Search Results (23)

Plasma electrolytic oxidation (PEO) is an electrochemical surface modification technique for producing dense oxide layers on valve metals. This review compiles the various modifications to the PEO process that have been used to improve the produced coatings and make them suitable for specific applications, with a focus on examples of aluminum, magnesium, and titanium substrates. An overview of the PEO process is given, highlighting the various process parameters and their effects on the final surface. The challenges with light metals that motivate the use of surface modifications are summarized, along with some of the other modifications that attempt to overcome them. Two broad categories of modifications to the PEO process are presented: in situ modifications, influencing the properties of the coating during its formation, and ex situ modifications, augmenting the properties of an already-formed coating. Finally, specific examples of applications for modified PEO processes are discussed, including battery, biomedical, water treatment, and energy production applications. Full article

Plasma electrolytic oxidation (PEO) is often used to improve the physical and mechanical properties of valve metals. This method allows for the formation of thicker and denser metal oxide coatings, which helps to improve physical and mechanical properties, especially the wear and corrosion resistance of the surface. The PEO process is widely used in areas such as mechanical engineering, aerospace, biomedical, and others. This review aims to summarize and explain the fundamental principles of the PEO process, with a focus on the influence of waveform types and their parameters on the properties of PEO coatings. This study found that a sinusoidal waveform promotes the generation of more stable discharges compared to a rectangular waveform, thereby enhancing the corrosion resistance of the coatings. Furthermore, it was demonstrated that using a rectangular waveform with adjustable parameters enables the production of thicker and more wear-resistant coatings. Meanwhile, the application of sawtooth and trapezoidal waveforms reduces sharp current spikes during the onset of discharges, minimizing defect formation and positively influencing the coating formation process. In addition, bipolar and unipolar modes are analyzed, and the promising future directions are discussed. Full article

Thermal energy storage systems for high temperatures >600 °C are currently mainly based on solid storage materials that are thermally charged and discharged by a gaseous heat transfer fluid. Usually, these systems benefit from low storage material costs but suffer from moderate heat transfer rates from the gas to the storage medium. Therefore, at the Karlsruhe Liquid Metal Laboratory, liquid metals are investigated as alternative heat transfer fluids for such heat storage systems, making use of the broad temperature range, in which the metals are in a liquid state, and their efficient heat transport capabilities. In this work, the design and construction of a high-temperature test rig using liquid lead is presented. The goal of the experiments is to demonstrate the operability of a pump, valves and measurement equipment at 700 °C in a challenging corrosive environment. Based on material pre-tests in stagnant lead at 700 °C, which are also shown in this study, aluminizing and pre-oxidation of the pipes and components are applied for enhanced corrosion protection. Full article

Ti15Zr15Mo (TMZ alloy) has been studied in recent years for biomedical applications, mainly due to phase beta formation. From the surface modification, it is possible to associate the volume and surface properties with a better biomedical response. This study aimed to evaluate the possibility of using anodization to obtain TiO₂ nanotubes due to the presence of valve-type metal (Zr) in their composition. X-ray photoelectron spectroscopy (XPS) was performed to determine the surface chemical composition in both after-processing conditions (passive layer) and after-processing plus anodization (TiO₂ nanotube growth). The anodization resulted in nanotubes with diameters and thicknesses of 126 ± 35 and 1294 ± 193 nm, respectively, and predominated anatase phase. Compared to the passive layer of titanium, which is less than ~10 nm, the oxide layer formed was continuous and thicker. High-resolution spectra revealed that the oxide layer of the element alloys contained different oxidation states. The major phase in all depths for the nanotube samples was TiO2. While the stable form of each oxide was found to predominate on the surface, the inner part of the oxide layer consisted of suboxides and metallic forms. This composition included different oxidation states of the substrate elements Ti, Zr, and Mo. Full article

High-frequency overvoltage generated in railways results in explosions of Electric Multiple Units’ (EMUs) arrestors. To solve this problem, the leakage current characteristics and heat transfer process of high-gradient MOA plates under high-frequency overvoltage has been studied. The leakage current characteristics of arrestor plates under high-frequency voltage was obtained and the element distribution has been analyzed. Heat transfer distribution and the thermal properties of the Metal Oxide Arrestor (MOA) have been modelled. According to the results, for a given voltage, the higher the harmonic frequency, the greater the leakage current of the arrestor valve plate, and the greater the resistive component of the leakage current. The Zn and O elements in high-gradient MOA plates are more uniform. Under the same leakage current as conventional ones, the undertake voltage of a high-gradient MOA plate will increase by 10%. Longtime high-order harmonic action will still significantly improve the core rod temperature when MOA plates are coated. The temperature rise in the power supply section of EMUs during operation is roughly 35 °C. This result will provide a foundation and supporting data for the applicability of high-gradient valve plates in railroads and coating improvements for traditional arrestor plates. Full article

Reanodizing metal underlayers through porous anodic alumina has already been used extensively to fabricate ordered columns of different metal oxides. Here, we present similar 3D multilayered nanostructures with unprecedented complexity. Two-level 3D column-like nanofilms have been synthesized by anodizing an Al/Nb metal layer in aqueous oxalic acid for forming the first level, and an Al/Ta layer in aqueous tartaric acid for forming the second level of the structure. Both levels were then reanodized in aqueous boric acid. The Ta layer deposited on partially dissolved porous anodic alumina of the first level, with protruding tops of niobia columns, acquired a unique hexagonally-packed structure. The morphology of the first and second levels was determined using scanning electron microscopy. Prolonged etching for 24 h in a 50%wt aqueous phosphoric acid was used to remove the porous anodic alumina. The formation mechanism of aluminum phosphates on the second-level columns in the process of long-time cold etching is considered. The model for the growth of columns on a Ta hexagonally-packed structure of the second level is proposed and described. The described approach can be applied to create 3D two- or three-level column-like systems from various valve metals (Ta, Nb, W, Hf, V, Ti), their combinations and alloys, with adjustable column sizes and scaling. The results of optical simulation show a high sensitivity of two-level column-like 3D nanofilms to biomedical objects and liquids. Among potential applications of these two-level column-like 3D nanofilms are photonic crystals for full-color displays, chemical sensors and biosensor, solar cells and thermoresponsive shape memory polymers. Full article

Plasma electrolytic oxidation (PEO) is a promising surface treatment for generating a thick, adherent coating on valve metals using an environmentally friendly alkaline electrolyte. In this study, the PEO method was used to modify the surface of AZ31 Mg alloy. The composite coatings were formed in a phosphate-based electrolyte containing hydroxyapatite nanoparticles (NPs) and different concentrations (1, 2, 3, and 4 g/L) of TiO₂ NPs. The results showed that the incorporation of TiO₂ NPs in the composite coatings increased the porosity, coating thickness, surface roughness, and surface wettability of the coatings. The corrosion-resistance results of coatings in simulated body fluid (SBF) were tested for up to 72 h and all coatings showed superior corrosion resistance compared to the bare substrate. Among samples containing TiO₂, the sample containing 1 g/L TiO₂ had the highest inner layer resistance (0.51 kΩ·cm²) and outer resistance (285 kΩ·cm²) and the lowest average friction coefficient (395.5), so it had the best wear and corrosion resistance performance. The antibacterial tests showed that the higher the concentration of TiO₂ NPs, the lower the adhesion of bacteria, resulting in enhanced antibacterial properties against S. aureus. The addition of 4 g/L of TiO₂ NPs to the electrolyte provided an antibacterial rate of 97.65% for the coating. Full article

Heavy metals can contaminate water through both natural processes and anthropogenic activities. Unlike organic contaminants, heavy metals are toxic, not biodegradable, and possess the ability to accumulate in organisms. Effective mixing between contaminated water and nanoparticles is of great importance in various purification applications of microfluidics, especially when heavy metals are involved. In these terms, a series of simulations were performed to succeed in an effective mixing of iron oxide nanoparticles in the duct. The selected geometry for the simulations was the Tesla valve which was used as a micromixer. In the present work, a stream loaded with nanoparticles and a stream with contaminated water are numerically studied for various inlet velocity ratios of the two streams. Better mixing is achieved, compared with relative works, under V_p/V_c = 10, for an inlet rate of the Fe₃O₄ nanoparticles per second equal to 1000. Full article

With plasma electrolytic oxidation (PEO), one can easily obtain thick (tens of microns), mechanically resilient and chemically stable oxide coating on aluminum and other valve metal alloys. The study of luminescent PEO coatings is a relatively new subfield of the already well-established coating preparation methods. In recent years, many new luminescence-based approaches have been developed, one of which is the detection of ionizing radiation of carbon-doped PEO alumina coating. This study presents an improved approach by doping the alumina coating with chromium using citric acid as an additive in the electrolyte. Trivalent chromium ions replacing aluminum in the crystalline lattice of the coating exhibit characteristic sharp lines in the luminescence spectrum. The effectiveness of different DC voltages, process times and citric acid concentrations in electrolyte were examined. The use of citric acid in the electrolyte also provides the conditions required for the formation of an energy trap in the bandgap of the material, thus opening up the possibility for the coating to be used as an ionizing radiation detector by measuring its thermoluminescence. Chromium atoms are incorporated in the coating from the Al6082 aluminum alloy itself and are not added in the electrolyte, therefore making the process much more reliable, repeatable, and environmentally friendly. Full article

Nanostructured aluminum, tantalum, and vanadium oxide layers on glass substrates were obtained by electrochemical anodizing in oxalic and sulfuric–oxalic electrolytes. The morphological and optical properties of the obtained structures were investigated experimentally by scanning electron microscopy and transmission spectroscopy. Obtained oxide coatings are quasi-ordered arrays of vertical (aluminum oxide/tantalum oxide, aluminum oxide/vanadium oxide, and aluminum oxide obtained in the oxalic electrolyte) or non-ordered tree-like (aluminum oxide obtained in the sulfuric–oxalic electrolyte) pores depending on the initial film metal and anodizing technology. The light transmission in the range of 750–1200 nm is up to 60% for aluminum oxide/tantalum oxide/glass (annealed) and quasi-ordered aluminum oxide/glass structures, and around 40% for aluminum oxide/tantalum oxide/glass (not annealed) and aluminum oxide/vanadium oxide. Non-ordered aluminum oxide is characterized by low transmission (no more than 8%) but has a developed surface and may be of interest for the formation of films with poor adhesion on smooth substrates, for example, photocatalytic active xerogels. The refractive indices of dispersion of the obtained layers were calculated from the transmission spectra by the envelope method. The dispersion of the refractive indices of the obtained oxide films is insignificant in a wide range of wavelengths, and the deviation from the average value is assumed to be observed near the intrinsic absorption edges of the films. The glasses with proposed semi-transparent nanostructured oxide layers are promising substrate structures for subsequent sol–gel coating layers used in photocatalytic purification systems or up-conversion modules of tandem silica solar cells with forward and reverse illumination. Full article

Sewerage systems consist of several different parts, components and materials. Many of them are metallic structures, such as pumps, valves, ladders and wells, which are necessary for the proper operation of wastewater transport systems. Wastewater pipelines can be a highly corrosive environment, mainly due to the presence of biogenic sulfuric acid. In the present study, seven magnesium hydroxide and one magnesium oxide materials were used as protective coatings applied onto the surface of certain stainless steel and mild steel specimens against sulfuric acid corrosion. The coated specimens were subjected to accelerated sulfuric acid spraying tests and their behavior was evaluated by using optical observation, mass measurements and electrochemical impedance spectroscopy. According to the results, the coating prepared from a magnesium hydroxide powder with relatively low specific surface area and smaller particle size was optimal for the protection of the examined steel specimens. Full article

The aim of this study was to develop memristors based on Nb₂O₅ grown by a simple and inexpensive electrochemical anodization process. It was confirmed that the electrolyte selection plays a crucial role in resistive switching due to electrolyte species incorporation in oxide, thus influencing the formation of conductive filaments. Anodic memristors grown in phosphate buffer showed improved electrical characteristics, while those formed in citrated buffer exhibited excellent memory capabilities. The chemical composition of oxides was successfully determined using HAXPES, while their phase composition and crystal structure with conductive filaments was assessed by TEM at the nanoscale. Overall, understanding the switching mechanism leads towards a wide range of possible applications for Nb memristors either as selector devices or nonvolatile memories. Full article

Magnetron-sputtered thin films of titanium and zirconium, with a thickness of 150 nm, were hydrogenated at atmospheric pressure and a temperature of 703 K, then anodized in boric, oxalic, and tartaric acid aqueous solutions, in potentiostatic, galvanostatic, potentiodynamic, and combined modes. A study of the thickness distribution of the elements in fully anodized hydrogenated zirconium samples, using Auger electron spectroscopy, indicates the formation of zirconia. The voltage- and current-time responses of hydrogenated titanium anodizing were investigated. In this work, fundamental possibility and some process features of anodizing hydrogenated metals were demonstrated. In the case of potentiodynamic anodizing at 0.6 M tartaric acid, the increase in titanium hydrogenation time, from 30 to 90 min, leads to a decrease in the charge of the oxidizing hydrogenated metal at an anodic voltage sweep rate of 0.2 V·s⁻¹. An anodic voltage sweep rate in the range of 0.05–0.5 V·s⁻¹, with a hydrogenation time of 60 min, increases the anodizing efficiency (charge reduction for the complete oxidation of the hydrogenated metal). The detected radical differences in the time responses and decreased efficiency of the anodic process during the anodizing of the hydrogenated thin films, compared to pure metals, are explained by the presence of hydrogen in the composition of the samples and the increased contribution of side processes, due to the possible features of the formed oxide morphologies. Full article

In the framework of the industry of secondary aluminum, the chemical neutralization of highly reactive materials that come from the pre-treatment screening processes of scraps (beverage cans and domestic appliances) was investigated through experiments in aqueous alkaline solutions. Metallic aluminum-rich by-products are classified, according to EU law, as dangerous waste, as they can potentially develop flammable gases capable of forming explosive mixtures with air. In this way they cannot be disposed of in landfills for non-hazardous wastes if chemical neutralization is not planned and performed beforehand. In this way, these experiments were mainly aimed at unraveling the oxidation rate and at quantifying the production of hydrogen-rich gases from the reactions of the metallic aluminum-rich by-products in a water-rich alkaline (liquid or vapor) environment. Reactions were carried out in a stainless-steel batch mini-reactor with metering and sampling valves, with the resulting gases analyzed by gas-chromatography (GC). The experimental setup was planned to avoid the following issues: (i) the corrosion of the reactor by the alkaline solution and (ii) the permeability of the system to hydrogen (i.e., possible leaks of H₂), related to the fast kinetics and short duration of the reactions (which may hinder a pile-up-effect) between the solid by-products and the liquid. The procedure was defined by a controlled interaction process between metals and liquid, using NaOH to increase reaction rates. The experimental runs performed in the mini-reactor proved to be effective for eliminating the reactive metallic aluminum, reaching a maximum hydrogen production of 96% of the total gases produced in the experiments. The relations between gas generation (up to 55 bar of H₂ in the experiments, which lasted for four days) and each specific parameter variation are discussed. All the obtained results can be transferred and applied to (i) the possible industrialization of the method for the chemical neutralization of these dangerous by-products, increasing sustainability and workplace safety, (ii) the use of the resulting hydrogen as a source of energy for the furnaces of the secondary aluminum industry itself, and (iii) new technological materials (e.g., “foamed geopolymers”), by using hydrogen as a foaming agent, coupled with aluminosilicate materials, during geopolymeric reactions. Full article

A room temperature liquid metal-based microvalve has been proposed in this work. The microvalve has the advantages of easy fabrication, high flexibility, and a low leak rate. By designing a posts array in the channel, the liquid metal can be controlled to form a deformable valve boss and block the flow path. Besides, through adjustment of the pressure applied to the liquid metal, the microvalve can perform reliable switching commands. To eliminate the problem that liquid metal is easily oxidized, which causes the microvalve to have poor repeatability, a method of electrochemical cathodic protection has been proposed, which significantly increases the number of open/close switch cycles up to 145. In addition, this microvalve overcomes the shortcomings of the traditional microvalve that requires an alignment process to assemble all the parts. When the valve is closed, no leak rate is detected at ≤320 mbar, and the leak rate is ≤0.043 μL/min at 330 mbar, which indicates it has good tightness. As an application, we also fabricate a chip that can control bubble flow based on this microvalve. Therefore, this microvalve has great prospects in the field of microfluidics. Full article