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Search Results (5,934)

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Keywords = powder compositions

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26 pages, 1979 KB  
Article
Composite Catalysts Based on Manganese Carbonate Ore for Environmental Ozone Decomposition and Decolourization of Malachite Green Dye
by Katerina Zaharieva, Rositsa Titorenkova, Vladislav Kostov-Kytin, Petya Karakashkova, Iliyana Yordanova, Petya Todorova and Liliya Tsvetanova
Environments 2026, 13(1), 11; https://doi.org/10.3390/environments13010011 - 24 Dec 2025
Abstract
Environmental pollution from ozone and wastewaters containing dyes from various industries is an important problem for humanity. In this study, novel composite catalysts based on manganese carbonate ore from the Obrochishte deposit, Bulgaria, were used successfully in two environmentally relevant catalytic processes—the ozone [...] Read more.
Environmental pollution from ozone and wastewaters containing dyes from various industries is an important problem for humanity. In this study, novel composite catalysts based on manganese carbonate ore from the Obrochishte deposit, Bulgaria, were used successfully in two environmentally relevant catalytic processes—the ozone decomposition and photocatalytic decolourization of Malachite Green (MG) dye under UV illumination. Manganese carbonate ore/NiO, manganese oxides, and silver-containing composites were synthesized via co-precipitation, followed by calcination at 500 °C or hydrothermal treatment at 160 °C, and then thermal treatment. The phase and elemental composition, structure, morphology, and textural characteristics of the obtained composites were investigated using powder X-ray diffraction analysis, wavelength-dispersive X-ray fluorescence, Fourier-transform infrared spectroscopy, scanning electron microscopy, nitrogen adsorption–desorption isotherms, and the BET method. The materials exhibit a mesoporous structure. The results established that the thermally treated MnCO3 ore/NiO, manganese oxides, and Ag-containing composites demonstrate a higher catalytic efficiency for the removal of ozone (85%, 93%, and 99%) in comparison with hydrothermally treated analogues—79%, 66%, and 98%, respectively. The thermally treated manganese carbonate ore/silver-containing composite exhibits the highest photocatalytic ability (83% degree of decolourization of MG dye) compared to the other investigated catalysts. Full article
19 pages, 1664 KB  
Article
Comparative Molecular Docking, Molecular Dynamics and Adsorption–Release Analysis of Calcium Fructoborate and Alendronate Salts on Hydroxyapatite and Hydroxyapatite–Titanium Implants
by Diana-Maria Trasca, Ion Dorin Pluta, Carmen Sirbulet, Renata Maria Varut, Cristina Elena Singer, Denisa Preoteasa and George Alin Stoica
Biomedicines 2026, 14(1), 44; https://doi.org/10.3390/biomedicines14010044 (registering DOI) - 24 Dec 2025
Abstract
Background/Objectives: Hydroxyapatite (HAp)-based implants and HAp–titanium (HApTi) composites are widely used in orthopedic and dental applications, but their long-term success is limited by peri-implant bone loss. Local delivery of osteoactive molecules from implant surfaces may enhance osseointegration and reduce periprosthetic osteolysis. This study [...] Read more.
Background/Objectives: Hydroxyapatite (HAp)-based implants and HAp–titanium (HApTi) composites are widely used in orthopedic and dental applications, but their long-term success is limited by peri-implant bone loss. Local delivery of osteoactive molecules from implant surfaces may enhance osseointegration and reduce periprosthetic osteolysis. This study combined in silico modeling and experimental assays to compare calcium fructoborate (CaFb), sodium alendronate, and calcium alendronate as functionalization agents for HAp and HApTi implants. Methods: Molecular docking (AutoDock 4.2.6) and 100 ns molecular dynamics (MD) simulations (AMBER14 force field, SPC water model) were performed to characterize ligand–substrate interactions and to calculate binding free energies (ΔG_binding) and root mean square deviation (RMSD) values for ligand–HAp/HApTi complexes. HAp and HApTi discs obtained by powder metallurgy were subsequently functionalized by surface adsorption with CaFb or alendronate salts. The amount of adsorbed ligand was determined gravimetrically, and in vitro release profiles were quantified by HPTLC–MS for CaFb and by HPLC after FMOC derivatization for alendronates. Results: CaFb–HAp and CaFb–HApTi complexes showed the lowest binding free energies (−1.31 and −1.63 kcal/mol, respectively), indicating spontaneous and stable interactions. For HAp-based complexes, the mean ligand RMSD values over 100 ns were 0.27 ± 0.17 nm for sodium alendronate, 0.72 ± 0.28 nm for calcium alendronate (range 0.35–1.10 nm), and 0.21 ± 0.19 nm for CaFb (range 0.15–0.40 nm). For HApTi-based complexes, the corresponding RMSD values were 0.30 ± 0.15 nm for sodium alendronate, 0.72 ± 0.38 nm for calcium alendronate and 0.26 ± 0.14 nm for CaFb. These distributions indicate that CaFb and sodium alendronate maintain relatively stable binding poses, whereas calcium alendronate shows larger conformational fluctuations, consistent with its less favorable binding energies. Experimentally, CaFb exhibited the greatest chemisorbed amount and percentage on both HAp and HApTi, followed by sodium and calcium alendronate. HApTi supported higher loadings than HAp for all ligands. Release studies demonstrated a pronounced burst and rapid plateau for both alendronate salts, whereas CaFb displayed a slower initial release followed by a prolonged, quasi-linear liberation over 14 days. Conclusions: The convergence between in silico and adsorption–release data highlights CaFb as the most promising candidate among the tested ligands for long-term functionalization of HAp and HApTi surfaces. Its stronger and more stable binding, higher loading capacity and more sustained release profile suggest that CaFb-coated HApTi implants may provide a favorable basis for future in vitro and in vivo studies aimed at improving osseointegration and mitigating periprosthetic osteolysis, although direct evidence for osteolysis prevention was not obtained in the present work. Full article
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22 pages, 8102 KB  
Article
Wetting and Interaction of Titanium Melt with Calcium Titanate
by Axaule Mamaeva, Alexander Panichkin, Bagdaulet Kenzhaliyev, Alma Uskenbayeva, Marzhan Chukmanova, Balzhan Kshibekova and Zhassulan Alibekov
Materials 2026, 19(1), 72; https://doi.org/10.3390/ma19010072 - 24 Dec 2025
Abstract
This study presents the results of a study of the reaction interaction and contact angle during contact between a titanium melt and a calcium metatitanate substrate. It is shown that at temperatures slightly above the melting point, the titanium melt poorly wets the [...] Read more.
This study presents the results of a study of the reaction interaction and contact angle during contact between a titanium melt and a calcium metatitanate substrate. It is shown that at temperatures slightly above the melting point, the titanium melt poorly wets the CaTiO3 substrate surface. The contact angle and the onset temperature of active reaction vary depending on the fractional composition of the CaTiO3 powders from which the substrates are made and their porosity. Under isothermal holding conditions below the onset temperature of active reaction, the contact angle changes insignificantly. At the onset temperature of the reaction interaction, after a short stabilization period of the contact angle, the reaction leads to rapid penetration of the molten droplet into the depth of the CaTiO3 substrate and, in some cases, to the expulsion of a Ca-Ti-O liquid phase from the reaction zone. The interaction of titanium melt with calcium titanate is accompanied by a series of physicochemical reactions associated with the reaction interaction, which intensifies with increasing temperature and causes the restoration of calcium to a metallic state and the dissolution of oxygen in the titanium melt, as well as the formation of a liquid Ca-Ti-O layer in the transition zone. Full article
(This article belongs to the Section Metals and Alloys)
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12 pages, 1186 KB  
Article
Three-Dimensional Chiral Metal–Organic Frameworks: Synthesis and Structural Transformations
by Vadim A. Dubskikh, Anna A. Lysova, Denis G. Samsonenko, Konstantin A. Kovalenko, Danil N. Dybtsev and Vladimir P. Fedin
Nanomaterials 2026, 16(1), 22; https://doi.org/10.3390/nano16010022 - 24 Dec 2025
Abstract
Four new porous homochiral metal–organic frameworks (MOFs), [M2(camph)2(bpa)]∙Solv (M = Co(II), Ni(II), Cu(II) and Zn(II)), based on (+)-camphoric acid (H2camph) and 1,2-bis(4-pyridyl)ethane (bpa) were synthesized and characterized. The crystal structures of [Ni2(camph)2(bpa)] and [...] Read more.
Four new porous homochiral metal–organic frameworks (MOFs), [M2(camph)2(bpa)]∙Solv (M = Co(II), Ni(II), Cu(II) and Zn(II)), based on (+)-camphoric acid (H2camph) and 1,2-bis(4-pyridyl)ethane (bpa) were synthesized and characterized. The crystal structures of [Ni2(camph)2(bpa)] and [Zn2(camph)2(bpa)] were established by single-crystal X-ray diffraction analysis. Powder X-ray data prove the phase purity and isostructural nature of all four compounds. The thermal stability of [M2(camph)2(bpa)] was found to depend on the electronic configuration, as well as on the redox properties of the metal cation, and varied from 225 °C (M = Zn2+) to 375 °C (M = Ni2+). The reversible, solvent-induced sponge-like dynamics of the coordination frameworks was thoroughly investigated. Changes in the positions of reflexes, related to the length of the flexible bpa linker, were observed by powder XRD, pointing to transitions between an open-framework phase and a squeezed, non-porous phase in a crystal-to-crystal manner, while the integrity and connectivity of the coordination network were maintained. Size-selective adsorption from a benzene–cyclohexane 1:1 mixture on [Zn2(camph)2(bpa)] was studied by 1H NMR analysis. The benzene-favorable composition of guest molecules (C6H6:C6H12 = 5:1) occluded within the host crystalline sponge revealed a preferable adsorption affinity towards smaller benzene compared with larger cyclohexane. High framework stability in various solvents, as well as successful molecular separation in the liquid state, validates the potential utilization of chiral porous metal(II) camphorate MOFs in important stereoselective applications. Full article
(This article belongs to the Section Inorganic Materials and Metal-Organic Frameworks)
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20 pages, 2564 KB  
Article
Effects of Synthetic Fibers and Rubber Powder from ELTs on the Rheology of Mineral Filler–Bitumen Compositions
by Krzysztof Maciejewski, Witalij Zankowicz, Anna Chomicz-Kowalska and Przemysław Zaprzalski
Materials 2026, 19(1), 52; https://doi.org/10.3390/ma19010052 - 23 Dec 2025
Abstract
This study investigates the influence of synthetic fibers and rubber powder derived from end-of-life tires (ELTs) on the rheological behavior of asphalt mastics composed of paving-grade bitumen and mineral filler. Nine asphalt mastic formulations were prepared with varying fiber and rubber contents, reflecting [...] Read more.
This study investigates the influence of synthetic fibers and rubber powder derived from end-of-life tires (ELTs) on the rheological behavior of asphalt mastics composed of paving-grade bitumen and mineral filler. Nine asphalt mastic formulations were prepared with varying fiber and rubber contents, reflecting the composition of stone mastic asphalt mixtures. Dynamic shear rheometer tests were conducted to assess dynamic stiffness modulus, phase angle, non-recoverable creep compliance, and elastic recovery. The results demonstrated that ELT-derived additives significantly enhanced high-temperature stiffness and elasticity, while maintaining satisfactory viscoelastic balance at lower temperatures. Synergistic effects between fibers and rubber were observed, improving both non-recoverable compliance and percent recovery, particularly at elevated shear stresses. Prolonged exposure to production temperatures (175 °C) confirmed the thermal stability of the modified mastics, with the most notable performance gains occurring during the first hour of heating. Based on the findings, it was concluded that ELT-based fiber–rubber additives can improve high-temperature performance of asphalt mastics without negative effects in intermediate and, possibly, also low service temperatures. This permits expanding the use cases for these kinds of additives beyond the role of inert stabilizers in stone mastic asphalt to an active modifier for extending asphalt mix performance. Full article
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20 pages, 2327 KB  
Article
Research on a Polyolefin Composite Modifier for High-Temperature and Heavy-Duty Pavement and Performance of Its Modified Asphalt
by Runduo Ding, Xianhe Wang, Wei Wang, Haoran Wang, Huaxin Chen and Yanjun Zhang
Polymers 2026, 18(1), 26; https://doi.org/10.3390/polym18010026 - 22 Dec 2025
Abstract
To address the challenges of rutting and performance balance in asphalt pavements under high-temperature and heavy-load conditions, a novel polyolefin composite modifier (PCM-H) was developed from waste tire rubber powder, recycled ethylene vinyl acetate (EVA), acrylonitrile butadiene styrene (ABS), petroleum resin, and polymer [...] Read more.
To address the challenges of rutting and performance balance in asphalt pavements under high-temperature and heavy-load conditions, a novel polyolefin composite modifier (PCM-H) was developed from waste tire rubber powder, recycled ethylene vinyl acetate (EVA), acrylonitrile butadiene styrene (ABS), petroleum resin, and polymer additives. The chemical characteristics, thermal stability, and compatibility mechanisms of PCM-H were compared with those of two commercial modifiers (PCM-1 and PCM-2) using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). PCM-H exhibited superior compatibility and thermal stability. In contrast, PCM-2 tends to crystallize and precipitate within the 180–200 °C range, which is detrimental to the stability of the composite system. At an optimal dosage of 10 wt% in styrene–butadiene–styrene (SBS) modified asphalt, PCM-H formed a uniform dispersion and, through crosslinking reactions, established a three-dimensional network structure. Subsequently, the performance of composite modified asphalts, prepared with each of the three modifiers at their respective optimal dosages, was evaluated comparatively. Performance evaluations demonstrated that all polyolefin-modified asphalts significantly outperformed the conventional SBS modified asphalt. The PCM-H modified asphalt (PCM-H MA) exhibited the most superior performance, achieving a performance grade (PG) exceeding 94 °C, along with exceptional high-temperature elasticity and creep resistance, superior low-temperature cracking resistance, and enhanced fatigue healing capability. The results indicated that the crosslinked network structure effectively enhances asphalt cohesion, thereby providing a synergistic improvement in both high- and low-temperature performance. This study provides an effective solution and theoretical basis for developing high-performance pavement materials resistant to high temperatures and heavy loads conditions. Full article
(This article belongs to the Special Issue Polymer Materials for Pavement Applications)
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21 pages, 4466 KB  
Article
Biogenic Fabrication of Ag-NPs@Hydroxyapatite from Goat Bone Waste: A Sustainable Route for Photocatalytic and Antioxidant Applications
by Ahmed Hamad Alanazi, Ali Atta, Hallouma Bilel, Riyadh F. Halawani, Fahed A. Aloufi, Amnah Salem Al Zbedy and Amr Mohammad Nassar
Inorganics 2026, 14(1), 2; https://doi.org/10.3390/inorganics14010002 - 22 Dec 2025
Viewed by 39
Abstract
In this study, we present a new, facile, and eco-friendly approach to the synthesis of silver nanoparticles using an aqueous extract obtained from wasted goat bone, which acted as a reducing and stabilizing agent. Hydroxyapatite (GHAP) derived from the same biogenic source was [...] Read more.
In this study, we present a new, facile, and eco-friendly approach to the synthesis of silver nanoparticles using an aqueous extract obtained from wasted goat bone, which acted as a reducing and stabilizing agent. Hydroxyapatite (GHAP) derived from the same biogenic source was then added to the Ag-NPs solution, resulting in the formation of a nanocomposite (Ag@GHAP). Biogenic GHAP and Ag@GHAP have been characterized using Fourier transform infrared spectroscopy (FTIR), dynamic light scattering (DLS), zeta potential, scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD), confirming the formation of crystalline GHAP with well-dispersed silver nanoparticles. According to AFM studies, the Ag@GHAP composite exhibits a higher surface roughness alteration than GHAP. XRD revealed that the crystalline sizes of GHAP and Ag@GHAP are 10.2 and 15.6 nm, respectively. Zeta potential showed that GHAP and Ag@GHAP possessed values of −12.4 and −11.7 mV, respectively. Ag@GHAP showed a promising performance in photocatalysis and antioxidant applications as compared to GHAP. The energy band gap (Eg) values are 5.1 eV and 4.5 eV for GHAP and Ag@GHAP, respectively. Ag@GHAP showed photocatalytic activity during the degradation of methylene blue dye (5 ppm) under solar irradiation with a removal efficiency of 99.15% in 100 min at the optimum conditions. The antioxidant activity of GHAP and Ag@GHAP was determined using the DPPH method. The results showed enhanced antioxidant activity of a silver decorated sample with IC50 values of 36.83 and 2.95 mg/mL, respectively. As a result, the Ag@GHAP composite is a promising candidate in environmental treatment and scavenging of free radicals. Full article
(This article belongs to the Special Issue Nanocomposites for Photocatalysis, 2nd Edition)
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15 pages, 5598 KB  
Article
Highly Printable Fe3Al Intermetallic Alloy
by Aliakbar Emdadi, Yitong Yang, Joanna Szyndler, Felix Jensch, Gökhan Ertugrul, Michael Tovar, Sebastian Härtel and Sabine Weiß
Metals 2026, 16(1), 5; https://doi.org/10.3390/met16010005 - 20 Dec 2025
Viewed by 107
Abstract
Intermetallic Fe3Al-based alloys reinforced with Laves-phase precipitates are emerging as potential replacements for conventional high-alloy steels and possibly polycrystalline Ni-based superalloys in structural applications up to 700 °C. Their impressive mechanical properties, however, are offset by limited fabricability and poor machinability [...] Read more.
Intermetallic Fe3Al-based alloys reinforced with Laves-phase precipitates are emerging as potential replacements for conventional high-alloy steels and possibly polycrystalline Ni-based superalloys in structural applications up to 700 °C. Their impressive mechanical properties, however, are offset by limited fabricability and poor machinability due to their severe brittleness. High tool wear during finish-machining, which is still required for components such as turbine blades, remains a key barrier to their broader adoption. In contrast to conventional manufacturing routes, additive manufacturing offers a viable solution by enabling near-net-shape manufacturing of difficult-to-machine iron aluminides. In the present study, laser powder bed fusion was used to produce an Fe-25Al-1.5Ta intermetallic containing strengthening Laves-phase precipitates, and the porosity, microstructure and phase composition were characterized as a function of the process parameters. The results showed that preheating the build plate to 650 °C effectively suppressed delamination and macrocrack formation, even though noticeable cracking still occurred at the high scan speed of 1000 mm/s. X-ray tomography revealed that samples fabricated with a lower scan speed (500 mm/s) and a higher layer thickness (0.1 mm) contained larger, irregularly shaped pores, whereas specimens printed at the same volumetric energy density (40 J/mm3) but with different parameter sets exhibited smaller fractions of predominantly spherical pores. All samples contained mostly elongated grains that were either oriented close to <001> relative to the build direction or largely texture-free. X-ray diffraction confirmed the presence of Fe3Al and C14-type (Fe, Al)2Ta Laves phase in all samples. Hardness values fell within a narrow range (378–398 HV10), with only a slight reduction in the specimen exhibiting higher porosity. Full article
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14 pages, 468 KB  
Article
Physicochemical Properties and Sensory Evaluation of Yanggaeng with Alternative Sweeteners and Cissus quadrangularis Powder
by Minseo Cho, Jisu Lee, Hyunsoo Jang, Miae Doo, Jung-Heun Ha and Hyun-Joo Lee
Appl. Sci. 2026, 16(1), 44; https://doi.org/10.3390/app16010044 - 19 Dec 2025
Viewed by 60
Abstract
This study investigated the effects of alternative sweeteners, allulose (AL), stevia (ST), and xylose (XY), on the physicochemical, antioxidant, textural, and sensory properties of Yanggaeng fortified with Cissus quadrangularis (CQ) powder. Replacing sucrose (SU) with alternative sweeteners significantly affected the proximate composition and [...] Read more.
This study investigated the effects of alternative sweeteners, allulose (AL), stevia (ST), and xylose (XY), on the physicochemical, antioxidant, textural, and sensory properties of Yanggaeng fortified with Cissus quadrangularis (CQ) powder. Replacing sucrose (SU) with alternative sweeteners significantly affected the proximate composition and overall quality of Yanggaeng. Formulations containing AL, ST, or XY exhibited higher moisture retention and lower carbohydrate content than those containing SU. Colorimetric analysis revealed that Yanggaeng prepared with alternative sweeteners developed a darker coloration and greater browning intensity, likely due to enhanced Maillard reactions during heating. Among the sweeteners tested, AL showed the highest total phenolic content and relatively high antioxidant activity, suggesting potential functional advantages beyond sweetness. Textural analysis indicated that ST enhanced gel strength and elasticity even under high-moisture conditions, whereas AL produced a softer texture, which may be desirable for products requiring reduced firmness. Although consumer preference scores did not differ significantly across most sensory attributes, both ST and AL achieved acceptable overall profiles, with sweetness ratings comparable to those of SU. These findings suggest that CQ-enriched Yanggaeng sweetened with alternative sweeteners can be developed as a promising low-sugar dessert option without compromising quality or consumer acceptability. Full article
(This article belongs to the Special Issue Assessments of Functional Food)
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23 pages, 611 KB  
Article
Comparative Study of Lipid Quality from Edible Insect Powders and Selected Cereal Flours Under Storage Conditions
by Zdzisław Domiszewski, Arkadiusz Szpicer, Sylwia Mierzejewska, Iwona Wojtasik-Kalinowska, Weronika Bińkowska, Karolina Maziarz and Joanna Piepiórka-Stepuk
Appl. Sci. 2026, 16(1), 13; https://doi.org/10.3390/app16010013 - 19 Dec 2025
Viewed by 107
Abstract
The increasing demand for sustainable food requires the development of raw materials and products that provide not only high-quality proteins but also valuable lipids. The aim of this study was to compare the lipid quality of insect powders with that of selected cereal [...] Read more.
The increasing demand for sustainable food requires the development of raw materials and products that provide not only high-quality proteins but also valuable lipids. The aim of this study was to compare the lipid quality of insect powders with that of selected cereal flours (millet, oat, and rice) during four months of storage at room temperature. To simulate increased oxidative conditions, the packages were filled only halfway, thereby increasing oxygen availability. Lipids were extracted using the Bligh–Dyer method, and their oxidation status was assessed based on peroxide value (PV), p-anisidine value (p-AsV), and the total oxidation (Totox) index. Fatty acid composition, antioxidant activity, and oxidative stability were determined using differential scanning calorimetry (DSC). Directly after purchase, none of the analyzed flours or insect powders exceeded a PV of 10 meq O2/kg lipids or a p-AsV of 20. After four months of storage, lipid oxidation increased in all samples, with changes ranging from 4.6% to 30%, depending on the parameter analyzed. Lipids extracted from insect powders consistently showed significantly higher oxidation levels than those from cereal flours. The proportion of PUFAs in the lipids of the flours ranged from 36.40% to 64.21%, whereas in insect powders it ranged from 30.01% to 37.29%. After storage, only minor changes in PUFA content were observed, and these did not indicate advanced destructive oxidative degradation. Overall, the lipids present in the analyzed flours demonstrated favorable nutritional quality indices, including AI (0.10–0.48), h/H (2.23–10.47), and TI (0.22–1.14). The results indicate that insect powders can serve as a valuable source of fatty acids; however, their susceptibility to lipid oxidation necessitates careful consideration during processing and storage. Full article
(This article belongs to the Special Issue Advanced Food Processing Technologies and Food Quality: 2nd Edition)
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17 pages, 4693 KB  
Article
From Waste to Cathode: A Comparative Evaluation of Sol–Gel and Co-Precipitation Routes for Closed-Loop Recycling of Lithium-Ion Battery Cathodes
by Alexandra Kosenko, Konstantin Pushnitsa, Pavel Novikov and Anatoliy A. Popovich
Batteries 2025, 11(12), 466; https://doi.org/10.3390/batteries11120466 - 18 Dec 2025
Viewed by 145
Abstract
The exponential growth of lithium-ion batteries (LIBs) in electric vehicles and energy storage systems has amplified the urgent need for sustainable recycling strategies. Conventional pyrometallurgical and hydrometallurgical methods for LIB recycling are energy-intensive, chemically demanding, and fail to preserve the structural integrity of [...] Read more.
The exponential growth of lithium-ion batteries (LIBs) in electric vehicles and energy storage systems has amplified the urgent need for sustainable recycling strategies. Conventional pyrometallurgical and hydrometallurgical methods for LIB recycling are energy-intensive, chemically demanding, and fail to preserve the structural integrity of cath-ode materials. Closed-loop recycling, in contrast, enables the recovery of layered oxides with minimal processing steps, reducing environmental footprint and supporting a circular economy. This study provides a systematic comparison of two regeneration approaches—sol–gel synthesis and hydroxide co-precipitation—for closed-loop recycling of layered NCM (LiNixCoyMnzO2) cathode materials recovered from spent LIBs. Spent cells were mechani-cally processed and leached using malic acid to recover Ni, Co, Mn, which were subsequently used to synthesize NCM622 cathode powders. The regenerated materials were characterized using SEM/EDX, XRD, and electrochemical testing in CR2032 coin cells. Both methods successfully produced phase-pure layered oxides with the R-3m structure, with distinct differences in structural ordering and electrochemical behavior. The sol–gel-derived NCM622 displayed higher crystallinity and reduced cation mixing, evidenced by an I(003)/I(104) ratio of 1.896 compared to 1.720 for the co-precipitated sample, and delivered a high initial discharge capacity of 170 mAh/g at 0.1 C. However, it exhibited significant capacity fade, retaining only 60 mAh/g after 40 cycles. In contrast, the co-precipitation route produced hierarchical porous spherical agglomerates that offered superior cycling stability, maintaining ~150 mAh/g after 40 cycles with lower polarization (ΔEp = 0.16 V). Both materials demonstrated electrochemical performance comparable to commercial NCM. Overall, hydroxide co-precipitation emerged as the most industrially viable method due to scalable processing, compositional robustness, and improved long-term stability of regenerated cathodes. This work highlights the critical influence of synthesis route selection in LIB closed-loop recycling and provides a technological framework for industrial recovery of high-value NCM cathode materials. Full article
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18 pages, 6466 KB  
Article
Copper-Mediated Leaching of LiCoO2 in H3PO4: Kinetics and Residue Transformation
by Dragana Medić, Ivan Đorđević, Maja Nujkić, Vladan Nedelkovski, Aleksandra Papludis, Stefan Đorđievski and Nataša Gajić
Chemistry 2025, 7(6), 203; https://doi.org/10.3390/chemistry7060203 - 17 Dec 2025
Viewed by 120
Abstract
The recycling of spent lithium-ion batteries (LIBs) requires efficient and sustainable methods for recovering critical metals. In this study, the leaching behavior of LiCoO2 cathode material obtained from spent LIBs was investigated in phosphoric acid, using copper powder recovered from waste LIBs [...] Read more.
The recycling of spent lithium-ion batteries (LIBs) requires efficient and sustainable methods for recovering critical metals. In this study, the leaching behavior of LiCoO2 cathode material obtained from spent LIBs was investigated in phosphoric acid, using copper powder recovered from waste LIBs as a reducing agent. Leaching experiments were conducted under various conditions (temperature, solid-to-liquid ratio, agitation rate) and compared with systems without copper. In the absence of copper, lithium and cobalt, recoveries after 30 min were approximately 77% and 23%, respectively. The addition of copper significantly enhanced leaching, achieving >96% recovery for both metals at 80 °C, with most extraction occurring within the first 30 min. Kinetic analysis using the shrinking core model indicated a mixed-control mechanism involving both surface chemical reaction and product layer diffusion. The calculated activation energies were 20.2 kJ·mol−1 for lithium and 16.1 kJ·mol−1 for cobalt. Solid residues were characterized by X-ray diffraction (XRD) and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS). XRD results revealed that the composition of the residues varied with leaching temperature: Co3O4 was consistently detected, whereas Cu8(PO3OH)2(PO4)4·7H2O appeared only when leaching was performed above 50 °C. Thermodynamic calculations supported the reductive role of copper and provided insight into possible reaction pathways. These findings confirm the effectiveness of copper-mediated leaching in phosphoric acid and demonstrate that temperature strongly influences residue phase evolution, thereby offering valuable guidance for the design of sustainable LIB recycling processes. Full article
(This article belongs to the Section Green and Environmental Chemistry)
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19 pages, 5492 KB  
Article
Influence of Printing Orientation on Tensile Strength and Surface Characterization of a Steel-Powder-Reinforced Thermoplastic Composite Manufactured by FDM Technology
by Paweł Szczygieł and Krystyna Radoń-Kobus
Materials 2025, 18(24), 5656; https://doi.org/10.3390/ma18245656 - 17 Dec 2025
Viewed by 193
Abstract
This study presents results on a thermoplastic polymer composite containing 95 wt.% steel powder, processed into samples using Fused Deposition Modeling (FDM) technology. Such a high filler loading exceeds the values commonly reported in the literature. Samples were printed with different build orientations [...] Read more.
This study presents results on a thermoplastic polymer composite containing 95 wt.% steel powder, processed into samples using Fused Deposition Modeling (FDM) technology. Such a high filler loading exceeds the values commonly reported in the literature. Samples were printed with different build orientations (0° and 90°) to evaluate the influence of printing direction on the tensile behavior of the material. Tensile tests were conducted to determine the effect of printing orientation on the composite’s strength. Additionally, surface structure analysis was performed using a contact profilometer, and wettability was evaluated by measuring the contact angle with a tensiometer. Dimensional measurements were also carried out using a digital caliper. The obtained results allowed determination of the relationship between printing orientation and the tensile and surface-related properties of the analyzed composite material. Full article
(This article belongs to the Special Issue 3D & 4D Printing—Metrological Problems)
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16 pages, 6543 KB  
Article
Phase Evolution by Annealing of Mechanically Activated Ni, Mn, and Sn Elemental Powders Mixture with the Ni2MnSn Heusler Compound Ratio
by Florin Popa, Andra Teodora Anastasia Man, Traian Florin Marinca and Ionel Chicinaș
Materials 2025, 18(24), 5642; https://doi.org/10.3390/ma18245642 - 15 Dec 2025
Viewed by 230
Abstract
A Ni2MnSn Heusler alloy composition of elemental powders was high-energy milled for a short time for powder activation. The milling times were chosen to be 1 and 4 h to study how mechanical mixing triggers the phase formation in the Ni-Mn-Sn [...] Read more.
A Ni2MnSn Heusler alloy composition of elemental powders was high-energy milled for a short time for powder activation. The milling times were chosen to be 1 and 4 h to study how mechanical mixing triggers the phase formation in the Ni-Mn-Sn system. After milling, the samples were analyzed by differential scanning calorimetry and the thermal events of Ni2MnSn L21 phase formation were investigated. The milled samples were compacted at 700 MPa and annealed in a vacuum for 10 min at different temperatures (230 °C, 330 °C, and 600 °C). The annealing temperatures were chosen to emphasize the activated powders’ behavior before and after Sn melting on L21 Structure formation. Using X-ray diffraction and Rietveld analysis, the phase quantity was computed, showing that the largest L21 phase (63%) can be obtained from the elemental powder mixture due to Sn melting during the annealing. For milled samples, a Ni3Sn4 phase was obtained by milling, and by annealing this phase, along with the remaining element, it reacts to form a Ni2MnSn L21 phase and a Ni3Sn2 phase. The microstructural evolution of the phase was illustrated by backscattering electron microscopy for milled and subsequent annealed samples, and, by image analysis, a correlation of the phase’s amount was performed. The results of the image analysis were correlated with the X-ray diffraction patterns. Full article
(This article belongs to the Special Issue Powder Metallurgy and Advanced Materials)
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Article
Comparative Efficacy of Latent Fingerprint Development Techniques in Varying Aquatic Environments of Rajasthan’s Shekhawati Region: Analyzing the Impact of Water Composition and Surface Interactions
by Abhaya Gupta, Mridu Sharma, Varsha Dabas, Kavita Kumari and Sameer Saharan
Forensic Sci. 2025, 5(4), 79; https://doi.org/10.3390/forensicsci5040079 - 15 Dec 2025
Viewed by 126
Abstract
Background/Objectives: The recovery of latent fingerprints from submerged evidence remains a critical challenge in forensic science, as ridge details deteriorate rapidly once under water. This study aims to compare the effectiveness of three established fingerprint development techniques—cyanoacrylate fuming, small particle reagent (SPR), and [...] Read more.
Background/Objectives: The recovery of latent fingerprints from submerged evidence remains a critical challenge in forensic science, as ridge details deteriorate rapidly once under water. This study aims to compare the effectiveness of three established fingerprint development techniques—cyanoacrylate fuming, small particle reagent (SPR), and powder dusting—on non-porous substrates (glass slides and stainless steel blades) immersed in different water types representative of Rajasthan’s Shekhawati region. The objective was to evaluate the influence of water composition and immersion duration on the quality and reproducibility of developed prints. Methods: Experiments were conducted under controlled laboratory conditions. Fingerprints were submerged in hard water, mineral water, and rainwater for durations of 10 min, 1 day, 5 days, and 10 days. Each condition was replicated three times. Developed fingerprints were assessed for ridge clarity using a five-point scoring scale, and the results were statistically analyzed using Chi-Square and correlation tests. Results: Cyanoacrylate fuming consistently produced the highest quality ridge detail across all submersion periods, particularly in mineral and rainwater environments. SPR exhibited moderate effectiveness, while powder dusting showed limited performance under all conditions. Statistical analysis indicated that fingerprint quality was significantly affected by water composition, substrate type, and immersion duration (p < 0.001). Conclusions: The study highlights that fingerprint recovery from submerged non-porous evidence depends strongly on water chemistry and exposure time. Cyanoacrylate fuming is confirmed as the most reliable method, while environmental variables such as ion content and water hardness play decisive roles in fingerprint preservation and visualization. Full article
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