Effect of the Synergistic Interaction of Micro- and Nanostructures with Silver Ions on the Biocompatibility and Antimicrobial Properties of Ti-15Mo-2.5Ag.

Titanium and titanium alloys have the advantages of a low density and a close elastic modulus to natural bone, which can reduce the stress-shielding effect and become one of the first choices for human hard tissue replacement and repair. However, implant site infection is still one of the main reasons for implantation failure. In this paper, 2.5 wt % Ag element was added to Ti-15Mo to obtain a low modulus, and a surface anodization was applied to improve the surface biocompatibility. The elastic modulus, micromorphology, surface elemental valence, corrosion resistance, antimicrobial properties, and cytocompatibility were investigated by mechanical tests, scanning electron microscopy, X-ray photoelectron spectroscopy, electrochemical tests, inductively coupled plasma spectroscopy, plate counting method, and cellular tests. The experimental results showed that the anodized Ti-15Mo-2.5Ag sample exhibited an elastic modulus of 79 GPa, a strong corrosion resistance, a strong antimicrobial ability of ≥99.99%, and good biocompatibility. It was demonstrated that the formation of Ag2O on the surface and Ag ion release improved the antimicrobial properties and that the structural synergism of silver ions with micro- and nanostructures played an important role in promoting the early spreading of cells and improving the cytocompatibility.

In situ deposition of bismuth on pre-anodized screen-printed electrode for sensitive determination of Cd2+ in water and rice with a portable device.

Electrochemical detection is favorable for the rapid and sensitive determination of heavy metal cadmium. However, the detection sensitivity needs to be further improved, and a portable, low-cost device is needed for on-site detection. Herein, an in-situ bismuth modified pre-anodized screen-printed carbon electrode (SPCE) was developed for Cd2+ determination by square wave anodic stripping voltammetry (SWASV). The in-situ bismuth modification enhances the enrichment of Cd2+, and together with pre-anodization improve the electron transfer rate of electrode, thus enhancing the detection sensitivity. The electrode modification method combines pre-anodization and in-situ bismuth deposition, which is very easy and effective. Furthermore, a self-made PSoC Stat potentiostat coupled with a stirring device was fabricated for portable and low-cost electrochemical detection. After comprehensive optimization, the developed method can reach a testing time of 3 min, a detection limit of 3.55 µg/L, a linear range of 5-100 µg/L, and a recovery rate of 91.7-107.1% in water and rice samples for Cd2+ determination. Therefore, our method holds great promise for the rapid, sensitive and on-site determination of Cd2+ in food samples.

Surface Engineering of Anodic WO3 Layers by In Situ Doping for Light-Assisted Water Splitting.

This study presents a novel approach to fabricating anodic Co-F-WO3 layers via a single-step electrochemical synthesis, utilizing cobalt fluoride as a dopant source in the electrolyte. The proposed in situ doping technique capitalizes on the high electronegativity of fluorine, ensuring the stability of CoF2 throughout the synthesis process. The nanoporous layer formation, resulting from anodic oxide dissolution in the presence of fluoride ions, is expected to facilitate the effective incorporation of cobalt compounds into the film. The research explores the impact of dopant concentration in the electrolyte, conducting a comprehensive characterization of the resulting materials, including morphology, composition, optical, electrochemical, and photoelectrochemical properties. The successful doping of WO3 was confirmed by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence measurements, X-ray photoelectron spectroscopy (XPS), and Mott-Schottky analysis. Optical studies reveal lower absorption in Co-doped materials, with a slight shift in band gap energies. Photoelectrochemical (PEC) analysis demonstrates improved PEC activity for Co-doped layers, with the observed shift in photocurrent onset potential attributed to both cobalt and fluoride ions catalytic effects. The study includes an in-depth discussion of the observed phenomena and their implications for applications in solar water splitting, emphasizing the potential of the anodic Co-F-WO3 layers as efficient photoelectrodes. In addition, the research presents a comprehensive exploration of the electrochemical synthesis and characterization of anodic Co-F-WO3, emphasizing their photocatalytic properties for the oxygen evolution reaction (OER). It was found that Co-doped WO3 materials exhibited higher PEC activity, with a maximum 5-fold enhancement compared to pristine materials. Furthermore, the studies demonstrated that these photoanodes can be effectively reused for PEC water-splitting experiments.

TiO2 nanotubes with customized diameters for local drug delivery systems.

In this study, we evaluated the drug release behavior of diameter customized TiO2 nanotube layers fabricated by anodization with various applied voltage sequences: conventional constant applied potentials of 20 V (45 nm) and 60 V (80 nm), a 20/60 V stepped potential (50 nm [two-diameter]), and a 20-60 V swept potential (49 nm [full-tapered]) (values in parentheses indicate the inner tube diameter at the top part of nanotube layers). The structures of the 50 nm (two-diameter) and 49 nm (full-tapered) samples had smaller inner diameters at the top part of nanotube layers than that of the 80 nm sample, while the outer diameters at the bottom part of nanotube layers were almost the same size as the 80 nm sample. The 80 nm sample, which had the largest nanotube diameter and length, exhibited the greatest burst release, followed by the 50 nm (two-diameter), 49 nm (full-tapered), and 45 nm samples. The initial burst released drug amounts and release rates from the 50 nm (two-diameter) and 49 nm (full-tapered) samples were significantly suppressed by the smaller tube top. On the other hand, the largest proportion of the slow released drug amount to the total released drug amount was observed for the 50 nm (two-diameter) sample. Thus, 50 nm (two-diameter) achieved suppressed initial burst release and large storage capacity. Therefore, this study has, for the first time, applied TiO2 nanotube layers with modulated diameters (two-diameter and full-tapered) to the realization of a localized drug delivery system (LDDS) with customized drug release properties.

Various Antibacterial Strategies Utilizing Titanium Dioxide Nanotubes Prepared via Electrochemical Anodization Biofabrication Method.

Currently, titanium and its alloys have emerged as the predominant metallic biomaterials for orthopedic implants. Nonetheless, the relatively high post-operative infection rate (2-5%) exacerbates patient discomfort and imposes significant economic costs on society. Hence, urgent measures are needed to enhance the antibacterial properties of titanium and titanium alloy implants. The titanium dioxide nanotube array (TNTA) is gaining increasing attention due to its topographical and photocatalytic antibacterial properties. Moreover, the pores within TNTA serve as excellent carriers for chemical ion doping and drug loading. The fabrication of TNTA on the surface of titanium and its alloys can be achieved through various methods. Studies have demonstrated that the electrochemical anodization method offers numerous significant advantages, such as simplicity, cost-effectiveness, and controllability. This review presents the development process of the electrochemical anodization method and its applications in synthesizing TNTA. Additionally, this article systematically discusses topographical, chemical, drug delivery, and combined antibacterial strategies. It is widely acknowledged that implants should possess a range of favorable biological characteristics. Clearly, addressing multiple needs with a single antibacterial strategy is challenging. Hence, this review proposes systematic research into combined antibacterial strategies to further mitigate post-operative infection risks and enhance implant success rates in the future.

Anodic Production and Characterization of Biomimetic Oxide Layers on Grade 4 Titanium for Medical Applications.

Biomaterials are the basis for the development of medicine because they allow safe contact with a living organism. The aim of this work was to produce innovative oxide layers with a microporous structure on the surface of commercially pure titanium Grade 4 (CpTi G4) and to characterize their properties as drug carriers. The anodization of the CpTi G4 subjected to mechanical grinding and electrochemical polishing was carried out in a solution of 1M ethylene glycol with the addition of 40 g of ammonium fluoride at a voltage of 20 V for 2, 18, 24, and 48 h at room temperature. It was found that the longer the anodization time, the greater the number of pores formed on the CpTi G4 surface as revealed using the FE-SEM method, and the greater the surface roughness determined in profilometric tests. As the anodizing time increases, the amount of the drug in the form of gentamicin sulfate incorporated into the resulting pores decreases. The most favorable drug release kinetics profile determined via UV-VIS absorption spectroscopy was found for the CpTi G4 anodized for 2 h.

A Rapid, Efficient Method for Anodic Aluminum Oxide Membrane Room-Temperature Multi-Detachment from Commercial 1050 Aluminum Alloy.

For commercial processes, through-hole AAO membranes are fabricated from high-purity aluminum by chemical etching. However, this method has the disadvantages of using heavy-metal solutions, creating large amounts of material waste, and leading to an irregular pore structure. Through-hole porous alumina membrane fabrication has been widely investigated due to applications in filters, nanomaterial synthesis, and surface-enhanced Raman scattering. There are several means to obtain freestanding through-hole AAO membranes, but a fast, low-cost, and repetitive process to create complete, high-quality membranes has not yet been established. Here, we propose a rapid and efficient method for the multi-detachment of an AAO membrane at room temperature by integrating the one-time potentiostatic (OTP) method and two-step electrochemical polishing. Economical commercial AA1050 was used instead of traditional high-cost high-purity aluminum for AAO membrane fabrication at 25 °C. The OTP method, which is a single-step process, was applied to achieve a high-quality membrane with unimodal pore distribution and diameters between 35 and 40 nm, maintaining a high consistency over five repetitions. To repeatedly detach the AAO membrane, two-step electrochemical polishing was developed to minimize damage on the AA1050 substrate caused by membrane separation. The mechanism for creating AAO membranes using the OTP method can be divided into three major components, including the Joule heating effect, the dissolution of the barrier layer, and stress effects. The stress is attributed to two factors: bubble formation and the difference in the coefficient of thermal expansion between the AAO membrane and the Al substrate. This highly efficient AAO membrane detachment method will facilitate the rapid production and applications of AAO films.

A Comprehensive Study of Aluminum Anodization in Transition Modes.

Anodization is a method to fabricate a tunable nanoporosity and thickness of alumina coating. This research is devoted to large-area hard anodization (HA), ultrahard anodization (UHA), and transitional modes. The phenomenon and challenges of UHA and the transition from HA are studied on large-area samples using linear-sweep voltammetry. The findings indicate that a uniform large-area thick coating can be achieved by utilizing pre-UHA modes. The study's results indicate that UHA leads only to coatings with non-uniform thickness in large-area anodization. The peculiarities of pre-UHA are studied using different temperatures (0, 5, 10, and 15 °C) and processing times (1, 2, 4, 6, and 12 h) in a 0.3 M oxalic acid electrolyte. The current study shows the possibility for the fast growth of thick nanoporous alumina up to 235 ± 4 µm for only 12 h.

Insight into antibacterial effect of titanium nanotubular surfaces with focus on Staphylococcus aureus and Pseudomonas aeruginosa.

Materials used for orthopedic implants should not only have physical properties close to those of bones, durability and biocompatibility, but should also exhibit a sufficient degree of antibacterial functionality. Due to its excellent properties, titanium is still a widely used material for production of orthopedic implants, but the unmodified material exhibits poor antibacterial activity. In this work, the physicochemical characteristics, such as chemical composition, crystallinity, wettability, roughness, and release of Ti ions of the titanium surface modified with nanotubular layers were analyzed and its antibacterial activity against two biofilm-forming bacterial strains responsible for prosthetic joint infection (Staphylococcus aureus and Pseudomonas aeruginosa) was investigated. Electrochemical anodization (anodic oxidation) was used to prepare two types of nanotubular arrays with nanotubes differing in dimensions (with diameters of 73 and 118 nm and lengths of 572 and 343 nm, respectively). These two surface types showed similar chemistry, crystallinity, and surface energy. The surface with smaller nanotube diameter (TNT-73) but larger values of roughness parameters was more effective against S. aureus. For P. aeruginosa the sample with a larger nanotube diameter (TNT-118) had better antibacterial effect with proven cell lysis. Antibacterial properties of titanium nanotubular surfaces with potential in implantology, which in our previous work demonstrated a positive effect on the behavior of human gingival fibroblasts, were investigated in terms of surface parameters. The interplay between nanotube diameter and roughness appeared critical for the bacterial fate on nanotubular surfaces. The relationship of nanotube diameter, values of roughness parameters, and other surface properties to bacterial behavior is discussed in detail. The study is believed to shed more light on how nanotubular surface parameters and their interplay affect antibacterial activity.

Silver-Doped Titanium Oxide Layers for Improved Photocatalytic Activity and Antibacterial Properties of Titanium Implants.

Titanium has a long history of clinical use, but the naturally forming oxide is not ideal for bacterial resistance. Anodization processes can modify the crystallinity, surface topography, and surface chemistry of titanium oxides. Anatase, rutile, and mixed phase oxides are known to exhibit photocatalytic activity (PCA)-driven bacterial resistance under UVA irradiation. Silver additions are reported to enhance PCA and reduce bacterial attachment. This study investigated the effects of silver-doping additions to three established anodization processes. Silver doping showed no significant influence on oxide crystallinity, surface topography, or surface wettability. Oxides from a sulfuric acid anodization process exhibited significantly enhanced PCA after silver doping, but silver-doped oxides produced from phosphoric-acid-containing electrolytes did not. Staphylococcus aureus attachment was also assessed under dark and UVA-irradiated conditions on each oxide. Each oxide exhibited a photocatalytic antimicrobial effect as indicated by significantly decreased bacterial attachment under UVA irradiation compared to dark conditions. However, only the phosphorus-doped mixed anatase and rutile phase oxide exhibited an additional significant reduction in bacteria attachment under UVA irradiation as a result of silver doping. The antimicrobial success of this oxide was attributed to the combination of the mixed phase oxide and higher silver-doping uptake levels.

Influence of Normal-to-High Anodizing Voltage on AAO Surface Hardness from 1050 Aluminum Alloy in Oxalic Acid.

Anodic aluminum oxide (AAO) has been widely applied for the surface protection of electronic component packaging through a pore-sealing process, with the enhanced hardness value reaching around 400 Vickers hardness (HV). However, the traditional AAO fabrication at 0~10 °C for surface protection takes at least 3-6 h for the reaction or other complicated methods used for the pore-sealing process, including boiling-water sealing, oil sealing, or salt-compound sealing. With the increasing development of nanostructured AAO, there is a growing interest in improving hardness without pore sealing, in order to leverage the characteristics of porous AAO and surface protection properties simultaneously. Here, we investigate the effect of voltage on hardness under the same AAO thickness conditions in oxalic acid at room temperature from a normal level of 40 V to a high level of 100 V and found a positive correlation between surface hardness and voltage. The surface hardness values of AAO formed at 100 V reach about 423 HV without pore sealing in 30 min. By employing a hybrid pulse anodization (HPA) method, we are able to prevent the high-voltage burning effect and complete the anodization process at room temperature. The mechanism behind this can be explained by the porosity and photoluminescence (PL) intensity of AAO. For the same thickness of AAO from 40~100 V, increasing the anodizing voltage decreases both the porosity and PL intensity, indicating a reduction in pores, as well as anion and oxygen vacancy defects, due to rapid AAO growth. This reduction in defects in the AAO film leads to an increase in hardness, allowing us to significantly enhance AAO hardness without a pore-sealing process. This offers an effective hardness enhancement in AAO under economically feasible conditions for the application of hard coatings and protective films.

Submerged nanoporous anodized alumina structure for solar-powered desalination.

Development of nanoporous structures utilizing a single step of anodization technique is well recognized as a cost-effective and straightforward approach for several applications. In the current work, anodized alumina was developed with nanoporous structure by utilizing oxalic acid as an electrolyte with a continuous voltage of 40 V. The formed nanoporous structure was subjected to desalination application because of its high absorbance of broadband solar spectrum energy. The desalination setup consists of two solar stills namely conventional and modified. The developed structure is placed in the modified still to examine its performance. It was observed that the structure distributing heat to surrounding water by absorbing photon energy from the sun through the nanopores and giving an efficient pathway to the water vapours for developing effective desalination. The nanoporous structure having ~ 45 nm average diameter. Furthermore, the band gap energy of nanoporous structure was found to be ~ 2.5 eV (absorption spectrum fitting) and ~ 2.8 eV (Tauc plot). The nanoporous structure possess the visible light spectra in solar region which helps the band gaps of nanoporous structure to provide an additional supply of energy for generating more water to evaporate. Moreover, the Urbach energy of the structure is 0.5 eV which reveals less defects in the modified still. The overall distillate yield of modified still was increased to 21% in contrast to conventional. Water quality analysis was also carried out before and after the desalination experiments, and the results were within acceptable limits set by World Health Organization (WHO).

Anodized CuO-based reusable non-enzymatic glucose sensor as an alternative method for the analysis of pharmaceutical glucose infusions: a cyclic voltammetric approach.

Analyzing pharmaceutical products is a quality control requirement in a production facility. This study presents a CuO electrode-based reusable non-enzymatic sensor as an alternative method for rapid analysis of glucose levels in glucose infusions. CuO is extensively employed as an electrode material in non-enzymatic glucose sensors. Conventionally, these electrodes are fabricated using chemical synthesis of CuO followed by immobilization to the electrode substrate. In contrast, here, Cu metal was mechanically modified to create a grooved surface, followed by electrochemical anodization and subsequent annealing process to grow a seamless CuO layer in situ with enhanced catalytic activity. The morphology of the electrodes was characterized using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). The direct electrocatalytic activity of the developed CuO-modified electrode towards glucose oxidation in alkaline media was investigated by cyclic voltammetry in detail. The CuO-modified electrode commenced the oxidation process around 0.10 V vs. Ag pseudo-reference electrode, demonstrating a significant reduction in the overvoltage for glucose oxidation compared to the bare Cu electrode. The sensor is capable of detecting glucose at low oxidation potentials such as 0.2 V with a sensitivity value of 0.37 µA ppm-1, a wide linear range (80-2300 ppm), limit of quantification (LOQ) of 1 ppm, greater repeatability, 1% precision, 3% bias, a short response time (80 s), good reproducibility and excellent reusability (196 consecutive attempts). The enhanced performance and cost-effectiveness make this sensor a promising alternative method for product analysis in glucose injection solutions.

Electrochemical and Mechanical Properties of Hexagonal Titanium Dioxide Nanotubes Formed by Sonoelectrochemical Anodization.

This study aimed to investigate the fabrication and characterization of hexagonal titanium dioxide nanotubes (hTNTs) compared to compact TiO2 layers, focusing on their structural, electrochemical, corrosion, and mechanical properties. The fabrication process involved the sonoelectrochemical anodization of titanium foil in various electrolytes to obtain titanium oxide layers with different morphologies. Scanning electron microscopy revealed the formation of well-ordered hexagonal TNTs with diagonals in the range of 30-95 nm and heights in the range of 3500-4000 nm (35,000-40,000 Å). The electrochemical measurements performed in 3.5% NaCl and Ringer's solution confirmed a more positive open-circuit potential, a lower impedance, a higher electrical conductivity, and a higher corrosion rate of hTNTs compared to the compact TiO2. The data revealed a major drop in the impedance modulus of hTNTs, with a diagonal of 46 ± 8 nm by 97% in 3.5% NaCl and 96% in Ringer's solution compared to the compact TiO2. Nanoindentation tests revealed that the mechanical properties of the hTNTs were influenced by their diagonal size, with decreasing hardness and Young's modulus observed with an increasing diagonal size of the hTNTs, accompanied by increased plastic deformation. Overall, these findings suggest that hTNTs exhibit promising structural and electrochemical properties, making them potential candidates for various applications, including biosensor platforms.

Uniaxial Magnetization and Electrocatalytic Performance for Hydrogen Evolution on Electrodeposited Ni Nanowire Array Electrodes with Ultra-High Aspect Ratio.

Ni nanowire array electrodes with an extremely large surface area were made through an electrochemical reduction process utilizing an anodized alumina template with a pore length of 320 µm, pore diameter of 100 nm, and pore aspect ratio of 3200. The electrodeposited Ni nanowire arrays were preferentially oriented in the (111) plane regardless of the deposition potential and exhibited uniaxial magnetic anisotropy with easy magnetization in the axial direction. With respect to the magnetic properties, the squareness and coercivity of the electrodeposited Ni nanowire arrays improved up to 0.8 and 550 Oe, respectively. It was also confirmed that the magnetization reversal was suppressed by increasing the aspect ratio and the hard magnetic performance was improved. The electrocatalytic performance for hydrogen evolution on the electrodeposited Ni nanowire arrays was also investigated and the hydrogen overvoltage was reduced down to ~0.1 V, which was almost 0.2 V lower than that on the electrodeposited Ni films. Additionally, the current density for hydrogen evolution at -1.0 V and -1.5 V vs. Ag/AgCl increased up to approximately -580 A/m2 and -891 A/m2, respectively, due to the extremely large surface area of the electrodeposited Ni nanowire arrays.

TiO2 Nanotube Arrays Inside Ultrafine Ti Tubes with an Aspect Ratio of 2500 for Sensing Needles: The Bubble Effect in a Confined Space.

Capillary metal tubes have attracted considerable interest for flexible electronics, portable devices, trace sampling, and detection. Tailoring the microstructure and wettability inside the capillary tubes is of paramount importance, yet it presents great difficulty because of the spatial confinement. Here, the coupling effect is revealed between the fluidic and electric field induced by bubble motion in a confined space during anodic oxidation. By controlling the bubble regeneration and flow rate, uniform and superhydrophilic TiO2 nanotube arrays are developed throughout the inner surface of an ultrafine Ti tube with a diameter of 0.4 mm and length of 1000 mm, equivalent to an aspect ratio of 2500 that is the largest value being ever reported. The inner surface of a capillary tube is further coated with a polytetrafluoroethylene layer and explored as a sensing needle for liquid detection in terms of concentration and species. This study provides an innovative approach to tailor the microstructure and wettability in a confined space for functional capillary tubes.

Detailed Insight into Photocatalytic Inactivation of Pathogenic Bacteria in the Presence of Visible-Light-Active Multicomponent Photocatalysts.

The use of heterogeneous photocatalysis in biologically contaminated water purification processes still requires the development of materials active in visible light, preferably in the form of thin films. Herein, we report nanotube structures made of TiO2/Ag2O/Au0, TiO2/Ag2O/PtOx, TiO2/Cu2O/Au0, and TiO2/Cu2O/PtOx obtained via one-step anodic oxidation of the titanium-based alloys (Ti94Ag5Au1, Ti94Cu5Pt1, Ti94Cu5Au1, and Ti94Ag5Pt1) possessing high visible light activity in the inactivation process of methicillin-susceptible S. aureus and other pathogenic bacteria-E. coli, Clostridium sp., and K. oxytoca. In the samples made from Ti-based alloys, metal/metal oxide nanoparticles were formed, which were located on the surface and inside the walls of the NTs. The obtained results showed that oxygen species produced at the surface of irradiated photocatalysts and the presence of copper and silver species in the photoactive layers both contributed to the inactivation of bacteria. Photocatalytic inactivation of E. coli, S. aureus, and Clostridium sp. was confirmed via TEM imaging of bacterium cell destruction and the detection of CO2 as a result of bacteria cell mineralization for the most active sample. These results suggest that the membrane ruptures as a result of the attack of active oxygen species, and then, both the membrane and the contents are mineralized to CO2.

Wide Response Range Photoelectrochemical UV Detector Based on Anodized TiO2-Nanotubes@Ti@quartz Structure.

Conventional sandwich structure photoelectrochemical UV detectors cannot detect UV light below 300 nm due to UV filtering problems. In this work, we propose to place the electron collector inside the active material, thus avoiding the effect of electrodes on light absorption. We obtained a TiO2-nanotubes@Ti@quartz photoanode structure by precise treatment of a commercial Ti mesh by anodic oxidation. The structure can absorb any light in the near-UV band and has superior stability to other metal electrodes. The final encapsulated photoelectrochemical UV detectors exhibit good switching characteristics with a response time below 100 ms. The mechanism of the oxidation conditions on the photovoltaic performance of the device was investigated by the electrochemical impedance method, and we obtained the optimal synthesis conditions. Response tests under continuous spectroscopy confirm that the response range of the device is extended from 300-400 nm to 240-400 nm. This idea of a built-in collector is an effective way to extend the response range of a photoelectrochemical detector.

Morphology and Structure of TiO2 Nanotube/Carbon Nanostructure Coatings on Titanium Surfaces for Potential Biomedical Application.

Titanium is the most used material for implant production. To increase its biocompatibility, continuous research on new coatings has been performed by the scientific community. The aim of the present paper is to prepare new coatings on the surfaces of the pure Ti Grade 2 and the Ti6Al4V alloy. Three types of coatings were achieved by applying anodization and chemical vapor deposition (CVD) methods: TiO2 nanotubes (TNTs) were formed by anodization, carbon nanotubes (CNTs) were obtained through a metal-catalyst-free CVD process, and a bilayer coating (TiO2 nanotubes/carbon nanostructures) was prepared via successive anodization and CVD processes. The morphology and structure of the newly developed coatings were characterized using SEM, EDX, AFM, XRD, and Raman spectroscopy. It was found that after anodization, the morphology of the TiO2 layer on pure Ti consisted of a "sponge-like" structure, nanotubes, and nano-rods, while the TNTs layer on the Ti alloy comprised mainly nanotubes. The bilayer coatings on both materials demonstrated different morphologies: the pure Ti metal was covered by a layer of nanotubular and nano-rod TiO2 structures, followed by a dense carbon layer decorated with carbon nanoflakes, and on the Ti alloy, first, a TNTs layer was formed, and then carbon nano-rods were deposited using the CVD method.

Anodization as a scalable nanofabrication method to engineer mechanobactericidal nanostructures on complex geometries.

Bacterial contamination of implant surfaces is one of the primary causes of their failure, and this threat has been further exacerbated due to the emergence of drug-resistant bacteria. Nanostructured mechanobactericidal surfaces that neutralize bacteria via biophysical forces instead of traditional biochemical routes have emerged as a potential remedy against this issue. Here, we report on the bactericidal activity of titania nanotubes (TNTs) prepared by anodization, a well-established and scalable method. We investigate the differences in bacterial behavior between three different topographies and demonstrate the applicability of this technique on complex three-dimensional (3D) geometries. It was found that the metabolic activity of bacteria on such surfaces was lower, indicative of disturbed intracellular processes. The differences in deformations of the cell wall of Gram-negative and positive bacteria were investigated from electron micrographs Finally, nanoindentation experiments show that the nanotubular topography was durable enough against forces typically experienced in daily life and had minimal deformation under forces exerted by bacteria. Our observations highlight the potential of the anodization technique for fabricating mechanobactericidal surfaces for implants, devices, surgical instruments, and other surfaces in a healthcare setting in a cheap, scalable way.