Anodic alumina membranes with defined pore diameters and thicknesses obtained by adjusting the anodizing duration and pore opening/widening time

The through-hole porous anodic aluminum oxide (AAO) membranes were fabricated by a simple two-step anodization of aluminum in 0.3 M oxalic acid, 0.3 M sulfuric acid, and 2 wt.% phosphoric acid solutions under different operating conditions followed by the removal of the remaining Al substrate and the pore opening/widening process. The effect of duration of the second anodizing step on the thickness of the porous oxide layer and the influence of other anodizing conditions such as applied voltage, type of electrolyte, and purity of the substrate on the rate of porous oxide growth were discussed in detail. The pore opening procedure for all synthesized membranes was optimized, and the influence of the duration of chemical etching on structural features of AAO membranes, especially pore diameter, was studied. The rate of pore widening was established for AAO membranes formed in various anodizing electrolytes and for different temperatures of 5 wt.% H3PO4 used for alumina dissolution

Tuning the photoelectrochemical properties of narrow band gap nanoporous anodic SnOxSnO_x films by simple soaking in water

Nanoporous tin oxide layers obtained via anodic oxidation of metallic tin at the potential of 4 V in the alkaline electrolyte (1 M NaOH) were soaked in distilled water for various durations (from 2 h to 120 h) to verify the influence of water-enabled crystallization on the morphology, composition, and related optical and photoelectrochemical properties of such kind of anodic SnOx. Although water soaking generally contributes to more stoichiometric and crystalline tin oxide, it was confirmed that at the initial stages of the water-induced dissolution–redeposition process, material exhibits enhanced photoelectrochemical performance under simulated sunlight irradiation. However, long-time exposure to water results in a gradual widening of the material’s band gap, shifting of the photoelectrochemical spectra towards higher energies, and almost complete deterioration of the photoelectrochemical activity under sunlight irradiation

Improving photoelectrochemical properties of anodic WO3WO_3 layers by optimizing electrosynthesis conditions

Although anodic tungsten oxide has attracted increasing attention in recent years, there is still a lack of detailed studies on the photoelectrochemical (PEC) properties of such kind of materials grown in different electrolytes under various sets of conditions. In addition, the morphology of photoanode is not a single factor responsible for its PEC performance. Therefore, the attempt was to correlate different anodizing conditions (especially electrolyte composition) with the surface morphology, oxide thickness, semiconducting, and photoelectrochemical properties of anodized oxide layers. As expected, the surface morphology of WO3 depends strongly on anodizing conditions. Annealing of as-synthesized tungsten oxide layers at 500 °C for 2 h leads to obtaining a monoclinic WO3 phase in all cases. From the Mott-Schottky analysis, it has been confirmed that all as prepared anodic oxide samples are n-type semiconductors. Band gap energy values estimated from incident photon−to−current efficiency (IPCE) measurements neither differ significantly for as−synthesized WO3 layers nor depend on anodizing conditions such as electrolyte composition, time and applied potential. Although the estimated band gaps are similar, photoelectrochemical properties are different because of many different reasons, including the layer morphology (homogeneity, porosity, pore size, active surface area), oxide layer thickness, and semiconducting properties of the material, which depend on the electrolyte composition used for anodization

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

The effect of anode surface area on nanoporous oxide formation during anodizing of low purity aluminum (AA1050 alloy)

Porous anodic alumina layers were obtained by a simple two-step anodization of low purity aluminum (99.5 % Al, AA1050 alloy) in a 0.3 M oxalic acid electrolyte at 45 V and 20 °C. The effect of anode surface area on structural features of nanoporous oxide and process of oxide formation was investigated. An ordered structure composed of nanostripes or nanopores was formed on the Al surface during electrochemical polishing in a mixture of perchloric acid and ethanol. This nanopattern is then replicated during the anodic oxide formation. It was found that the pore diameter, interpore distance, and porosity increase slightly with increasing surface area of the aluminum sample exposed to the anodizing electrolyte. On the other hand, a slight decrease in pore density and cell wall thickness was observed with increasing surface area of the sample. The detailed inspection of current density vs. time curves was also performed. The obtained results revealed that the higher surface area of the anode, the local current density minimum, was reached faster during first step of anodization and the increase in current density corresponding to the pore rearrangement process was observed earlier. Finally, a dense array of Pd nanowires (∼90 nm in diameter) was synthesized by simple electrodeposition of metal inside the channels of through-hole nanoporous anodic alumina templates with relatively large surface areas (4 cm2)

Analysis of nanopore arrangement and structural features of anodic alumina layers formed by two-step anodizing in oxalic acid using the dedicated executable software

Anodic porous alumina layers were fabricated by a two-step self-organized anodization in 0.3 M oxalic acid under various anodizing potentials ranging from 30 to 60 V at two different temperatures (10 and 17 ◦ C). The ef- fect of anodizing conditions on structural features and pore arrangement of AAO was investigated in detail by using the dedicated executable publication combined with ImageJ software. With increasing anodizing potential, a linear in- crease of the average pore diameter, interpore distance, wall thickness and barrier layer thickness, as well as a decrease of the pore density, were observed. In addition, the higher pore diameter and porosity values were obtained for samples an- odized at the elevated temperature, independently of the an- odizing potential. A degree of pore order was investigated on the basis of Delaunay triangulations (defect maps) and cal- culation of pair distribution or angle distribution functions (PDF or ADF), respectively. All methods confirmed that in order to obtain nanoporous alumina with the best, hexag- onal pore arrangement, the potential of 40 V should be ap- plied during anodization. It was confirmed that the dedicated executable publication can be used to a fast and complex analysis of nanopore arrangement and structural features of nanoporous oxide layers

Hierarchical nanoporous Sn/SnOxSn/SnO_x systems obtained by anodic oxidation of electrochemically deposited Sn Nanofoams

A simple two-step electrochemical method for the fabrication of a new type of hierarchical Sn/SnOx micro/nanostructures is proposed for the very first time. Firstly, porous metallic Sn foams are grown on Sn foil via hydrogen bubble-assisted electrodeposition from an acidulated tin chloride electrolyte. As-obtained metallic foams consist of randomly distributed dendrites grown uniformly on the entire metal surface. The estimated value of pore diameter near the surface is ~35 µm, while voids with a diameter of ~15 µm appear in a deeper part of the deposit. Secondly, a layer of amorphous nanoporous tin oxide (with a pore diameter of ~60 nm) is generated on the metal surface by its anodic oxidation in an alkaline electrolyte (1 M NaOH) at the potential of 4 V for various durations. It is confirmed that if only optimal conditions are applied, the dendritic morphology of the metal foam does not change significantly, and an open-porous structure is still preserved after anodization. Such kinds of hierarchical nanoporous Sn/SnOx systems are superhydrophilic, contrary to those obtained by thermal oxidation of metal foams which are hydrophobic. Finally, the photoelectrochemical activity of the nanostructured metal/metal oxide electrodes is also presented