the ALD growth rate of ZnO films is strongly influenced by the concentration of surface hydroxyl (-OH) groups on the microstructured gamma-Fe2O3 films. Detailed structural and surface characterization were performed using SEM, TEM, AFM, XPS and GIXRD. Under UV irradiation, the ZnO/gamma-Fe2O3 heterostructures exhibited up to threefold higher methylene blue degradation rates compared to ZnO films on flat silicon. This enhancement arises from two distinct factors observed in different samples: increased surface roughness and microstructured morphology led to larger catalytic surface area in case of samples with the intermediate silica layer; and the formation of a type I heterojunction between ZnO and gamma-Fe2O3-enabled by the direct contact between the two metal oxides for samples without an intermediate silica layer-promoted efficient separation of photogenerated charge carriers. These results demonstrate how both surface architecture and band alignment engineering can independently contribute to improved photocatalytic performance.

Background/Objectives: Nanoparticles (NPs) were previously explored as enhancers in electroporation due to their potential to locally amplify electric fields near cell membranes, with gold nanoparticles (AuNPs) in particular showing promise in improving membrane permeability and gene electrotransfer (GET). In this study, we systematically investigated the influence of NP properties—including size, shape, surface functionalization, and material—on electroporation efficacy. Methods: A combined approach using theoretical modeling and experimental validation was employed, encompassing numerical simulations, membrane permeabilization assays, transmission electron microscopy, and GET efficiency measurements. Results: Numerical results revealed that the presence of NPs alters local electric field distributions, but the amplification is highly localized, regardless of NP conductivity or geometry. Experimentally, only two out of six tested NP types produced a statistically significant, yet modest, increase in membrane permeability at one electric field intensity. Similarly, GET improvement was observed with only one NP type, with no dependence on concentration or functionalization. Conclusions: Overall, our findings demonstrate that NPs, under tested conditions, do not substantially enhance cell membrane permeability or GET efficacy. These conclusions are supported by both computational modeling and in vitro experiments.

Bacterial resistance is gaining ground and novel, unconventional strategies are required to improve antibiotic treatments. As a synthetic analog of planktonic bacilli, the natural bacterial swimmers that can penetrate bacterial biofilms, ultra-short propelling magnetic nanochains are presented as bioinspired magnetic nanorobots, enhancing the antibiotic treatment in biofilm-forming Staphylococcus epidermidis . Propelling nanochains, activated by a low intensity (<20 mT) and low frequency (<10 Hz) rotating magnetic field (RMF), prompt the otherwise resistant biofilm-forming bacteria to become sensitive to methicillin, resulting in the killing of 99.99% of bacteria. While magnetic force-driven spherical magnetic nanoparticles were previously reported as unidirectional biofilm channel diggers, propelling nanochains emerge as second-generation magnetic nanorobots, which, due to their magnetic core, shape anisotropy, and negative zeta potential, combine magnetic responsiveness, torque-driven movement, and attractive electrostatic interactions to attach to bacterial aggregates and multi-directionally protrude throughout the biofilm, indulging mechanical forces. These synergistic effects, in combination with an antibiotic drug, destroy the bacterial extracellular matrix and eradicate the formed biofilm, as confirmed with several complementary techniques.

The study aimed to develop a superhydrophobic coating on the aluminium alloy 2024-T3 surface. The desired surface roughness and low surface energy were achieved with SiO2 nanoparticles, synthesised via the Stöber method and modified with alkyl silane (AS) or perfluoroalkyl silane (FAS). To enhance particle adhesion to the alloy substrate, nanoparticles were incorporated into a hybrid sol–gel coating composed of tetraethyl orthosilicate, methyl methacrylate, and 3-methacryloxypropyl trimethoxysilane. The coated substrates were characterised using field emission scanning and transmission electron microscopy with energy-dispersive spectroscopy for surface topography, nanoparticle size distribution, composition, and coating thickness. The corrosion resistance of the coatings on AA2024-T3 was evaluated in a 0.1 M NaCl solution using electrochemical impedance spectroscopy. The synthesised SiO2 nanoparticles had an average size between 25 and 35 nm. The water contact angles on coated aluminium surfaces reached 135° for SiO2 + AS and 151° for SiO2 + FAS. SiO2 + FAS, indicating superhydrophobic properties, showed the most uniform surface with the most consistent size distribution of the SiO2 nanoparticles. Incorporation of nanoparticles into the hybrid sol–gel coating further improved particle adhesion. The ~2 µm-thick coating also demonstrated efficient barrier properties, significantly enhancing corrosion resistance for over two months under the test conditions.