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14 pages, 2180 KiB  
Article
Study on Preparation of Nano-CeO2 Modified Aluminized Coating by Low Temperature Pack Aluminizing on γ-TiAl Intermetallic Compound
by Jiahui Song, Yunmei Long, Yifan He, Yichen Li, Dianqi Huang, Yan Gu, Xingyao Wang, Jinlong Wang and Minghui Chen
Coatings 2025, 15(8), 914; https://doi.org/10.3390/coatings15080914 - 5 Aug 2025
Viewed by 40
Abstract
TiAl alloy offers advantages including low density, high specific strength and stiffness, and excellent high-temperature creep resistance. It is widely used in the aerospace, automotive, and chemical sectors, as well as in other fields. However, at temperatures of 800 °C and above, it [...] Read more.
TiAl alloy offers advantages including low density, high specific strength and stiffness, and excellent high-temperature creep resistance. It is widely used in the aerospace, automotive, and chemical sectors, as well as in other fields. However, at temperatures of 800 °C and above, it forms a porous oxide film predominantly composed of TiO2, which fails to provide adequate protection. Applying high-temperature protective coatings is therefore essential. Oxides demonstrating protective efficacy at elevated temperatures include Al2O3, Cr2O3, and SiO2. The Pilling–Bedworth Ratio (PBR)—defined as the ratio of the volume of the oxide formed to the volume of the metal consumed—serves as a critical criterion for assessing oxide film integrity. A PBR value greater than 1 but less than 2 indicates superior film integrity and enhanced oxidation resistance. Among common oxides, Al2O3 exhibits a PBR value within this optimal range (1−2), rendering aluminum-based compound coatings the most extensively utilized. Aluminum coatings can be applied via methods such as pack cementation, thermal spraying, and hot-dip aluminizing. Pack cementation, being the simplest to operate, is widely employed. In this study, a powder mixture with the composition Al:Al2O3:NH4Cl:CeO2 = 30:66:3:1 was used to aluminize γ-TiAl intermetallic compound specimens via pack cementation at 600 °C for 5 h. Subsequent isothermal oxidation at 900 °C for 20 h yielded an oxidation kinetic curve adhering to the parabolic rate law. This treatment significantly enhanced the high-temperature oxidation resistance of the γ-TiAl intermetallic compound, thereby broadening its potential application scenarios. Full article
(This article belongs to the Special Issue High-Temperature Protective Coatings)
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20 pages, 1743 KiB  
Article
Encapsulation of Lactobacillus reuteri in Chia–Alginate Hydrogels for Whey-Based Functional Powders
by Alma Yadira Cid-Córdoba, Georgina Calderón-Domínguez, María de Jesús Perea-Flores, Alberto Peña-Barrientos, Fátima Sarahi Serrano-Villa, Rigoberto Barrios-Francisco, Marcela González-Vázquez and Rentería-Ortega Minerva
Gels 2025, 11(8), 613; https://doi.org/10.3390/gels11080613 - 4 Aug 2025
Viewed by 226
Abstract
This study aimed to develop a functional powder using whey and milk matrices, leveraging the protective capacity of chia–alginate hydrogels and the advantages of electrohydrodynamic spraying (EHDA), a non-thermal technique suitable for encapsulating probiotic cells under stress conditions commonly encountered in food processing. [...] Read more.
This study aimed to develop a functional powder using whey and milk matrices, leveraging the protective capacity of chia–alginate hydrogels and the advantages of electrohydrodynamic spraying (EHDA), a non-thermal technique suitable for encapsulating probiotic cells under stress conditions commonly encountered in food processing. A hydrogel matrix composed of chia seed mucilage and sodium alginate was used to form a biopolymeric network that protected probiotic cells during processing. The encapsulation efficiency reached 99.0 ± 0.01%, and bacterial viability remained above 9.9 log10 CFU/mL after lyophilization, demonstrating the excellent protective capacity of the hydrogel matrix. Microstructural analysis using confocal laser scanning microscopy (CLSM) revealed well-retained cell morphology and homogeneous distribution within the hydrogel matrix while, in contrast, scanning electron microscopy (SEM) showed spherical, porous microcapsules with distinct surface characteristics influenced by the encapsulation method. Encapsulates were incorporated into beverages flavored with red fruits and pear and subsequently freeze-dried. The resulting powders were analyzed for moisture, protein, lipids, carbohydrates, fiber, and color determinations. The results were statistically analyzed using ANOVA and response surface methodology, highlighting the impact of ingredient ratios on nutritional composition. Raman spectroscopy identified molecular features associated with casein, lactose, pectins, anthocyanins, and other functional compounds, confirming the contribution of both matrix and encapsulants maintaining the structural characteristics of the product. The presence of antioxidant bands supported the functional potential of the powder formulations. Chia–alginate hydrogels effectively encapsulated L. reuteri, maintaining cell viability and enabling their incorporation into freeze-dried beverage powders. This approach offers a promising strategy for the development of next-generation functional food gels with enhanced probiotic stability, nutritional properties, and potential application in health-promoting dairy systems. Full article
(This article belongs to the Special Issue Food Gels: Fabrication, Characterization, and Application)
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16 pages, 1265 KiB  
Article
Enhancing Stability of Boesenbergia rotunda Bioactive Compounds: Microencapsulation via Spray-Drying and Its Physicochemical Evaluation
by Fahmi Ilman Fahrudin, Suphat Phongthai and Pilairuk Intipunya
Foods 2025, 14(15), 2699; https://doi.org/10.3390/foods14152699 - 31 Jul 2025
Viewed by 263
Abstract
This study aimed to microencapsulate Boesenbergia rotunda (fingerroot) extract using maltodextrin (MD) and gum arabic (GA) as wall materials via spray-drying to improve powder physicochemical properties and protect bioactive compounds. MD and GA were employed as wall materials in varying ratios (MD:GA of [...] Read more.
This study aimed to microencapsulate Boesenbergia rotunda (fingerroot) extract using maltodextrin (MD) and gum arabic (GA) as wall materials via spray-drying to improve powder physicochemical properties and protect bioactive compounds. MD and GA were employed as wall materials in varying ratios (MD:GA of 1:0, 0:1, 1:1, 2:1, 1:2) to evaluate their effects on the physicochemical properties of the resulting microcapsules. Spray-dried microcapsules were evaluated for morphology, flowability, particle size distribution, moisture content, hygroscopicity, solubility, encapsulation efficiency, major bioactive compound retention, and thermal stability. The extract encapsulation using MD:GA at 1:1 ratio (MD1GA1) demonstrated a favorable balance, with high solubility (98.70%), low moisture content (8.69%), low hygroscopicity (5.08%), and uniform particle morphology, despite its moderate EE (75.06%). SEM images revealed spherical particles with fewer surface indentations in MD-rich formulations. Microencapsulation effectively retained pinostrobin and pinocembrin in all formulations with pinostrobin consistently retained at a higher value, indicating its higher stability. The balanced profile of physical and functional properties of fingerroot extract with MD1GA1 microcapsule makes it a promising candidate for food and nutraceutical applications. Full article
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16 pages, 1006 KiB  
Article
Spray Drying of Jackfruit (Artocarpus heterophyllus Lam.) Seeds Protein Concentrate: Physicochemical, Structural, and Thermal Characterization
by Dulce María de Jesús Miss-Zacarías, Montserrat Calderón-Santoyo, Victor Manuel Zamora-Gasga, Gabriel Ascanio and Juan Arturo Ragazzo-Sánchez
Processes 2025, 13(7), 2319; https://doi.org/10.3390/pr13072319 - 21 Jul 2025
Viewed by 372
Abstract
Jackfruit seeds (Artocarpus heterophyllus Lam.) are a viable option for supporting a sustainable protein supply. The objective was to obtain protein powder from jackfruit seeds protein concentrate (JSPC) by spray drying. A central composite design was used; the independent variables were inlet [...] Read more.
Jackfruit seeds (Artocarpus heterophyllus Lam.) are a viable option for supporting a sustainable protein supply. The objective was to obtain protein powder from jackfruit seeds protein concentrate (JSPC) by spray drying. A central composite design was used; the independent variables were inlet temperature (110, 115, and 120 °C) and the solids of the JSPC solution (5, 7.5, and 10%). With the desirability function, the optimal drying parameters to maximize the process yield and achieve a low moisture content were 7.5% solids in the JSPC solution and an inlet temperature of 115 °C, resulting in a process yield of 71.51 ± 1.21%. Moisture (5.33 ± 0.11%), water activity (0.15 ± 0.02), bulk density (0.40 ± 0.01 g/mL), and color (L*: 70.56 ± 0.38, a*: 7.80 ± 0.11 and b*: 15.18 ± 0.15) were measured; these parameters are within the allowed ranges for stable food powders. Hydrosolubility (82.46 ± 1.68%), foaming capacity (48.33 ± 1.66%), and emulsifying activity (105.74 ± 10.20 m2/g) were evaluated. Glass transition temperature (129.49 °C) of the JSPC powder enables the establishment of optimal storage and processing conditions for the protein. JSPC powder could be applied to the elaboration of food products with nutritional and functional value. Full article
(This article belongs to the Section Food Process Engineering)
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17 pages, 6250 KiB  
Article
Microstructure and Chemical Stability of Al2O3-ZrO2-ReB2 Composite Coatings Obtained by Air Plasma Spraying
by Adriana Wrona, Kinga Czechowska, Katarzyna Bilewska, Monika Czerny, Anna Czech, Marcin Lis, Anna Brudny, Grzegorz Muzia and Lucyna Jaworska
Materials 2025, 18(14), 3363; https://doi.org/10.3390/ma18143363 - 17 Jul 2025
Viewed by 300
Abstract
This study investigated the effect of adding superhard ReB2 to atmospheric plasma sprayed (APS) coatings based on 60 wt% Al2O3 and 40 wt% ZrO2. The amorphous phases commonly present in such coatings are known to impair their [...] Read more.
This study investigated the effect of adding superhard ReB2 to atmospheric plasma sprayed (APS) coatings based on 60 wt% Al2O3 and 40 wt% ZrO2. The amorphous phases commonly present in such coatings are known to impair their performance. ReB2 was introduced as a crystallization nucleus due to its high melting point. ReB2 decomposes in the presence of moisture and oxygen into H3BO3, ReO3, HBO2, and HReO4. ReB2 was encapsulated with Al2O3 via metallothermic synthesis to improve moisture stability, yielding a powder with d90 = 15.1 μm. After milling, it was added at 20 wt% to the Al2O3-ZrO2 feedstock. Agglomeration parameters were optimized, and coatings were deposited under varying APS conditions onto 316L steel substrates with a NiAl bond coat. In the coating with the highest ReB2 content, the identified phases included ReB2 (2.6 wt%), Re (0.8 wt%), α-Al2O3 (30.9 wt%), η-Al2O3 (32.4 wt%), and monoclinic and tetragonal ZrO2. The nanohardness of the coating, measured using a Vickers indenter at 96 mN and calculated via the Oliver–Pharr method, was 9.2 ± 1.0 GPa. High abrasion resistance was obtained for the coating with a higher content of η-Al2O3 (48.7 wt%). The coefficient of friction, determined using a ball-on-disc test with a corundum ball, was 0.798 ± 0.03. After 15 months, the formation of (H3O)(ReO4) was observed, suggesting initial moisture-induced changes. The results confirm that Al2O3-encapsulated ReB2 can enhance phase stability and crystallinity in APS coatings. Full article
(This article belongs to the Section Materials Physics)
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18 pages, 1790 KiB  
Article
Development of Co-Amorphous Systems for Inhalation Therapy—Part 1: From Model Prediction to Clinical Success
by Eleonore Fröhlich, Aurora Bordoni, Nila Mohsenzada, Stefan Mitsche, Hartmuth Schröttner and Sarah Zellnitz-Neugebauer
Pharmaceutics 2025, 17(7), 922; https://doi.org/10.3390/pharmaceutics17070922 - 16 Jul 2025
Viewed by 418
Abstract
Background/Objectives: The integration of machine learning (ML) and artificial intelligence (AI) has revolutionized the pharmaceutical industry by improving drug discovery, development and manufacturing processes. Based on literature data, an ML model was developed by our group to predict the formation of binary [...] Read more.
Background/Objectives: The integration of machine learning (ML) and artificial intelligence (AI) has revolutionized the pharmaceutical industry by improving drug discovery, development and manufacturing processes. Based on literature data, an ML model was developed by our group to predict the formation of binary co-amorphous systems (COAMSs) for inhalation therapy. The model’s ability to develop a dry powder formulation with the necessary properties for a predicted co-amorphous combination was evaluated. Methods: An extended experimental validation of the ML model by co-milling and X-ray diffraction analysis for 18 API-API (active pharmaceutical ingredient) combinations is presented. Additionally, one COAMS of rifampicin (RIF) and ethambutol (ETH), two first-line tuberculosis (TB) drugs are developed further for inhalation therapy. Results: The ML model has shown an accuracy of 79% in predicting suitable combinations for 35 APIs used in inhalation therapy; experimental accuracy was demonstrated to be 72%. The study confirmed the successful development of stable COAMSs of RIF-ETH either via spray-drying or co-milling. In particular, the milled COAMSs showed better aerosolization properties (higher ED and FPF with lower standard deviation). Further, RIF-ETH COAMSs show much more reproducible results in terms of drug quantity dissolved over time. Conclusions: ML has been shown to be a suitable tool to predict COAMSs that can be developed for TB treatment by inhalation to save time and cost during the experimental screening phase. Full article
(This article belongs to the Special Issue New Platform for Tuberculosis Treatment)
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16 pages, 10539 KiB  
Article
Comparative Corrosion and Wear Behaviors of Cermet Coatings Obtained from Conventional and Recycled Powders
by Dino Woelk, Julian Eßler, Ion-Dragos Utu and Gabriela Marginean
Appl. Sci. 2025, 15(14), 7654; https://doi.org/10.3390/app15147654 - 8 Jul 2025
Viewed by 346
Abstract
Many components in industry are subjected to high loads during operation and therefore often do not reach their intended service life. Conventional steels frequently do not provide sufficient protection against wear and corrosion. One solution is to coat these components using methods like [...] Read more.
Many components in industry are subjected to high loads during operation and therefore often do not reach their intended service life. Conventional steels frequently do not provide sufficient protection against wear and corrosion. One solution is to coat these components using methods like thermal spraying to apply cermet coatings such as Cr3C2-NiCr or WC-Co-Cr. In light of increasingly strict environmental regulations, more eco-friendly alternatives are needed, especially ones that use little or no Cr, Ni, Co, or W. Another alternative is the recycling of powder materials, which is the focus of this research project. This study investigated whether filter dust from an HVOF system could be used to develop a new coating suitable for use in applications requiring resistance to wear and corrosion. This is challenging as the filter dusts have heterogeneous compositions and irregular particle sizes. Nevertheless, this recycled material, referred to as “Green Cermets” (GCs), offers previously untapped potential that may also be of ecological interest. An established WC-Co-Cr coating served as a reference. In addition to friction wear and corrosion resistance, the study also examined particle size distribution, hardness, microstructure, and susceptibility to crack formation at the interface and inside the coating. Even though the results revealed a diminished performance of the GC coatings relative to the conventional WC-CoCr, they may still be applicable in various industrial applications. Full article
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22 pages, 2427 KiB  
Article
Cyclodextrin-Based Quercetin Powders for Potential Nose-to-Brain Transport: Formulation and In Vitro Assessment
by Elmina-Marina Saitani, Paraskevi Papakyriakopoulou, Theodora Bogri, Georgia Choleva, Kyriaki Kontopoulou, Spyridon Roboras, Maria Samiou, Antiopi Vardaxi, Stergios Pispas, Georgia Valsami and Natassa Pippa
Molecules 2025, 30(13), 2878; https://doi.org/10.3390/molecules30132878 - 7 Jul 2025
Viewed by 492
Abstract
Quercetin (Que) is widely recognized for its antioxidant and neuroprotective properties; however, its clinical potential remains limited due to poor solubility and low oral bioavailability. Nasal powders have emerged as a promising strategy to overcome these limitations, taking advantage of nose-to-brain delivery, offering [...] Read more.
Quercetin (Que) is widely recognized for its antioxidant and neuroprotective properties; however, its clinical potential remains limited due to poor solubility and low oral bioavailability. Nasal powders have emerged as a promising strategy to overcome these limitations, taking advantage of nose-to-brain delivery, offering a direct, non-invasive route to the central nervous system while bypassing first-pass metabolism. This study aims to extend previous work by systematically investigating the impact of different preparation methods (spray drying vs. lyophilization) and the incorporation of hydroxypropyl methylcellulose (HPMC) and mannitol/lecithin microparticles (MLMPs) on the physicochemical characteristics, structural properties, and in vitro diffusion behavior of HPβCD-based nasal powder formulations of Que. Thermal behavior and stability were analyzed using TGA, while morphology and particle distribution were assessed via Scanning Electron Microscopy. In vitro diffusion studies using Franz cells and regenerated cellulose membranes were conducted under simulated nasal conditions. Among all tested formulations, the spray-dried HPβCD/Que powder (F4) showed the highest permeation (0.11 ± 0.01 mg/cm2 at 120 min). The inclusion of HPMC improved thermal stability but reduced Que diffusion, likely due to increased viscosity and matrix formation. Blending with MLMPs enhanced powder flow and dose placement, although it modestly reduced diffusion efficiency. Overall, this study highlights the potential of HPβCD-based spray-dried powders for nasal Que delivery and demonstrates how HPMC and MLMPs can be strategically employed to tailor performance characteristics. Full article
(This article belongs to the Section Macromolecular Chemistry)
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13 pages, 11057 KiB  
Article
Microstructure, Hardness and Tribological Characteristics of High-Entropy Coating Obtained by Detonation Spraying
by Zhuldyz Sagdoldina, Laila Sulyubayeva, Dastan Buitkenov and Yedilzhan Kambarov
Crystals 2025, 15(7), 625; https://doi.org/10.3390/cryst15070625 - 4 Jul 2025
Viewed by 260
Abstract
In this study, powders based on a high-entropy AlCoCrFeNi alloy obtained by mechanical alloying were successfully applied to a 316L stainless steel substrate by detonation spraying under various conditions. Their microstructural features, phase composition, hardness, and wear resistance were studied. A comparative analysis [...] Read more.
In this study, powders based on a high-entropy AlCoCrFeNi alloy obtained by mechanical alloying were successfully applied to a 316L stainless steel substrate by detonation spraying under various conditions. Their microstructural features, phase composition, hardness, and wear resistance were studied. A comparative analysis between the initial powder and the coatings was performed, including phase transformation modeling using Thermo-Calc under non-equilibrium conditions. The results showed that the phase composition of the powder and coatings includes body-centered cubic lattice (BCC), its ordered modification (B2), and face-centered cubic lattice FCC phases, which is consistent with the predictions of the Scheil solidification model, describing the process of non-equilibrium solidification, assuming no diffusion in the solid phase and complete mixing in the liquid phase. Rapid solidification and high-speed impact deformation of the powder led to significant grain refinement in the detonation spraying coating, which ultimately improved the mechanical properties at the micro level. The data obtained demonstrate the high efficiency of the AlCoCrFeNi coating applied by detonation spraying and confirm its potential for use in conditions of increased wear and mechanical stress. AlCoCrFeNi coatings may be promising for use as structural materials in the future. Full article
(This article belongs to the Section Crystalline Metals and Alloys)
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31 pages, 4803 KiB  
Review
Advanced HVOF-Sprayed Carbide Cermet Coatings as Environmentally Friendly Solutions for Tribological Applications: Research Progress and Current Limitations
by Basma Ben Difallah, Yamina Mebdoua, Chaker Serdani, Mohamed Kharrat and Maher Dammak
Technologies 2025, 13(7), 281; https://doi.org/10.3390/technologies13070281 - 3 Jul 2025
Viewed by 541
Abstract
Thermally sprayed carbide cermet coatings, particularly those based on tungsten carbide (WC) and chromium carbide (Cr3C2) and produced with the high velocity oxygen fuel (HVOF) process, are used in tribological applications as environmentally friendly alternatives to electroplated hard chrome [...] Read more.
Thermally sprayed carbide cermet coatings, particularly those based on tungsten carbide (WC) and chromium carbide (Cr3C2) and produced with the high velocity oxygen fuel (HVOF) process, are used in tribological applications as environmentally friendly alternatives to electroplated hard chrome coatings. These functional coatings are especially prevalent in the automotive industry, offering excellent wear resistance. However, their mechanical and tribological performances are highly dependent on factors such as feedstock powders, spray parameters, and service conditions. This review aims to gain deeper insights into the above elements. It also outlines emerging advancements in HVOF technology—including in situ powder mixing, laser treatment, artificial intelligence integration, and the use of novel materials such as rare earth elements or transition metals—which can further enhance coating performance and broaden their applications to sectors such as the aerospace and hydro-machinery industries. Finally, this literature review focuses on process optimization and sustainability, including environmental and health impacts, critical material use, and operational limitations. It uses a life cycle assessment (LCA) as a tool for evaluating ecological performance and addresses current challenges such as exposure risks, process control constraints, and the push toward safer, more sustainable alternatives to traditional WC and Cr3C2 cermet coatings. Full article
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13 pages, 1022 KiB  
Article
Fluorinated Analogs of Organosulfur Compounds from Garlic (Allium sativum): Synthesis and Chemistry
by Eric Block, Benjamin Bechand, Sivaji Gundala, Abith Vattekkatte and Kai Wang
Molecules 2025, 30(13), 2841; https://doi.org/10.3390/molecules30132841 - 2 Jul 2025
Viewed by 432
Abstract
We report the first syntheses—from commercially available 3-chloro-2-fluoroprop-1-ene (9)—of key garlic-derived compounds containing sp2-fluorine. We also report synthesis of fluoro-5,6-dihydrothiopyrans by trapping 2-fluorothioacrolein (15). Thus, difluoroallicin (12, S-(2-fluoro-2-propenyl) 2-fluoroprop-2-ene-1-sulfinothioate) is prepared by peracid oxidation [...] Read more.
We report the first syntheses—from commercially available 3-chloro-2-fluoroprop-1-ene (9)—of key garlic-derived compounds containing sp2-fluorine. We also report synthesis of fluoro-5,6-dihydrothiopyrans by trapping 2-fluorothioacrolein (15). Thus, difluoroallicin (12, S-(2-fluoro-2-propenyl) 2-fluoroprop-2-ene-1-sulfinothioate) is prepared by peracid oxidation of 1,2-bis(2-fluoro-2-propenyl)disulfane (11). S-2-Fluoro-2-propenyl-l-cysteine (2-fluorodeoxyalliin, 13), synthesized from cysteine and characterized by X-ray crystallography, is oxidized to its S-oxide, 2-fluoroalliin (22). The latter, with alliinase-containing powdered fresh garlic, gives a mixture of 12, allicin (1), and isomers of monofluoroallicin (23), indicating that 22 serves as a substrate for garlic alliinase. Upon heating, 12 generates transient 15, which dimerizes giving difluoro vinyl dithiins 6 and 7. Ethyl acrylate trapping of 15 affords 5- and 6-substituted 3-fluoro-5,6-dihydro-4H-thiopyrans (19 and 20). In 1,1,1,3,3,3-hexafluoro-2-propanol (HEFP) as solvent, 12 is converted into trifluoroajoene ((E,Z)-1-(2-fluoro-3-((2-fluoro-2-propenyl)sulfinyl)prop-1-en-1-yl)-2-(2-fluoro-2-propenyl)disulfane; 18). Liquid sulfur converts 11 to a (CH2=CFCH2)2Sn mixture (n = 4–15), characterized by UPLC-(Ag+)-coordination ion spray-mass spectrometry. Full article
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12 pages, 5865 KiB  
Article
Recovery of Titanium and Aluminum from Secondary Waste Solutions via Ultrasonic Spray Pyrolysis
by Srećko Stopić, Duško Kostić, Vladimir Damjanović, Mitar Perušić, Radislav Filipović, Nenad Nikolić and Bernd Friedrich
Metals 2025, 15(7), 701; https://doi.org/10.3390/met15070701 - 24 Jun 2025
Viewed by 329
Abstract
The synthesis of oxide nanopowders through ultrasonic spray pyrolysis (USP) represents a sustainable method for producing high-purity, spherical particles tailored for advanced material applications. Recent developments in USP synthesis leverage the continuous transport of aerosols from an ultrasonic generator to a high-temperature furnace, [...] Read more.
The synthesis of oxide nanopowders through ultrasonic spray pyrolysis (USP) represents a sustainable method for producing high-purity, spherical particles tailored for advanced material applications. Recent developments in USP synthesis leverage the continuous transport of aerosols from an ultrasonic generator to a high-temperature furnace, with nanopowders collected efficiently using an electrostatic precipitator. This study explored the use of USP for titanium oxysulfate and aluminum nitrate solutions derived from the aluminum industry, focusing on resource recovery and waste reduction. Titanium oxysulfate was synthesized by leaching slag, generated during the reduction of red mud, with sulfuric acid under oxidizing, high-pressure conditions. After purification, the titanium oxysulfate solution was processed using USP in a hydrogen reduction atmosphere to yield spherical titanium dioxide (TiO2) nanopowders. The hydrogen atmosphere enabled precise control over the nanoparticles’ morphology and crystallinity, enhancing their suitability for use in applications such as photocatalysis, pigments, and advanced coatings. In parallel, both synthetic and laboratory solutions of aluminum nitrate [Al(NO3)3] were prepared. The laboratory solution was prepared by leaching aluminum hydroxide oxide (AlOOH) with hydrochloric acid to form aluminum chloride (AlCl3), followed by a conversion to aluminum nitrate through the addition of nitric acid. The resulting aluminum nitrate solution was subjected to USP, producing highly uniform, spherical alumina (Al2O3) nanopowders with a narrow size distribution. The resulting nanopowders, characterized by their controlled properties and potential applicability, represent an advancement in oxide powder synthesis and resource-efficient manufacturing techniques. Full article
(This article belongs to the Special Issue Advances in Recycling of Valuable Metals—2nd Edition)
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22 pages, 2559 KiB  
Article
Viability of Microencapsulated Probiotics in Cross-Linked Alginate Matrices and Chia Seed or Flaxseed Mucilage During Spray-Drying and Storage
by Mariela Bustamante, B. Dave Oomah, César Burgos-Díaz, Daniela Vergara, Liset Flores and Carolina Shene
Microorganisms 2025, 13(7), 1457; https://doi.org/10.3390/microorganisms13071457 - 23 Jun 2025
Cited by 1 | Viewed by 753
Abstract
Interest in probiotics has not diminished, and techniques to protect them from the environment in which they are found are constantly being innovated. Spray-drying is the most studied and industrially used technique to encapsulate probiotics. Recently, a new process has been developed in [...] Read more.
Interest in probiotics has not diminished, and techniques to protect them from the environment in which they are found are constantly being innovated. Spray-drying is the most studied and industrially used technique to encapsulate probiotics. Recently, a new process has been developed in which particle formation, alginate cross-linking, and drying are carried out in a single step. In this study, Bifidobacterium infantis, Bifidobacterium longum, Lactobacillus plantarum, and Lactobacillus rhamnosus were microencapsulated by spray-drying using a cross-linked alginate matrix supplemented with chia seed mucilage (CM) or flaxseed mucilage (FM) as the coating material. All formulations evaluated, supplemented with 0.4% (w/v) of CM or FM, including the control formulation showed high survival rates, varying between 87% and 97%. The viability of microencapsulated probiotics was affected by storage temperature. At 4 °C, viability decreased slightly, and after 90 days, the viable probiotic count ranged from 7 to 11 Log CFU/g of dry powder. Meanwhile, viability did not exceed 4 Log CFU/g of dry powder at 37 °C. Probiotic microencapsulation in cross-linked alginate matrices and chia or flaxseed mucilage by spray-drying is presented as a promising alternative for their protection, potentially improving the long-term stability and efficacy of the probiotic product. Full article
(This article belongs to the Section Food Microbiology)
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26 pages, 8375 KiB  
Article
Water-Soluble Formulations of Curcumin and Eugenol Produced by Spray Drying
by Iskra Z. Koleva, Katya Kamenova, Petar D. Petrov and Christo T. Tzachev
Pharmaceuticals 2025, 18(7), 944; https://doi.org/10.3390/ph18070944 - 23 Jun 2025
Viewed by 600
Abstract
Background/Objectives: In this study, we present a green, scalable platform for the production of water-dispersible powders co-encapsulating the lipophilic bioactives curcumin (Cur) and eugenol (Eug) within the amphiphilic polymer Soluplus® (SP) via low-temperature spray drying. Methods: The amount of Cur [...] Read more.
Background/Objectives: In this study, we present a green, scalable platform for the production of water-dispersible powders co-encapsulating the lipophilic bioactives curcumin (Cur) and eugenol (Eug) within the amphiphilic polymer Soluplus® (SP) via low-temperature spray drying. Methods: The amount of Cur (1%, 5%, and 10%) and Eug (5%, 10%, 15%, and 20%) was varied to achieve single- and double-loaded water-soluble powders with the maximum amount of active substances. The powders containing a higher loading of Cur, 5% and 10% (and Eug), were obtained from water/ethanol mixtures (2:1 and 5:1 v/v ratio), while the formulation with 1% of Cur was spray-dried by using water as a solvent. Results: By leveraging aqueous or aqueous–ethanolic feed systems, we achieved high loading of the bioactive substances—up to 10% Cur and 20% Eug (w/w)—while minimizing organic solvent use. Myo-inositol was incorporated as a stabilizing excipient to modulate particle morphology, improve powder flowability, and enhance redispersibility. Physicochemical characterization revealed nanoscale micellization (53–127 nm), amorphization of both actives as confirmed by XRD and DSC, and the absence of crystalline residue. Encapsulation efficiencies exceeded 95% for Cur and 93% for Eug. Dissolution tests demonstrated a rapid release from the 5% Cur/5% Eug formulation (>85% in 5 min), while higher-loaded single-formulations showed progressively slower release (up to 45 min). Conclusions: This work demonstrates a robust and environmentally responsible encapsulation strategy, suitable for delivering poorly water-soluble phytochemicals with potential applications in oral nutraceuticals and pharmaceutical dosage forms. Full article
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19 pages, 3569 KiB  
Article
Comprehensive Assessment and Freeze–Thaw Durability Prediction of Wet-Sprayed Concrete for Cold-Region Tunnels
by Haiyan Wang, Yanli Wang, Zhaohui Sun, Lichuan Wang, Hongtao Zhang, Wenhua Zheng and Qianqian Wang
Materials 2025, 18(13), 2955; https://doi.org/10.3390/ma18132955 - 22 Jun 2025
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Abstract
This study examines freeze–thaw deterioration patterns and predicts the service life of wet-sprayed concrete with composite cementitious materials in cold-region tunnels. The microstructure and particle size distribution of four materials (cement, fly ash, silica fume, and mineral powder) were analyzed. Subsequent tests evaluated [...] Read more.
This study examines freeze–thaw deterioration patterns and predicts the service life of wet-sprayed concrete with composite cementitious materials in cold-region tunnels. The microstructure and particle size distribution of four materials (cement, fly ash, silica fume, and mineral powder) were analyzed. Subsequent tests evaluated the rebound rate, mechanical properties, and durability of wet-sprayed concrete with various compositions and proportions of cementitious materials, emphasizing freeze–thaw resistance under cyclic freezing and thawing. A freeze–thaw deterioration equation was developed using damage mechanics theory to predict the service life of early-stage wet-sprayed concrete in tunnels. The results indicate that proportionally combining cementitious materials with different particle sizes and gradations can enhance concrete compactness. Adding mineral admixtures increases concrete viscosity, effectively reducing rebound rates and dust generation during wet spraying. Concrete incorporating binary and ternary mineral admixtures shows reduced early-age strength but significantly enhanced later-age strength. Its frost resistance is also improved to varying degrees. The ternary composite binder fills voids between cement particles and at the interface between paste and aggregate, resulting in a dense microstructure due to a ‘composite superposition effect.’ This significantly enhances the frost resistance of wet-mixed shotcrete, enabling it to withstand up to 200 freeze–thaw cycles, compared to failure after 75 cycles in plain cement concrete. The relative dynamic modulus of elasticity of wet-shotcrete follows a parabolic deterioration trend with increasing freeze–thaw cycles. Except for specimen P5 (R2 = 0.89), the correlation coefficients of deterioration models exceed 0.94, supporting their use in durability prediction. Simulation results indicate that, across all regions of China, the service life of wet-shotcrete with ternary admixtures can exceed 100 years, while that of plain cement concrete remains below 41 years. Full article
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