Fabrication of Multiferroic Co-Substituted BiFeO3 Epitaxial Films on SrTiO3 (100) Substrates by Radio Frequency Magnetron Sputtering

The 10 at.% Co-substituted BiFeO₃ films (of thickness 50 nm) were successfully prepared by radio frequency (r.f.) magnetron sputtering on SrTiO₃ (100) substrates with epitaxial relationships of [001](001)Co-BiFeO₃//[001](001)SrTiO₃. In this study, a single phase Co-substituted BiFeO₃ epitaxial film was fabricated by r.f. magnetron sputtering. Sputtering conditions such as Ar, O₂ gas pressure, annealing temperature, annealing atmosphere, and sputtering power were systematically changed. It was observed that a low Ar gas pressure and low sputtering power is necessary to suppress the formation of the secondary phases of BiO_x. The Co-substituted BiFeO₃ films were crystalized with post-annealing at 600 °C in air. The process window for single phase films is narrower than that for pure BiFeO₃ epitaxial films. By substituting Fe with Co in BiFeO₃, the magnetization at room temperature increased to 20 emu/cm³. This result suggests that Co-substituted BiFeO₃ films can be used in spin-filter devices.     

A High-Efficiency TiO2/ZnO Nano-Film with Surface Oxygen Vacancies for Dye Degradation

Photocatalytic degradation of organic pollutants in water is a highly efficient and green approach. However, the low quantum efficiency is an intractable obstacle to lower the photocatalytic efficiency of photocatalysts. Herein, the TiO₂/ZnO heterojunction thin films combined with surface oxygen vacancies (OVs) were prepared through magnetron sputtering, which was designed to drive rapid bulk and surface separation of charge carriers. The morphology and structural and compositional properties of films were investigated via different techniques such as SEM, XRD, Raman, AFM, and XPS. It has been found that by controlling the O₂/Ar ratio, the surface morphology, thickness, chemical composition, and crystal structure can be regulated, ultimately enhancing the photocatalytic performance of the TiO₂/ZnO heterostructures. In addition, the heterojunction thin film showed improved photocatalytic properties compared with the other nano-films when the outer TiO₂ layer was prepared at an O₂/Ar ratio of 10:35. It degraded 88.0% of Rhodamine B (RhB) in 90 min and 90.8% of RhB in 120 min. This was attributed to the heterojunction interface and surface OVs, which accelerated the separation of electron–hole (e–h) pairs.     

Tuning Stoichiometry and Structure of Pd-WO3−x Thin Films for Hydrogen Gas Sensing by High-Power Impulse Magnetron Sputtering

By tuning the deposition parameters of reactive high-power impulse magnetron sputtering, specifically the pulse length, we were able to prepare WO_3−x films with various stoichiometry and structure. Subsequently, the films were annealed in air at moderate temperature (350 °C). We demonstrate that the stoichiometry of the as-deposited films influences considerably the type of crystalline phase formed in the annealed films. The appropriate sub-stoichiometry of the films (approx. WO_2.76) enabled crystallization of the monoclinic phase during the annealing. This phase is favorable for hydrogen sensing applications. To characterize the sensory behavior of the films, the tungsten oxide films were decorated by Pd nanoparticles before annealing and were assembled as a conductometric gas sensor. The sensory response of the films that crystallized in the monoclinic structure was proven to be superior to that of the films containing other phases.     

Molybdenum Oxide Thin Films Grown on Flexible ITO-Coated PET Substrates

Molybdenum oxide thin films were deposited on stiff and flexible substrates by reactive DC magnetron sputtering. Two sets of samples were prepared. The first with different O₂/Ar flow rate ratios and the second, fixing the oxygen content, with different time of deposition. As the O₂/Ar flow rate ratio varies from 0 up to 0.56, a threshold was found, ranging from crystalline to amorphous nature, and from a nontransparent appearance with metallic-like electrical conductivity to transparent and dielectric behaviour. From the second set, all transparent, the MoO_x films present a compact/dense and featureless morphology with thickness from 190 up to 910 nm, depending on the time of deposition. Their structure was corroborated by XPS and Rutherford Backscattering Spectrometry (RBS) and density measurements were performed by RBS and X-ray reflectivity (XRR), revealing a value of 2.4 g/cm³. The surface roughness is in the order of a few nanometers and the maxima optical transmission, in the visible range, is around 89%. Electrochemical cyclic voltammograms showed noticeable color reversibility and reproducibility on the flexible substrates opening new framework possibilities for new electrochomic devices.     

Influence of Ti3C2Tx MXene and Surface-Modified Ti3C2Tx MXene Addition on Microstructure and Mechanical Properties of Silicon Carbide Composites Sintered via Spark Plasma Sintering Method

This article presents new findings related to the problem of the introduction of MXene phases into the silicon carbide matrix. The addition of MXene phases, as shown by the latest research, can significantly improve the mechanical properties of silicon carbide, including fracture toughness. Low fracture toughness is one of the main disadvantages that significantly limit its use. As a part of the experiment, two series of composites were produced with the addition of 2D-Ti₃C₂T_x MXene and 2D-Ti₃C₂T_x surface-modified MXene with the use of the sol-gel method with a mixture of Y₂O₃/Al₂O₃ oxides. The composites were obtained with the powder metallurgy technique and sintered with the Spark Plasma Sintering method at 1900 °C. The effect adding MXene phases had on the mechanical properties and microstructure of the produced sinters was investigated. Moreover, the influence of the performed surface modification on changes in the properties of the produced composites was determined. The analysis of the obtained results showed that during sintering, the MXene phases oxidize with the formation of carbon flakes playing the role of reinforcement. The influence of the Y₂O₃/Al₂O₃ layer on the structure of carbon flakes and the higher quality of the interface was also demonstrated. This was reflected in the higher mechanical properties of composites with the addition of modified Ti₃C₂T_x. Composites with 1 wt.% addition of Ti₃C₂T_x M are characterized with a fracture toughness of 5 MPa × m^0.5, which is over 50% higher than in the case of the reference sample and over 15% higher than for the composite with 2.5 wt.% addition of Ti₃C₂T_x, which showed the highest fracture toughness in this series.     

Biocompatibility and Surface Properties of TiO2 Thin Films Deposited by DC Magnetron Sputtering

We present the study of the biocompatibility and surface properties of titanium dioxide (TiO₂) thin films deposited by direct current magnetron sputtering. These films are deposited on a quartz substrate at room temperature and annealed with different temperatures (100, 300, 500, 800 and 1100 °C). The biocompatibility of the TiO₂ thin films is analyzed using primary cultures of dorsal root ganglion (DRG) of Wistar rats, whose neurons are incubated on the TiO₂ thin films and on a control substrate during 18 to 24 h. These neurons are activated by electrical stimuli and its ionic currents and action potential activity recorded. Through X-ray diffraction (XRD), the surface of TiO₂ thin films showed a good quality, homogeneity and roughness. The XRD results showed the anatase to rutile phase transition in TiO₂ thin films at temperatures between 500 and 1100 °C. This phase had a grain size from 15 to 38 nm, which allowed a suitable structural and crystal phase stability of the TiO₂ thin films for low and high temperature. The biocompatibility experiments of these films indicated that they were appropriated for culture of living neurons which displayed normal electrical behavior.     

Optically Active TiO2:Er Thin Films Deposited by Magnetron Sputtering

Titanium dioxide photoanodes for hydrogen generation suffer from a profound mismatch between the optical absorption of TiO₂ and the solar spectrum. To solve the problem of low solar-to-chemical efficiency, optically active materials are proposed. In this work, TiO₂ thin films containing erbium were deposited by radio frequency RF magnetron sputtering under ultrahigh vacuum conditions UHV. Morphology, structural, optical and electronic properties were studied. TiO₂:Er thin films are homogenous, with uniform distribution of Er ions and high transparency over the visible VIS range of the light spectrum. However, a profound 0.4 eV blue shift of the fundamental absorption edge with respect to undoped TiO₂ was observed, which can be attributed either to the size effect due to amorphization of TiO₂ host or to the onset of precipitation of Er₂Ti₂O₇ nanocrystals. Near-infrared NIR to VIS up-conversion is demonstrated upon excitation at 980 nm, while strong green photoluminescence at 525 and 550 nm occurs upon photon absorption at 488 nm.     

Photocatalytic Inactivation of Salmonella typhimurium by Floating Carbon-Doped TiO2 Photocatalyst

Photocatalysis application is considered as one of the most highly promising techniques for the reduction in wastewater pollution. However, the majority of highly efficient photocatalyst materials are obtained as fine powders, and this causes a lot of photocatalyst handling and reusability issues. The concept of the floating catalyst proposes the immobilization of a photocatalytic (nano)material on relatively large floating substrates and is considered as an encouraging way to overcome some of the most challenging photocatalysis issues. The purpose of this study is to examine floating photocatalyst application for Salmonella typhimurium bacteria inactivation in polluted water. More specifically, high-density polyethylene (HDPE) beads were used as a photocatalyst support for the immobilization of carbon-doped TiO₂ films forming floating photocatalyst structures. Carbon-doped TiO₂ films in both amorphous and anatase forms were deposited on HDPE beads using the low-temperature magnetron sputtering technique. Bacteria inactivation, together with cycling experiments, revealed promising results by decomposing more than 95% of Salmonella typhimurium bacteria in five consecutive treatment cycles. Additionally, a thorough analysis of the deposited carbon-doped TiO₂ film was performed including morphology, elemental composition and mapping, structure, and depth profiling. The results demonstrate that the proposed method is a suitable technique for the formation of high-quality photocatalytic active films on thermal-sensitive substrates.     

Osteoblast-like Cell Proliferation,ALP Activity and Photocatalytic Activity on Sintered Anatase and Rutile Titanium Dioxide

This study aimed to create a biomaterial from titanium dioxide (TiO₂), which has been known to have photocatalytic and bone formation promoting effects. I expected that anatase titanium dioxide-based implants could promote bone augmentation and induce bone formation. Powdery anatase TiO₂ was compression molded and sintered at 700, 800, 900, and 1000 °C to prepare sintered compact samples. X-ray diffraction and scanning electron microscopy were used to observe the surface of these samples. Furthermore, mouse osteoblast-like cells (MC3T3-E1 cell line) were seeded on the samples sintered at different temperatures, and cell proliferation was observed to evaluate the cell proliferation of the samples. The sample sintered at 700 °C was composed of anatase TiO₂. The samples sintered at 800 °C and 900 °C were confirmed to consist of a mixture of anatase and rutile TiO₂ crystalline phases. Moreover, the sample sintered at 700 and 800 °C, which contained anatase TiO₂, showed remarkable photocatalytic activity. Those samples sintered at 1000 °C were transformed to the rutile TiO₂. The cell proliferation after 7–14-days culturing revealed that cells cultured on the 700 °C sample decreased in number immediately after initiation of culturing. The cells cultured on TiO₂ sintered at 900 °C markedly proliferated over time with an increase in the alkaline phosphatase activity, showing good MC3T3-E1 cell compatibility of the samples. The sample sintered at 1000 °C, which is rutile TiO₂, showed the highest increase.     

Synthesis and Characterization of TiO2 Nanotubes (TiO2-NTs) with Ag Silver Nanoparticles (Ag-NPs): Photocatalytic Performance for Wastewater Treatment under Visible Light

In this work, we present the influence of the decoration of TiO₂ nanotubes (TiO₂-NTs) with Ag silver nanoparticles (Ag-NPs) on the photocatalysis of emerging pollutants such as the antibiotic diclofenac sodium. The Ag-NPs were loaded onto the TiO₂-NTs by the anodization of metallic titanium foils. Diclofenac sodium is an emerging pollutant target of the pharmaceutical industry because of its negative environmental impact (high toxicity and confirmed carcinogenicity). The obtained Ag-NP/TiO₂-NT nanocomposites were characterized by X-ray diffraction (XRD), photoluminescence spectroscopy (PL), scanning electron microscopy (SEM), transmission spectroscopy (TEM), and X-ray photoelectron spectroscopy (XPS). In order to study the photocatalytic behavior of Ag-NPs/TiO₂-NTs with visible cold LEDs, the possible photocatalytic mechanism of antibiotic degradation with reactive species (O₂°⁻ and OH°) was detailed. Moreover, the Langmuir–Hinshelwood model was used to correlate the experimental results with the optimized catalyst. Likewise, reuse tests showed the chemical stability of the catalyst.     

Electrical Properties of Aluminum Nitride Thick Films Magnetron Sputtered on Aluminum Substrates

The realization of a c-axis oriented aluminum nitride thick film on aluminum substrates is a promising step in the development of transducers for applications with a working temperature up to about 600 °C. The present paper deals with the realization of AlN thick films by means of reactive magnetron sputtering with a pulsed DC power supply, operating in continuous mode for 50 h. Two values (0.4 and 0.8) of nitrogen concentration were used; operative pressure and power were set at 0.3 Pa and 150 W, respectively. The thickness of the obtained aluminum nitride films on the aluminum substrate, assessed with a profilometer, varied from 20 to 30 µm. The preferential orientation of AlN crystals was verified by X-ray diffraction. Finally, as the main focus of the investigation, the films underwent electrical characterization by means of an LCR-meter used on a parallel plate capacitor set-up and a test system based on a cantilever beam configuration. AlN conductivity and ε₃₃ permittivity were derived in the 100 Hz–300 kHz frequency range. Magnetron sputtering operation with nitrogen concentration equal to 0.4 resulted in the preferred operative condition, leading to a d₃₁ piezoelectric coefficient, in magnitude, of 0.52 × 10⁻¹² C/N.     

Potentiodynamic Polarization Studies and Surface Chemical Composition of Bismuth Titanate (BixTiyOz) Films Produced through Radiofrequency Magnetron Sputtering

The applications of Bismuth Titanate (Bi_xTi_yO_z) materials have been focused on their electronic and optical properties, but with respect to the use of these compounds in applications like corrosion resistance, have been very few or nonexistent. For this reason, in the present investigation Bi_xTi_yO_z thin films were deposited using RF magnetron sputtering onto silicon wafers, stainless steel 316L, and titanium alloy (Ti₆Al₄V) substrates, in order to carry out a study of the corrosion behavior of this compound. The structural properties of the coatings were studied through X-ray diffraction (XRD), the morphology was determined using Scanning Electron Microscopy (SEM), the corrosion resistance behavior of the coated and uncoated substrates was evaluated via the Potentiodynamic Polarization technique, and surface chemical composition was evaluated through X-ray photoelectron spectroscopy (XPS). The XRD results indicated that the films were amorphous. The SEM micrographs showed that the deposited films were homogeneous, but in some cases there were cracks. The potentiodynamic polarization technique showed that the corrosion current in the coated substrates decreased by an order of two magnitudes with respect to the uncoated substrates, but in both cases the corrosion mechanism was pitting due to the pores in the film. The XPS analysis shows that the deposited films contain both Bi³⁺ and Ti⁴⁺.     

High-Temperature Chemical Stability of Cr(III) Oxide Refractories in the Presence of Calcium Aluminate Cement

Al₂O₃-CaO-Cr₂O₃ castables are used in various furnaces due to excellent corrosion resistance and sufficient early strength, but toxic Cr(VI) generation during service remains a concern. Here, we investigated the relative reactivity of analogous Cr(III) phases such as Cr₂O₃, (Al_1−xCr_x)₂O₃ and in situ Cr(III) solid solution with the calcium aluminate cement under an oxidizing atmosphere at various temperatures. The aim is to comprehend the relative Cr(VI) generation in the low-cement castables (Al₂O₃-CaO-Cr₂O₃-O₂ system) and achieve an environment-friendly application. The solid-state reactions and Cr(VI) formation were investigated using powder XRD, SEM, and leaching tests. Compared to Cr₂O₃, the stability of (Al_1−xCr_x)₂O₃ against CAC was much higher, which improved gradually with the concentration of Al₂O₃ in (Al_1−xCr_x)₂O₃. The substitution of Cr₂O₃ with (Al_1−xCr_x)₂O₃ in the Al₂O₃-CaO-Cr₂O₃ castables could completely inhibit the formation of Cr(VI) compound CaCrO₄ at 500–1100 °C and could drastically suppress Ca₄Al₆CrO₁₆ generation at 900 to 1300 °C. The Cr(VI) reduction amounting up to 98.1% could be achieved by replacing Cr₂O₃ with (Al_1−xCr_x)₂O₃ solid solution. However, in situ stabilized Cr(III) phases as a mixture of (Al_1−xCr_x)₂O₃ and Ca(Al_12−xCr_x)O₁₉ solid solution hardly reveal any reoxidation. Moreover, the CA₆ was much more stable than CA and CA₂, and it did not participate in any chemical reaction with (Al_1−xCr_x)₂O₃ solid solution.     

Annealing Effect on the Structural and Optical Properties of Sputter-Grown Bismuth Titanium Oxide Thin Films

The aim of this work is to assess the evolution of the structural and optical properties of Bi_xTi_yO_z films grown by rf magnetron sputtering upon post-deposition annealing treatments in order to obtain good quality films with large grain size, low defect density and high refractive index similar to that of single crystals. Films with thickness in the range of 220–250 nm have been successfully grown. After annealing treatment at 600 °C the films show excellent transparency and full crystallization. It is shown that to achieve larger crystallite sizes, up to 17 nm, it is better to carry the annealing under dry air than under oxygen atmosphere, probably because the nucleation rate is reduced. The refractive index of the films is similar under both atmospheres and it is very high (n =2.5 at 589 nm). However it is still slightly lower than that of the single crystal value due to the polycrystalline morphology of the thin films.     

Impact of Li3BO3 Addition on Solid Electrode-Solid Electrolyte Interface in All-Solid-State Batteries

All-solid-state lithium-ion batteries raise the issue of high resistance at the interface between solid electrolyte and electrode materials that needs to be addressed. The article investigates the effect of a low-melting Li₃BO₃ additive introduced into LiCoO₂- and Li₄Ti₅O₁₂-based composite electrodes on the interface resistance with a Li₇La₃Zr₂O₁₂ solid electrolyte. According to DSC analysis, interaction in the studied mixtures with Li₃BO₃ begins at 768 and 725 °C for LiCoO₂ and Li₄Ti₅O₁₂, respectively. The resistance of half-cells with different contents of Li₃BO₃ additive after heating at 700 and 720 °C was studied by impedance spectroscopy in the temperature range of 25–340 °C. It was established that the introduction of 5 wt% Li₃BO₃ into LiCoO₂ and heat treatment at 720 °C led to the greatest decrease in the interface resistance from 260 to 40 Ω cm² at 300 °C in comparison with pure LiCoO₂. An SEM study demonstrated that the addition of the low-melting component to electrode mass gave better contact with ceramics. It was shown that an increase in the annealing temperature of unmodified cells with Li₄Ti₅O₁₂ led to a decrease in the interface resistance. It was found that the interface resistance between composite anodes and solid electrolyte had lower values compared to Li₄Ti₅O₁₂|Li₇La₃Zr₂O₁₂ half-cells. It was established that the resistance of cells with the Li₄Ti₅O₁₂/Li₃BO₃ composite anode annealed at 720 °C decreased from 97.2 (x = 0) to 7.0 kΩ cm² (x = 5 wt% Li₃BO₃) at 150 °C.     

Impact of Annealing on Magnetic Properties and Structure of Co40Fe40W20 Thin Films on Si(100) Substrate

Co₄₀Fe₄₀W₂₀ monolayers of different thicknesses were deposited on Si(100) substrates by DC magnetron sputtering, with Co₄₀Fe₄₀W₂₀ thicknesses from 10 to 50 nm. Co₄₀Fe₄₀W₂₀ thin films were annealed at three conditions (as-deposited, 250 °C, and 350 °C) for 1 h. The structural and magnetic properties were then examined by X-ray diffraction (XRD), low-frequency alternative-current magnetic susceptibility (χ_ac), and an alternating-gradient magnetometer (AGM). The XRD results showed that the CoFe (110) peak was located at 2θ = 44.6°, but the metal oxide peaks appeared at 2θ = 38.3, 47.6, 54.5, and 56.3°, corresponding to Fe₂O₃ (320), WO₃ (002), Co₂O₃ (422), and Co₂O₃ (511), respectively. The saturation magnetization (Ms) was calculated from the slope of the magnetization (M) versus the CoFeW thickness. The Ms values calculated in this manner were 648, 876, 874, and 801 emu/cm³ at the as-deposited condition and post-annealing conditions at 250, 350, and 400 °C, respectively. The maximum M_S was about 874 emu/cm³ at a thickness of 50 nm following annealing at 350 °C. It indicated that the M_S and the χ_ac values rose as the CoFeW thin films’ thickness increased. Owing to the thermal disturbance, the M_S and χ_ac values of CoFeW thin films after annealing at 350 °C were comparatively higher than at other annealing temperatures. More importantly, the Co₄₀Fe₄₀W₂₀ films exhibited a good thermal stability. Therefore, replacing the magnetic layer with a CoFeW film improves thermal stability and is beneficial for electrode and strain gauge applications.     

3D Porous MXene (Ti3C2Tx) Prepared by Alkaline-Induced Flocculation for Supercapacitor Electrodes

2D layered MXene (Ti₃C₂T_x) with high conductivity and pseudo-capacitance properties presents great application potential with regard to electrode materials for supercapacitors. However, the self-restacking and agglomeration phenomenon between Ti₃C₂T_x layers retards ion transfer and limits electrochemical performance improvement. In this study, a 3D porous structure of Ti₃C₂T_x was obtained by adding alkali to a Ti₃C₂T_x colloid, which was followed by flocculation. Alkaline-induced flocculation is simple and effective, can be completed within minutes, and provides 3D porous networks. As 3D porous network structures present larger surface areas and more active sites, ions transfer accelerates, which is crucial with regard to the improvement of the superior capacitance and rate performance of electrodes. The sample processed with KOH (K-a-Ti₃C₂T_x) exhibited a high capacity of approximately 300.2 F g⁻¹ at the current density of 1 A g⁻¹. The capacitance of the samples treated with NaOH and LiOH is low. In addition, annealing is essential to further improve the capacitive performance of Ti₃C₂T_x. After annealing at 400 °C for 2 h in a vacuum tube furnace, the sample treated with KOH (K-A-Ti₃C₂T_x) exhibited an excellent specific capacitance of approximately 400.7 F g⁻¹ at a current density of 1 A g⁻¹, which is considerably higher than that of pristine Ti₃C₂T_x (228.2 F g⁻¹). Furthermore, after 5000 charge–discharge cycles, the capacitance retention rate reached 89%. This result can be attributed to annealing, which can further remove unfavourable surface groups, such as –F or –Cl, and then improve conductivity capacitance and rate performance. This study can provide an effective approach to the preparation of high-performance supercapacitor electrode materials.     

Preparation and Properties of (YCa)(TiMn)O3?δ Ceramics Interconnect of Solid Oxide Fuel Cells

(YCa)(TiMn)O_3–δ ceramics prepared using a reaction-sintering process were investigated. Without any calcination involved, the mixture of raw materials was pressed and sintered directly. Y₂Ti₂O₇ instead of YTiO₃ formed when a mixture of Y₂O₃ and TiO₂ with Y/Ti ratio 1/1 were sintered in air. Y₂Ti₂O₇, YTiO_2.085 and some unknown phases were detected in Y_0.6Ca_0.4Ti_0.6Mn_0.4O_3–δ. Monophasic Y_0.6Ca_0.4Ti_0.4Mn_0.6O_3–δ ceramics were obtained after 1400–1500 °C sintering. Dense Y_0.6Ca_0.4Ti_0.4Mn_0.6O_3–δ with a density 4.69 g/cm³ was observed after 1500 °C/4 h sintering. Log σ for Y_0.6Ca_0.4Ti_0.6Mn_0.4O_3–δ increased from –3.73 Scm^–1 at 350 °C to –2.14 Scm^–1 at 700 °C. Log σ for Y_0.6Ca_0.4Ti_0.4Mn_0.6O_3–δ increased from –2.1 Scm^–1 at 350 °C to –1.36 Scm^–1 at 700 °C. Increasing Mn content decreased activation energy E_a and increased electrical conductivity. Reaction-sintering process is proved to be a simple and effective method to obtain (YCa)(TiMn)O_3–δ ceramics for interconnects in solid oxide fuel cells.     

Synthesis and Characterization of a Nearly Single Bulk Ti2AlN MAX Phase Obtained from Ti/AlN Powder Mixture through Spark Plasma Sintering

MAX phases are an advanced class of ceramics based on ternary carbides or nitrides that combine some of the ceramic and metallic properties, which make them potential candidate materials for many engineering applications under severe conditions. The present work reports the successful synthesis of nearly single bulk Ti₂AlN MAX phase (>98% purity) through solid-state reaction and from a Ti and AlN powder mixture in a molar ratio of 2:1 as starting materials. The mixture of Ti and AlN powders was subjected to reactive spark plasma sintering (SPS) under 30 MPa at 1200 °C and 1300 °C for 10 min in a vacuum atmosphere. It was found that the massive formation of Al₂O₃ particles at the grain boundaries during sintering inhibits the development of the Ti₂AlN MAX phase in the outer zone of the samples. The effect of sintering temperature on the microstructure and mechanical properties of the Ti₂AlN MAX phase was investigated and discussed.     

One-Step Formation of WO3-Loaded TiO2 Nanotubes Composite Film for High Photocatalytic Performance

High aspect ratio of WO₃-loaded TiO₂ nanotube arrays have been successfully synthesized using the electrochemical anodization method in an ethylene glycol electrolyte containing 0.5 wt% ammonium fluoride in a range of applied voltage of 10–40 V for 30 min. The novelty of this research works in the one-step formation of WO₃-loaded TiO₂ nanotube arrays composite film by using tungsten as the cathode material instead of the conventionally used platinum electrode. As compared with platinum, tungsten metal has lower stability, forming dissolved ions (W⁶⁺) in the electrolyte. The W⁶⁺ ions then move towards the titanium foil and form a coherent deposit on titanium foil. By controlling the oxidation rate and chemical dissolution rate of TiO₂ during the electrochemical anodization, the nanotubular structure of TiO₂ film could be achieved. In the present study, nanotube arrays were characterized using FESEM, EDAX, XRD, as well as Raman spectroscopy. Based on the results obtained, nanotube arrays with average pore diameter of up to 74 nm and length of 1.6 µm were produced. EDAX confirmed the presence of tungsten element within the nanotube arrays which varied in content from 1.06 at% to 3.29 at%. The photocatalytic activity of the nanotube arrays was then investigated using methyl orange degradation under TUV 96W UV-B Germicidal light irradiation. The nanotube with the highest aspect ratio, geometric surface area factor and at% of tungsten exhibited the highest photocatalytic activity due to more photo-induced electron-hole pairs generated by the larger surface area and because WO₃ improves charge separation, reduces charge carrier recombination and increases charge carrier lifetime via accumulation of electrons and holes in the two different metal oxide semiconductor components.