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Keywords = melt-recrystallization

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20 pages, 24137 KB  
Article
Effect of WAAM Process Parameters on Structure and Mechanical Properties of Low-Carbon Steel Thin Walls
by Margarita Klimova, Konstantin Nasonovskiy, Dmitrii Mukin, Ilya Astakhov, Artem Voropaev, Alexey Evstifeev, Alexey Silkin, Rudolf Korsmik and Nikita Stepanov
J. Manuf. Mater. Process. 2026, 10(4), 144; https://doi.org/10.3390/jmmp10040144 - 21 Apr 2026
Viewed by 589
Abstract
Wire Arc Additive Manufacturing (WAAM) has emerged as a promising additive manufacturing technique due to its high deposition rate and low material cost. WAAM is increasingly adopted in various industries for the production of large-scale metal components, yet optimizing productivity without sacrificing mechanical [...] Read more.
Wire Arc Additive Manufacturing (WAAM) has emerged as a promising additive manufacturing technique due to its high deposition rate and low material cost. WAAM is increasingly adopted in various industries for the production of large-scale metal components, yet optimizing productivity without sacrificing mechanical integrity remains a critical challenge, particularly for low-carbon steels. This study systematically investigates the influence of key WAAM parameters—welding current (100–350 A) and travel speed (5–30 mm/s) on the deposition stability, microstructure, and mechanical properties of thin walls made of low-carbon Fe–0.09 C–1.10 Cr–1.47 Mn–0.59 Si–0.56 Mo–0.11 Ni–0.23 V steel. A stable processing window for defect-free wall fabrication was established for currents of 100–250 A, while higher currents of 300–350 A resulted in melt pool instability and geometrical distortions due to excessive heat input. Microstructural characterization revealed a dual-phase structure consisting of allotriomorphic ferrite (ALF) and acicular ferrite (AF) in all samples. The microstructural evolution was critically governed by variations in the cooling time in the critical temperature range of 800 °C to 500 °C (t8/5) within the thermal cycles, a direct consequence of the heat input quantified through volumetric energy density. Low heat input at 100 A, 5 mm/s promoted a microstructure with minimal ALF fraction of ~10%, whereas high heat input at 350 A, 30 mm/s induced significant ferrite recrystallization and coarsening, increasing ALF fraction to ~55%. These microstructural changes directly affected mechanical properties: YS/UTS decreased from 512 MPa/668 MPa to 401 MPa/602 MPa, respectively. Concurrently, the deposition rate increased substantially from ~1.6 kg/h to ~6.3 kg/h. The results demonstrate a critical trade-off between productivity and mechanical performance, providing a practical framework for parameter selection in WAAM-fabricated low-carbon steel components. Full article
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12 pages, 4376 KB  
Article
Laser-Induced In Situ Crystallization of Hybrid Manganese(II) Bromide Arrays for X-Ray Imaging
by Zhaoran Lin, Guansheng Xing, Wei Wang and Bing Chen
Sensors 2026, 26(8), 2373; https://doi.org/10.3390/s26082373 - 12 Apr 2026
Viewed by 490
Abstract
Hybrid metal-halide scintillators are promising for X-ray imaging, but direct fabrication of patterned arrays with high spatial precision remains challenging. Here, we report a laser-induced in situ crystallization strategy for constructing pixelated scintillator arrays from a melt-processable manganese(II) bromide glass precursor, (BuTPP)2 [...] Read more.
Hybrid metal-halide scintillators are promising for X-ray imaging, but direct fabrication of patterned arrays with high spatial precision remains challenging. Here, we report a laser-induced in situ crystallization strategy for constructing pixelated scintillator arrays from a melt-processable manganese(II) bromide glass precursor, (BuTPP)2MnBr4 (BuTPP+, butyltriphenylphosphonium). The (BuTPP)2MnBr4 undergoes low-temperature glass formation and can be selectively recrystallized under femtosecond laser irradiation, enabling programmable spatial patterning. Structural analyses confirm the recovery of the crystalline phase after laser writing, while photophysical measurements show markedly enhanced photoluminescence and radioluminescence compared with the glassy state. Benefiting from efficient X-ray-to-light conversion and precise array definition, the patterned scintillators exhibit a high light yield of 24,600 photons MeV−1, an X-ray detection limit of 4.89 µGyair s−1, and a spatial resolution of 10 lp mm−1. This work establishes the laser-induced in situ crystallization strategy as an effective route to integrated hybrid scintillator arrays and offers a versatile platform for customizable and low-temperature processed X-ray imaging devices for imaging uses. Full article
(This article belongs to the Special Issue Next-Generation X-Ray Detection and Imaging Materials and Devices)
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18 pages, 3663 KB  
Article
Cooling–Heating Phase Behavior of Hypersaline Culture Media Studied by DSC and Cryomicroscopy
by Olena Bobrova, Nadiia Chernobai, Nadiia Shevchenko, Viktor Husak and Alexander Shyichuk
Water 2026, 18(6), 738; https://doi.org/10.3390/w18060738 - 21 Mar 2026
Viewed by 427
Abstract
Hypersaline culture media used for cultivation of Dunaliella salina represent complex multicomponent aqueous systems whose cooling–heating phase behavior remains insufficiently characterized. In this study, the thermal transitions of two biologically relevant hypersaline media (Artari and Ramaraj) were investigated using differential scanning calorimetry (DSC) [...] Read more.
Hypersaline culture media used for cultivation of Dunaliella salina represent complex multicomponent aqueous systems whose cooling–heating phase behavior remains insufficiently characterized. In this study, the thermal transitions of two biologically relevant hypersaline media (Artari and Ramaraj) were investigated using differential scanning calorimetry (DSC) and cryomicroscopy. The media were examined at NaCl concentrations of 1.5, 2.0, and 4.0 M, corresponding to moderate to highly concentrated brine conditions comparable to natural salt lakes and evaporative basins. DSC analysis revealed pronounced salinity-dependent suppression of ice crystallization and modification of melting transitions relative to classical NaCl–water systems. Increased NaCl concentration reduced recrystallization during heating and shifted peak temperatures, indicating kinetic and compositional effects in the unfrozen fraction. Rapid cooling promoted formation of partially amorphous phases, consistent with limited vitrification in highly concentrated media. Cryomicroscopy directly confirmed changes in ice morphology, nucleation density, and crystal growth dynamics under varying salinity and thermal histories. The combined calorimetric and microscopic approach demonstrates that complete hypersaline cultivation media exhibit phase behavior that cannot be fully extrapolated from simplified binary systems. These findings provide new insight into the physicochemical stability of multicomponent brines during cooling and highlight the critical role of salinity and thermal history in controlling crystallization pathways in hypersaline aqueous environments. Full article
(This article belongs to the Section Water, Agriculture and Aquaculture)
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22 pages, 4150 KB  
Article
Closed-Loop Chemical Recycling of Polylactide via Glycolysis: From Water-Soluble Oligomers to High-Purity Lactide
by Gadir Aliev, Roman Toms, Matvey Marinichev, Daniil Ismailov, Kirill Kirshanov and Alexander Gervald
Polymers 2026, 18(5), 655; https://doi.org/10.3390/polym18050655 - 7 Mar 2026
Viewed by 758
Abstract
Polylactide (PLA) has become widely adopted across biomedical, packaging, and manufacturing sectors due to its biodegradability and renewable sourcing. However, the rapid growth in PLA consumption has created urgent challenges related to waste management and the cleaning of processing equipment. This study investigates [...] Read more.
Polylactide (PLA) has become widely adopted across biomedical, packaging, and manufacturing sectors due to its biodegradability and renewable sourcing. However, the rapid growth in PLA consumption has created urgent challenges related to waste management and the cleaning of processing equipment. This study investigates glycolysis as a promising chemical depolymerization pathway for PLA recycling and in situ reactor cleaning. A systematic analysis of four glycolysis agents (GA) (ethylene glycol, diethylene glycol, propylene glycol, and glycerol) was performed across molar PLA:GA ratios from 1:0.125 to 1:4 at 220 °C, targeting the efficient conversion of high-molecular-weight PLA (Mn ≈ 165 kDa) into low-molecular-weight oligomers. Gel permeation chromatography (GPC) demonstrated that propylene glycol exhibited the highest depolymerization efficiency, yielding oligomers with Mn as low as 200 g·mol−1 even at minimal glycolysis agent ratios, while glycerol produced hydroxyl-rich oligomers optimal for subsequent lactide synthesis. Hydroxyl value (HV) measurements showed excellent agreement with theoretical values (<5% deviation), allowing us to make an assumption about an approximate, close to near-quantitative con-version. Glycolysis products with Mw below 400 g·mol−1 displayed excellent water solubility, making them particularly attractive for reactor cleaning applications. Using glycerol-derived (GL) oligomers (PLA:GL = 1:0.25), purified L-lactide with a melting point of 98.1 °C and high purity (>99%) was obtained through thermocatalytic depolymerization and five recrystallization cycles, as confirmed by 1H nuclear magnetic resonance (1H NMR) and differential scanning calorimetry (DSC) analyses. The recovered lactide’s high purity renders it suitable for ring-opening polymerization, enabling closed-loop PLA recycling schemes. Overall, glycolysis emerges as a highly promising chemical recycling route complementary to hydrolysis and pyrolysis: propylene glycol maximizes depolymerization efficiency for cleaning applications, while glycerol optimizes oligomer functionality for lactide recovery and advanced material synthesis. Our results provide practical guidelines for selecting glycolysis agents and conditions for cleaning and recycling applications. Full article
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15 pages, 5266 KB  
Article
Tailoring a Heterogeneous Bimodal Structure for Superior Strength–Ductility Synergy in Dilute Mg-0.4Al-0.3Ca-0.2Mn-xSn Alloy: The Critical Role of Trace Sn Microalloying
by Guo Li, Jiahao Zhang, Li Sun, Xinyang Ge, Bin Li and Guobing Wei
Materials 2026, 19(3), 507; https://doi.org/10.3390/ma19030507 - 27 Jan 2026
Viewed by 487
Abstract
To achieve an optimal balance of mechanical properties in low-cost alloy systems, this study tailored a heterogeneous bimodal structure in dilute Mg-0.4Al-0.3Ca-0.2Mn-xSn alloys (x = 0, 0.1 wt.%) and systematically investigated the critical role of trace Sn microalloying during hot extrusion. Mg-0.4Al-0.3Ca-0.2Mn-xSn alloys [...] Read more.
To achieve an optimal balance of mechanical properties in low-cost alloy systems, this study tailored a heterogeneous bimodal structure in dilute Mg-0.4Al-0.3Ca-0.2Mn-xSn alloys (x = 0, 0.1 wt.%) and systematically investigated the critical role of trace Sn microalloying during hot extrusion. Mg-0.4Al-0.3Ca-0.2Mn-xSn alloys were fabricated via melting, homogenization, and subsequent hot extrusion at 320 °C. Trace Sn addition induced the formation of uniformly distributed CaMgSn phases within the homogenized matrix, facilitating a synergistic enhancement of strength and ductility. Specifically, the extruded alloys exhibited a characteristic bimodal grain structure consisting of coarse un-dynamic recrystallized (unDRXed) grains and fine dynamic recrystallized (DRXed) grains. Sn microalloying effectively refined the DRXed grains from 2.66 μm to 2.11 μm and significantly boosted the elongation (EL) from 12.9% to 26.3% while maintaining an Ultimate Tensile Strength (UTS) of 274 MPa. The Sn-containing secondary phases served as potent sites for particle-stimulated nucleation (PSN), thereby promoting the DRX process and reducing the texture intensity from 20.89 to 9.99. Overall, the superior strength-ductility synergy is primarily governed by the formation of the heterogeneous bimodal structure, where trace Sn facilitates grain refinement and texture weakening through PSN mechanisms, providing a robust strategy for the design of high-performance dilute magnesium alloys. Full article
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21 pages, 10212 KB  
Article
Numerical Investigation of Material Flow and Defect Formation in FRAM-6061 Al Alloy Ring Component Using CEL Simulation
by Yan Ji and Bin Yang
Materials 2026, 19(2), 236; https://doi.org/10.3390/ma19020236 - 7 Jan 2026
Viewed by 343
Abstract
In this study, a novel and efficient solid-state additive manufacturing technique, friction rolling additive manufacturing (FRAM), was employed to fabricate an aluminum alloy ring component, significantly reducing process complexity and mitigating solidification defects typical of melt-based techniques. However, previous studies on FRAM have [...] Read more.
In this study, a novel and efficient solid-state additive manufacturing technique, friction rolling additive manufacturing (FRAM), was employed to fabricate an aluminum alloy ring component, significantly reducing process complexity and mitigating solidification defects typical of melt-based techniques. However, previous studies on FRAM have primarily focused on the microstructural characteristics and mechanical properties of flat components, with limited attention paid to ring-shaped components. Owing to the unique geometric constraints imposed during the forming process, ring components exhibit markedly different microstructural evolution and defect formation mechanisms compared with flat counterparts, and these mechanisms remain insufficiently and systematically understood. To address this knowledge gap, the coupled Eulerian–Lagrangian (CEL) method was introduced for the first time to numerically simulate the temperature distribution and residual stress evolution during the FRAM process of ring-shaped components. In addition, tracer particles were incorporated into the simulations to analyze the material flow behavior, thereby systematically elucidating the forming behavior and microstructural evolution characteristics under geometric constraint conditions. Moreover, scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) were employed to systematically characterize the microstructural evolution and defect morphology. The CEL numerical simulations exhibited good consistency with the experimental observations, demonstrating the reliability and accuracy of the simulation method. The results showed that the peak temperatures were primarily concentrated at the advancing side of the rotation tool, and the temperature on the outer diameter side of the ring was consistently higher than that on the inner diameter side. The lack of shoulder friction on the inner side led to an increased heat dissipation rate, thereby resulting in higher residual stress compared to other regions. The particle analysis revealed that, due to ring geometry, material flow varied across radial regions, resulting in distinct microstructures. Further EBSD analysis revealed that, after the rotating tool passed, the material first developed a preferential orientation with {111} planes parallel to the shear direction, and with more layers, dynamic recrystallization produced an equiaxed grain structure. This study provides a theoretical basis and process reference for the application of the FRAM technique in the manufacturing of large ring components. Full article
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24 pages, 7874 KB  
Article
Experimental Study and Numerical Modeling of Inter-Pass Forging in Wire-Arc Additive Manufacturing of Inconel 718
by Oleg Yu. Smetannikov, Gleb L. Permyakov, Sergey D. Neulybin, Ivan P. Ovchinnikov, Alexander A. Oskolkov and Dmitriy N. Trushnikov
Materials 2026, 19(1), 182; https://doi.org/10.3390/ma19010182 - 4 Jan 2026
Cited by 1 | Viewed by 594
Abstract
Inter-pass forging with different degrees of deformation during WAAM of Inconel 718 specimens (single-stage, three passes; two-stage, six passes) was investigated. Macrostructural analysis of the specimens showed that inter-pass forging led to a recrystallized structure. Alternation of layers with different grain shapes (columnar [...] Read more.
Inter-pass forging with different degrees of deformation during WAAM of Inconel 718 specimens (single-stage, three passes; two-stage, six passes) was investigated. Macrostructural analysis of the specimens showed that inter-pass forging led to a recrystallized structure. Alternation of layers with different grain shapes (columnar and equiaxed) is observed throughout the height of the specimens. Increasing the number of passes improves the mechanical properties of the material (tensile strength, yield strength, microhardness). A finite element model of inter-pass forging was developed to determine the effect of inter-pass surface deformation during WAAM on the residual stress–strain state. The non-stationary formulation was replaced with a quasi-static one. Johnson–Cook material constants were obtained for the deposited Inconel 718 material, including the effect of forging. Verification of the mathematical model was performed using a wall (specimen 2) deposited with single-stage forging. The deviation between the simulation results and the experiment did not exceed 15%. It was found that the sequence and number of passes significantly affect residual strain and displacements but have little effect on residual stress. Numerical modeling showed that the depth of plastic deformation exceeds the melting depth when depositing the subsequent layer, ensuring the preservation and accumulation of the inter-pass forging effect throughout the deposition process. Full article
(This article belongs to the Section Manufacturing Processes and Systems)
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24 pages, 3342 KB  
Article
Effects of Grass Carp Antifreeze Peptide on Freeze-Thaw Characteristics and Structure of Wet Gluten Protein
by Meizhu Dang, Bing Huang, Yangyang Jia, Yuanyuan Shao, Xingxing Mei and Chunmei Li
Foods 2025, 14(24), 4336; https://doi.org/10.3390/foods14244336 - 16 Dec 2025
Cited by 1 | Viewed by 701
Abstract
This study uniquely explores the impact of a novel natural antifreeze peptide derived from grass carp (GCAFP) on the freeze–thaw characteristics and structural stability of wet gluten protein, providing new insights into the development of natural cryoprotectants for frozen foods. The effects of [...] Read more.
This study uniquely explores the impact of a novel natural antifreeze peptide derived from grass carp (GCAFP) on the freeze–thaw characteristics and structural stability of wet gluten protein, providing new insights into the development of natural cryoprotectants for frozen foods. The effects of GCAFP on the physicochemical and structural properties of gluten protein were investigated using differential scanning calorimetry (DSC), nuclear magnetic resonance imaging (NMR), rheology, and scanning electron microscopy (SEM). The results showed that the addition of 0.5% GCAFP significantly reduced the freezing temperature (Tf, from −8.50 ± 1.31 °C to −10.75 ± 2.49 °C) and expanded the melting temperature range (Tm,δ, from 3.60 ± 1.40 °C to 5.65 ± 0.12 °C), indicating improved freezing stability. After five weeks of frozen storage, the ice crystal melting enthalpy (ΔHm) of gluten protein in the GCAFP group increased by only 20.17 J/g, compared with 27.23 J/g in the control, representing a 6.35% reduction (p < 0.05). Similarly, after five freeze–thaw cycles, the freezable water fraction (Fw) and ΔHm were reduced by 5.19% and 1.55%, respectively, demonstrating that GCAFP inhibited water migration and ice recrystallization. Low-field NMR revealed that GCAFP maintained a higher proportion of bound water (T21) and decreased free water (T23), confirming its role in restricting water mobility. Rheological analysis showed that GCAFP preserved the viscoelasticity of gluten protein, maintaining higher storage (G′) and loss (G″) moduli than the control after five freeze–thaw cycles, thus mitigating the decline in network elasticity. Structural characterization indicated that GCAFP stabilized the α-helix and β-sheet contents, reduced glutenin macropolymer depolymerization from 24.85% to 18.95%, and strengthened hydrogen bonding within the protein matrix. Overall, GCAFP effectively protected wet gluten protein against ice crystal damage by maintaining water distribution, viscoelasticity, and secondary structure integrity, highlighting its potential as a natural antifreeze ingredient for frozen food applications. Full article
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13 pages, 34475 KB  
Article
Characteristics of Tungsten Prepared by Hot Pressing at High Pressure
by Jiří Matějíček, Monika Vilémová, Andrii Rednyk, Hynek Hadraba, Zdeněk Chlup, František Lukáč, Romain Génois and Jakub Klečka
Materials 2025, 18(23), 5265; https://doi.org/10.3390/ma18235265 - 21 Nov 2025
Viewed by 804
Abstract
Tungsten is a prime candidate material for the plasma-facing components of fusion reactors, thanks to its high melting point, high temperature strength, good thermal conductivity, high erosion resistance, etc. Yet, it has some limitations, mainly its brittle nature, difficulty of machining, and propensity [...] Read more.
Tungsten is a prime candidate material for the plasma-facing components of fusion reactors, thanks to its high melting point, high temperature strength, good thermal conductivity, high erosion resistance, etc. Yet, it has some limitations, mainly its brittle nature, difficulty of machining, and propensity to recrystallize at elevated temperatures. Among the approaches to the improvement of particular properties are alloying, dispersion strengthening, thermomechanical processing, and modifications to the sintering process. This study explores the possibility of combining fine powder size with ultra-high pressure to achieve significant densification at moderate temperatures during hot pressing. Two powder sizes and a range of temperatures from 1000 to 2000 °C were used, and their effects were observed. The resulting tungsten compacts were characterized for their microstructure, density, and mechanical and thermal properties. The high pressure enabled substantial densification already at relatively low temperatures, thanks to the plastic deformation of the powder particles. A significant degree of sintering, as manifested by the microstructural and property evolution, occurred however only at higher temperatures. The compacts exhibited brittleness, calling for further optimization of the method. Full article
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21 pages, 8013 KB  
Article
Analysis of Microstructure Evolution, Mechanical Properties, and Strengthening Mechanisms in Extruded 2014Al-GNP Composites
by Junjie Xiong, Shaolong Ma, Jinsheng Zhou and Yu Zhou
Metals 2025, 15(11), 1213; https://doi.org/10.3390/met15111213 - 31 Oct 2025
Viewed by 560
Abstract
A 2014Al matrix composite reinforced with 0.8 wt.% graphene nanoplatelets (GNPs) was prepared by pre-dispersion and ultrasonic melt casting. Subsequently, the as-cast 2014Al-GNP composite was subjected to hot extrusion under different parameters, followed by a comparative analysis of the microstructure and properties of [...] Read more.
A 2014Al matrix composite reinforced with 0.8 wt.% graphene nanoplatelets (GNPs) was prepared by pre-dispersion and ultrasonic melt casting. Subsequently, the as-cast 2014Al-GNP composite was subjected to hot extrusion under different parameters, followed by a comparative analysis of the microstructure and properties of the various alloys. Microstructure and phase composition of the prepared samples were characterized using OM, SEM, EDS, EBSD and TEM inspections. The results indicate that the addition of GNPs effectively promoted the refinement of the as-cast matrix alloy microstructure, while hot extrusion with appropriate parameters further refined the microstructure of the as-cast matrix alloy. At an extrusion ratio of 16, the Al2Cu, Al2CuMg, and GNPs in the microstructure displayed a band-like distribution along the extrusion direction, with reduced size and enhanced uniformity. Concurrently, the dislocation density and Kernel Average Misorientation (KAM) values of the composite increased significantly, dynamic recrystallization intensified, and the texture was further enhanced. The tensile strength reached 572.1 MPa, hardness was 369.6 HV, and elongation was 11.9%, representing improvements of 89.0%, 92.0%, and 142.9%, respectively, compared to the as-cast matrix alloy. Fracture surface analysis exhibited brittle fracture characteristics in the matrix alloy, while the extruded composite with optimal parameters displayed distinct ductile fracture features. In the extruded aluminum matrix composite, the interface between GNPs and the matrix was clean, with mutual diffusion of Al and C atoms, achieving an excellent interfacial bonding state. The significant enhancement in mechanical properties of the extruded alloy was primarily attributed to grain refinement strengthening, dislocation strengthening, and load transfer strengthening by GNPs. Full article
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21 pages, 14113 KB  
Article
Microstructure and Properties of Sm2O3 Micro-Dispersed Tungsten-Based Alloy and Its Sintering Evolution
by Song Ye, Ping Wang, Zhiqiang Cui, Ningfei Zhang, Yuhao Wang and Zhenyi Huang
Materials 2025, 18(21), 4973; https://doi.org/10.3390/ma18214973 - 31 Oct 2025
Viewed by 637
Abstract
Tungsten (W) is regarded as the most promising plasma-facing material in thermonuclear fusion reactors due to its excellent properties, such as high strength, a high melting point, and a low sputtering rate. However, its low-temperature brittleness, recrystallization embrittlement, and irradiation embrittlement seriously limit [...] Read more.
Tungsten (W) is regarded as the most promising plasma-facing material in thermonuclear fusion reactors due to its excellent properties, such as high strength, a high melting point, and a low sputtering rate. However, its low-temperature brittleness, recrystallization embrittlement, and irradiation embrittlement seriously limit the practical application of W. In this research, the properties of tungsten-based materials were improved by introducing second phases into W. Core–shell composite powders with W particles as core and Sm(OH)3 thin films as shell were prepared by electroless plating, and sintered by spark plasma sintering (SPS) to obtain bulk. After sintering, the Sm(OH)3 shell transformed into the Sm2O3 phase with a different size, mainly distributed at W grain boundaries. The average size of W grains in the composite material was smaller than that of pure W sintered bulk due to the pinning of W grain boundaries by Sm2O3, while the porosity of the composite is reduced. Compared with pure W sintered bulk, the composites exhibited better mechanical properties and radiation resistance; although the thermal conductivity decreased somewhat, it still maintained a high level. With the increase in sintering temperature and pressure, the evolution of core–shell powders during the sintering process could be simplified into six stages, which occurred approximately in sequence. Full article
(This article belongs to the Section Metals and Alloys)
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15 pages, 2257 KB  
Article
The Development and Characterization of Layered Pellets Containing a Combination of Amorphized Amlodipine Besylate and Hydrochlorothiazide Using a High-Shear Granulator
by Azza A. K. Mahmoud, Krisztina Ludasi, Dorina Gabriella Dobó, Dániel Sebők, Ákos Kukovecz, Viktória Hornok, Kadosa Sajdik, Tamás Szabó, Tamás Sovány, Géza Regdon and Katalin Kristó
Pharmaceuticals 2025, 18(10), 1496; https://doi.org/10.3390/ph18101496 - 5 Oct 2025
Viewed by 1114
Abstract
Background/Objective: The high-shear granulator is considered an effective piece of equipment for layering pelletization because it enhances drug amorphization and improves drug dissolution. This study aimed to apply a high-shear granulator to prepare layered pellets containing a combination of hydrochlorothiazide and amlodipine besylate [...] Read more.
Background/Objective: The high-shear granulator is considered an effective piece of equipment for layering pelletization because it enhances drug amorphization and improves drug dissolution. This study aimed to apply a high-shear granulator to prepare layered pellets containing a combination of hydrochlorothiazide and amlodipine besylate with improved physicochemical properties. Methods: Different molar ratios (2:1, 1:1, and 1:2) of the hydrochlorothiazide and amlodipine besylate mixture were deposited on the surface of the inert spheres of the microcrystalline cellulose (MCC) core by the mechanical effect of the high impeller speed. The resulting layered pellets were characterized using X-ray powder diffractometry (XRPD) and differential scanning calorimetry (DSC) to estimate the degree of the drug amorphization, and consequently a dissolution test was performed to determine the degree of the enhancement of the percentage of release. Additionally, micro-computed tomography (micro-CT) and a texture analyzer were used to determine the morphological characteristics and hardness of the resulting pellets, and then a stability study was performed. Results: On the basis of the micro-CT images, the MCC core was successfully loaded with a uniform layer of the drug combination at the pellet surface, which exhibited higher diameters than pure cellets. Furthermore, the drug combination in layered pellets was partially amorphized with a lower crystallinity percentage, a lower intensity, a broadening of the hydrochlorothiazide melting peak, and a higher cumulative release of both drugs with good stability, except pellets with a molar ratio of 1:2 that were recrystallized with a higher crystallinity percentage of 79.9%. Conclusions: Modifying the physical form and dissolution behavior of the hydrochlorothiazide and amlodipine besylate combination was achieved by single-step layering pelletization. Full article
(This article belongs to the Section Pharmaceutical Technology)
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33 pages, 6726 KB  
Review
Recent Techniques to Improve Amorphous Dispersion Performance with Quality Design, Physicochemical Monitoring, Molecular Simulation, and Machine Learning
by Hari Prasad Bhatta, Hyo-Kyung Han, Ravi Maharjan and Seong Hoon Jeong
Pharmaceutics 2025, 17(10), 1249; https://doi.org/10.3390/pharmaceutics17101249 - 24 Sep 2025
Cited by 5 | Viewed by 3818
Abstract
Amorphous solid dispersions (ASDs) represent a promising formulation strategy for improving the solubility and bioavailability of poorly water-soluble drugs, a major challenge in pharmaceutical development. This review provides a comprehensive analysis of the physicochemical principles underlying ASD stability, with a focus on drug–polymer [...] Read more.
Amorphous solid dispersions (ASDs) represent a promising formulation strategy for improving the solubility and bioavailability of poorly water-soluble drugs, a major challenge in pharmaceutical development. This review provides a comprehensive analysis of the physicochemical principles underlying ASD stability, with a focus on drug–polymer miscibility, molecular mobility, and thermodynamic properties. The main manufacturing techniques including hot-melt extrusion, spray drying, and KinetiSol® dispersing are discussed for their impact on formulation homogeneity and scalability. Recent advances in excipient selection, molecular modeling, and in silico predictive approaches have transformed ASD design, reducing dependence on traditional trial-and-error methods. Furthermore, machine learning and artificial intelligence (AI)-based computational platforms are reshaping formulation strategies by enabling accurate predictions of drug–polymer interactions and physical stability. Advanced characterization methods such as solid-state NMR, IR, and dielectric spectroscopy provide valuable insights into phase separation and recrystallization. Despite these technological innovations, ensuring long-term stability and maintaining supersaturation remain significant challenges for ASDs. Integrated formulation design frameworks, including PBPK modeling and accelerated stability testing, offer potential solutions to address these issues. Future research should emphasize interdisciplinary collaboration, leveraging computational advancements together with experimental validation to refine formulation strategies and accelerate clinical translation. The scientists can unlock the full therapeutic potential with emerging technologies and a data-driven approach. Full article
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17 pages, 3511 KB  
Article
In Vitro Digestibility of Starch Gel in Cooked Rice Prepared with Thermo-Reversible Short-Chain Glucan Aggregates (SCGAs)
by So-Eun Yoon, Sang-Jin Ye, Min-Seok Kim, Seon-Min Oh, Jae-Sung Shin, Ji-Eun Bae, Hyun-Wook Choi and Moo Yeol Baik
Gels 2025, 11(9), 701; https://doi.org/10.3390/gels11090701 - 2 Sep 2025
Cited by 1 | Viewed by 1488
Abstract
To enhance the food applicability of SCGAs, this study investigated the thermo-reversible behavior of SCGAs after cooking and evaluated the in vitro digestibility of starch gels in a real food system, i.e., cooked rice. For the thermo-reversibility of SCGAs, the DSC double-helical melting [...] Read more.
To enhance the food applicability of SCGAs, this study investigated the thermo-reversible behavior of SCGAs after cooking and evaluated the in vitro digestibility of starch gels in a real food system, i.e., cooked rice. For the thermo-reversibility of SCGAs, the DSC double-helical melting enthalpy and relative crystallinity of SCGAs decreased after cooking but increased upon cooling. In addition, cooling SCGAs to 30 °C after cooking led to increased slowly digestible starch (SDS) and RS contents associated with a lower glycemic index. These results indicate that cooked SCGAs undergo rapid recrystallization during the cooling process and maintain their resistance to digestion. For application in a real food system, RS content increased with the increasing amount of SCGAs. Furthermore, when the cooked rice was frozen and thawed, the RS content further increased due to the retrogradation of both cooked rice and SCGAs during storage. The appearance and textural characteristics of the cooked rice were not affected by adding SCGAs up to 20%. Nevertheless, the addition of SCGAs to the rice positively increased SDS and RS contents as well as reducing the estimated glycemic index (eGI), indicating low digestibility of starch gels. Consequently, SCGAs exhibited unique thermo-reversibility and low digestibility, which could be applied to real food systems. Overall, this study highlights the potential of SCGAs as a functional material for a wide range of thermally processed starch gel foods. Full article
(This article belongs to the Special Issue Food Gels: Structures, Properties and Applications)
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11 pages, 2162 KB  
Article
Synthesis and Purification of [Eu(BA)4(pip)] Rare-Earth Molecular Crystals
by Xiangtai Xi, Wenli Fan, Jun Huang, Haoyang Chen, Huan Chen, Zhengkun Fu and Zhenglong Zhang
Nanomaterials 2025, 15(17), 1348; https://doi.org/10.3390/nano15171348 - 2 Sep 2025
Viewed by 1236
Abstract
Europium mononuclear complexes are able to form organic molecular crystals by aggregation of molecules through non-covalent bonding interactions. These crystals have many unique optical properties. However, this kind of crystal still faces some difficulties and challenges in the process of research and application, [...] Read more.
Europium mononuclear complexes are able to form organic molecular crystals by aggregation of molecules through non-covalent bonding interactions. These crystals have many unique optical properties. However, this kind of crystal still faces some difficulties and challenges in the process of research and application, such as the high difficulty of synthesis and purification, and the difficulty of spectral property modulation. In this work, an europium-containing rare-earth molecular crystal material [Eu(BA)4(pip)], was prepared via a solvothermal method. It is characterized by low melting point, low polarity, stable structure, high luminescence intensity, and has the potential for the preparation of quantum optical devices. After that, optimized the structure of the molecular crystals by petroleum ether solvent. Through the recrystallization process, a uniform and continuous film was formed, which resulted with a more regular surface morphology, and the changes in the optimized crystal structure had an effect on the europium ion electron-leap energy level, the fluorescence emission spectra also showed higher fluorescence resolving ratio. This study particular emphasis on enhancing the quality of [Eu(BA)4(pip)] molecular crystals and investigating their impact on their spectral properties. Full article
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