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Search Results (2,673)

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Keywords = crystalline stabilization

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26 pages, 5455 KiB  
Article
Features of Thermal Stabilization of PVC Modified with Microstructured Titanium Phosphate
by Irina N. Vikhareva, Anton Abramian, Dragan Manojlović and Oleg Bol’shakov
Polymers 2025, 17(15), 2140; https://doi.org/10.3390/polym17152140 - 5 Aug 2025
Abstract
Poly(vinyl chloride) (PVC) undergoes thermal degradation during processing and operation, which necessitates the use of effective thermal stabilizers. The purpose of this work is to comprehensively evaluate the potential of new hierarchically structured titanium phosphates (TiP) with controlled morphology as thermal stabilizers of [...] Read more.
Poly(vinyl chloride) (PVC) undergoes thermal degradation during processing and operation, which necessitates the use of effective thermal stabilizers. The purpose of this work is to comprehensively evaluate the potential of new hierarchically structured titanium phosphates (TiP) with controlled morphology as thermal stabilizers of plasticized PVC, focusing on the effect of morphology and Ti/P ratio on their stabilizing efficiency. The thermal stability of the compositions was studied by thermogravimetric analysis (TGA) in both inert (Ar) and oxidizing (air) atmospheres. The effect of TiP concentration and its synergy with industrial stabilizers was analyzed. An assessment of the key degradation parameters is given: the temperature of degradation onset, the rate of decomposition, exothermic effects, and the carbon residue yield. In an inert environment, TiPMSI/TiPMSII microspheres demonstrated an optimal balance by increasing the temperature of degradation onset and the residual yield while suppressing the rate of decomposition. In an oxidizing environment, TiPR rods and TiPMSII microspheres provided maximum stability, enhancing resistance to degradation onset and reducing the degradation rate by 10–15%. Key factors of effectiveness include ordered morphology (spheres, rods); the Ti-deficient Ti/P ratio (~0.86), which enhances HCl binding; and crystallinity. The stabilization mechanism of titanium phosphates is attributed to their high affinity for hydrogen chloride (HCl), which catalyzes PVC chain scission, a catalyst for the destruction of the PVC chain. The unique microstructure of titanium phosphate provides a high specific surface area and, as a result, greater activity in the HCl neutralization reaction. The formation of a sol–phosphate framework creates a barrier to heat and oxygen. An additional contribution comes from the inhibition of oxidative processes and the possible interaction with unstable chlorallyl groups in PVC macromolecules. Thus, hierarchically structured titanium phosphates have shown high potential as multifunctional PVC thermostabilizers for modern polymer materials. Potential applications include the development of environmentally friendly PVC formulations with partial or complete replacement of toxic stabilizers, the optimization of thermal stabilization for products used in aggressive environments, and the use of hierarchical TiP structures in flame-resistant and halogen-free PVC-based compositions. Full article
(This article belongs to the Section Polymer Processing and Engineering)
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25 pages, 13119 KiB  
Article
Spatial and Temporal Variability of C Stocks and Fertility Levels After Repeated Compost Additions: A Case Study in a Converted Mediterranean Perennial Cropland
by Arleen Rodríguez-Declet, Maria Teresa Rodinò, Salvatore Praticò, Antonio Gelsomino, Adamo Domenico Rombolà, Giuseppe Modica and Gaetano Messina
Soil Syst. 2025, 9(3), 86; https://doi.org/10.3390/soilsystems9030086 (registering DOI) - 4 Aug 2025
Abstract
Land use conversion to perennial cropland often degrades the soil structure and fertility, particularly under Mediterranean climatic conditions. This study assessed spatial and temporal dynamics of soil properties and tree responses to 3-year repeated mature compost additions in a citrus orchard. Digital soil [...] Read more.
Land use conversion to perennial cropland often degrades the soil structure and fertility, particularly under Mediterranean climatic conditions. This study assessed spatial and temporal dynamics of soil properties and tree responses to 3-year repeated mature compost additions in a citrus orchard. Digital soil mapping revealed strong baseline heterogeneity in texture, CEC, and Si pools. Compost application markedly increased total organic C and N levels, aggregate stability, and pH with noticeable changes after the first amendment, whereas a limited C storage potential was found following further additions. NDVI values of tree canopies monitored over a 3-year period showed significant time-dependent changes not correlated with the soil fertility variables, thus suggesting that multiple interrelated factors affect plant responses. The non-crystalline amorphous Si/total amorphous Si (iSi:Siamor) ratio is here proposed as a novel indicator of pedogenic alteration in disturbed agroecosystems. These findings highlight the importance of tailoring organic farming strategies to site-specific conditions and reinforce the value to combine C and Si pool analysis for long-term soil fertility assessment. Full article
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15 pages, 5007 KiB  
Article
In Situ Construction of Thiazole-Linked Covalent Organic Frameworks on Cu2O for High-Efficiency Photocatalytic Tetracycline Degradation
by Zhifang Jia, Tingxia Wang, Zhaoxia Wu, Shumaila Razzaque, Zhixiang Zhao, Jiaxuan Cai, Wenao Xie, Junli Wang, Qiang Zhao and Kewei Wang
Molecules 2025, 30(15), 3233; https://doi.org/10.3390/molecules30153233 - 1 Aug 2025
Viewed by 155
Abstract
The strategic construction of heterojunctions through a simple and efficient strategy is one of the most effective means to boost the photocatalytic activity of semiconductor materials. Herein, a thiazole-linked covalent organic framework (TZ-COF) with large surface area, well-ordered pore structure, and high stability [...] Read more.
The strategic construction of heterojunctions through a simple and efficient strategy is one of the most effective means to boost the photocatalytic activity of semiconductor materials. Herein, a thiazole-linked covalent organic framework (TZ-COF) with large surface area, well-ordered pore structure, and high stability was developed. To further boost photocatalytic activity, the TZ-COF was synthesized in situ on the surface of Cu2O through a simple multicomponent reaction, yielding an encapsulated composite material (Cu2O@TZ-COF-18). In this composite, the outermost COF endows the material with abundant redox active sites and mass transfer channels, while the innermost Cu2O exhibits unique photoelectric properties. Notably, the synthesized Cu2O@TZ-COF-18 was proven to have the heterojunction structure, which can efficiently restrain the recombination of photogenerated electron–hole pairs, thereby enhancing the photocatalytic performance. The photocatalytic degradation of tetracycline demonstrated that 3-Cu2O@TZ-COF-18 had the highest photocatalytic efficiency, with the removal rate of 96.3% within 70 min under visible light, which is better than that of pristine TZ-COF-18, Cu2O, the physical mixture of Cu2O and TZ-COF-18, and numerous reported COF-based composite materials. 3-Cu2O@TZ-COF-18 retained its original crystallinity and removal efficiency after five cycles in photodegradation reaction, displaying high stability and excellent cycle performance. Full article
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17 pages, 3877 KiB  
Article
Efficient Tetracycline Hydrochloride Degradation by Urchin-like Structured MoS2@CoFe2O4 Derived from Steel Pickling Sludge via Peroxymonosulfate Activation
by Jin Qi, Kai Zhu, Ming Li, Yucan Liu, Pingzhou Duan and Lihua Huang
Molecules 2025, 30(15), 3194; https://doi.org/10.3390/molecules30153194 - 30 Jul 2025
Viewed by 155
Abstract
Steel pickling sludge serves as a valuable iron source for synthesizing Fe-based catalysts in heterogeneous advanced oxidation processes (AOPs). Here, MoS2@CoFe2O4 catalyst derived from steel pickling sludge was prepared via a facile solvothermal approach and utilized to activate [...] Read more.
Steel pickling sludge serves as a valuable iron source for synthesizing Fe-based catalysts in heterogeneous advanced oxidation processes (AOPs). Here, MoS2@CoFe2O4 catalyst derived from steel pickling sludge was prepared via a facile solvothermal approach and utilized to activate peroxymonosulfate (PMS) for tetracycline hydrochloride (TCH) degradation. Comprehensive characterization using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) confirmed the supported microstructure, composition, and crystalline structure of the catalyst. Key operational parameters—including catalyst dosage, PMS concentration, and initial pH—were systematically optimized, achieving 81% degradation efficiency within 30 min. Quenching tests and EPR analysis revealed ∙SO4 as the primary oxidative species, while the catalyst maintained high stability and reusability across cycles. TCH degradation primarily occurs through hydroxylation, decarbonylation, ring-opening, and oxidation reactions. This study presents a cost-effective strategy for transforming steel pickling sludge into a high-performance Fe-based catalyst, demonstrating its potential for practical AOP applications. Full article
(This article belongs to the Section Nanochemistry)
16 pages, 1702 KiB  
Article
Does Salt Form Matter? A Pilot Randomized, Double-Blind, Crossover Pharmacokinetic Comparison of Crystalline and Regular Glucosamine Sulfate in Healthy Volunteers
by Chuck Chang, Afoke Ibi, Yiming Zhang, Min Du, Yoon Seok Roh, Robert O’Brien and Julia Solnier
Nutrients 2025, 17(15), 2491; https://doi.org/10.3390/nu17152491 - 30 Jul 2025
Viewed by 264
Abstract
Background: Crystalline glucosamine sulfate (cGS) claims to be a stabilized form of glucosamine sulfate with a defined crystalline structure intended to enhance chemical stability. It is proposed to offer pharmacokinetic advantages over regular glucosamine sulfate (rGS) which is stabilized with potassium or [...] Read more.
Background: Crystalline glucosamine sulfate (cGS) claims to be a stabilized form of glucosamine sulfate with a defined crystalline structure intended to enhance chemical stability. It is proposed to offer pharmacokinetic advantages over regular glucosamine sulfate (rGS) which is stabilized with potassium or sodium chloride. However, comparative human bioavailability data are limited. Since both forms dissociate in gastric fluid into constituent ions, the impact of cGS formulation on absorption remains uncertain. This pilot study aimed to compare the bioavailability of cGS and rGS using a randomized, double-blind, crossover design. Methods: Ten healthy adults received a single 1500 mg oral dose of either cGS or rGS with a 7-day washout between interventions. Capillary blood samples were collected over 24 h. Glucosamine and its metabolite concentrations were quantified by Liquid Chromatography-High Resolution Mass Spectrometry (LC-HRMS), and pharmacokinetic parameters—including maximum concentration (Cmax), time to reach Cmax (Tmax), and area under the curve (AUC)—were calculated. Results: Mean AUC0–24, Cmax, Tmax, and T½ values for glucosamine and glucosamine-6-sulfate (GlcN-6-S) were comparable between cGS and rGS. Although the AUC0–24 for glucosamine was modestly higher with rGS (18,300 ng·h/mL) than with cGS (12,900 ng·h/mL), the difference was not statistically significant (p = 0.136). GlcN-6-S exposure was also similar between formulations (rGS: 50,700 ng·h/mL; cGS: 50,600 ng·h/mL), with a geometric mean ratio of 1.39, a delayed Tmax (6–8 h) and longer half-life, consistent with its role as a downstream metabolite. N-acetylglucosamine levels remained stable, indicating potential homeostatic regulation. Conclusions: This pilot study found no significant pharmacokinetic advantage of cGS over rGS. These preliminary findings challenge claims of cGS’ pharmacokinetic superiority, although the small sample size limits definitive conclusions. Larger, adequately powered studies are needed to confirm these results. Full article
(This article belongs to the Special Issue Bone-Health-Promoting Bioactive Nutrition)
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17 pages, 4077 KiB  
Article
The Impact of Sm Promoter on the Catalytic Performance of Ni/Al2O3-SiO2 in Methane Partial Oxidation for Enhanced H2 Production
by Salwa B. Alreshaidan, Rasha S. A. Alanazi, Omalsad H. Odhah, Ahmed A. Ibrahim, Fekri Abdulraqeb Ahmed Ali, Naif Alarifi, Khaled M. Banabdwin, Sivalingam Ramesh and Ahmed S. Al-Fatesh
Catalysts 2025, 15(8), 721; https://doi.org/10.3390/catal15080721 (registering DOI) - 29 Jul 2025
Viewed by 319
Abstract
This study investigates the effects of samarium (Sm) promotion on the catalytic activity of 5 weight percent Ni catalysts for partial oxidation of methane (POM)-based hydrogen production supported on a Si-Al mixed oxide (10SiO2+90Al2O3) system. Several 5% [...] Read more.
This study investigates the effects of samarium (Sm) promotion on the catalytic activity of 5 weight percent Ni catalysts for partial oxidation of methane (POM)-based hydrogen production supported on a Si-Al mixed oxide (10SiO2+90Al2O3) system. Several 5% Ni-based catalysts supported on silica–alumina was used to test the POM at 600 °C. Sm additions ranged from 0 to 2 wt.%. Impregnation was used to create these catalysts, which were then calcined at 500 °C and examined using BET, H2-TPR, XRD, FTIR, TEM, Raman spectroscopy, and TGA methods. Methane conversion (57.85%) and hydrogen yield (56.89%) were greatly increased with an ideal Sm loading of 1 wt.%, indicating increased catalytic activity and stability. According to catalytic tests, 1 wt.% Sm produced high CH4 conversion and H2 production, as well as enhanced stability and resistance to carbon deposition. Nitrogen physisorption demonstrated a progressive decrease in pore volume and surface area with the addition of Sm, while maintaining mesoporosity. At moderate Sm loadings, H2-TPR and XRD analyses showed changes in crystallinity and increased NiO reducibility. Sm incorporation into the support and its impact on the ordering of carbon species were indicated by FTIR and Raman spectra. The optimal conditions to maximize H2 yield were successfully identified through optimization of the best catalyst, and there was good agreement between the theoretical predictions (87.563%) and actual results (88.39%). This displays how successfully the optimization approach achieves the intended outcome. Overall, this study demonstrates that the performance and durability of Ni-based catalysts for generating syngas through POM are greatly enhanced by the addition of a moderate amount of Sm, particularly 1 wt.%. Full article
(This article belongs to the Section Industrial Catalysis)
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18 pages, 3793 KiB  
Review
Research Progress on Vaterite Mineral and Its Synthetic Analogs
by Guoxi Sun, Xiuming Liu, Bin Lian and Shijie Wang
Minerals 2025, 15(8), 796; https://doi.org/10.3390/min15080796 - 29 Jul 2025
Viewed by 244
Abstract
As the most unstable crystalline form of calcium carbonate, vaterite is rarely found in nature due to being highly prone to phase transitions. However, its high specific surface area, excellent biocompatibility, and high solubility properties have led to a research boom and the [...] Read more.
As the most unstable crystalline form of calcium carbonate, vaterite is rarely found in nature due to being highly prone to phase transitions. However, its high specific surface area, excellent biocompatibility, and high solubility properties have led to a research boom and the following breakthroughs in the last two decades: (1) From primitive calculations and spectroscopic analyses to modern multidimensional research methods combining calculations and experiments, the crystal structure of vaterite has turned from early identifications in orthorhombic and hexagonal crystal systems to a complex polymorphic structure within the monoclinic crystal system. (2) The formation process of vaterite not only conforms to the classical crystal growth theory but also encompasses the nanoparticle aggregation theory, which incorporates the concepts of oriented nanoparticle assembly and mesoscale transformation. (3) Regardless of the conditions, the formation of vaterite depends on an excess of CO32− relative to Ca2+, and its stability duration relates to preservation conditions. (4) Vaterite demonstrates significant value in biomedical applications—including bone repair scaffolds, targeted drug carriers, and antibacterial coating materials—leveraging its porous structure, high specific surface area, and exceptional biocompatibility. While it also shows utility in environmental pollutant adsorption and general coating technologies, the current research remains predominantly concentrated on its medical applications. Currently, the rapid transformation of vaterite presents the primary limitation for its industrial application. Future research should prioritize investigating its formation kinetics and stability. Full article
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29 pages, 14906 KiB  
Article
Hydrothermal Engineering of Ferroelectric PZT Thin Films Tailoring Electrical and Ferroelectric Properties via TiO2 and SrTiO3 Interlayers for Advanced MEMS
by Chun-Lin Li and Guo-Hua Feng
Micromachines 2025, 16(8), 879; https://doi.org/10.3390/mi16080879 - 29 Jul 2025
Viewed by 207
Abstract
This work presents an innovative hydrothermal approach for fabricating flexible piezoelectric PZT thin films on 20 μm titanium foil substrates using TiO2 and SrTiO3 (STO) interlayers. Three heterostructures (Ti/PZT, Ti/TiO2/PZT, and Ti/TiO2/STO/PZT) were synthesized to enable low-temperature [...] Read more.
This work presents an innovative hydrothermal approach for fabricating flexible piezoelectric PZT thin films on 20 μm titanium foil substrates using TiO2 and SrTiO3 (STO) interlayers. Three heterostructures (Ti/PZT, Ti/TiO2/PZT, and Ti/TiO2/STO/PZT) were synthesized to enable low-temperature growth and improve ferroelectric performance for advanced flexible MEMS. Characterizations including XRD, PFM, and P–E loop analysis evaluated crystallinity, piezoelectric coefficient d33, and polarization behavior. The results demonstrate that the multilayered Ti/TiO2/STO/PZT structure significantly enhances performance. XRD confirmed the STO buffer layer effectively reduces lattice mismatch with PZT to ~0.76%, promoting stable morphotropic phase boundary (MPB) composition formation. This optimized film exhibited superior piezoelectric and ferroelectric properties, with a high d33 of 113.42 pm/V, representing an ~8.65% increase over unbuffered Ti/PZT samples, and displayed more uniform domain behavior in PFM imaging. Impedance spectroscopy showed the lowest minimum impedance of 8.96 Ω at 10.19 MHz, indicating strong electromechanical coupling. Furthermore, I–V measurements demonstrated significantly suppressed leakage currents in the STO-buffered samples, with current levels ranging from 10−12 A to 10−9 A over ±3 V. This structure also showed excellent fatigue endurance through one million electrical cycles, confirming its mechanical and electrical stability. These findings highlight the potential of this hydrothermally engineered flexible heterostructure for high-performance actuators and sensors in advanced MEMS applications. Full article
(This article belongs to the Special Issue Manufacturing and Application of Advanced Thin-Film-Based Device)
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33 pages, 2684 KiB  
Review
Biocompatible Natural Polymer-Based Amorphous Solid Dispersion System Improving Drug Physicochemical Properties, Stability, and Efficacy
by Arif Budiman, Helen Ivana, Kelly Angeline Huang, Stella Aurelia Huang, Mazaya Salwa Nadhira, Agus Rusdin and Diah Lia Aulifa
Polymers 2025, 17(15), 2059; https://doi.org/10.3390/polym17152059 - 28 Jul 2025
Viewed by 359
Abstract
Poor aqueous solubility still disqualifies many promising drug candidates at late stages of development. Amorphous solid dispersion (ASD) technology solves this limitation by trapping the active pharmaceutical ingredient (API) in a high-energy, non-crystalline form, yet most marketed ASDs rely on synthetic carriers such [...] Read more.
Poor aqueous solubility still disqualifies many promising drug candidates at late stages of development. Amorphous solid dispersion (ASD) technology solves this limitation by trapping the active pharmaceutical ingredient (API) in a high-energy, non-crystalline form, yet most marketed ASDs rely on synthetic carriers such as polyvinylpyrrolidone (PVP) and hydroxypropyl methylcellulose (HPMC), which raise concerns about long-term biocompatibility, residual solvent load, and sustainability. This study summarizes the emergence of natural polymer-based ASDs (NP-ASDs), along with the bond mechanism reactions through which these natural polymers enhance drug performance. As a result, NP-ASDs exhibit improved physical stability and significantly enhance the dissolution rate of poorly soluble drugs. The structural features of natural polymers play a critical role in stabilizing the amorphous state and modulating drug release profiles. These findings support the growing potential of NP-ASDs as sustainable and biocompatible alternatives to synthetic carriers in pharmaceutical development. Full article
(This article belongs to the Section Biobased and Biodegradable Polymers)
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15 pages, 2865 KiB  
Article
Mitigation of Alkali–Silica Reactivity of Greywacke Aggregate in Concrete for Sustainable Pavements
by Kinga Dziedzic, Aneta Brachaczek, Dominik Nowicki and Michał A. Glinicki
Sustainability 2025, 17(15), 6825; https://doi.org/10.3390/su17156825 - 27 Jul 2025
Viewed by 358
Abstract
Quality requirements for mineral aggregate for concrete used to construct pavement for busy highways are high because of the fatigue traffic loads and environmental exposure. The use of local aggregate for infrastructure projects could result in important sustainability improvements, provided that the concrete’s [...] Read more.
Quality requirements for mineral aggregate for concrete used to construct pavement for busy highways are high because of the fatigue traffic loads and environmental exposure. The use of local aggregate for infrastructure projects could result in important sustainability improvements, provided that the concrete’s durability is assured. The objective of this study was to identify the potential alkaline reactivity of local greywacke aggregate and select appropriate mitigation measures against the alkali–silica reaction. Experimental tests on concrete specimens were performed using the miniature concrete prism test at 60 °C. Mixtures of coarse greywacke aggregate up to 12.5 mm with natural fine aggregate of different potential reactivity were evaluated in respect to the expansion, compressive strength, and elastic modulus of the concrete. Two preventive measures were studied—the use of metakaolin and slag-blended cement. A moderate reactivity potential of the greywacke aggregate was found, and the influence of reactive quartz sand on the expansion and instability of the mechanical properties of concrete was evaluated. Both crystalline and amorphous alkali–silica reaction products were detected in the cracks of the greywacke aggregate. Efficient expansion mitigation was obtained for the replacement of 15% of Portland cement by metakaolin or the use of CEM III/A cement with the slag content of 52%, even if greywacke aggregate was blended with moderately reactive quartz sand. It resulted in a relative reduction in expansion by 85–96%. The elastic modulus deterioration was less than 10%, confirming an increased stability of the elastic properties of concrete. Full article
(This article belongs to the Special Issue Sustainability of Pavement Engineering and Road Materials)
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9 pages, 12041 KiB  
Article
Facile Synthesis of Te and Ag2Te Microrods for Light-Activated Bending-Responsive Photodetectors
by Hsueh-Shih Chen, Kapil Patidar and Pen-Ru Chen
Nanomaterials 2025, 15(15), 1156; https://doi.org/10.3390/nano15151156 - 26 Jul 2025
Viewed by 258
Abstract
In this study, we report the synthesis of Te and Ag2Te micron-sized rods (MRs) via a controlled hot-injection-based quenching process, enabling the control of rod morphology and enhanced crystallinity. Structural analysis confirmed that the synthesized Te MRs exhibit a trigonal phase, [...] Read more.
In this study, we report the synthesis of Te and Ag2Te micron-sized rods (MRs) via a controlled hot-injection-based quenching process, enabling the control of rod morphology and enhanced crystallinity. Structural analysis confirmed that the synthesized Te MRs exhibit a trigonal phase, growing along the (110) direction, while Ag2Te MRs undergo a phase transformation into a monoclinic structure upon Ag doping. A simple and scalable photodetector (PD) was fabricated by drop-casting Te and Ag2Te MRs onto PET plastic films, followed by the application of Ag paste electrodes. The PD demonstrated room-light-induced photocurrent responses, which increased significantly upon mechanical bending due to the formation of additional conductive pathways between MRs. The Ag2Te-based bending sensor exhibited a fivefold enhancement in photocurrent compared to its Te counterpart and maintained high stability over 1000 bending cycles. These results highlight the potential of Te and Ag2Te MRs for use in flexible and wearable motion-sensing technologies, offering a simple yet effective approach for integrating 1D telluride nanostructures into scalable optoelectronic applications. Full article
(This article belongs to the Section Nanoelectronics, Nanosensors and Devices)
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19 pages, 10374 KiB  
Article
Nanoscale Nickel Oxide: Synthesis, Characterization, and Impact on Antibacterial Activity Against Representative Microorganisms
by Daniela Istrate, Mihai Oproescu, Ecaterina Magdalena Modan, Sorin Georgian Moga, Denis Aurelian Negrea and Adriana-Gabriela Schiopu
ChemEngineering 2025, 9(4), 77; https://doi.org/10.3390/chemengineering9040077 - 25 Jul 2025
Viewed by 244
Abstract
Among the various available synthesis approaches, hydrolytic precipitation offers a simple, cost-effective, and scalable route for producing phase-pure NiO with a controlled morphology and crystallite size. However, the influence of calcination temperature on its crystalline phase, particle size, and antimicrobial activity remains an [...] Read more.
Among the various available synthesis approaches, hydrolytic precipitation offers a simple, cost-effective, and scalable route for producing phase-pure NiO with a controlled morphology and crystallite size. However, the influence of calcination temperature on its crystalline phase, particle size, and antimicrobial activity remains an active field of research. This study aims to investigate the structural, morphological, and antibacterial properties of NiO nanoparticles synthesized via hydrolytic methods and thermally treated at different temperatures. XRD data indicate the presence of the hexagonal crystallographic phase of NiO (space group 166: R-3m), a structural variant less commonly reported in the literature, stabilized under mild hydrolytic synthesis conditions. The average crystallite size increases significantly from 4.97 nm at 300 °C to values of ~17.8 nm at 500–700 °C, confirming the development of the crystal lattice. The ATR-FTIR analysis confirms the presence of the characteristic Ni–O band for all samples, positioned between 367 and 383 cm−1, with a reference value of 355 cm−1 for commercial NiO. The displacements and variations in intensity reflect a thermal evolution of the crystalline structure, but also an important influence of the size of the crystallites and the agglomeration state. The results reveal a systematic evolution in particle morphology from porous, flake-like nanostructures at 300 °C to dense, well-faceted polyhedral crystals at 900 °C. With an increasing temperature, particle size increases. EDS spectra confirm the high purity of the NiO phase across all samples. Additionally, the NiO nanoparticles exhibit calcination-temperature-dependent antibacterial activity, with the complete inhibition of Escherichia coli and Enterococcus faecalis observed after 24 h for the sample calcined at 300 °C and over 90% CFU reduction within 4 h. A significant reduction in E. faecalis viability across all samples indicates time- and strain-specific bactericidal effects. Due to its remarkable multifunctionality, NiO has emerged as a strategic nanomaterial in fields ranging from energy storage and catalysis to antimicrobial technologies, where precise control over its structural phase and particle size is essential for optimizing performance. Full article
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14 pages, 1884 KiB  
Article
Ag/ZrO2 Hybrid Coating for Tribological and Corrosion Protection of Ti45Nb Alloy in Biomedical Environments
by Mevra Aslan Çakir
Metals 2025, 15(8), 831; https://doi.org/10.3390/met15080831 - 24 Jul 2025
Viewed by 241
Abstract
In this study, a Ag/ZrO2 hybrid coating prepared by the sol–gel method on a β-type Ti45Nb alloy was applied by the spin coating technique, and the microstructural, mechanical, electrochemical, and tribological properties of the surface were evaluated in a multi-dimensional manner. The [...] Read more.
In this study, a Ag/ZrO2 hybrid coating prepared by the sol–gel method on a β-type Ti45Nb alloy was applied by the spin coating technique, and the microstructural, mechanical, electrochemical, and tribological properties of the surface were evaluated in a multi-dimensional manner. The hybrid solution was prepared using zirconium propoxide and silver nitrate and stabilized through a low-temperature two-stage annealing protocol. The crystal structure of the coating was determined by XRD, and the presence of dense tetragonal ZrO2 phase and crystalline Ag phases was confirmed. SEM-EDS analyses revealed a compact coating structure of approximately 1.8 µm thickness with homogeneously distributed Ag nanoparticles on the surface. As a result of the electrochemical corrosion tests, it was determined that the open circuit potential shifted to more noble values, the corrosion current density decreased, and the corrosion rate decreased by more than 70% on the surfaces where the Ag/ZrO2 coating was applied. In the tribological tests, a decrease in the coefficient of friction, narrowing of wear marks, and significant reduction in surface damage were observed in dry and physiological (HBSS) environments. The findings revealed that the Ag/ZrO2 hybrid coating significantly improved the surface performance of the Ti45Nb alloy both mechanically and electrochemically and offers high potential for biomedical implant applications. Full article
(This article belongs to the Special Issue Corrosion Behavior and Surface Engineering of Metallic Materials)
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13 pages, 2459 KiB  
Article
Green Synthesis of Zinc Oxide Particles Using Cladophora glomerata L. (Kütz) Extract: Comparative Study of Crystal Structure, Surface Chemistry, and Antimicrobial Efficacy with Different Zinc Precursors
by Göksal Sezen and Ramazan Aktan
Processes 2025, 13(8), 2350; https://doi.org/10.3390/pr13082350 - 24 Jul 2025
Viewed by 272
Abstract
This study examined the eco-friendly synthesis of zinc oxide (ZnO) nanoparticles using Cladophora glomerata extracts as reducing and stabilizing agents, comparing zinc acetate and zinc chloride precursors for biomedical and environmental applications. Zinc acetate-synthesized ZnO nanoparticles showed a significant absorption peak around 320–330 [...] Read more.
This study examined the eco-friendly synthesis of zinc oxide (ZnO) nanoparticles using Cladophora glomerata extracts as reducing and stabilizing agents, comparing zinc acetate and zinc chloride precursors for biomedical and environmental applications. Zinc acetate-synthesized ZnO nanoparticles showed a significant absorption peak around 320–330 nm, indicating stable, quasi-spherical ZnO nanoparticles with a narrow size distribution, primarily around 100 nm. Zeta potential measurements revealed a value of −25 mV for these particles, suggesting moderate colloidal stability. XRD analysis confirmed a highly crystalline hexagonal wurtzite structure for zinc acetate-derived ZnO, and SEM images supported a proper microstructure with approximately 2 µm particle size. FTIR analysis indicated higher-quality ZnO from zinc acetate due to the absence of moisture and hydroxyl groups. Conversely, zinc chloride-derived ZnO particles displayed a broader absorption spectrum around 370 nm, indicative of significant aggregation. Their narrower zeta potential distribution around +10 mV suggested diminished colloidal stability and a heightened aggregation tendency. While a peak around 100 nm was observed, many particles exceeded 1000 nm, reaching up to 10,000 nm. XRD results showed that zinc chloride adversely affected crystallinity, and SEM analysis indicated smaller particles (approx. 1 µm). FTIR analysis demonstrated that zinc chloride samples retained hydroxyl groups. Both zinc acetate- and zinc chloride-derived ZnO nanoparticles produced notable inhibitory zones against Gram-positive (L. monocytogenes, S. aureus) and specific Gram-negative bacteria (E. coli, K. pneumoniae). Zinc acetate-derived ZnO showed a 21 mm inhibitory zone against P. vulgaris, while zinc chloride-derived ZnO showed a 10.1 mm inhibitory zone against C. albicans. Notably, zinc chloride-derived ZnO exhibited broad-spectrum antimicrobial activity. MIC readings indicated that zinc acetate-derived ZnO had better antibacterial properties at lower concentrations, such as 3.125 µg/mL against L. monocytogenes. These findings emphasize that the precursor material selection critically influences particle characteristics, including optical properties, surface charge, and colloidal stability. Full article
(This article belongs to the Topic Advanced Materials in Chemical Engineering)
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15 pages, 2393 KiB  
Article
Determination of Time and Concentration Conditions Affecting Polylactic Acid (Pla) Production
by Jorge Braulio Amaya and Gabriela Vaca
Polymers 2025, 17(15), 2009; https://doi.org/10.3390/polym17152009 - 23 Jul 2025
Viewed by 233
Abstract
Polylactic acid (PLA) is a renewable biopolymer that has attracted considerable interest due to its ability to replace petroleum-based synthetic polymers, thereby offering a more sustainable alternative to global environmental concerns. This study focused on evaluating the effect of catalyst concentration and reaction [...] Read more.
Polylactic acid (PLA) is a renewable biopolymer that has attracted considerable interest due to its ability to replace petroleum-based synthetic polymers, thereby offering a more sustainable alternative to global environmental concerns. This study focused on evaluating the effect of catalyst concentration and reaction time on the efficiency of PLA synthesis via the Ring-Opening Polymerization (ROP) technique. The process involved a lactic acid esterification stage (using 88% lactic acid) to obtain lactide, employing 40% and 60% (v/v) sulfuric acid concentrations, followed by polymerization at various reaction times (10, 15, 20, and 30 min). Analysis of variance (ANOVA) results revealed that the 40% catalyst concentration had a statistically significant effect on polymer yield (p = 0.032), whereas reaction time showed no statistical significance (p = 0.196), although the highest yields were recorded at 10 and 15 min. Fourier Transform Infrared Spectroscopy (FTIR) confirmed the presence of the characteristic functional groups of PLA, and Differential Scanning Calorimetry (DSC) revealed a semi-crystalline structure with a high melting temperature, indicating good thermal stability. These results validate the viability of PLA as a functional and sustainable biopolymer. Full article
(This article belongs to the Special Issue Advanced Polymer Materials: Synthesis, Structure, and Properties)
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