Ethylene Glycol-based Electrolyte Research Articles

Preparation of highly active and durable electrodes for alkaline water electrolysis by anodizing of commercial FeNi and FeNiCo alloys

Anodizing is gaining popularity as a binder-free fabrication route for obtaining catalyst materials directly on the current collector without using noble metals, binders, or conductive carbon additives. Here, we fabricate promising highly active electrodes for alkaline water electrolysis by anodizing commercial FeNi and FeNiCo alloys (%wt. Fe range between 22 and 63) in an ethylene glycol-based fluoride electrolyte. Anodizing forms metal fluoride coatings, which are converted to OER active compounds (γ-NiOOH:Fe) during potential cycling in an alkaline aqueous solution (1 mol L−1 (M) KOH at 293 K) as a result of leaching of fluoride ions. The morphology, thickness, and number of active sites are influenced by the amount of Fe in the alloy, and the electrode with the highest electrochemical active surface area (Kovar alloy with a 54 %wt. Fe) shows the largest OER activity enhancement by anodizing. The performance evaluation in practical conditions (7 mol L−1 KOH at 343 K) demonstrated a highly active performance with an OER potential as low as 1.52 V at a current density of 600 mA cm−2 even for electrodes obtained in alloys with a low amount of Fe (78-Permalloy with a 22 %wt. Fe), demonstrating that anodizing is an effective way to develop highly active OER electrodes from commercially available alloys. On the other hand, anodizing is a good fluoridation route for transition metals with good results in the formation of F-enriched precursors that efficiently promote active phase formation during the catalytic process, offering the possibility of obtaining catalysts directly on the current collector in a one-step process, easily implemented in industrial applications.

Electrodeposition of Zn and Cu Nanoparticles into TiO2 Nanotubes on Ti6Al4V: Antimicrobial Effect against S. Epidermidis and Cytotoxicity Assessment

Surface modification of the Ti6Al4V alloy (ASTM grade 5), with the fabrication of vertically oriented TiO2 nanotubes, has been receiving increasing attention both as a way to provide advanced bioactive features and the ability to act as reservoirs for a localized, controlled drug release. In this work, TiO2 nanotubes were grown on the surface of a Ti6Al4V alloy through electrochemical anodization. An ethylene glycol-based electrolyte containing 0.5 wt.% NH4F and 2.5% (v/v) H2O was used. Post-anodizing heat treatments at 500 °C in air atmosphere were performed to achieve a crystalline oxide layer with a higher mechanical stability. Following these treatments, Zn or Cu nanoparticles were incorporated into the nanotubular structures through electrodeposition processes. Then, the antimicrobial performance of the obtained surfaces was assessed against Staphylococcus epidermidis, a Gram-positive bacterium common in implant-related infections. Lastly, the cytotoxicity of the produced surface was evaluated against MC3T3-E1 mouse pre-osteoblast cells. In general, Cu-doped TiO2 nanotubes presented an almost total antimicrobial action, while Zn doped samples had a lower, but still significant antibacterial effect. However, a highly cytotoxic effect against MC3T3-E1 cells was observed on all anodized samples due to the release of vanadium from the alloy. In spite of this, the surface modification reported in this work can be a valid solution for existing commercially available orthopedic implants, considering that similar solutions were already studied in in vivo assays.

CO2 Photoreduction Activity Enhancement and Unexpected Observation of Carbon Monoxide Adsorbates on the Surface of TiO2 Nanotube Arrays Synthesized in Formamide Electrolytes.

TiO2 nanotube arrays grown through electrochemical anodization in a formamide-based electrolyte (TNTA-FA) exhibited a whole host of unusual properties compared to nanotubes grown in the conventional ethylene glycol-based electrolyte (TNTA-EG). TNTA-FA exhibited shorter phonon lifetimes, lower lattice strain, more visible light absorption, lower work function, and a highly unusual adsorbate structure consisting of physisorbed and chemisorbed CO along with linearly adsorbed CO2 and various monodentate and bidentate carbonate species. The observation of adsorbed CO in the dark is highly unusual and indicates spontaneous deoxygenation of CO2 on the surface of TNTA-FA. The significance of this finding is that the formation of CO2•- is no longer the rate-limiting bottleneck for the reduction of CO2 on TNTA-FA surfaces as it is for all TiO2 surfaces. TNTA-FA samples are strongly colored (inclusive of a fluorescent green color) and consist of rounded, vertically oriented hollow cylinders as opposed to the honeycomb-like morphology of TNTA-EG arranged in an approximate triangular lattice. The photocatalytic activity was tested through the CO2 photoreduction and dye degradation tests. Formamide-based nanotubes outperformed the EG-based nanotubes by almost 1.7 and 2 times, respectively, in CO2 reduction and dye degradation tests done on methylene blue, brilliant green, and rhodamine B dyes. These results are attributed to stronger surface band bending in TNTA-FA which facilitates more efficient separation of photogenerated electron-hole pairs.

Real-time monitoring of process current and its correlation with micro-feature accuracy and surface topography in electrochemical micromachining of nitinol

The nickel-titanium alloy known as Nitinol classified as a shape memory alloy is distinguished by its exceptional attributes, including shape memory effect, biocompatibility, and superelasticity. However, its thermo-mechanical dependent transformation behavior makes it difficult to process using traditional methods. Electrochemical micromachining (ECMM), a non-traditional fabrication method, uses anodic dissolution process to produce microfeatures on Nitinol. The current work emphasizes the impact of process current on the machining accuracy and surface topography of microchannels produced during ECMM of Nitinol utilizing ethylene glycol-based sodium nitrate electrolyte. The ECMM process parameters that were studied are pulsed potential, molar concentration, and micro-tool scan rate, and the development of the process current resulting in variation of these parameters during microchannel fabrication was closely observed. The statistical parameters, namely, the average process current and the process current fluctuation, were derived from the process current data that were further analyzed with respect to input parameters. The machining accuracy and the surface topography of the microchannel are analyzed by measuring the width overcut, channel depth, stray region, width standard deviation, and average surface roughness of the fabricated microchannel. The results showed that monitoring the process current in real-time is an effective way of controlling the process, particularly when it comes to fabricating micro-features that must adhere to strict predetermined criteria.

Electrodeposition of zinc-nickel alloys from ethylene glycol-based electrolytes in presence of additives for corrosion protection

In the present work the electrodeposition of zinc-nickel alloys with 15-20 wt.% nickel from non-aqueous solutions based on ethylene glycol is investigated. Potentiostatic deposition conditions are used, which are found to offer optimal coating quality and superior control over composition. In addition, ammonium chloride is evaluated as additive to partially suppress zinc incorporation into the deposit and to enhance layer quality. Layers composition, surface morphology of the deposits and their anticorrosive properties are investigated. The electrochemical characteristics of the Zn-Ni electrolytes are studied using cyclic voltammetry measurements. From the phase composition point view, X-ray diffraction results confirm that a metastable γ phase is present in the as deposited Zn-Ni alloys with nickel content 16-18 wt.%. Corrosion tests show that the barrier behaviour against corrosion of Zn-Ni films electrodeposited from the NH4Cl containing bath is superior in comparison to layers plated from an additive-free bath. The use of the additive enlarges the grains and provides a compact surface structure, which upskills the anticorrosive behaviour of the deposit.

Influence of the microstructure of sputtered Ti films on the anodization toward TiO2 nanotube arrays

The microstructure of sputtered Ti films plays a crucial role in the formation of TiO2 nanotube arrays (TNTs) via anodization. Magnetron sputtering under controllable parameters was used to create diverse microstructures of Ti films, followed by anodization in an ethylene glycol-based electrolyte. The relationship between the microstructures of Ti films and the resulting TiO2 layers was analyzed, and the film density was identified as the key microstructure affecting the TNTs formation. The electron aggregation theory explained why denser Ti films facilitate TNTs formation, and confirmatory experiments were performed to validate this theory..

Electrochemical removal of secondary roughness on selective laser melted titanium with an ethylene–glycol-based electrolyte

Partially sintered satellite particles in scaffolds produced via Selective Laser Melting (SLM) create discrepancies between the as-designed and the as-manufactured properties (esp. porosity). These discrepancies impede direct comparison of manufactured parts performance to computer simulations. We propose anodic electrolysis using an electrolyte based on non-aqueous ethlylene-glycol TiCl4 (EthaTi) to remove the secondary roughness on titanium SLM-ed porous scaffolds. Post-processed gyroid scaffolds regained 10% porosity with respect to their as-manufactured value (65.20 ± 0.23%), which was close to the as-designed value (75.12%). Compared to other well-established electrolytes, this method is cost-effective, user-friendly and practical, as it requires shorter processing times, is temperature-stable and of gentler chemistry.

Multi-objective optimization in electrochemical micro-drilling of Ti6Al4V using nature-inspired techniques

ABSTRACT Current study investigates the efficacy of electrochemical micro-drilling (ECMD) process during micro-hole fabrication on a Ti6Al4V alloy sheet of 1.2 mm thickness using a cylindrical-shaped micro-tool. Ethylene glycol-based electrolyte was selected to overcome excessive passivation. Experiments were conducted by altering voltage, feed rate (FR), and electrolyte concentration (EC) using a central-composite-design to observe their effects on the output parameters. The desired response parameters, such as radial overcut (ROC), and taper were examined while fabricating dimensionally accurate micro-holes including the volume removal rate (VRR) that occurred during the process. ANOVA results established voltage as the major significant input parameter that affects all the responses, followed by FR. In addition, different nature-inspired optimization techniques, namely Multi-Objective Grey-Wolf Optimizer (MOGWO), Multi-Objective Bonobo Optimizer (MOBO), and Multi-Objective Particle Swarm Optimization (MOPSO), were employed. MOBO reported the best Pareto-surface in terms of uniformity and spread measures and suggested a FR of 0.3 μm/s for optimal micro-drilling operations.

TiO2 nanotube arrays grown in ethylene glycol-based media containing fluoride: Understanding the effect of early anodization stages on the morphology

In this work, we develop a phenomenological model describing the growth of TiO2 nanotube arrays (NTA-TiO2) by titanium anodization in ethylene glycol-based electrolytes containing fluoride. NTA-TiO2 formation is described in terms of the well-known High-Field mechanism (HFM) considering film thinning by dissolution, and the electronic current contribution according to the Oxygen Bubble Mold (OBM) model, as it has been previously reported. For the first time, the inclusion of the nucleation of oxygen bubbles as the rate determining step at early anodization times is considered. By simultaneous fitting of the potentiostatic j/t profiles and the time evolution of morphological features such as pore radius, layer thickness and density of pores, the behavior observed for several experimental conditions is accurately described, in contrast to previously reported Field Assisted Dissolution (FAD) and OBM models. Proposed model allows obtaining physical and phenomenological information concerning the formation and growth of nanoporous oxide films as well as their morphological properties. Results also indicate that fluoride species play a key role at the early anodization stages, determining the subsequent film morphology evolution. Also, conclusive evidence for a chemical-type instead of field-assisted film dissolution process is obtained.

New insights into the mechanism of coupled photocatalysis and Fenton-based processes using Fe surface-modified TiO2 nanotube layers: The case study of caffeine degradation

TiO2 nanotube (TNT) layers are prepared via electrochemical anodization of Ti foil in ethylene glycol-based electrolyte containing fluoride ions. Using spin-coating of Fe(III) precursor solutions of different concentrations (10 µM to 10 mM), iron surface-modified TNT (Fe-TNT) layers are formed after annealing at 450 °C for 2 h in air. The Fe-TNT layers are comprehensively characterized by XRD, SEM, DRS and XPS. To identify and assess the contribution of photocatalysis and Fenton-based processes that are simultaneously triggered by Fe-TNT layers, degradation of caffeine is investigated in the dark and under UVA with and without the presence of 500 µM H2O2. It has been found that in the presence of H2O2 under UVA, 100 µM Fe-TNT can degrade 67 % of caffeine after 3 h, of which 4 % is from photolysis, 23.5 % from photocatalysis and 39.5 % from Fenton-based processes. It is important to note that Fenton-based reactions are due to the iron leaching, while the main reactive oxygen species are identified as hydroxyl radicals. In addition, the main degradation by-products are identified by LC-MS and IC-MS techniques, thus leading to the proposal of different degradation pathways of caffeine. To sum up, the research's findings provide novel insights into the concept of photochemical versatility, which is only obliquely explored in the corpus of previous research.

Study of the Photocatalytic Properties of Ni-Doped Nanotubular Titanium Oxide

Nanotubular titanium oxide is widely known as a prospective semiconductor photocatalyst for the process of water splitting. Its photoelectrochemical (PEC) efficiency can be improved by doping with 3d metal. In this work, the synthesis of nanotubular titanium oxide (NTO) was carried out by anodizing titanium substrates using two doping techniques. First, Ni-doped TiO2 was obtained by immersion in Ni salt solution; second, an ethylene glycol-based fluoride electrolyte containing Ni2+ ions solution was used. The obtained samples were analyzed using SEM, XRD, and photoelectrochemical methods. The produced Ni-doped NTO exhibited photocatalytic activity twice as high as that of nondoped NTO. Additionally, it was found that the immersion technique initiated a shift of the incident photon to converted electron (IPCE) spectra to the visible part of the spectrum.

Porous vs. Nanotubular Anodic TiO2: Does the Morphology Really Matters for the Photodegradation of Caffeine?

Herein, the preparation of nanotubular and porous TiO2 structures (TNS) is presented for photocatalytic applications. Different TNS were prepared in three different types of glycerol- and ethylene glycol-based electrolytes on a large area (approx. 20 cm2) via anodization using different conditions (applied potential, fluoride concentration). Morphology, structure, and optical properties of TNS were characterized by Scanning Electron Microscopy (SEM), X-ray Diffractometry (XRD), and Diffuse Reflectance Spectroscopy (DRS), respectively. All TNS possess optical band-gap energy (EBG) in the range from 3.1 eV to 3.2 eV. Photocatalytic degradation of caffeine was conducted to evaluate the efficiency of TNS. Overall, nanotubular TiO2 possessed enhanced degradation efficiencies (up to 50% degradation) compared to those of porous TiO2 (up to 30% degradation). This is due to the unique properties of nanotubular TiO2, e.g., improved incident light utilization. As the anodization of large areas is, nowadays, becoming a trend, we show that both nanotubular and porous TiO2 are promising for their use in photocatalysis and could be potentially applicable in photoreactors for wastewater treatment. We believe this present work can be the foundation for future development of efficient TiO2 nanostructures for industrial applications.

Single-step fabrication of highly stable amorphous TiO2 nanotubes arrays (am-TNTA) for stimulating gas-phase photoreduction of CO2 to methane

This study investigates the facile fabrication of interfacial defects assisted amorphous TiO2 nanotubes arrays (am-TNTA) for promoting gas-phase CO2 photoreduction to methane. The am-TNTA catalyst was fabricated via a one-step synthesis, without heat treatment, by anodization of Titanium in Ethylene glycol-based electrolyte in a shorter anodizing time. The samples presented a TiO2 nanostructured array with a nanotubular diameter of 100 ± 10 nm, a wall thickness of 26 ± 5 nm, and length of 3.7 ± 0.3 μm, resulting in a specific surface of 0.75 m2 g. The am-TNTA presented prolonged chemical stability, a high exposed surface area, and a large number of surface traps that can reduce the recombination of the charge carriers. The am-TNTA showed promising photoactivity when tested in the CO2 reduction reaction with water under UV irradiation with a methane production rate of 14.0 μmol gcat−1 h−1 for a pure TiO2 material without any modification procedure. This enhanced photocatalytic activity can be explained in terms of surface defects of the amorphous structure, mainly OH groups that can act as electron traps for increasing the electron lifetime. The CO2 interacts directly with those traps, forming carbonate species, which favors the catalytic conversion to methane. The am-TNTA also exhibited a high stability during six reaction cycles. The photocatalytic activity, the significantly reduced time for synthesis, and high stability for continuous CH4 production make this nanomaterial a potential candidate for a sustainable CO2 reduction process and can be employed for other energy applications.

Band gap reduction of (Mo+N) co-doped TiO2 nanotube arrays with a significant enhancement in visible light photo-conversion: A combination of experimental and theoretical study

The present research aimed to evaluate the effects of co-doping TiO2 nanotube aligned arrays (TNAs) with molybdenum and nitrogen on photocatalytic activity/performance under visible light irradiation. The surface morphology, electronic and optical properties of the pure and modified TNAs based on experimental characterization and theoretical calculations are reported. Both, pure and doped/modified TNAs were synthesized using a single step/low cost anodization method. Titanium sheets were immersed in ethylene glycol-based electrolytes containing NH4F and NH4F + K2MoO4 to fabricate highly ordered TNAs and Mo-doped TNAs, respectively. Mo–N-doped TNAs were fabricated by a thermal annealing process of Mo-doped samples in nitrogen environment (N2-gas flow rate of 400 cc/min) for 2hr at 520 °C. Physical/chemical characteristics, structural and photo-electrochemical/electronic properties of the photo-electrodes were observed using several techniques including, field emission scanning electron microscopy (FESEM), Energy Dispersive X-Ray Spectroscopy (EDX), XRD, X-ray photoelectron spectroscopy (XPS), Raman and UV–Vis spectroscopy. We further used a full potential density functional theory (DFT) method to estimate the morphological and electronic structure of the synthesized photo-anodes and also observed a good agreement between theoretical calculations and characterization results. The characterization techniques confirm that Mo and N atoms have been incorporated into the lattice of anodized TNAs and molybdenum atoms partially substituted titanium atoms in the structure of TNAs. UV–Vis DRS spectroscopy experiments and theoretical results reveal that (Mo + N) co-doping creates a positive synergic effect on the band structure of TNAs which can enhance photo-conversion activity, compared to the single Mo/N-doped TNAs samples. In presence of sacrificial agent/electrolyte (aqueous solution of Na2S/Na2SO3) and visible light irradiation, average photocurrent density of the co-doped TNAs photo-anode is 14 times greater than that of the undoped TNAs.

Insights into the Intrinsic Creation of Heterojunction-Based Ordered TiO2 Nanotubes Obtained from the One-Step Anodic Oxidation of Titanium Alloys

To gain insights into how the presence of the second metal in Ti alloys affects the morphology, crystallinity, chemical structure, and photocatalytic/photoelectrochemical activity of mixed-oxide nanotubes (TiO2–MxOy), five systems were electrochemically synthesized in a fluoride-containing ethylene glycol-based electrolyte by using Ti alloys, with 10 wt % of the second metal, as precursors. The level of self-organization and -orientation in the obtained samples followed the order: Ag < Cu < Mn < V < Co, being the Ti90Ag10_40V sample, the only presenting single Ag nanoparticles embedded in the oxide layer. The highest photocatalytic and photoelectrochemical activities were reported for the Ti90Ag10_40V sample, which can be attained to the heterojunction between the oxides, the formation of single Ag nanoparticles, and the high level of self-organization. Apparently, the intrinsic heterojunction between the oxides depends on the still-needed-to-be-estimated stability of the oxides produced during the anodization of each system.

Suitability of Different Titanium Dioxide Nanotube Morphologies for Photocatalytic Water Treatment.

Photocatalysis has long been touted as one of the most promising technologies for environmental remediation. The ability of photocatalysts to degrade a host of different pollutants, especially recalcitrant molecules, is certainly appealing. Titanium dioxide (TiO2) has been used extensively for this purpose. Anodic oxidation allows for the synthesis of a highly ordered nanotubular structure with a high degree of tunability. In this study, a series of TiO2 arrays were synthesised using different electrolytes and different potentials. Mixed anatase-rutile photocatalysts with excellent wettability were achieved with all the experimental iterations. Under UVA light, all the materials showed significant photoactivity towards different organic pollutants. The nanotubes synthesised in the ethylene glycol-based electrolyte exhibited the best performance, with near complete degradation of all the pollutants. The antibacterial activity of this same material was similarly high, with extremely low bacterial survival rates. Increasing the voltage resulted in wider and longer nanotubes, characteristics which increase the level of photocatalytic activity. The ease of synthesis coupled with the excellent activity makes this a viable material that can be used in flat-plate reactors and that is suitable for photocatalytic water treatment.

Design and characterization of a chloride-free organic copper solution: Electrochemical synthesis of Zn/Cu/Sn precursor stack for CZTS-based photoconversion devices

In the present study, an ethylene glycol-based electrolyte is used to electrodeposit copper onto zinc for the synthesis of the Zn/Cu/Sn stack, precursor of Cu2ZnSnS4. The employed solution contains diethanolamine (DEA) which supports the formation of amine-complexes, whose features are studied by UV–vis absorption, ESI-MS, and FTIR measurements, providing insight on the optimal concentration of DEA for copper complexation. Cyclic voltammetries (CVs) are carried out at increasing [DEA]/[Cu2+] ratios, highlighting the amine effect on the reduction potential of the copper species. The displacement reaction between copper and zinc is investigated by immersion potential measurements, showing a direct correlation to the voltammetric data. The optimized copper solution resulted in a negligible displacement contribution, allowing the electrochemical synthesis of Mo(sub)/Zn/Cu/Sn stack on a relatively large area (4 cm2). The metallic precursor is analyzed by SEM/EDS, AFM, XRD, and GDOES techniques. Finally, the kesterite CZTS phase is obtained through reactive annealing with elemental sulfur and it is characterized by SEM/EDS, XRD, and Raman spectroscopy. Photoelectrochemical water splitting on CZTS/CdS/Pt heterostructure is carried out in an aqueous solution at pH 6.85, showing a photocurrent of -5.05 mA/cm2 at 0 V vs RHE. A maximum applied bias photon-to-current efficiency (ABPE) value of 2.15% was found at 0.84 V bias.

Electrodeposition of Bi-Se thin films involving ethylene glycol based electrolytes

The work is devoted to the electrochemical deposition of Bi-Se thin films from ethylene glycol-based electrolytes. The studies have been carried out by potentiodynamic and galvanostatic methods under various conditions, using Pt and Ni electrodes. By recording cyclic and linear polarization curves, the potential range of deposition of thin Bi-Se films on Pt (-0.75 to -1.2 V) and Ni (0.2 to -0.85 V) electrodes was determined. A comparison of the polarization curves of two electrodes showed that co-electrodeposition of Bi and Se occurs in approximately the same potential range. In order to find the optimal mode and composition of the electrolyte, the effect of various factors (concentration of initial components, temperature, etc.) on the process of co-electrodeposition of Bi with Se was studied. In addition, the samples of Bi-Se thin films obtained on Ni electrodes using the galvanostatic method were studied by scanning electron microscope (SEM) and X-ray phase analysis. The results of X-ray phase analysis confirmed the formation of thin Bi2Se3 films with and without additional heat treatment step. Elemental analysis of obtained films carried out by EDS shows that films contained 62.79 wt. % Bi and 37.21 wt. % Se.

Photocatalytic oxidation of benzyl alcohol and the photoelectrochemical water splitting of visible light-activated TiO2 nanostructures prepared by one-step titanium anodization

Doped TiO2 nanostructures have been prepared by one-step anodization of titanium in an ethylene glycol-based electrolyte with different concentrations of potassium hexacyanocobaltate and their catalytic activity in photocatalytic oxidation of benzyl alcohol to benzaldehyde, and photoelectrochemical water splitting under visible light has been investigated in this work. Field emission scanning electron microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, X-ray diffraction, energy-dispersive X-ray spectroscopy and UV–visible techniques have been used to determine the effect of the concentration of the doping agent on the morphology, structure and optical properties of doped TiO2 thin films. Doped TiO2 nanostructures show significant morphological differences in comparison with commercial bare TiO2 nanotube samples, based on SEM analysis. Different electrochemical methods have been used to study the effect of the concentration of the doping agents on the photoelectrocatalytic activity of the samples. The as-anodized doped TiO2 electrodes were observed to show higher photocatalytic activity compared with the bare TiO2 due to the high absorption of visible light and reduction in the recombination of photogenerated charges. Very high surface area, good photocatalytic performance, moderate conversion (about 42%) and high selectivity ( > 99%) for oxidation of benzyl alcohol to benzaldehyde at ambient temperature under visible light illumination in acetonitrile solvent were shown by the doped TiO2 nanoporous sample anodized in electrolyte containing 0.015 M potassium hexacyanocobaltate (sample CT15). Finally, the photoelectrochemical water splitting efficiency of the samples prepared has also been investigated.

Electrochemical Oxidation of Ti15Mo Alloy-The Impact of Anodization Parameters on Surface Morphology of Nanostructured Oxide Layers.

It is well-known that the structure and composition of the material plays an important role in the processes occurring at the surface. In this paper, a surface morphology of nanostructured oxide layers electrochemically grown on Ti15Mo, tuned by applying different anodization parameters, was investigated in detail. The one-step anodization of Ti15Mo alloy was performed at room temperature in an ethylene glycol-based electrolyte containing 0.11 M NH4F and 1.11 M H2O. Different anodization times (ranging from 5 to 60 min) and applied potentials (40–100 V) were tested, and the surface morphology, elemental content, and crystalline structure were monitored by scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), and X-ray diffractometry (XRD), respectively. The results showed that contrary to the multistep anodization of titanium foil, the surface morphology of anodic oxide obtained via the one-step process contains the nanoporous outer layer covering the nanotubular structure. What is more, the pore diameter (Dp) and interpore distance (Dint) of such layers exhibit different trends than those observed for anodization of pure titanium. In particular, at a certain potential range, a decrease in both Dp and Dint with increasing potential was observed. However, independently on the used anodization conditions, the elemental content of oxide layers remained similar, showing the amount of molybdenum at c.a. 15 wt.%. Finally, the amorphous nature of as-anodized layers was confirmed, and their optical band-gap was determined from the diffuse reflectance UV–Vis spectra. It was found that Eg is tunable to some extent by changing the anodizing potential. However, further thermal treatment in air at 400 °C resulted in the anatase phase formation that was accompanied by a significant Eg reduction. Therefore, we believe that the presented results will greatly contribute to the understanding of anodic formation of nanostructured functional oxide layers with tunable properties that can be applied in various fields.