Search Results (169)

High-entropy alloys (HEAs) exhibit superior properties for extreme environments, yet the effects of laser scanning speed on the microstructure and performance of laser-clad NiAlNbTiV HEA coatings remain unclear. This study systematically investigates NiAlNbTiV coatings on 316 stainless steel fabricated at scanning speeds of 800–1100 mm/min via laser cladding. Characterizations via XRD, SEM/EDS, microhardness testing, high-temperature wear testing, and electrochemical measurements reveal that increasing scanning speed enhances the cooling rate, promoting γ-(Ni, Fe) solid solution formation, intensifying TiV peaks, and reducing Fe-Nb intermetallics. Higher speeds refine grains and needle-like crystal distributions but introduce point defects and cracks at 1100 mm/min. Microhardness decreases from 606.2 HV (800 mm/min) to 522.4 HV (1100 mm/min). The 800 mm/min coating shows optimal wear resistance (wear volume: 0.0117 mm³) due to dense eutectic hard phases, while higher speeds degrade wear performance via increased defects. Corrosion resistance follows a non-linear trend, with the 900 mm/min coating achieving the lowest corrosion current density (1.656 μA·cm⁻²) due to fine grains and minimal defects. This work provides parametric optimization guidance for laser-clad HEA coatings in extreme-condition engineering applications. Full article

The present study focused on 10 wt.% TiB₂@Ti/AlCoCrFeNi_2.1 eutectic high-entropy alloy matrix composites (EHEAMCs), which were treated with furnace cooling (FC), air cooling (AC), and water cooling (WC) after being held at 1000 °C for 12 h, aiming to investigate the effect of cooling methods on their microstructure and mechanical properties. The results showed that the composites in all states consisted of FCC phase, BCC phase, TiB₂ phase, and Ti phase. The cooling methods did not change the phase types but affected the diffraction peak characteristics. With the increase in cooling rate, the diffraction peaks of FCC and BCC phases gradually separated from overlapping, and the diffraction peak of the FCC (111) crystal plane shifted to a lower angle (due to the increase in lattice constant caused by Ti element diffusion), while the diffraction peak intensity showed a downward trend. In terms of microstructure, all composites under the three cooling conditions were composed of eutectic matrix, solid solution zone, and grain boundary zone. The cooling rate had little effect on the morphology but significantly affected the element distribution. During slow cooling (FC, AC), Ti and B diffused sufficiently from the grain boundary to the matrix, resulting in higher concentrations of Ti and B in the matrix (Ti in FCC phase: 7.4 at.%, B in BCC phase: 8.1 at.% in FC state). During rapid cooling (WC), diffusion was inhibited, leading to lower concentrations in the matrix (Ti in FCC phase: 4.6 at.%, B in BCC phase: 4.3 at.%), but the element distribution was more uniform. Mechanical properties decreased with the increase in cooling rate: the FC state showed the optimal average hardness (627.0 ± 26.1 HV), yield strength (1574 MPa), fracture strength (2824 MPa), and fracture strain (24.2%); the WC state had the lowest performance (hardness: 543.2 ± 35.4 HV and yield strength: 1401 MPa) but was still better than the as-sintered state. Solid solution strengthening was the main mechanism, and slow cooling promoted element diffusion to enhance lattice distortion, achieving the synergistic improvement of strength and plasticity. Full article

A novel behavior of fluid inclusions (FIs) in crystals is reported in this study. Typically, at “high” temperature, FIs in molecular crystals become faceted, adopting the morphology of a single crystal. Usually, upon cooling, these faceted FIs develop into rounded cavities containing the mother solution with a retreat gas bubble. After annealing at low temperature, the FIs reshape back into a negative-crystal morphology, but the gas bubble remains. This latter process can take from minutes to very long times depending on the storage temperature and solubility. Investigations into the behavior of FIs of dicumyl peroxide (DCP) under fast cooling rates have revealed a morphological transition from negative crystals to FIs with a holly-leaf shape. The spikes of the holly-leaf-shaped FIs point toward the corners of the former negative crystal, and the sizes of the gas bubbles exceed those of conventional retreat bubbles. Therefore, it is likely that this phenomenon is linked to rapid cooling and an excess of CO₂ dissolved in the mother solution from which the DCP single crystals were grown. The concentration of the solution inside the FIs rapidly increases after the nucleation of this large gas bubble. This is consistent with a sharp acceleration of inward crystal growth immediately after its appearance. Interestingly, FIs in pyroclastic olivine crystals grown from CO₂-rich lava can also present a holly-leaf shape. Thus, this non-equilibrium morphological transition may be relatively common. Full article

The effect of severe plastic deformation during milling and conventional and Spark Plasma Sintering (SPS) on the wt. % microstructural, structural, thermal, magnetic, and mechanical properties of the Al–16 wt. % Mn–7 wt. % Cu alloy was studied. A milling process for up to 24 h (A24) leads to microstructure refinement and the presence of Al, Mn, and Cu solid solutions. The energy dispersive spectroscopy (EDS) analysis reveals the existence of Cu–Al, Mn–Al, and Al–Mn enriched particles. The powders exhibit weak ferromagnetism and an exchange bias (EB) behaviour that decreases with increasing milling time. The Ms values fitted using the law of approach to saturation (LAS) are comparable to the experimental values. The exothermic and endothermic peaks that appear in the differential scanning calorimetry (DSC) scans in the 500–900 °C range on heating/cooling are related to different phase transformations. The crystal structure of the A24 powders heated up to 900 °C (A24_900 °C) consists of a dual-phase microstructure of Al₂₀Cu₂Mn₃ nanoprecipitates (~28%) and Al matrix (~72%). The sintering of the A24 powders at 500 °C for one hour (A24S) leads to the precipitation of Al₆Mn, Al₂Cu, and the Al₂₀Cu₂Mn₃ T-phase into the Al-enriched matrix. In contrast, the consolidation by SPS (A24SPS) leads to a mixture of an Al solid solution, Al₆Mn, T-phase, and α-Mn with an increased weight fraction of the T-phase and Al₆Mn. The sintered samples exhibit the coexistence of a significant PM/AFM contribution to the M-H curves, with increasing Hc and decreasing EB. A higher microhardness value of about 581 HV is achieved for the A24SPS sample compared to those of the A24 (68 HV) and A24S (80 HV) samples. Full article

Rare earth elements (REEs) have garnered significant global attention due to their essential role in advanced technologies. Sri Lanka is endowed with various REE-bearing minerals, including the apatite-rich deposit in the Eppawala area, commonly known as Eppawala rock phosphate (ERP). However, direct extraction of REEs from ERP is technically challenging and economically unfeasible. This study introduces a novel, integrated approach for recovering REEs from ERP as a by-product of nitrophosphate fertilizer production. The process involves nitric acid-based acidolysis of apatite, optimized at 10 M nitric acid for 2 h at 70 °C with a pulp density of 2.4 mL/g. During cooling crystallization, 42 wt% of calcium was removed as Ca(NO₃)₂.4H₂O while REEs remained in the solution. REEs were then selectively precipitated as REE phosphates via pH-controlled addition of ammonium hydroxide, minimizing the co-precipitation with calcium. Further separation was achieved through selective dissolution in a sulfuric–phosphoric acid mixture, followed by precipitation as sodium rare earth double sulfates. The process achieved over 90% total REE recovery with extraction efficiencies in the order of Pr > Nd > Ce > Gd > Sm > Y > Dy. Samples were characterized for their phase composition, elemental content, and morphology. The fertilizer results confirmed the successful production of a nutrient-rich nitrophosphate (NP) with 18.2% nitrogen and 13.9% phosphorus (as P₂O₅) with a low moisture content (0.6%) and minimal free acid (0.1%), indicating strong agronomic value and storage stability. This study represents one of the pioneering efforts to valorize Sri Lanka’s apatite through a novel, dual-purpose, and circular approach, recovering REEs while simultaneously producing high-quality fertilizer. Full article

Nylons 6,7, 8,7 and 10,7 have been synthesized by interfacial polycondensation and characterized. Thermal properties and thermally induced structural transitions have been evaluated to complement the reported data on nylon 4,7. Therefore, the complete even–odd series derived from pimelic acid is here fully characterized, in order to insist on their peculiar structural polymorphism. Real-time WAXD synchrotron experiments were conducted during heating, cooling and reheating processes. Basically, three structures were involved: a modified α-form, a distorted pseudohexagonal form and a pseudohexagonal form. The modified α-form was stable up to relatively low temperatures (i.e., lower than 140 °C), was mainly produced by solution crystallization and was progressively disfavored when the number of methylene groups of the diamine moiety increased. A progressive transition from the modified α-form to the distorted pseudohexagonal structure was observed during heating. Also, a continuous reverse transition was detected on cooling, although the yield on the modified α-form was low. A Brill transition towards a pseudohexagonal structure was observed in all cases. This transition was reversible, although with some hysteresis degree. Oriented fiber patterns corresponding to the distorted pseudohexagonal structure were obtained by melt stretching. In all cases, the 00l reflections appeared with a meridional orientation and indicated a shortening close to 0.05 nm/amide group with respect to the expected values for fully extended conformations. Full article

To improve the convective heat transfer in internal cooling channels of heavy-duty gas turbine blades, this study experimentally and numerically investigates the thermal performance of rectangular channels with hybrid pin-fins and micro V-ribs turbulators. The transient thermochromic liquid crystal (TLC) technique and ANSYS 2019 R3 (ICEM CFD 2019 R3, Fluent 2019 R3, CFD-Post 2019 R3) were employed under Reynolds numbers ranging from 10,000 to 50,000, with the numerical model rigorously validated against experimental data (the maximum RMSE is 2.5%). It is found that hybrid pin-fins and continuous V-ribs configuration exhibits the maximum heat transfer enhancement of 27.6%, with an average friction factor increase of 13.3% and 21.9% improvement in thermal performance factor (TPF) compared to the baseline pin-fin channel. In addition, compared to the baseline pin-fin channel, hybrid pin-fins and broken V-ribs configuration exhibits average heat transfer enhancement (Nu/Nu0) of 24.4%, an average friction factor increase of 7.2% and 22.5% improvement across the investigated Reynolds number range (10,000~50,000) based on computational results. The synergistic effects of hybrid pin-fin and micro V-rib structures demonstrate superior coolant flow control, offering a promising solution for next-generation turbine blade cooling designs. This work provides actionable insights for high-efficiency gas turbine thermal management. Full article

This work presents a data-driven modeling framework for predicting image-derived crystal size metrics in seeded cooling crystallization using Long Short-Term Memory (LSTM) neural networks. The model leverages in situ microscopy data to predict square-weighted D10, D50, D90, and particle counts based solely on seed loading and temperature profiles, without requiring real-time supersaturation measurements. To enhance predictive power, engineered process descriptors—including temperature derivatives and integrals—were incorporated as dynamic features. Experimental validation was performed using creatine monohydrate crystallization from aqueous solution, with LSTM models trained on a diverse dataset encompassing variable seed loadings and cooling profiles. The feature-engineered LSTM model consistently outperformed its non-engineered counterpart, particularly under nonlinear cooling conditions where crystallization dynamics were the most complex. This approach offers a practical alternative to mechanistic models and spectroscopic process analytical technology (PAT) tools by enabling accurate prediction of chord length distribution (CLD) metrics from routinely collected data. The framework is easily transferable to other crystallization systems and provides a low-complexity, high-accuracy tool for accelerating lab-scale crystallization development. Full article

A high-pressure torsion (HPT) with a number of revolutions (n) of up to 10 and an advanced method of accumulative HPT (AccHPT), n = 10 with subsequent post-deformation annealing (PDA) at 500 and 600 °C, were applied to a biodegradable Fe-30Mn-5Si (wt.%) alloy. The effect of HPT, AccHPT and AccHPT with PDA on the microstructure, phase composition, microhardness and electrochemical behavior in Hanks’ solution was studied. HPT with n = 1 and 5 resulted in forming a mixed submicrocrystalline (SMCS) and nanocrystalline (NCS)structure, while HPT, n = 10 and AccHPT, n = 10 resulted in a predominant NCS with grain/subgrain sizes of 15–100 nm and 5–40 nm, respectively. PDA after AccHPT resulted in a mixture of SMCS and NCS. HPT, n = 5, n = 10 and AccHPT, n = 10 led to a transition from a two-phase (γ-austenite and ε-martensite) state after reference quenching, and HPT, n = 1 to a single-phase state (stress-induced and deformed ε-martensite), while the AccHPT, n = 10 with PDA results in a two-phase state of γ-austenite and cooling-induced ε-martensite, similarly to reference heat treatment (RHT). The increase in n resulted in the microhardness increasing up to its maximum after AccHPT, followed by a slight decrease after PDA. HPT and AccHPT led the biodegradation rate to decrease as compared to the initial state. PDA after AccHPT at 500 and 600 °C resulted in a two-phase state corresponding to an elevated biodegradation rate without significant material softening. The observed electrochemical behavior features are explained by changes in a combination of the phase state and the overall level of crystal lattice distortion. Full article

This research examines the influence of ammonium (NH₄⁺) impurities on the kinetic behavior, activation energy, crystal structure, morphology, and purity of cobalt sulfate hexahydrate using the cooling crystallization method. Characterization results indicate that ammonium at all concentrations affects the crystallization process, with a minimum concentration required to alter crystal characteristics. At ammonium concentrations up to 3.75 g/L, the crystal growth rate decreases, while activation energy increases. Furthermore, the crystal structure does not change, and crystal purity decreases by approximately 0.2%. This decline is insignificant and tends to stagnate, suggesting a maximum adsorption limit of impurities onto the crystal. At ammonium concentrations of 5 g/L, the crystal growth rate increases, and activation energy decreases. This shift in behavior is caused by the formation of Tutton’s salt, (NH₄)₂Co(SO₄)₂·6H₂O, which significantly reduces crystal purity by 1%. Additionally, the presence of ammonium does not alter the crystal shape. Full article

Compounds of the general composition A₂B^IB^IIIX₆ with a double perovskite (elpasolite) structure are currently considered as an alternative to lead halide perovskites APbX₃ in electronics and photovoltaics due to their greater compositional flexibility and low toxicity. One such alternative is the recently synthesized double perovskite Cs₂AgNaBiBr₆ and a number of various substituted compounds. The close values of the radii of silver and sodium cations make tuning the optoelectronic properties of the double perovskite via the substitution of Ag⁺ by Na⁺ promising if the formation of the substitution solid solution Cs₂Ag_1−xNa_xBiBr₆ takes place. We explored different possible routes for the synthesis of this class of materials, including solid-phase or melt crystallization ampoule syntheses. Varying heating temperature and duration and using standard cooling processing or a quenching-like process, we demonstrate the instability of Cs₂NaBiBr₆ and Na-substituted compounds Cs_2−xNa_xAgBiBr₆ in the temperature range of 300–650 °C. It is worth noting that the formation of Cs₂Ag_1−xNa_xBiBr₆ solid solutions by a solid-phase method is more favorable. Full article

Impurities significantly constrain the production of high-purity magnesium sulfate crystals, essential for advanced magnesium-based materials. Sodium–magnesium co-precipitation affects the crystals’ purity and surface smoothness, with NaCl embedding into crystal surfaces during cooling crystallization in the MgSO₄-NaCl-H₂O system. Trace impurities, however, inhibit NaCl adhesion, alter SO₄²⁻ coordination structures, and enhance the purity and morphology of MgSO₄·6H₂O crystals. Adding 300 mmol/L K₂SO₄ reduces sodium content in crystals from 0.57% to 0.03% and surface roughness from 2.76 nm to 0.415 nm. The binding energies of Na⁺ on MgSO₄·6H₂O crystal planes are lower than those of impurity ions, which compete for active growth sites and prevent Na⁺ nucleation. This finding challenges the assumption that higher-purity solutions yield higher-purity crystals. Full article

The Bridgman method for single-crystal growth enables the formation of crystals at the lower end of the molten material by cooling it under a precisely controlled temperature gradient. This makes it particularly suitable for producing high-quality single-crystal materials. Over the years, the Bridgman technique has become widely adopted for growing single crystals of semiconductors, oxides, sulfides, fluorides, as well as various optoelectronic, magnetic, and piezoelectric materials. Recently, there has been growing interest in metal halide materials, with the growth of high-quality metal halide single crystals emerging as a major focus for both the scientific community and industry. However, traditional solution-based single-crystal growth methods have several limitations, such as slow growth rates, inconsistent crystal quality, challenges in solvent selection, and difficulties in controlling saturation levels. These issues present significant obstacles, particularly when large, defect-free, high-quality single crystals are needed for certain high-performance materials. As a result, the Bridgman method has emerged as an effective solution to overcome these challenges. This review provides an overview of various categories of metal halide single-crystal systems grown using the Bridgman method in recent years. The systems are classified based on their dimensionality into three-dimensional, two-dimensional, and zero-dimensional metal halide structures. Furthermore, we highlight novel metal halide single crystals developed through the Bridgman technique. Additionally, we offer a brief introduction to the structures, properties, and applications of these single crystals, underscoring the crucial role of the Bridgman method in advancing research in this field. Full article

Tracking the microstructural evolution during high-pressure die casting of Al-Si alloys is challenging due to the rapid solidification, varying thermal conditions, and severe turbulence. The process involves a transition from slower cooling in the shot sleeve to rapid cooling in the die cavity, resulting in a bimodal dendritic microstructure and nucleation of new finer dendrite arms on fragmented externally solidified crystals. In this study, a two-dimensional phase-field model was employed to investigate the solidification behaviour of a hypoeutectic Al-7% Si alloy during high-pressure die casting. The model is based on thermodynamic formulations that account for temperature changes due to phase transformation heat, thermal boundary conditions, and solute diffusion in both liquid and solid phases. To replicate the observed bimodal microstructure, solid–liquid interface properties such as thickness, energy, and mobility were systematically varied to reflect the transition from the shot sleeve to the die cavity. The results demonstrated the model’s ability to capture the growth of dendrites under shot sleeve conditions and nucleation and development of new dendrite arms under the rapid cooling conditions of the die cavity. Full article

Treating the surfaces of dental implants in an alkaline medium allows us to obtain microstructures of sodium titanate crystals that favor the appearance of apatite in the physiological environment, producing osteoconductive surfaces. In this research, 385 discs made of titanium used in dental implants underwent different NaOH treatments with a 6M concentration at 600 °C and cooling rates of 20, 50, 75, and 115 °C/h. Using high-resolution electron microscopy, the microstructures were observed, and the different crystal sizes were determined and compared with control samples (those without biomimetic treatment). Roughness, wettability, surface energy and the sodium content of the surface were determined. The different surfaces were cultured with human osteoblastic cells; cell adhesion was determined at 3 and 14 days, and the degree of mineralization was determined at 14 days via alkaline phosphatase levels. Variations in the microstructure and size of sodium titanate crystals in NaOH solutions rich (1 g/L) or low in calcium (approximately 100 ppm) were determined. The results show that as the cooling rate increases, the size of the crystals decreases (from 0.4 μm to 0.8 μm) except for the case of 115 °C/h, when the rate is too fast for crystalline nucleation to occur on the surface of the titanium. The thermochemical treatment does not influence the roughness or the cooling rate since a Sa of 0.21 μm is maintained. However, the presence of titanate causes a decrease in the contact angle from 70° to 42° and, in turn, causes an increase in the total surface energy from 35 to 49.5 mJ/m², with the polar component standing out in this energy increase. No variations were observed in the thermochemical treatments in the presence of sodium, which was around 1200 ppm. It was observed that as the size of the crystals decreases, cell adhesion increases at 3 days and decreases at 14 days. This is because finer crystals on the surface are already in the mineralization process, as demonstrated using the level of alkaline phosphatase that is maximal for the cooling rate of 75 °C/h. It was possible to confirm that the variations in the concentrated NaOH solutions with different calcium contents did not affect the crystal sizes or the microstructure of the surface. This research makes it possible to obtain dental implants with different mineralization speeds depending on the cooling rate applied. Full article