Search Results (1,259)

The Mako Belt in the Kédougou-Kéniéba Inlier (eastern Senegal) preserves Paleoproterozoic (2.3–1.9 Ga) mafic and ultramafic rocks that record early crustal growth processes within the southern West African Craton (WAC). Basalt bulk rock compositions preserve primary melt signatures, whereas the associated ultramafic cumulates are variably serpentinized and are better assessed through mineral chemistry. Basalts occur as massive and pillow lavas, with MgO contents of 5.9–9.1 wt.% and flat to slightly LREE-depleted patterns (La/Smₙ = 0.73–0.88). Primitive mantle-normalized diagrams show subduction-related signatures, including enrichment in Ba, Pb, and Rb and depletion in Nb and Ta. Most basalts and all ultramafic rocks display (Nb/La)_PM > 1, consistent with enriched mantle melting in a back-arc setting. Harzburgites and lherzolites have cumulate textures, high Cr and Ni contents, and spinel with chromian cores (Cr# > 0.6) zoned sharply to Cr-rich magnetite rims that overlap basalt spinel compositions. Integration of the petrographic, mineralogical, and whole-rock geochemical data indicates the presence of mafic melts derived from a subduction-modified mantle wedge and likely formed in a back-arc basin above a subducting slab, rather than from a plume or mid-ocean ridge setting. Regional comparisons with other greenstone belts across the WAC suggest that the Mako Belt was part of a broader arc–back-arc system accreted during the Eburnean orogeny (~2.20–2.00 Ga). This study supports the view that modern-style plate tectonics—including subduction and back-arc magmatism—was already active by the Paleoproterozoic, and highlights the Mako Belt as a key archive of early lithospheric evolution in the WAC. Full article

The development of high-performance supercapacitor electrodes is crucial to meet the increasing demand for efficient and sustainable energy storage systems. Cobalt oxide (Co₃O₄), with its high theoretical capacitance, is a promising electrode material, but its practical application is hindered by poor conductivity limitations and structural instability during cycling. In this work, lanthanum La³⁺-doped Co₃O₄ nanocubes were synthesized via a hydrothermal approach to tailor their structural and electrochemical properties. Different doping concentrations (1, 3, and 5%) were introduced to investigate their influence systematically. X-ray diffraction confirmed the retention of the spinel phase with clear evidence of La³⁺ incorporation into the Co₃O₄ lattice. Also, Raman spectroscopy validated the structural integrity through characteristic Co-O vibrational modes. Scanning electron microscopy analysis revealed uniform cubic morphologies across all samples. The formation of the cubic spinel structure of 1% La³⁺-doped Co₃O₄ are confirmed from XPS and TEM studies. Electrochemical evaluation in a 3 M KOH electrolyte demonstrated that 1% La³⁺-doped Co₃O₄ nanocubes delivered the highest performance, achieving a specific capacitance of 1312 F g⁻¹ at 1 A g⁻¹ and maintaining a 79.8% capacitance retention and a 97.12% Coulombic efficiency over 10,000 cycles at 5 Ag⁻¹. It can be demonstrated that La³⁺ doping is an effective strategy to enhance the charge storage capability and cycling stability of Co₃O₄, offering valuable insights for the rational design of next-generation supercapacitor electrodes. Full article

The chemical looping steam reforming of methane (CLSR) employing Fe-containing oxygen carriers can produce syngas and hydrogen simultaneously. However, Fe-based oxygen carriers exhibit low CH₄ activation ability and cyclic stability. In this work, oxygen carriers with fixed Fe content and different Fe/Ni ratios were synthesized by the sol–gel method to investigate the effects of Ni-Fe-Al interactions on CLSR performance. Ni-Fe-Al interactions promote the growth of the spinel structure and regulate both the catalytic sites and the available lattice oxygen, resulting in the CH₄ conversion and CO selectivity being maintained at 96–98% and above 98% for the most promising oxygen carrier, with an Fe₂O₃ content of 20 wt% and Fe/Ni molar ratio of 10. The surface, phase, and particle size were kept the same over 90 cycles, leading to high stability. During the CLSR cycles, conversion from Fe³⁺ to Fe²⁺/Fe⁰ occurs, along with transformation between Ni²⁺ in NiAl₂O₄ and Ni⁰. Overall, the results demonstrate the feasibility of using spinel containing earth-abundant elements in CLSR and the importance of cooperation between oxygen release and CH₄ activation. Full article

ZrO₂-MgO-Al₂O₃ ceramics, despite a long history of research, still attract the attention of researchers due to the high potential of their applications as refractories and matrices for metal ceramics. A unique composition combining high strength and temperature stability is particularly in demand. In this paper, a comprehensive study of ceramics of the composition (90−x)·ZrO₂-10·MgO-x·Al₂O₃ (x = 10–80 wt.%) obtained by solid-phase sintering with preliminary annealing is carried out. Preliminary annealing was used for the possible formation of metastable phases with outstanding mechanical properties. Using the X-ray diffraction method, it was found that most of the samples consist of monoclinic zirconium oxide, magnesium–aluminum spinel, and corundum phases. The exception is the sample with x = 10 wt.%, in which the main phase was a cubic modification of zirconium oxide. By formation this type of ZrO₂ polymorph in the composition hardness and flexural strength significantly increased from 400 to 1380 and 50 to 210 MPa, respectively. The total porosity of ceramics under study lies in the range 6–28%. Using the scanning electron microscopy method, it was found that the phase composition significantly affects the morphology of the microstructure of the sintered bodies. Thus, for sintered ceramics with a high corundum content, the microstructure is characterized by high porosity and a large grain size. For the first time, by applying preliminary annealing, a new type of ternary ceramic ZrO₂-MgO-Al₂O₃ was sintered with potentially outstanding mechanical properties. The presence of a stabilized zirconium oxide phase, stresses in the crystal lattice of the matrix phase, and the formation of cracks in the microstructure are the main factors influencing shrinkage, porosity, microhardness, and biaxial flexural strength. Full article

Herein, nanoscale MgAl₂O₄ (MOA), 10%CuO@MgAl₂O₄ (10Cu@MOA), 10%NiO@MgAl₂O₄ (10Ni@MOA), and 10%CoO@MgAl₂O₄ (10Co@MOA) were synthesized employing butylated hydroxytoluene (the food additive BHT) as a capping agent. The SEM images illustrated average sizes of 38.8, 30.0, 40.8, and 32.7 nm for MOA, 10Cu@MOA, 10Ni@MOA, and 10Co@MOA, respectively, and their BET surface area were 84.4, 141.8, 126.7, and 105.3, respectively. Doxycycline DXC removal was studied employing the MOA, 10Cu@MOA, 10Ni@MOA, and 10Co@MOA, which resulted in q_t values of 57.3, 106.1, 97.7, and 73.9 mg g⁻¹, respectively. The pseudo-second order model best described the DXC sorption onto MOA, 10Cu@MOA, 10Ni@MOA, and 10Co@MOA, and both film diffusion models influenced the DXC sorptions onto the sorbents. The DXC sorption onto the 10Cu@MOA fitted the Freundlich model. The thermodynamics implied endothermic-spontaneous DXC sorption onto the10Cu@MOA. The pH study exposed that the DXC removal by 10Cu@MOA was more effective in a mildly acidic medium (pH = 6.0). Furthermore, the 10Cu@MOA effectiveness in treating surface water contaminated by 5.0 and 10.0 mg L⁻¹ DXC was 99.9% and 98.1%, respectively, while it was 94.7% and 92.5% in treating the concentrations above in seawater, respectively. The reusability study showed a 10% reduction in the 10Cu@MOA’s removal efficiency at the fourth cycle, which is encouraging for real-life applications. Full article

This paper studies the formation process of a composite material based on an organic substance, biochar from sunflower husks, and an inorganic substance, nickel (II)-copper (II) ferrites of the composition Cu_xNi_1−xFe₂O₄ (x = 0.0; 0.5; 1.0). The obtained materials were characterized by X-ray phase analysis, scanning electron microscopy, and FTIR spectroscopy. It is shown that when replacing copper (II) cations with nickel (II) cations, the average parameters and volume of the unit cell gradually decrease, and the cation–anion distances in both the tetrahedral and octahedral spinel grids also decrease with regularity. The oxide materials were found to form a film on the surface of biochar, repeating its porous structure. The obtained materials exhibit high catalytic activity in the methyl orange decomposition reaction under the action of hydrogen peroxide in an acidic medium; the degradation of methyl orange in an aqueous solution occurs 30 min after the start of the reaction. This result may be associated with the formation of the Fenton system during the oxidation–reduction process. A significant increase in the reaction rate in the system containing mixed nickel–copper ferrite as a catalyst may be associated with the formation of a more defective structure due to the Jahn–Teller effect manifestation, which creates additional active centers on the catalyst surface. Full article

The method of obtaining functional materials almost always influences the physicochemical properties of the resulting substances. The plasma treatment of solid materials is considered to be a more energy efficient method when compared with thermal destruction. Our work is the first to treat double complex salt (DCS) [Co(NH₃)₆][Fe(CN)₆] with different plasma discharge modes. We have demonstrated the possibility of obtaining a single-phase spinel with a CoFe₂O₄ structure as a result of the calcination in air of the plasma destruction product. The crystallite sizes of the obtained spinel are 40 nm, with a lattice constant 8.38 Å. Full article

In this study, we investigate the phase transition process during high-alumina, low-lithium glass-ceramics (ZnO-MgO-Li₂O-SiO₂-Al₂O₃) crystallization. The differential scanning calorimetry and high-temperature X-ray diffraction results show that approximately 10 wt.% of (Zn, Mg)Al₂O₄ crystals precipitated when the heat treatment temperature reached 850 °C, indicating that a large number of nuclei had already formed during the earlier stages of heat treatment. Field emission transmission electron microscopy used to observe the microstructure of glass-ceramics after staged heat treatment revealed that cation migration occurred during the nucleation process. Zn and Mg aggregated around Al to form (Zn, Mg)Al₂O₄ nuclei, which provided sites for crystal growth. Moreover, high-valence Zr aggregated outside the glass network, leading to the formation of nanocrystals. Raman spectroscopy analysis of samples at different stages of crystallization revealed that during spinel precipitation, the Q³ and Q⁴ structural units in the glass network increased significantly, along with an increase in the number of bridging oxygens. Highly coordinated Al originally present in the network mainly participated in spinel nucleation, effectively suppressing the subsequent formation of Li_xAl_xSi_1−xO₂, which eventually resulted in the successful preparation of glass-ceramics with (Zn, Mg)Al₂O₄ and ZrO₂ as the main crystalline phases. The grains in this glass-ceramic are all nanocrystals. Its Vickers hardness and flexural strength can reach up to 875 Hv and 350 MPa, respectively, while the visible light transmittance of the glass-ceramic reaches 81.5%. This material shows potential for applications in touchscreen protection, aircraft and high-speed train windshields, and related fields. Full article

Lithium (Li) ion sieve is considered to have great potential in the selective extraction of Li⁺ from complex Li⁺-containing brine owing to its cost-effectiveness, excellent adsorption performance, and environmental friendliness. Nevertheless, the defects of complex regulation and control of technological parameters in the preparation process of Li ion sieve and poor recycling efficiency limit its application. In this study, spinel-type H₄Ti₅O₁₂ ion sieves (HTO) were successfully prepared through a high-temperature solid-state method for recovering Li⁺ from aqueous resources. Through the experiment of optimizing the key preparation process parameters of HTO, it was found that the optimum preparation conditions were as follows: lithium ion source of CH₃COOLi‧H₂O, calcination temperature of 800 °C, and acid (HCl) washing concentration of 0.3 mol/L. The uptake of Li⁺ by HTO aligned with the pseudo-second-order kinetic model, which was a chemical adsorption process controlled by reversible Li–H ion exchange reaction. HTO exhibited extremely high regeneration cycle characteristics, and after five cycles, it retained 96.06% of its initial adsorption capacity. The present work highlighted that spinel-type HTO has high industrial application potential in the field of Li⁺ recovery from oilfield brine. Full article

The citrate–nitrate method was employed to synthesize the magnesium chromite (MgCr₂O₄) spinel, followed by calcination at 700 °C for 3 h. The synthesized compound was analyzed using techniques including powder XRD, SEM-EDAX, FTIR, UV-DRS, and LCR Meter. The structural analysis was conducted using an X-ray diffractometer, which revealed the formation of the cubic crystal symmetry of the sample with the corresponding Fd-3 m space group. The average crystallite size of the sample was calculated around 15.38 nm. Using tetrahedral and octahedral positions, the lattice vibrations of the associated chemical bonds were identified using Fourier transform infrared (FTIR) spectroscopy. SEM (scanning electron microscopy) micrographs showed that the spherical nature of the particles and the constituent particles were between 10 and 40 nm in size. The optical bandgap value was evaluated using Tauc’s plot. Pellets of the powdered sample were prepared for determining the dielectric aspects, such as the dielectric constant (ε′) and tangent loss (tanδ), in the frequency range of 10 Hz–8 MHz at room temperature. The charge transport mechanism was explored from the complex impedance spectroscopy study. The obtained results indicate that magnesium chromite may be a potential candidate in the fabrication of sensors, micro-electronic devices, etc. Full article

The development of multifunctional nanostructured catalysts with high electrochemical activity and stability is crucial for sustainable technologies. Herein, we report the synthesis of CTAB-capped NiCo₂O₄ (CNC) spinel nanostructures via a facile co-precipitation method, engineered to enhance surface activity and charge transport. The optical and structural properties of the nanocomposite were confirmed by UV-Vis and TEM analysis, and the functional group present in the composite was confirmed by FT-IR study. The cubic spinel phase of the CNC was confirmed by XRD analysis. The band gap value was determined to be 2.15 eV, which confirmed the semiconductor nature of the nanocomposite. The photocatalytic degradation efficiency was achieved up to approximately 97% against malachite green. Additionally, CNC demonstrated excellent electrocatalytic performance in non-enzymatic glucose detection, exhibiting high sensitivity and reproducibility across a broad concentration range. Hence, the CNC acted as a potent oxidant for photoelectrochemical reactions. Full article

The growing demand for lithium-ion batteries (LIBs) has led to an urgent need for sustainable recycling strategies for spent cathode materials. In this study, a mechanochemical approach was developed for the recovery of lithium and cobalt from end-of-life LiCoO₂ cathodes using high-energy ball milling. For the first time, aluminum and carbon were employed as internal reducing agents, facilitating the in situ decomposition of LiCoO₂ into CoO, Li₂O, and metallic Co. X-ray diffraction analysis confirmed significant structural disorder, phase transitions, and the formation of CoO, AlCo, and spinel-like CoAl₂O₄. The Taguchi method was applied to optimize milling parameters, identifying 800 rpm, 60 min, and a ball-to-powder ratio of 50:1 as the most effective conditions for structural activation. Subsequent ammonia leaching under fixed conditions (3.0 M NH₃·H₂O, 1.0 M (NH₄)₂CO₃, 60 °C, 25 mL/g, 6 h) demonstrated high recovery efficiencies: up to 94.6% for lithium and 83.7% for cobalt in the best-performing samples. These results highlight the synergistic benefits of mechanical activation and reductant-assisted phase engineering for enhancing metal recovery. The proposed method offers a simple, scalable, and eco-friendly route for the hydrometallurgical recycling of LIB cathodes without requiring extensive chemical pretreatment. Full article

This study evaluates the corrosion behavior of Fe-22Mn-0.6C TWIP steels containing 0%, 5%, and 10% chromium after 28 days of exposure to a neutral sulfate solution. By combining electrochemical testing with a surface and spectroscopic analysis, we explored how Cr influences the formation and stability of oxide layers. The results reveal a clear trend: as the chromium content increases, the corrosion resistance improves significantly. The 10% Cr alloy stood out for its high impedance and stable electrochemical response, pointing to the development of a dense, protective oxide layer that limits the corrosive attack. The SEM/EDS and Raman spectroscopy revealed that chromium not only enhances the oxide’s compactness but also alters its composition, transitioning from iron-rich, porous oxides to Cr-containing spinels and oxyhydroxides with superior barrier properties. These structural and chemical improvements were confirmed by electrochemical parameters, which showed a reduced capacitance and increased film homogeneity. To tie these findings together, we propose a schematic model describing how chromium shapes the passivation process in these steels. Altogether, this study highlights the essential role of Cr in enhancing long-term corrosion protection in high-Mn TWIP steels under sulfate-rich conditions. Full article

This study is focused on the hydrothermal synthesis of iron–manganese oxide nanostructures, focusing on the influence of Fe:Mn precursor ratios, temperature, and reaction time on phase formation, morphology, and structural characteristics. Three molar ratios (Fe:Mn = 2:1, 1:1, and 1:2) were explored under variable conditions (80 °C, 120 °C, and 200 °C; 4, 12, and 24 h). X-ray diffraction (XRD) analysis revealed distinct phase selectivity depending on precursor composition: FeMn₂O₄ was obtained with 1:2 ratio, Fe₃Mn₃O₈ with 1:1, and Fe₂MnO₄ with 2:1, each without phase mixing. Scanning electron microscopy (FESEM) showed a pronounced effect of temperature and time on nanoparticle morphology, ranging from compact agglomerates to well-defined rod-like structures at 200 °C/24 h. Dynamic light scattering (DLS) indicated narrow size distributions for samples synthesized at 120 °C/12 h, with hydrodynamic diameters between 20 and 50 nm. Raman spectroscopy confirmed the presence of characteristic vibrational modes of spinel-type structures and validated structural integrity. High-resolution transmission electron microscopy (HRTEM) evidenced well-ordered lattice fringes with interplanar spacings of ~0.48–0.52 nm, consistent with spinel phases and indicative of high crystallinity. These findings demonstrate that controlled atomic binding and thermal parameters enable selective synthesis of pure iron–manganese oxide phases with tailored morphologies, offering a scalable route for designing advanced functional materials in catalysis, energy, and biomedical applications. Full article

As internal combustion engine (ICE) systems are increasingly exposed to severe thermal and oxidative environments, the oxidation resistance and structural integrity of exhaust valve materials have become critical for maintaining long-term engine reliability and efficiency. This study presents a comparative evaluation of the cyclic oxidation behavior of two candidate valve steels, 1.4718 (ferritic stainless steel) and 1.4871 (austenitic stainless steel), under service-temperature conditions. The specimens were exposed to repeated oxidation at 550 °C, 650 °C and 750 °C for 25 cycles in ambient air. The surface and cross-sectional morphologies of the oxide layers were analyzed using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) to investigate oxide scale composition, thickness, and growth characteristics. The oxidation behavior of both alloys proceeded in two distinct stages: an initial phase marked by accelerated oxidation, followed by a slower, more stable growth period. The extent of oxidation intensified with increasing temperature. The 1.4718 alloy developed relatively porous but compositionally stable oxide layers consisting primarily of Fe- and Cr-based spinels such as FeCr₂O₄ and Cr₂SiO₄. In contrast, the 1.4871 alloy formed a dense, adherent, dual-layered oxide scale composed of an outer Mn₂O₃-rich layer and an inner Cr₂O₃-rich layer, attributable to its high Mn and Cr content. The results underscore the critical influence of elemental composition, particularly Cr, Mn and Si, on oxide scale stability and spallation resistance, demonstrating the superior cyclic oxidation resistance of the 1.4871 alloy and its potential suitability for exhaust valve applications in thermally aggressive environments. Full article