Search Results (1,330)

The corrosion protection of copper in acidic urban rain environments was studied using self-assembled hydrophobic layers (SAHLs) based on stearic acid (SA), with and without rosehip seed oil (RH). The limited durability of fatty acid-based self-assembled layers under acidic conditions was addressed by correlating surface wettability, morphology, and electrochemical behaviour. Contact angle and SEM analyses showed that SA alone forms a moderately hydrophobic but structurally irregular layer, whereas the addition of 2.0 wt.% RH produces a hierarchical micro/nanostructure with near-superhydrophobic characteristics (CA ≈ 149°). Electrochemical measurements in simulated acid rain solutions (pH 5, 3, and 1) revealed a strong pH dependence of protective performance. While SA-derived layers provided effective protection at pH 5, they deteriorated at lower pH due to protonation of carboxylate anchoring groups and electrolyte ingress. In contrast, SAHLs containing 2.0 wt.% RH maintained polarisation resistance in the MΩ cm² range and inhibition efficiencies above 99% at pH 3, and remained effective even at pH 1. Long-term EIS results indicate a predominantly diffusion-controlled, barrier-type inhibition mechanism associated with defects sealing and interfacial reorganisation. Notably, the rosehip seed oil used is a commercially available, bio-based material with expired shelf life, highlighting the potential of waste-derived resources for sustainable corrosion protection. Full article

The objective of this study is to develop and assess the feasibility of utilizing lotus (Nelumbo nucifera Gaertn.) leaf extract as a green corrosion inhibitor for copper in a sulfuric acid environment. The inhibitory efficacy was comprehensively evaluated using a multi-technique approach, incorporating electrochemical measurements, weight loss analysis, theoretical analysis, and surface morphological characterization. The experimental results demonstrate that the lotus leaf extract functions as an efficient corrosion inhibitor for copper, achieving an inhibition efficiency of 88.07% at 700 mg/L by effectively suppressing both cathodic and anodic corrosion processes. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) confirmed the protective effect, whereas X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) identified functional groups and surface interaction between metal and inhibitor. Theoretical calculations further confirmed the involvement of nitrogen (N) and oxygen (O) as the key active sites. Adsorption behavior adheres to the Langmuir isotherm model, involving both physical and chemical adsorption processes that inhibit the Cu⁺→Cu²⁺ oxidation reaction. This study demonstrates acid-resistant protection of copper using lotus leaf extract. Full article

In the present study, room temperature (RTR) and cryogenic (CR) rolling of electrolytic tough pitch copper (ETP-Cu) was performed to elucidate how deformation temperature and reduction ratio (40% and 80% thickness reductions) control dislocation storage, local stored energy (SE), and self-annealing. Correlated SEM/EDS and EBSD analyses were used to (i) locate Cu₂O particles, (ii) quantify local misorientation, and (iii) map the SE for self-annealing. Point EDS confirms that the intermetallic particles are copper oxides (Cu₂O), with apparent O content varying with particle size and EDS interaction volume. RTR80 (80% rolled) exhibits systematically higher KAM values and a larger area fraction of high SE than RTR40 (40% rolled), explaining the greater frequency and spatial density of self-annealed grains at higher reduction. Cryogenic rolling produces more severe fragmentation and a higher fraction of subgrains than RTR at equivalent reductions. CR80 shows the high KAM structures and locally highest SE regions among all conditions, and a higher fraction of self-annealed grains. Nevertheless, the mapped average SE for CR80 (2.93 × 10⁶ J/m³) was lower than for RTR80 (3.34 × 10⁶ J/m³) due to rapid post-deformation dislocation annihilation/self-annealing upon warming at RT. In all conditions, Cu₂O particles and bulged/irregular grain boundaries concentrate dislocations and SE and act as dominant particle-stimulated nucleation (PSN) sites and RT recrystallization, respectively. These results demonstrate that deformation temperature and reduction jointly determine the spatial distribution of SE and hence the propensity for self-annealing in ETP Cu. Full article

Metal anodes offer substantially higher specific and volumetric capacities than conventional anode materials such as graphite in lithium-ion batteries or hard carbon in sodium-ion batteries. However, the integration of metal anodes into solid-state batteries poses significant challenges, particularly with respect to processing, interfacial stability, and cell assembly. Anode-free solid-state batteries (AFSSBs) address these challenges by eliminating the pre-installed metal anode, instead forming the metal in situ during the initial charging (formation) step. In anode-free solid-state batteries, the quality of the interfacial contact is particularly critical, as insufficient contact can lead to locally increased current densities. Consequently, the initial metal plating during the formation step plays a decisive role in determining the homogeneity and stability of the anode interface. Furthermore, conventional battery-grade copper foils (~10 µm) are considerably thicker than required for the targeted C-rates and are difficult to use as stand-alone anode-free current collectors, thereby hindering the industrial production of anode-free solid-state batteries. In this publication, we demonstrate the application of atmospheric plasma spraying (APS) to fabricate thin copper current collectors directly on the ceramic solid electrolytes LAGP (lithium aluminium germanium phosphate) and BASE (beta-alumina solid electrolyte) with superior interface contact. No mechanical damage or diffusion of copper into the solid electrolyte nor formation of secondary phases at the interfaces were observed in SEM or EDS despite the elevated process temperature. LAGP with a thickness as low as 300 µm was successfully coated and subsequently used for plating/stripping experiments. Finally, dense sodium metal was plated at the copper-substrate interface of a 1.4 mm thick BASE sample. Full article

The study of wide-bandgap nanomaterials has gained considerable attention in recent years, especially in the case of semiconductor oxides that exhibit full or partial optical transparency in fundamental research and technological applications. These include optoelectronic devices, gas sensors and photovoltaic cells, among others. The activation or adjustment of optical and structural properties, especially the bandgap and the parameters of unit cell lattice, can be achieved by varying the dopant concentration during the synthesis of semiconductor thin films in these applications. In this context, copper oxide has emerged as a valuable material, owing to its thoroughly analyzed structural behavior and its broad potential across multiple technological fields. The present work focuses on the synthesis of zinc-doped copper oxide (Zn_xCu_1−xO) thin films on silicon and quartz substrates through ultrasonic spray pyrolysis. The effects of varying the zinc doping concentration (0.0, 5.0, 10.0 and 20.0 at. %) on the morphological, structural, and optical characteristics of the Zn_xCu_1−xO films were analyzed. Scanning electron microscopy (SEM) analysis indicated a gradual increase in nanoparticle size, rising from 221 nm for CuO to approximately 322 nm for the Zn_0.2Cu_0.8O samples as the zinc content increased. Structural characterization via X-ray diffraction (XRD) confirmed a monoclinic crystal arrangement belonging to the $C_{2h}^6$ (c2/c) space group. As the percentage of zinc increased, the XRD peaks shifted to lower angles, consequently increasing the volume and crystal lattice parameters of the Zn_xCu_1−xO structure; this finding was additionally supported by a redshift observed in the Raman analysis. The transmittance spectra of the films showed low transmittance between 40 and 44%. The optical bandgap of the Zn_xCu_1−xO thin films was estimated from the transmittance data by applying the Tauc plot method. A decrease in the band gap was observed at higher doping concentrations. It can be confirmed that no secondary phases are observed at a doping level of 20.0 at. % of zinc, indicating good solubility of zinc in CuO. The analysis and discussion of these findings are included throughout this work to elucidate the controversies noted in the literature. Full article

This study presents a combined process of sulfide precipitation followed by hydrogen peroxide leaching for rhenium recovery from copper smelting waste acid under ambient temperature and pressure. The process first removed copper through selective sulfide precipitation, then achieved co-precipitation of rhenium and arsenic to obtain a rhenium-rich precipitate. Subsequently, exploration of rhenium-containing precipitate leaching using H₂O₂ solution was conducted under isothermal conditions at 20 °C. The effects of H₂O₂ concentration, liquid-to-solid ratio, acidity, and leaching time rhenium extraction efficiency were examined systematically. The optimal leaching conditions were determined as: H₂O₂ concentration of 150 g/L, liquid-to-solid ratio of 5:1 mL/g, stirring speed of 350 r/min, and leaching time of 30 min. Under these conditions, the leaching conversions of rhenium and arsenic reached 96.0% and 93.8%, respectively. Through characterization of precipitate and leaching residue using ICP, SEM-EDS, XRD, and XPS analyses, the process and related reactions were elucidated. Results demonstrated that low-valence rhenium oxides and sulfides serve as the main reactive species during H₂O₂ leaching, whereas organic sulfur, high-valence oxides, and copper sulfide remained stable and resistant to leaching. Selective precipitation of copper effectively eliminated insoluble metal sulfides from rhenium-containing precipitates, thereby enabling efficient separation of rhenium under mild conditions. Full article

Pulse repetition frequency (PRF) controls pulse off-time and, therefore, the extent of thermal accumulation, melt expulsion, and dielectric recovery in finishing electrical discharge machining (EDM). This study clarifies how PRF modifies crater evolution and surface integrity in finishing EDM of 4Cr13 martensitic stainless steel, a corrosion-resistant mold steel used in precision dies and molds. A 2D axisymmetric electro-thermo-fluid model was established in COMSOL, where Gaussian current density, heat-flux, and plasma pressure were periodically imposed at PRFs of 25–100 kHz, while pulse-on time (6 μs) and peak current (8 A) were kept constant. The simulations tracked the transient pressure, heat-flux, velocity, and temperature fields over a common elapsed time of 25 μs. Finishing experiments were then carried out on flat 4Cr13 coupons at 50, 75, and 100 kHz using a copper electrode and deionized water, followed by characterization by laser confocal microscopy, SEM/EDS, and X-ray diffraction using the cosα method. Increasing PRF localized the coupled pressure-heat-flow fields near the crater rim, but shortened off-time and intensified inter-pulse heat accumulation. Accordingly, the surface roughness decreased from Ra = 1.18 μm at 50 kHz to 0.63 μm at 75 kHz, and then slightly increased to 0.71 μm at 100 kHz because of crater overlap, re-melting, and incomplete gap recovery. SEM observations confirmed large irregular craters with cracks at 50 kHz, more uniform fine craters at 75 kHz, and overlapping re-solidified traces at 100 kHz. The residual stress remained compressive for all tested conditions (−341 to −409 MPa). Overall, 75 kHz offers the best compromise between crater uniformity, roughness, and compressive stress for finishing EDM of 4Cr13 steel. Full article

Successive ionic layer adsorption reaction (SILAR) was used to deposit Cu₂O nanosheets on anodized TiO₂ nanotubes at different deposition cycles (4, 8, 15, and 20). Compared to the bare TiO₂ nanotubes, these coatings were investigated for their tribological behavior (friction, wear and energy loss), scanning and transmission electron microscopy (SEM, TEM), X-ray Diffraction (XRD) was used to characterize Cu₂O/TiO₂ coatings to study the effect of number of cycles on the morphological and structural properties of the samples; these characteristics engage in determining the wear mechanisms. The assessment of the coating’s adhesion was determined by the obtained critical loads from the scratch test; the 15 cycles Cu₂O/TiO₂ exhibited higher critical loads, which corresponds to improved adhesion. This sample also showed a low wear volume of 7.5 × 10⁶ µm³ compared to other samples but higher energy loss due to the low shear strength of copper oxide. The friction coefficient, however, decreased from 0.7 for bare TiO₂ nanotubes to 0.48 for 20 cycles Cu₂O/TiO₂ coatings at higher loads, which proves the wear resistance enhancement. Since these coatings will be manufactured for orthopedic and dental implant applications, the corrosion resistance was tested, and the 15 cycles Cu₂O-NPs/TiO₂-NTs where these coatings exhibited the most favorable combination of a low corrosion current density (1.9 × 10⁻⁴ A/cm²) and a noble corrosion potential (−0.3 V/SCE); furthermore, there was a polarization resistance of 2.4 × 10⁴ Ω·cm² and a protection efficiency of 96.7%, indicating significantly enhanced corrosion resistance as opposed to the other samples. Full article

Large-scale reuse of copper tailings can mitigate environmental hazards and recover strategic elements; this work investigates the feasibility of producing foam glass-ceramics with high copper-tailing content (>70 wt%) by tuning the CaO/SiO₂ ratio to couple melt viscosity and crystallisation. The comprehensive utilisation of these tailings helps mitigate environmental pollution and enhance resource efficiency. In this study, foam glass-ceramics with varying CaO/SiO₂ ratios were synthesised through melt quenching followed by foaming heat treatment. The effects of different CaO/SiO₂ ratios on the foaming behaviour, crystallisation, and microstructure were investigated using DSC, FTIR, viscosity, XRD, SEM, and CT. The results indicate that increasing the CaO/SiO₂ ratio disrupts the three-dimensional network structure of the glass, which lowers the glass viscosity and influences the bubble size and distribution in the foam glass-ceramics. Additionally, the increased CaO content promotes crystal precipitation and enhances the compressive strength of the foam glass-ceramics. At a CaO/SiO₂ mass ratio of 0.22, the foam glass-ceramics exhibited the lower bulk density (240 kg/m³) and thermal conductivity (0.07 W/m·K). The materials also demonstrated good water absorption and compressive strength. This study highlights the potential of using copper tailings in foam glass-ceramics to improve their overall performance, offering promising energy-saving and environmentally friendly solutions. Full article

Cold-mercury gilding uses mercury as an adhesive to bond gold foil onto the surface of copper and silver artifacts. This technique and mercury gilding (fire gilding) both belong to the Au-Hg system and are closely related in technology. Clarifying the technical differences between them is of great significance for revealing the developmental sequence of ancient gilding technologies. On the basis of reconstructing traditional fire gilding, simulated cold-mercury-gilded samples were successfully prepared using experimental archeological methods, and multi-scale characterization was performed using SEM-EDS, XRD, and XPS. The results show that the surface of cold-mercury-gilded samples displays a micromorphology of folded and overlapped gold foil accompanied by locally dense particle aggregation. The cross-section of the gold layer exhibits a multilayer stacked structure, in which mercury is enriched at the gold layer/substrate interface and forms an AuHgCu/Ag diffusion layer. Room-temperature-stable Au-Hg and Ag-Hg phases such as Au₂Hg and AgHg are present in the gold layer, reflecting complex phase transformation behavior of the Au-Hg/Ag-Hg system at room temperature. During cold-mercury gilding, liquid mercury first adheres to the gold foil, and then interdiffusion and phase reactions occur between mercury, gold, and copper/silver atoms at room temperature. Intermetallic compounds and diffusion layers formed at the interface achieve firm bonding between the gold layer and the substrate. Both cold-mercury gilding and mercury gilding achieve metallurgical bonding through atomic interdiffusion. However, affected by differences in the initial state of mercury and operating temperature, the phase transformation and atomic diffusion behaviors of the system differ significantly, which are ultimately reflected in the cross-sectional structure of the gold layer, the composition of the interfacial diffusion layer, and the types of phases. Therefore, mercury-gilded artifacts show superior gold layer durability and bonding strength with the substrate compared with cold-mercury-gilded artifacts. Both techniques pioneered the application of mercury in metallic gilding and represent important innovations in ancient surface decoration technology. Full article

Janus nanoparticles (JNPs) synthesis has caught the scientific community’s attention due to their amphiphilic properties and extensive areas of application. In this work, different new copper–silica-based and silica-based JNPs were synthesized using a novel masking methodology and a self-assembly method based on sol–gel procedures, respectively. Moreover, various techniques were used to characterize the developed nanomaterials, including scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Two types of copper–silica-based Janus nanoparticles were synthesized with a 40 to 70 nm size, while SiO₂-based JNPs of around 135 nm were obtained. The duality of different JNPs was confirmed by SEM and by a simple and economical route based on an emulsion stabilization path: analyzing dispersion/aggregation and associated behavior at the immiscible solvent interface. JNPs exhibited an extended residence time over 20 days at an immiscible solvent interface, thereby enhancing the resulting emulsion interface stability. This behavior highlighted their amphiphilic characteristics in comparison to conventional nanoparticles. Consequently, a procedure to determine nanoparticle amphiphilicity could be further standardized. Full article

This research investigates the optimization of surface integrity in powder-mixed electrical discharge machining (PMEDM) through the innovative use of Jatropha biodielectric fluid enhanced with titanium dioxide (TiO₂) nanoparticles. A comprehensive experimental framework was developed using design expert software (DOE) with Response Surface Methodology (RSM) to systematically analyze the machining of AISI D2 tool steel using copper electrodes. The study examined five critical process parameters, gap current (Ip), pulse-on duration (Ton), pulse-off time (Toff), gap voltage (V), and powder concentration, evaluating their combined effects on surface roughness (SR), surface crack density (SCD), and residual stress characteristics. Advanced characterization techniques including scanning electron microscopy (SEM) were employed to analyze surface topography and subsurface microstructural changes. The optimization process successfully identified optimal machining conditions of current = 9 A, Ton = 100 µs, Toff = 10 µs, and gap voltage = 65 V, achieving exceptional surface quality with a minimum surface roughness of 3.22 µm. Remarkably, these optimized parameters resulted in crack-free surfaces with zero surface crack density and minimal residual stress values across the 2θ range of 90° to 180°. To enhance predictive capabilities, supervised machine learning algorithms were implemented to model surface roughness behavior. Comparative analysis of classification algorithms demonstrated that Support Vector Machine (SVM), k-Nearest Neighbors (kNNs), and Gaussian Naïve Bayes achieved superior performance with F1-scores of 0.88 and prediction accuracies of 90%. The integration of sustainable Jatropha biodielectric with TiO₂ nanoparticles represents a significant advancement in environmentally conscious precision machining, while the machine learning approach establishes a robust framework for intelligent process optimization and quality prediction in advanced manufacturing applications. Full article

Saxony was ruled by two cousins in 1544: John Frederick I (Elector of Saxony) and his cousin Maurice (Duke of Saxony). Both rulers’ names appear on each side of the quarter thalers produced in this year. They were enemies involved in religious wars, although they were both Protestants. Two types of quarter thalers from 1544 occur: a pierced random find from Transylvania (Romania) with four shields on the reverse, heavily worn, and another one with three shields on the obverse side, found in the Głogów Hoard (Poland), which is well preserved. Why did they issue two types in the same year? Was it a matter of silver title or other historical factors? Nondestructive investigation methods were used: XRD revealed the phases within the alloy and patina layer; SEM-EDS revealed the morphological aspects and their elemental compositions, which were correlated with XRF results. The results show that both coins have closer silver amounts, from 91 to 96 wt.%. The EDS results were in good agreement with the XRF results. Lead traces indicated a difference between them: the four-shielded coin is lead-free, while the three-shielded coin has a moderate amount of lead, about 0.5 wt.%. The archeological data evidence that the four-shielded coin issued in 1544 is rarer than the three-shielded one because it was issued during specific historical conditions. Black patina is formed by a mixture rich in copper oxides mixed with silver oxides and Ag₂S. The presence of silver sulfide in the patina layer confirms that the pierced coin was in prolonged contact with the skin surface. Also, the finest traces of minerals embedded in the patina layer (e.g., quartz, kaolinite, and calcite) suggest that they were embedded in the patina via prolonged exposure to particulate matter. The mineral inclusions in the patina would have been more numerous if they were formed underground. Thus, the pierced four-shielded coin was probably worn as jewelry by nomads, while the three-shielded coin was most likely treasured in a well-preserved hoard. Full article

The brittleness of 18-karat purple gold originates from the AuAl₂ intermetallic compound. This study investigates the microstructural modification of the AuAl₂ intermetallic compound by adding silicon (Si) and cobalt (Co) and by rapid solidification in copper molds. The samples with alloy additions from a traditional investment casting were compared with copper mold casting for grain boundary characteristics using SEM, EBSD, and TEM. SEM micrographs showed a reduction in grain size of copper mold casting from approximately within 150–200 μm to within 12–20 μm. EBSD showed a narrow grain size distribution in the Si–Co-modified alloy than in the Si-modified alloy, using the copper mold casting technique. TEM observations show that grain boundaries were closely packed, with ~80 nm-sized voids. XRD confirmed that all alloys retained the AuAl₂ intermetallic phase, with peak broadening in the modified and fast-cooling samples indicating crystallographic refinement. These results confirm that Si-Co additions with a fast cooling rate effectively refine the microstructure of the AuAl₂ intermetallic compound, making the alloy less brittle while preserving the purple gold color. Full article

In this study, the in situ solvothermal synthesis of a copper-based metal–organic framework (Cu-BTC MOF) into two porous ceramic substrates with a 10 cm diameter and 2 cm thickness was reported. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, diffuse reflectance spectroscopy (DRS), Tauc plot analysis, optical microscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were the techniques that were utilized to verify the formation and incorporation of the MOF into ceramics (two samples, with different SiO₂ particles; 500 µm (Ceramic 1), and 150 µm (Ceramic 2)). The synthesized Cu-MOF exhibited a crystalline structure. Both the composites and the Cu-MOF exhibited visible-light absorption, with optical band gaps of 2.5 eV and 2.4 eV, respectively, as determined by DRS. TEM images demonstrated that crystalline MOF domains were successfully included inside the ceramics. Methyl orange (MO), Congo red (CR), and methylene blue (MB) were used to assess the composites’ ability to remove dyes. Catalytic hydrogenation, powered by in situ hydrogen production from NaBH₄ hydrolysis, demonstrated high removal efficiencies of 91–97% after 60 min. Adsorption, on the other hand, was ineffective. Despite undergoing four consecutive cycles without performance degradation, the materials demonstrated remarkable recyclability. Cu-MOF@ceramic composites are effective, durable, and practically applicable for improved wastewater treatment. Full article