Implant-associated infections (IAI) are a significant concern within the field of orthopedics. To develop an implant with antimicrobial properties, titania nanotubes (TNTs) supported with iodine were synthesized on 3D-printed Ti-6Al-4V implants using the electrochemical anodization (ECA) technique. This study aims to analyze the release profile of iodine and the antimicrobial efficacy and cytotoxicity of the iodine-supported TNT (I-TNTs) on the 3D-printed Ti-6Al-4V implant. 3D-printed Ti-6Al-4V samples were doped with six different iodine formulations, including four test groups containing TNT and two control groups without TNT. As printed 3D Ti-6Al-4V samples and TNTs samples without iodine were also utilized as control groups. In vitro assays were performed to assess the drug elution, cytotoxicity, and antimicrobial efficacy. All tested I-TNTs samples exhibited sustained iodine release over 28 days without an initial burst. Notably, the amount of iodine released from I-TNTs was significantly higher compared to the control group. TNTs with a higher aspect ratio (AR) and the ECA process using higher potassium iodide (KI) concentration were found to have better cumulative iodine release profiles. No cytotoxicity was observed when tested against the mouse calvaria-derived preosteoblast cell line (MC3T3-E1). The antibacterial property of the implant surface became evident within 24 hours, with complete inhibition of S. aureus and MRSA in I-TNTs samples. This innovative approach is an intriguing alternative for preventing infections on 3D-printed Ti-6Al-4V implants.

WO3 nanorods were fabricated following electrochemical anodization of tungsten, under controlled hydrodynamic conditions, in electrolytes containing three distinct carboxylic acids: citric, tartaric and L-aspartic acids, to study the influence of these complexing agents on the morphology and arrangement of the oxide layers. The samples were characterized by FESEM, TEM and XRD, and electrochemical analyses (EIS and ECSA) to assess their potential as anode materials for lithium-ion batteries. This characterization showed the nanostructures anodized in the presence of tartaric acid exhibit uniform morphology and lower total charge transfer resistance associated with the nanostructured layer of WO3 and cycling stability, resulting in more efficient electrochemical processes, better conductivity and stability, making these nanostructures promising for anodes in lithium-ion batteries. The cycling of the batteries was also conducted to understand the behavior of the nanostructures as anodes against metallic lithium. The results showed that the nanostructures analyzed in the presence of tartaric acid exhibited the best initial specific capacity, improving the capacity provided by the graphite ones. These samples also showed a good recovery after faster cycling. These findings demonstrate the effectiveness of complexing-agent-assisted anodization as a strategy for tailoring WO3 nanostructures with enhanced electrochemical performance.

The majority of volatile organic compounds (VOCs) are hazardous pollutants that pose significant risks to human health and the environment. Thus, the development of a smart sensing system for the early identification of VOCs would be in high demand, particularly those enabling rapid detection with high sensitivity and long-term stability. In this study, an interferometric optical sensor was rationally devised through the facile non-atmospheric thermolysis of polystyrene (PS) pre-loaded into a porous silicon (pSi) template prepared via electrochemical anodization. During the thermolysis, styrenic carbon fragments were covalently grafted onto the pore walls of pSi to form a PS-grafted pSi composite (pSi-PS). This composite was subsequently utilized as a scaffold for grafting poly(4-chlorostyrene) (PPCS) via a second thermolysis step, consequently yielding the double-grafted pSi composite (pSi-PS-PPCS). The obtained samples were subsequently employed as an interferometric optical sensor for the sensitive detection of various VOCs, including ethanol, isopropanol, isobutanol, n-hexane, methyl ethyl ketone (M. E. K.), and ethyl acetate. The sensitivity of the optical response to those VOCs exhibited the following order: n-hexane < ethanol < isopropanol < M. E. K. < isobutanol < ethyl acetate. Notably, the double-grafted pSi-PS-PPCS sensor exhibited significantly higher sensitivity than both pristine pSi and single-grafted pSi-PS. The highly enhanced sensitivity of pSi-PS-PPCS, particularly toward isobutanol and ethyl acetate vapors, was mainly attributed to strong intermolecular interactions (such as hydrophobic, hydrogen bonding effects and/or strong interplay of π–π interactions) between the VOC analytes and the chlorine-substituted phenyl moieties of the grafted PPCS.

Alzheimer’s disease (AD) is a growing challenge worldwide, with current treatments largely symptomatic and limited. The current study aimed to introduce coated nanoporous membranes for localized drug delivery of donepezil, combining both antifouling activity and sustained drug release, unlike traditional Alzheimer’s treatments that rely on systemic administration. Nanoporous membranes were prepared by electrochemical anodization, coated with Polymethyl methacrylate (PMMA) or a PMMA/polyurethane (PU) mixture to mitigate biofouling. The fabricated nanoporous membranes before and after coating were characterized using SEM/EDX, FTIR, BET, and contact angle measurements. In vitro drug release and release kinetics were studied in artificial cerebrospinal fluid (ACSF). Coated and donepezil loaded membranes were implanted on the dura surface in Wistar rats AD model via intracerebral streptozotocin (STZ) injection. The activity was evaluated on behavioral, biochemical and histological levels. PMMA enhanced membrane hydrophobicity (contact angle increased from 62.8° to 79°) and sustained drug release over 7 days, making it the preferred coating. The PMMA membrane demonstrated a reduction in beta-amyloid levels without being loaded with donepezil, while the donepezil-loaded membrane showed cognitive function improvement in Morris water maze and Y-maze. Acetylcholinesterase activity was elevated after STZ-induction of AD and got ameliorated by the membranes implantation. Brain-Derived Neurotrophic Factor (BDNF) was lowered by STZ, while increased in treated animals. Histological examination revealed the neuronal regeneration after donepezil-loaded PMMA coated membrane. These findings suggest that coated nanoporous membranes are promising systems for localized active donepezil drug delivery for AD-like symptoms modulation in STZ-induced AD model, warranting further validation in other AD paradigms.Supplementary InformationThe online version contains supplementary material available at 10.1038/s41598-025-26181-z.

Solar energy conversion into fuels and added-value chemicals is a promising alternative to existing technologies based on fossil fuels and thermally-driven processes. In this realm, the use of metallic nanoparticles supporting surface plasmon resonances has shown the capability to drive industrially-relevant chemical reactions at high rates and control over product selectivity. However, deciphering energy transfer channels underlining photo-reactivity is often complex, due to the concomitant action of several plasmonic effects such as intense near-fields, generation of hot carriers, and significant local heating. Several challenges are associated to their detection in nanoparticle ensemble forming packed-bad reactors under operando conditions. In this talk, I will discuss an alternative approach to powdered photocatalysis that makes use of scalable periodic arrays of plasmonic nanoantennas organized on a flat substrate, i.e. metasurfaces. I will show that, in these systems, the investigation and determination of plasmonic effects is more precise than in traditional settings, while different challenges emerges. We fabricate self-organized one-dimensional nanostructures on metallic substrates by using electrochemical anodization. This process produces cm-scale plasmonic metasurfaces with exceptional opto-thermal properties that, depending on the employed materials, enable either to create high temperatures under modest light concentration or highly intense non-thermal effects that drive photochemistry locally. In one example, we demonstrate the use of refractory plasmonic metasurfaces for carbon dioxide reduction. I will discuss the impact of thermal and non-thermal effects in both one-electron and multi-electron multi-proton reduction reactions. In a second example, I will show the possibility of using only non-thermal effects to catalyze ammonia decomposition for hydrogen production.

Achieving global environmental sustainability requires the development of high-efficiency, low-energy materials and technologies, with an emphasis on passive systems that minimize or eliminate external power requirements. At the same time, the limited availability of critical raw materials is accelerating the search for abundant, safe alternatives. Current catalytic approaches to environmental purification and solar fuel production depend heavily on precious metals and energy-intensive processes, while functional CO₂ conversion to solar fuels remains a major challenge.Titanium dioxide (TiO₂) is a widely used, chemically stable, and non-toxic material employed across diverse industries. However, its catalytic activity as a stand-alone material is constrained by its wide band gap—limiting activation to UV light—and rapid charge carrier recombination. Nanostructuring TiO₂ into self-organized nanotube (NT) arrays via electrochemical anodization can enhance surface area and improve charge separation. Despite these improvements, TiO₂ still suffers from poor CO₂ adsorption, limiting its application in photocatalytic CO₂ reduction.To overcome these limitations, this study explores the functionalization of nanotubular TiO₂ with copper (Cu) co-catalysts to enhance CO₂ adsorption and catalytic activity. The research focuses on the controlled synthesis of Cu-modified TiO₂ NTs and the in situ investigation of their photocatalytic performance. The influence of structural parameters—such as NT morphology, surface area, and co-catalyst loading—on CO₂ reduction efficiency is analyzed.Our findings demonstrate that co-catalyst integration enhances TiO₂’s photocatalytic response, offering a promising, cost-effective route for solar fuel production and environmental remediation. This work contributes to the development of sustainable catalytic systems by coupling earth-abundant materials with scalable nanostructuring techniques.

Energy storage forms an important role in net-zero energy transition and greening the energy grid. Lithium batteries with nonaqueous electrolytes are the major electrochemical energy storage devices used in day-to-day activities. However, high fabrication costs and recent safety incidents have forced researchers to search for safe and cost-effective alternatives. [1] Tapping into alternative energy storage is crucial for reducing the impact of lithium battery and green energy transition. Aqueous rechargeable zinc-ion batteries with high theoretical capacity (820 mAh g-1/ 5855 mAh cm-3) and economical fabrication costs are emerging as a strong contender in the post the lithium era.[2] Despite the advantages, its practical application is hindered by its short cycle life and low capacity. Zinc anode suffers from dendrites formation and other parasitic reactions due to uneven stripping and plating and cathode suffers from active material dissolution.[3] Dendritic growth during cycling causes the battery to short-circuit and cell failure. In the recent times, engineering strategies are adopted at the anode to enhance the performance of battery. These involves modification of zinc interface to artificially generate uniform electric fields and directing uniform ion flux during plating to suppress the unwanted reaction .Herein, an electrochemical anode modification strategy is demonstrated to curb the uncontrolled dendritic growth of zinc and side reaction. It involves the in situ generation of a zincophilic solid-electrolyte interface (SEI) based on a Zn nanoparticle-integrated poly(acrylic acid) hybrid layer on the anode.[4] The characterization of the polymer hybrid layer reveals the Zn nanoparticle integrated hybrid polymer with hydrophilic nature, porous morphology and polar functionalities (-C=O and >N-H). The porous polymeric interface with homogeneously distributed polar functionalities regulates the uniform zinc ion flux during plating, while the Zn nanoparticles serve as the nucleation sites for the deposition. The electrochemical characterization was performed to understand the role of hybrid layer in zinc deposition and suppressing side reactions. Cyclic voltammetry (1 mVs-1) in asymmetric set-up (Zn||Ti) for the modified anode shows better plating and stripping compared to unmodified anode. Current transient analysis with Scharifker-Hills model shows the instantaneous mode of nucleation. The galvanic charge-discharge (GCD) in asymmetric cell shows enhanced coulombic efficiency and low polarization voltage for modified anode. Tafel analysis and hydrogen overpotential experiment shows the suppressed corrosion and hydrogen evolution. The polymer hybrid layer was further tested in symmetrical cell (Zn||Zn) GCD at current density 1 mA cm-2 and 1mAh cm-2. Polymer hybrid layer has an enhanced lifecycle of > 860 h with a reduced voltage gap of 28 mV compared to 198 h of unmodified zinc. Impedance analysis in symmetric cell set-up shows the low charge transfer value for modified zinc. The full cell fabricated by pairing the engineered anode with α-MnO2 cathode showed a high discharge specific capacity of 238.3 mAh g-1 at 0.2 A g-1 with a capacity retention of 81.76% after 200 cycles and a long lifecycle. The cyclic voltametric studies (Zn||MnO2) show increased current response and small ΔEP for the modified zinc. The full cell exhibits a good rate capability which demonstrates its dynamic ability to sustain charge-discharge at varied current densities. The zincophilic hybrid SEI layer protects the anode from unwanted dendritic growth and side reactions and increasing the performance of the battery.

The self-organized TiO2 nanotube layers have attracted considerable scientific and technological interest over the past 20 years motivated for their wide range of applications including (photo-) catalysis, hydrogen generation and biomedical uses (1,2). The synthesis of the 1D TiO2 nanotube layers is carried out by a conventional electrochemical anodization of valve Ti metal sheets in various electrolytes or eventually by bipolar anodization in the wireless fashion (3).By now, the synthesis of TiO2 nanotube layers with different nanotube dimensions (diameter, length) and the application of these nanotube layers is well established on the laboratory scale. However, for real applications outside the laboratory scale, such as photocatalysis (3), TiO2 nanotube layers of much larger size are necessary. Until our efforts, just a few efforts were carried out to scale up the size of the nanotube layers to more than a few cm2 (3-8) due to the difficulty of controlling the parameters of the anodization process on a larger scale. The main challenge is the huge current received during the anodization of large substrates. This, in turn, leads to an increase in the electrolyte temperature that may result in dielectric breakdown of the growing nanotube layers. However, upon extensive optimization of the anodization conditions, we managed to overcome these challenges.In this presentation, the preparation of TiO2 nanotube layers on larger area titanium substrates (dozens of cm2) will be discussed, taking into account the control of the anodization parameters. The TiO2 nanotube layers were employed for the photocatalytic degradation of hexane, according to ISO standards, and show a superior behaviour compared to reference TiO2 nanoparticle layers of the same thickness (9-11). The use of 3D-printed Ti (12) and TiNb substrates (13) for synthesis of highly photocatalytically active TiO2 nanotube layers will be demonstrated too.References(1) Macak, J.M., Tsuchiya, H., Ghicov, A., Yasuda, K., Hahn, R., Bauer, S., Schmuki, P., Curr. Opin. Solid State Mater., 11, 3 (2007).(2) Lee, K., Mazare, A., Schmuki, P., Chem. Rev., 114, 9385 (2014).(3) Loget, G., So, S., Hahn, R., Schmuki, P., J. Mater. Chem. A, 2, 17740−17745 (2014)(4) Franz, S., Perego, D., Marchese, O., Bestetti, M., J. Water Chem. Tech. 37, 108 (2015).(5) Kim, H.-I., Kim, D., Kim, W., Ha, Y.-C., Sim, S.-J., Kim, S., Choi, W., Appl. Catal. A: Gen. 521, 174 (2016).(6) Ghosh, J.P., Achari, G., Langford, C.H., Water Environ. Res. 88, 785 (2016).(7) Xiang, C., et al., J. Phys. Chem. C 121, 15448 (2017).(8) Mena, E., de Vidales, M., Mesones, S., Marugan J., Catal. Today 313, 33 (2018).(9) Sopha, H., & Macak, J.M., Electrochem. Commun., 97, 91 (2018).(10) Sopha, H., & Macak, J.M., et al., Appl. Mater. Today, 29, 101567 (2022).(11) Sopha, H., & Macak, J.M., et al., ACS Appl. Nano Mater. 6, 17053−17059 (2023).(12) Sopha H., & Macak, J.M., et al., Nano Lett., 21, 8701-8706 (2021)(13) Sopha, H., Sepúlveda, M., & Macak, J.M., et al., Nano Lett., 23, 6406-6413 (2023)

Lithium sulfur (Li/S) batteries offer high energy density but suffer from pronounced self-discharge during rest. While commonly attributed to chemical parasitic reactions or polysulfide shuttling, this work emphasizes the overlooked electrochemical processes at the anode. A 1D physics-based model, implemented in COMSOL Multiphysics, incorporates lithium-metal oxidation and stepwise polysulfide reduction to simulate galvanostatic discharge followed by open-circuit rest. Excluding anode reactions yields stable voltage and species concentrations, whereas their inclusion causes gradual voltage decay, continued sulfur reduction, and Li₂S precipitation trends consistent with experimental observations. These results establish electrochemical anode reactions as a primary driver of self-discharge and provide a mechanistic basis for predictive Li/S battery models. As part of future work, in-house experimental data will be compared with model predictions to further validate and refine the proposed framework.

BackgroundDental implant success critically depends on soft tissue integration (STI) to prevent peri-implantitis. Macrophages, key immune regulators, exhibit distinct pro-inflammatory (M1) or anti-inflammatory/pro-healing (M2) phenotypes, significantly impacting peri-implant tissue responses. While implant surface nanostructures modulate macrophage polarization, the effects of specific topographies and underlying mechanisms require further elucidation. This study investigated the ability of an anodized anisotropic titanium dioxide nanoporous (TNP) surface to direct human macrophage polarization toward the M2 phenotype and explored the associated mechanisms.MethodsAn anisotropic nanoporous titanium topography was fabricated via electrochemical anodization followed by annealing. Surface characterization included morphological analysis (FE-SEM, AFM), wettability assessment (contact angle measurement), and evaluation of mechanical properties (nanoindentation, nanoscratch testing). THP-1-derived macrophages were utilized for in vitro evaluation. Cell viability and adhesion were measured using the CCK-8 assay. Macrophage morphology was observed via scanning electron microscopy (SEM). Polarization status was assessed by flow cytometry (CD68, CD86, CD206) and RT-qPCR (CD86, CD206, TNF-α, IL-1β, iNOS, TGF-β). Subsequently, transcriptomic profiling through RNA sequencing (RNA-Seq) was conducted to analyze underlying molecular pathways.ResultsThe TNP surface featured uniform 30 nm diameter nanopores, significantly increased hydrophilicity and surface energy, and adequate mechanical properties. Macrophage early adhesion and spreading (enhanced pseudopodia formation) were significantly increased on TNP compared to control. Flow cytometry and RT-qPCR revealed that TNP induced M2 polarization, as evidenced by significantly upregulated CD206 and TGF-β expression, while downregulating pro-inflammatory markers (CD86, TNF-α, IL-1β, and iNOS). RNA-Seq analysis further identified significant alterations in genes associated with cell projection membranes, collagen fiber organization, and actin binding.ConclusionsAnodization followed by annealing successfully created a mechanically stable, hydrophilic titanium nanoporous surface. The in vitro study demonstrated that the specific nano-topographical structure enhanced macrophage adhesion and spreading, inducing a shift towards the anti-inflammatory M2 phenotype characterized. The observed polarization is potentially associated with cytoskeletal reorganization and the activation of mechanotransduction pathways triggered by the nanostructure. This surface modification strategy offers significant potential for enhancing dental implant abutment soft tissue integration by favorably modulating the local immune response.Supplementary InformationThe online version contains supplementary material available at 10.1186/s12903-025-07131-7.

This work reports the controlled synthesis and characterization of nanoenergetic composites composed of porous silicon (PS) impregnated with sodium perchlorate (NaClO4) for precision energy-release applications. PS films were fabricated by electrochemical anodization of p-type silicon (10–20 Ω·cm), with systematic variation in current density (50–200 mA cm−2) and anodization time (10–25 min) to tailor pore morphology. The energetic behavior of the composites was evaluated through thermal ignition tests, optical emission spectroscopy (300–1000 nm), acoustic analysis (0–500 Hz), and high-speed imaging. Optimal energy release was obtained for PS films anodized at 100 mA cm−2 for 15–20 min, attributed to their hierarchical pore architecture that facilitated complete oxidant infiltration. Overall, this work provides additional insights beyond previous reports by correlating the explosive efficiency with both anodization time—linked to PS film thickness—and current density—associated with porosity. A portable multispectral optical system with fiber-optic access to the explosion chamber was developed for in situ characterization, offering a safe and versatile approach for measurements in explosive environments. To the best of our knowledge, no prior studies have analyzed the correlation between the acoustic signatures and explosion intensity in PS–NaClO4 systems as proposed here.

This study presents a systematic investigation into the fabrication and corrosion behavior of nanoporous titanium dioxide (TiO2) films formed via electrochemical anodization. Optimized anodization parameters, including electrolyte composition, applied voltage, and processing duration, yielded uniform nanoporous TiO2 layers with pore diameters of 60-70 nm and thicknesses of 2-3 μm. Structural and compositional analyses using SEM, EDS, and XRD confirmed the formation of a well-ordered anatase TiO2 phase. Post-anodization annealing further enhanced oxide purity by eliminating residual fluorides, as evidenced by XPS depth profiling. Electrochemical characterization in 25 mM Na2SO4 with increasing H2O2 concentrations revealed significantly improved corrosion resistance of anodized Ti compared to untreated Ti. Despite the lower polarization resistance (R p) observed in EIS, the anodized oxide exhibited stable passivation, reduced corrosion current densities, and favorable capacitive behavior, attributed to its porous morphology and chemical stability. These findings demonstrate that engineered nanoporous TiO2 films offer robust corrosion protection in oxidizing environments, supporting their application in biomedical devices, catalytic systems, and advanced nuclear materials.

WO3 nanostructures for photoelectrocatalytic emerging pollutants degradation: influence of carboxylic acids on electrochemical anodization

Photothermal conversion is an important compensation to the current energy system, which is capable of converting the sunlight into thermal energy. Copper serves as an excellent heat conductor but exhibits limited absorption over the solar spectrum, even with oxide coatings upon annealing. Herein, vertically aligned copper oxides are tailored on the copper surfaces by electrochemical anodization. The current transient renders a unique stepped profile, which corresponds to the structure evolution from a double-layered stack, i.e., the Cu(OH)2 nanowires sitting atop the CuO nanosheets, to a single-layered CuO nanosheets. The as-anodized CuO nanosheets impart strong light absorption in the range of 200-1200nm. Under one sun illumination, the water rises up to 102.6°C in 20min inside copper tubes with the CuO coatings, as compared to the 60.6°C without the coatings. Under frozen conditions, the CuO nanosheets also result in a rapid de-icing process in just 700 s, in obvious contrast to the 1200 s for pristine copper. This is attributed to the high photothermal conversion efficiency of 73.6% for the CuO coatings, being more than doubled with respect to the copper. The photothermal coatings may find important applications in seawater desalination, evaporation-induced electricity generation, hydrogen evolution reaction, etc.

Electrosynthesis offers a promising method to make valuable chemicals under mild conditions; however, its application has been greatly hampered by issues including the requirement of a supporting electrolyte, the limited solubility of reactant(s) in electrochemical compartments, the complex product(s) separation processes, etc. Herein, we innovatively present a four-compartment electrochemical reactor equipped with delicately designed active species diffusion membrane electrodes. Four compartments include two chemical (reduction and oxidation) compartments and two electrochemical (cathode and anode) compartments. The unique membrane electrodes physically separate the chemical compartments (containing organic reactants in pure solvent) from the electrochemical compartments (containing supporting electrolytes), while allowing electrosynthesis of high-value-added chemicals in both nonconducting aqueous and organic environments without the need of a supporting electrolyte. The reactor is able to drive both the anodic electrosynthesis (e.g., oxidation with a halogenation yield > 93%) and the cathodic electrosynthesis (e.g., reduction with a hydrogenation yield > 95% and a deuteration incorporation > 85%). The batch four-compartment electrochemical reactor can be engineered into a continuous type, where substrates in pure solvent can be converted into products with a conversion > 90% as they travel from the inlet to the outlet of the continuous reactor.

The production of H2 via water electrolysis is limited by the kinetically sluggish oxygen evolution reaction (OER) that occurs on the anode of water electrolysis. In alkaline water electrolysis, OER is catalyzed equally well by non-noble metals-based catalysts. In this study, we report one such advanced OER electrocatalyst developed by an unconventional electrochemical anodization in acid from a readily available, abundant, and cheap permalloy (Ni0.8Fe0.2). The unconventionally activated (in sulfuric acid (pH 0)) commercially purchased Ni0.8Fe0.2 sheets delivered 10 mA cm-2 at 264 mV in 1.0 M KOH for OER while maintaining an impressive 95% activity retention after 12 h. All this while exhibiting smaller Tafel slope (38 mV dec-1) testifying ultrafast OER kinetics. Our analysis revealed that the unconventional acid activation led to the increased surface roughness of the permalloy substrate that featured intrinsically OER active NiFeOOH nanostructures on the surface. Such intentional design converted the otherwise moderately active permalloy into a high-performance OER electrocatalyst. This study can also be extended to other prospective substrates for similar electrochemical activation and their subsequent use in OER and in other energy conversion electrocatalytic reactions.

Electrochemical anodization of β-Ti35Nb5Ta alloy for enhanced surface and mechanical properties

This work investigates the thermal and structural transformation of TiO 2 nanoparticles (TiO 2 NPs) generated through electrochemical anodization in a fluoride‐based electrolyte, with a focus on understanding their formation via nanotube fragmentation. This disintegration pathway, characteristic of a top‐down progression, is modeled and visualized to clarify the origin of the nanoparticles. Temperature‐controlled annealing (100–1000 °C) governs phase behavior, crystallinity, and surface properties, with Na 2 Ti 6 O 13 emergence linked to a suppressed anatase‐to‐rutile transformation. TiO 2 NPs annealed at 400 °C demonstrate peak photocatalytic activity, achieving 77% caffeine degradation. These insights bridge formation mechanism and functional performance, offering a pathway‐based perspective on material tailoring.

This study investigatesthe synthesis and electrochemical performanceof NiCo2O4 anodes for water electrolysis inboth alkaline and anion exchange membrane (AEM) configurations. Anengineered direct growth method using a urea-mediated sono-hydrothermalapproach was used to synthesize NiCo2O4 on Nifelt, creating a binder-free electrode optimized for an alkaline environment.We evaluated the electrode’s performance in AEM water electrolysis,comparing it with a spray-coated electrode incorporating ionomersand the same electrocatalyst. Our findings highlight that direct-grownbinder-free electrodes, produced through varied synthesis routes,exhibit remarkable activity and stability in AEM cells operated indry cathode mode (1.90 V @ 1 A cm–2), with seamlessinteraction between the catalyst layer and the membrane. Moreover,this binder-free NiCo2O4 on Ni felt is alsoan efficient anode under alkaline electrolysis configuration, exhibitinghigh stability and remarkable performance (1.78 V @ 1 A cm–2, 1.92 V @ 2 A cm–2), ascribable to the increasedconductivity and improved charge transfer resistance of the catalystlayer.

Abstract A novel nonenzymatic glucose sensor based on a CuO nanoflowers‐decorated reduced graphene oxide (CuONFs@rGO) nanocomposite was successfully fabricated via a facile, green, and cost‐effective electrochemical anodization method. In this synthesis, NaOH served both as the electrolyte and reducing agent, enabling the efficient deposition of CuO nanoflowers onto rGO sheets through electrochemical etching.The structural and morphological characteristics of the CuONFs@rGO nanocomposite were thoroughly investigated using high‐resolution transmission electron microscopy (HR‐TEM), field emission scanning electron microscopy (FE‐SEM), X‐ray diffraction (XRD), and electrochemical impedance spectroscopy (EIS). Electrochemical performance was evaluated using cyclic voltammetry and chronoamperometry techniques.The CuONFs@rGO‐modified electrode exhibited outstanding electrocatalytic activity toward glucose oxidation in alkaline media, with a significant reduction in overpotential compared to previously reported systems. The sensor demonstrated high sensitivity (2294.33 µA·mM−1·cm−2), a low detection limit (0.9 µM, S/N = 3), and a wide linear detection range (0.01–3 mM). Additionally, the sensor showed excellent selectivity, reproducibility, and stability, confirming its potential for practical applications in nonenzymatic glucose sensing.