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20 pages, 6127 KB  
Article
Ultra-High-Performance Concrete Prepared with Manufactured Sand: Effects of Stone Powder Content on Fresh-State Fluidity and Mechanical Properties
by Yanzhou Peng, Hefei Yin, Jinlong Ma, Zhenyu Bao, Jian Yang and Gang Xu
Coatings 2026, 16(4), 414; https://doi.org/10.3390/coatings16040414 (registering DOI) - 29 Mar 2026
Abstract
This study investigates the preparation and performance of ultra-high-performance concrete (UHPC) incorporating manufactured sand as a full replacement for quartz sand. The mix design was optimized by integrating the compressible packing model (CPM) with an orthogonal experimental design. The influence of stone powder [...] Read more.
This study investigates the preparation and performance of ultra-high-performance concrete (UHPC) incorporating manufactured sand as a full replacement for quartz sand. The mix design was optimized by integrating the compressible packing model (CPM) with an orthogonal experimental design. The influence of stone powder content in manufactured sand—0, 5, 10, and 15% by mass of fine aggregate—on fresh-state fluidity and 7d-mechanical properties was systematically evaluated. Hydration products and microstructural features were analyzed using X-ray diffraction (XRD), scanning electron microscope (SEM), and mercury intrusion porosimetry (MIP). Results show that the manufactured sand-based UHPC achieved a fresh-state fluidity of 185 mm and a 7-day compressive strength of 152.4 MPa. Both fluidity and compressive strength exhibited a unimodal trend with increasing stone powder content, reaching maxima at 10%. Microstructural analysis revealed intimate interfacial bonding between unhydrated particles and calcium silicate hydrate (C–S–H) gel; notably, the UHPC matrix with 10% stone powder displayed the densest microstructure. MIP results further demonstrated that an optimal stone powder content effectively reduced total porosity, with the lowest overall porosity and the highest volume fractions of harmless (≤20 nm) and less harmful (20–100 nm) pores observed at 10%. These microstructural refinements collectively underpin the superior mechanical performance of manufactured sand-based UHPC. Full article
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35 pages, 2567 KB  
Review
Waste Glass Powder as a Circular-Economy Precursor in Geopolymer Binders
by Sri Ganesh Kumar Mohan Kumar, John M. Kinuthia, Jonathan Oti and Blessing O. Adeleke
Materials 2026, 19(7), 1357; https://doi.org/10.3390/ma19071357 (registering DOI) - 29 Mar 2026
Abstract
The transition toward low-carbon and resource-efficient construction materials has intensified interest in geopolymer binders incorporating industrial and post-consumer wastes. Waste glass powder (WGP), a silica-rich component of the global glass waste stream, has emerged as a promising circular-economy precursor in alkali-activated systems; however, [...] Read more.
The transition toward low-carbon and resource-efficient construction materials has intensified interest in geopolymer binders incorporating industrial and post-consumer wastes. Waste glass powder (WGP), a silica-rich component of the global glass waste stream, has emerged as a promising circular-economy precursor in alkali-activated systems; however, reported durability trends remain inconsistent and are often interpreted without mechanistic integration. This review synthesises current knowledge of WGP reactivity, gel chemistry, and long-term performance through an explicit reaction–transport–ageing (R–T–A) framework that links dissolution behaviour and phase assemblage development to pore connectivity, ion ingress, and time-dependent degradation. Under alkaline activation, the amorphous structure of WGP promotes silica release, modifying Si/Al ratios and governing the formation of N-A-S-H or hybrid N-A-S-H/C-(A)-S-H gels. These reaction products determine transport characteristics and ageing evolution, which collectively control chemical resistance, chloride ingress, alkali–silica reaction-type instability, and dimensional stability. Variability across studies is shown to arise from imbalances in particle fineness, replacement level, precursor chemistry, and activator design rather than intrinsic inconsistency in WGP behaviour. The R–T–A framework clarifies how reaction completeness, pore network architecture, and long-term phase stability interact to produce system-dependent durability outcomes. WGP demonstrates strong potential as a circular-economy precursor in alkali-activated binders; however, reliable structural application requires durability-informed mix design grounded in coupled reaction–transport–ageing mechanisms and supported by extended exposure testing under realistic service conditions. Full article
(This article belongs to the Special Issue Advanced Sustainable Cement-Based Materials)
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19 pages, 8877 KB  
Article
Comparative Performance of Ni- and Fe-Based Mixed Alloy Brazed Coatings via Laser Remelting
by Marco Brand, Mareen Goßling, Ion-Dragoş Uțu and Gabriela Mărginean
Lubricants 2026, 14(4), 142; https://doi.org/10.3390/lubricants14040142 (registering DOI) - 29 Mar 2026
Abstract
Traditionally, repairing coated substrates requires completely removing damaged, wear-resistant layers before recoating. This process leads to high costs, extended downtime, and material waste. Flexible brazing tapes, which are composed of alloy powder and an organic binder, offer an alternative to full coating removal [...] Read more.
Traditionally, repairing coated substrates requires completely removing damaged, wear-resistant layers before recoating. This process leads to high costs, extended downtime, and material waste. Flexible brazing tapes, which are composed of alloy powder and an organic binder, offer an alternative to full coating removal for targeted repairs. Despite this, the process of vacuum brazing these tapes may lead to the formation of defects, including pores caused by trapped gases or residual binder, which compromise coating durability and corrosion resistance. This study focuses on the utilization of laser remelting as a method for post-processing nickel- and iron-based mixed alloy brazing tapes, with the aim of improving the integrity of the coating. Surface quality was assessed via microscopy and microhardness testing by systematically varying laser power, scanning speed, and hatch distance. Among the parameters studied, the most suitable laser parameter combination was found to be 350 W laser power, 250 mm/s scanning speed, and a hatch distance of 0.02 mm. These parameters yielded crack- and pore-free coatings with a remelting depth of 160.3 ± 17.2 µm and a microhardness of 701 ± 23 HV1, which is an 85% increase over as-brazed samples. Wear testing revealed a reduced coefficient of friction, and electrochemical corrosion tests showed lower corrosion current density and enhanced repassivation behavior in remelted coatings. These improvements demonstrate that laser remelting significantly enhances the microstructure, hardness, wear resistance, and corrosion performance of brazed coatings, providing an effective method for localized repair while minimizing material consumption and processing duration. Full article
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39 pages, 4635 KB  
Article
Rice Husk Ash Geopolymers Modified with Fe3O4 or ZnTiO3/TiO2 Nanoparticles for the Adsorption and Photodegradation of Organic Dyes
by Ximena Jaramillo-Fierro, Juan-Pablo Cueva, John Ramón and Eduardo Valarezo
Nanomaterials 2026, 16(7), 413; https://doi.org/10.3390/nano16070413 (registering DOI) - 29 Mar 2026
Abstract
Hybrid nanomaterials integrating magnetic and semiconductor phases offer promising multifunctional platforms for wastewater remediation; however, their stabilization and recovery remain challenging. In this study, Fe3O4 and ZnTiO3/TiO2 nanoparticles were incorporated into a rice husk ash-based geopolymer matrix [...] Read more.
Hybrid nanomaterials integrating magnetic and semiconductor phases offer promising multifunctional platforms for wastewater remediation; however, their stabilization and recovery remain challenging. In this study, Fe3O4 and ZnTiO3/TiO2 nanoparticles were incorporated into a rice husk ash-based geopolymer matrix to develop hybrid nanocomposites for synergistic adsorption–photodegradation of methylene blue (MB) and methyl orange (MO). The materials were synthesized via alkaline activation followed by nanoparticle incorporation, and characterized by XRD, XRF, FTIR, SEM, EDX, BET surface area analysis, and pHPZC determination. XRD confirmed the presence of nanocrystalline Fe3O4 and ZnTiO3/TiO2 phases while preserving the amorphous aluminosilicate framework. Modified powders exhibited higher specific surface areas (up to 198 m2 g−1) compared to the unmodified geopolymer. Adsorption followed the Langmuir isotherm and pseudo-second-order kinetics, with spontaneous and exothermic behavior. Under UV irradiation, the ZnTiO3/TiO2-modified composite achieved photodegradation efficiencies up to 94% for MB and 92% for MO, whereas the Fe3O4-modified material combined adsorption capacity with magnetic recoverability. These results demonstrate that nanoparticle incorporation enables multifunctional performance while maintaining structural integrity of the geopolymeric matrix. Full article
(This article belongs to the Section Nanocomposite Materials)
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20 pages, 1151 KB  
Article
Response Surface Methodology-Optimized Ultrasonic-Assisted Extraction Combined with Folin–Ciocalteu Assay for Total Polyphenol Determination in Grape Seeds: Development and Application
by Chujun Li, Ruiqi Liu, Linlin Meng, Yuxin Meng, Shuang Xu, Xin Wang, Lihong Wang, Tao Lan and Tong Zhou
Appl. Sci. 2026, 16(7), 3306; https://doi.org/10.3390/app16073306 (registering DOI) - 29 Mar 2026
Abstract
A robust Folin–Ciocalteu method, coupled with an optimized ultrasonic-assisted extraction, was established for accurate quantification of total polyphenols in high-oil grape seed matrices, where lipid interference and low extraction efficiency have been persistent challenges. Samples were first defatted with n-hexane to eliminate lipid [...] Read more.
A robust Folin–Ciocalteu method, coupled with an optimized ultrasonic-assisted extraction, was established for accurate quantification of total polyphenols in high-oil grape seed matrices, where lipid interference and low extraction efficiency have been persistent challenges. Samples were first defatted with n-hexane to eliminate lipid interference. Key colorimetric parameters—Folin–Ciocalteu reagent volume, Na2CO3 concentration, reaction temperature, and time—were systematically optimized and validated for linearity, precision, and recovery. Subsequently, using defatted grape seed powder as the raw material, a four-factor, three-level Box–Behnken design combined with response surface methodology was employed to optimize the four extraction parameters: solid-to-liquid ratio, ethanol concentration, extraction temperature, and extraction time. The optimal conditions were 0.5 mL of Folin–Ciocalteu reagent, 20% Na2CO3, and reaction at 30 °C for 2.0 h, yielding a linear calibration curve (R2 = 0.9991) with satisfactory methodological validation. Optimal extraction (52% ethanol, 1:50 w/v, 68 °C, 21 min) achieved a total polyphenol content of 2.93 × 104 mg·kg−1, closely matching the predicted value (relative error = 0.34%). Analysis of seven grape seed varieties from the Hebei Province revealed significant content variation (p < 0.05), ranging from 3.24 to 7.47 × 104 mg·kg−1, with Rose grape seeds exhibiting the highest level. The developed method effectively overcame matrix interference from high oil content, offering a reliable, efficient tool for screening high-polyphenol grape seed varieties and supporting the development of value-added functional products. Full article
19 pages, 34013 KB  
Article
Correlation Between Manufacturing Conditions, Microstructure, and Electrical–Mechanical Properties of Cu Matrix Composites
by Marko Simić, Emilija Nidžović, Svetlana Butulija, Željko Radovanović, Marija M. Vuksanović and Jovana Ružić
Materials 2026, 19(7), 1347; https://doi.org/10.3390/ma19071347 (registering DOI) - 28 Mar 2026
Abstract
The continuous demand for advanced composite materials with superior mechanical and electrical properties has driven the exploration of copper matrix composites for high-performance applications. The Cu–2Zr–0.6B (wt.%) powder mixtures were mechanically alloyed (MA) using two different ball-to-powder weight ratios (BPR: 10:1 and 15:1) [...] Read more.
The continuous demand for advanced composite materials with superior mechanical and electrical properties has driven the exploration of copper matrix composites for high-performance applications. The Cu–2Zr–0.6B (wt.%) powder mixtures were mechanically alloyed (MA) using two different ball-to-powder weight ratios (BPR: 10:1 and 15:1) to investigate the influence of milling conditions on the final composite material’s properties. MA powders milled with BPR 15:1 exhibited the highest values of dislocation densities, which induce higher hardness of Cu–ZrB2 bulk materials. The MA powders were consolidated using three different methods: conventional cold pressing followed by sintering (CPS), hot pressing (HP), and spark plasma sintering (SPS). The in situ forming of ZrB2 (3.5 vol.%) reinforcements during consolidation processes in Cu matrix proved to have a major impact on enhancing the hardness and structural stability, while the use of SPS and HP offered superior control over grain growth and porosity reduction compared to CPS. Main findings related to electrical and mechanical properties showed similar values for SPS (~38% IACS, ~173 HV1) and HP compacts (~39% IACS, ~155 HV1) but proved to be much higher compared to values of CPS compacts (~21% IACS, ~80 HV1). Full article
(This article belongs to the Section Advanced Composites)
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27 pages, 3188 KB  
Article
From Cell Physiology to Process Design: Spray-Drying-Based Production of a Stable and Functional Ensifer meliloti Bioinoculant
by Florencia Belén Alvarez Strazzi, María Evangelina Carezzano, Martina Guerrieri Magrini, Ladislao Iván Díaz Vergara, Walter Giordano and Pablo Bogino
Processes 2026, 14(7), 1094; https://doi.org/10.3390/pr14071094 (registering DOI) - 28 Mar 2026
Abstract
The formulation of rhizobial bioinoculants remains a critical bottleneck for the large-scale deployment of biological nitrogen fixation in sustainable agriculture, mainly due to limitations in the stability and viability of conventional liquid products. In this study, a spray-drying-based process was developed and optimized [...] Read more.
The formulation of rhizobial bioinoculants remains a critical bottleneck for the large-scale deployment of biological nitrogen fixation in sustainable agriculture, mainly due to limitations in the stability and viability of conventional liquid products. In this study, a spray-drying-based process was developed and optimized to produce a stable and functional bioinoculant using Ensifer meliloti Rm8530, an EPS II–producing strain with enhanced stress tolerance. Strain robustness was evaluated through thermal and osmotic stress assays, together with growth performance across relevant temperature and pH ranges. Six carrier-based formulations combining polysaccharides and proteins were then tested under controlled spray-drying conditions. Process performance was assessed in terms of powder recovery, residual moisture, bacterial survival, yield, and storage stability over 16 weeks. The morphological integrity of spray-dried particles and rehydrated cells was analyzed by scanning electron microscopy. The biological functionality of selected formulations was subsequently validated in planta using alfalfa as a host model. Among the formulations tested, a mixed alginate–gum Arabic matrix showed the best overall balance between process efficiency, post-drying viability, long-term stability, and symbiotic performance. Spray-dried cells retained the ability to induce nodulation and support early plant responses under the conditions evaluated. These results demonstrate that spray drying, combined with appropriate strain selection and formulation design, constitutes a viable and scalable platform for producing stable, functional rhizobial bioinoculants. Full article
(This article belongs to the Section Biological Processes and Systems)
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23 pages, 11197 KB  
Article
Determination of Particle Size of Active Pharmaceutical Ingredients in Dry Powder Inhaler Formulations
by Stefani Fertaki, Malvina Orkoula and Christos Kontoyannis
Pharmaceuticals 2026, 19(4), 543; https://doi.org/10.3390/ph19040543 (registering DOI) - 28 Mar 2026
Abstract
Background/Objectives: Accurate determination of active pharmaceutical ingredient (API) particle size within dry powder inhaler (DPI) formulations is essential for ensuring effective pulmonary delivery but remains analytically challenging due to low API content and micronized particle size. Methods: In this study, scanning electron microscopy [...] Read more.
Background/Objectives: Accurate determination of active pharmaceutical ingredient (API) particle size within dry powder inhaler (DPI) formulations is essential for ensuring effective pulmonary delivery but remains analytically challenging due to low API content and micronized particle size. Methods: In this study, scanning electron microscopy (SEM) coupled with energy-dispersive X-ray microanalysis (EDX) was used to directly identify and calculate the API particle size within several different commercial DPI products fit for purpose under regulatory constraints. The method exploits unique elemental markers inherent to each API, enabling reliable discrimination from excipients without prior sample modification or API extraction. Results: Large-area SEM–EDX mapping was used to localize API particles, followed by high-magnification imaging and confirmatory spot microanalysis. Particle sizes were manually measured for at least 50 API particles per formulation using image analysis software, and particle size distribution parameters were calculated from equivalent spherical diameters. Conclusions: The methodology was successfully applied to Spiriva®, Anoro® Ellipta, and Relvar® Ellipta inhalation powders, revealing micronized APIs with distinct morphological features and verifying systematic application across products. Cross-validation against laser diffraction measurements of pure APIs demonstrated statistical equivalence, confirming the robustness and analytical utility of the proposed method for particle size assessment in DPI formulations. Full article
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23 pages, 5229 KB  
Article
Experimental Investigation of Surface Integrity Analysis Using Machine Learning for Nano-Powder Mixed Electrical Discharge Machining
by Amreeta R. Kaigude, Nitin K. Khedkar and Vijaykumar S. Jatti
J. Manuf. Mater. Process. 2026, 10(4), 115; https://doi.org/10.3390/jmmp10040115 (registering DOI) - 28 Mar 2026
Abstract
This research investigates the optimization of surface integrity in powder-mixed electrical discharge machining (PMEDM) through the innovative use of Jatropha biodielectric fluid enhanced with titanium dioxide (TiO2) nanoparticles. A comprehensive experimental framework was developed using design expert software (DOE) with Response [...] Read more.
This research investigates the optimization of surface integrity in powder-mixed electrical discharge machining (PMEDM) through the innovative use of Jatropha biodielectric fluid enhanced with titanium dioxide (TiO2) nanoparticles. A comprehensive experimental framework was developed using design expert software (DOE) with Response Surface Methodology (RSM) to systematically analyze the machining of AISI D2 tool steel using copper electrodes. The study examined five critical process parameters, gap current (Ip), pulse-on duration (Ton), pulse-off time (Toff), gap voltage (V), and powder concentration, evaluating their combined effects on surface roughness (SR), surface crack density (SCD), and residual stress characteristics. Advanced characterization techniques including scanning electron microscopy (SEM) were employed to analyze surface topography and subsurface microstructural changes. The optimization process successfully identified optimal machining conditions of current = 9 A, Ton = 100 µs, Toff = 10 µs, and gap voltage = 65 V, achieving exceptional surface quality with a minimum surface roughness of 3.22 µm. Remarkably, these optimized parameters resulted in crack-free surfaces with zero surface crack density and minimal residual stress values across the 2θ range of 90° to 180°. To enhance predictive capabilities, supervised machine learning algorithms were implemented to model surface roughness behavior. Comparative analysis of classification algorithms demonstrated that Support Vector Machine (SVM), k-Nearest Neighbors (kNNs), and Gaussian Naïve Bayes achieved superior performance with F1-scores of 0.88 and prediction accuracies of 90%. The integration of sustainable Jatropha biodielectric with TiO2 nanoparticles represents a significant advancement in environmentally conscious precision machining, while the machine learning approach establishes a robust framework for intelligent process optimization and quality prediction in advanced manufacturing applications. Full article
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15 pages, 684 KB  
Article
Odor-Free Lyophilized Trout (Oncorhynchus mykiss) Powder in Gluten-Free Pasta: Nutritional, Techno-Functional, Sensory and Digestibility Evaluation
by Özlem Emir Çoban, Hülya Gül, Mücahit Eroğlu, Tuba Okutan, İlhan Firat Kilinçer and Feray Çağiran Yilmaz
Foods 2026, 15(7), 1155; https://doi.org/10.3390/foods15071155 (registering DOI) - 28 Mar 2026
Abstract
Gluten-free (GF) products developed for individuals with celiac disease and gluten sensitivity often suffer from low protein and mineral content. Fish proteins offer a promising solution to address these deficiencies; however, the characteristic “fishy odor” and related technological challenges limit consumer acceptance. This [...] Read more.
Gluten-free (GF) products developed for individuals with celiac disease and gluten sensitivity often suffer from low protein and mineral content. Fish proteins offer a promising solution to address these deficiencies; however, the characteristic “fishy odor” and related technological challenges limit consumer acceptance. This study aimed to develop an innovative GF pasta with improved nutritional density and acceptable sensory quality by incorporating deodorized and lyophilized trout powder. GF pasta formulations were prepared using buckwheat flour, xanthan gum, and 5% or 10% odorless trout powder. Vinegar pretreatment was applied to reduce fish odor, while lyophilization was chosen to minimize nutrient losses. The samples were analyzed for nutritional composition, techno-functional properties, in vitro digestibility, and sensory attributes. Results showed that trout powder significantly increased protein and ash content compared to the control (p < 0.05). A slight darkening was observed in color analysis due to fish pigments and buckwheat phenolics, but overall visual stability remained high. In vitro digestibility revealed enhanced protein digestibility (p < 0.05) and a slight reduction in starch digestibility. Sensory evaluation demonstrated that odor scores (8) at 10% trout inclusion remained close to the control, reversing the commonly reported decline in acceptance with increasing fish content. These findings indicate that combining vinegar pretreatment with lyophilization enables the incorporation of fish proteins into GF pasta without sensory disadvantages, while simultaneously improving nutritional quality. Full article
(This article belongs to the Section Grain)
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22 pages, 12860 KB  
Article
Valorization of Spent Coffee Grounds and Brewer’s Spent Grain Waste Toward Toughening of a Biodegradable PBAT/PHBH Blend
by Shabnam Yavari, Nima Esfandiari, Elsa Lasseuguette, Mohd Shahneel Saharudin and Reza Salehiyan
J. Compos. Sci. 2026, 10(4), 185; https://doi.org/10.3390/jcs10040185 (registering DOI) - 28 Mar 2026
Abstract
Plastic pollution from packaging waste is driving the development of biodegradable composites for sustainable packaging. In this work, poly(butylene adipate-co-terephthalate)/poly(3-hydroxybutyrate) (PBAT/PHBH) blends (50/50 wt.%) were reinforced with agro-industrial waste fillers—spent coffee grounds (SCG), brewer’s spent grain (BSG), and cellulose powder (CP)—at 1–15 wt.% [...] Read more.
Plastic pollution from packaging waste is driving the development of biodegradable composites for sustainable packaging. In this work, poly(butylene adipate-co-terephthalate)/poly(3-hydroxybutyrate) (PBAT/PHBH) blends (50/50 wt.%) were reinforced with agro-industrial waste fillers—spent coffee grounds (SCG), brewer’s spent grain (BSG), and cellulose powder (CP)—at 1–15 wt.% loading. The effects of these fillers on tensile properties, impact strength, and thermal stability were examined and supported by scanning electron microscopy (SEM) of fracture surfaces and thermogravimetric analysis (TGA). The neat PBAT/PHBH blend exhibited balanced stiffness and ductility. Low BSG loadings (≤5 wt.%) produced the greatest toughening, with impact strength increasing by ~92% and elongation at break significantly improving over the neat blend. SEM analysis indicated crack deflection and particle pull-out as dominant energy-dissipation mechanisms at low BSG loading. At higher BSG loading (15 wt.%), particle clustering and larger voids acted as stress concentrators, reducing impact performance. SCG improved ductility at low loading (1 wt.%), whereas increasing SCG content led to progressive reductions in tensile strength and elongation due to increased debonding and microvoid formation. In contrast, CP exhibited minimal reinforcement efficiency within the investigated range (1–5 wt.%). Overall, filler addition generally reduced tensile strength and, in several cases, tensile modulus, reflecting limited interfacial compatibility between the hydrophilic lignocellulosic fillers and the hydrophobic polyester matrix. TGA indicated a modest improvement in thermal stability at higher BSG loadings, reflected by shifts in T5% and Tmax1 (PHBH) toward higher temperatures. Overall, this study demonstrates that upcycled coffee and beer waste fillers can impart specific toughness benefits to biodegradable PBAT/PHBH blends, but interfacial incompatibility currently limits their reinforcement efficiency. The findings highlight the potential and challenges of these biocomposites for sustainable packaging applications and suggest that interface engineering (e.g., compatibilizers) will be key to unlocking optimal performance. Full article
(This article belongs to the Special Issue Sustainable Polymer Composites: Waste Reutilization and Valorization)
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17 pages, 3090 KB  
Article
Recovery of Separator from Battery Waste by Supercritical Carbon Dioxide Extraction: Removal of Electrolyte and Electrode Contaminants
by Martin Östergren, Philipp Mikšovsky and Burçak Ebin
Batteries 2026, 12(4), 118; https://doi.org/10.3390/batteries12040118 (registering DOI) - 28 Mar 2026
Abstract
Hazardous compounds from used batteries pose a great threat to the environment. To prevent pollution and to recover critical materials from battery waste, efficient recycling is required. Until now, battery recycling has focused on the recovery of valuable metals from cathode materials, while [...] Read more.
Hazardous compounds from used batteries pose a great threat to the environment. To prevent pollution and to recover critical materials from battery waste, efficient recycling is required. Until now, battery recycling has focused on the recovery of valuable metals from cathode materials, while organic fractions have often been neglected due to their low material value. New approaches to battery recycling are therefore necessary, where recycling methods based on supercritical carbon dioxide (SC-CO2) extraction show great potential. In this work, a SC-CO2 method was implemented to extract electrolyte solvents for the purification and recovery of a separator waste material (SWM) sorted out from lithium-ion battery (LIB)-based black mass. In addition, two other separation routes (ultrasonic washing and thermal treatment) were used for comparison. Based on the results from the three routes, mass balances revealed the gravimetric composition of the SWM, which includes separator, electrolyte, and electrode powder. The composition of electrolyte solvents was determined via Gas Chromatography-Mass Spectroscopy analysis. Furthermore, the polymeric separator was analyzed using Fourier Transform Infrared Spectroscopy, Thermogravimetric Analysis, and Differential Scanning Calorimetry analysis to evaluate the effects of SC-CO2 extraction on the physicochemical properties. The recovery of electrolyte by the SC-CO2 route is more efficient than the others, with extraction yields of 162 mg of electrolyte per gram of SWM. Moreover, no changes are observed in the analyzed properties of the polymeric separator material due to the SC-CO2 extraction. Thus, the SC-CO2 process proves to be a promising method for an efficient and sustainable recycling of electrolyte solvent and purifying of separator material from LIB waste. Full article
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33 pages, 5971 KB  
Article
Energy-Efficient and Reliable Hydrodynamic Separation of Spent Drilling Fluids: Experiments, Modeling, and Process Stability
by Bakytzhan Kaliyev, Beibit Myrzakhmetov, Bulbul Mauletbekova, Bibinur Akhymbayeva, Gulzada Mashatayeva, Yerik Merkibayev, Vladimir I. Golik and Boris V. Malozyomov
Energies 2026, 19(7), 1659; https://doi.org/10.3390/en19071659 - 27 Mar 2026
Abstract
The treatment of spent drilling fluids generated during the drilling of technological wells for uranium production represents an important engineering and environmental challenge associated with high energy consumption, significant waste generation, and the need for rational water use under arid regional conditions. Conventional [...] Read more.
The treatment of spent drilling fluids generated during the drilling of technological wells for uranium production represents an important engineering and environmental challenge associated with high energy consumption, significant waste generation, and the need for rational water use under arid regional conditions. Conventional phase separation methods based on gravitational settling and chemical–mechanical treatment are characterized by limited process controllability, long processing times, and increased consumption of reagents and energy. This study proposes an energy-efficient and reliable hydrodynamic technology for the treatment of spent drilling fluids based on the formation of controlled turbulent structures without the use of mechanical drives. The research object comprised spent drilling fluids (SDFs) generated during the drilling of technological wells for uranium production in the southern regions of the Republic of Kazakhstan and the Kyzylorda region. Experimental investigations were carried out using a laboratory–pilot hydrodynamic disperser with variations in velocity gradient, treatment time, flocculant dosage, and suspension flow rate. A mathematical model linking hydrodynamic process parameters with phase separation kinetics and energy characteristics was developed. Model calibration by weighted nonlinear least squares yielded a stable parameter set with 95% confidence intervals, and model validation demonstrated good agreement between calculated and experimental data (MAPE 8.4%; maximum relative error 11.8%). It was established that the use of a hydrodynamic disperser provides separation efficiency of up to 90–95% under optimal operating conditions while reducing specific energy consumption and maintaining stable repeated-cycle performance within the investigated operating window. Experimental results confirm that implementation of the hydrodynamic technology enables a reduction in sludge volume by 40–60%, recovery of up to 60–80% of process water, and a significant decrease in waste requiring transportation and disposal. The obtained results demonstrate the high environmental and resource-saving efficiency of the proposed technology and its suitability for scaling and industrial implementation at facilities drilling technological wells for uranium production. The developed hydrodynamic approach can be considered an effective engineering platform for creating energy-efficient and sustainable systems for drilling fluid treatment in regions with limited water resources and remote industrial infrastructure. Full article
(This article belongs to the Section B: Energy and Environment)
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26 pages, 3344 KB  
Article
Influence of Ethanol on Ultrasound-Assisted Extraction of Bioactive Compounds from Cocoa Pod Husk and Their Antioxidant, Antihypertensive, and Antihyperglycemic Activity
by Fanny Adabel González-Alejo, Areli Carrera-Lanestosa, Mario Moscosa-Santillán, Ricardo García-Alamilla, Jesús Alfredo Araujo-León, Diakaridia Sangaré, Juan José Acevedo-Fernández and Pedro García-Alamilla
ChemEngineering 2026, 10(4), 43; https://doi.org/10.3390/chemengineering10040043 - 27 Mar 2026
Abstract
Cocoa pod husk (CPH), a major agro-industrial residue, contains valuable bioactive compounds whose recovery can support sustainable waste valorization. This study evaluated the influence of increasing ethanol concentrations on the ultrasound-assisted extraction (UAE) of bioactive compounds from CPH and their antioxidant, antihypertensive, and [...] Read more.
Cocoa pod husk (CPH), a major agro-industrial residue, contains valuable bioactive compounds whose recovery can support sustainable waste valorization. This study evaluated the influence of increasing ethanol concentrations on the ultrasound-assisted extraction (UAE) of bioactive compounds from CPH and their antioxidant, antihypertensive, and antihyperglycemic activity. Dried and milled CPH was extracted using ethanol–water mixtures (0–100% ethanol) under fixed ultrasonic conditions. Cocoa pod husk powder characterization and the resulting extracts were analyzed in terms of chemical composition (lignocellulosic compounds, proximate and elemental composition, and bromatological composition), antioxidant capacity, and in vivo antihypertensive and antihyperglycemic effects in Wistar rats. The results showed that solvent polarity strongly modulated extraction efficiency: absolute ethanol yielded the highest phenolic (171.43 mg GAE/g) and flavonoid (132.05 mg QE/g) content, whereas hydroalcoholic mixtures, particularly 50:50, enhanced overall antioxidant performance, especially in FRAP. The chemical analysis results showed the selective recovery of compounds such as quercetin, hesperidin, and theobromine, and FTIR-PCA results revealed distinct solvent-dependent chemical profiles. In vivo assays indicated modest blood pressure stabilization and a more pronounced antihyperglycemic effect after chronic administration. Overall, UAE proved an effective, rapid, and solvent-efficient method for CPH valorization, highlighting its potential for producing natural antioxidants applicable to food, nutraceutical, and cosmetic formulations. Full article
(This article belongs to the Topic Separation Techniques and Circular Economy)
19 pages, 11526 KB  
Article
Pharmaceutical Co-Crystal Formulation of Rivaroxaban with Niacinamide: Preparation, Characterization, and In Vitro Release Evaluation
by Cristina Solomon, Iulian Sarbu, Valentina Anuța, Emma Adriana Ozon, Adina Magdalena Musuc, Adriana Rusu, Vasile-Adrian Surdu, Abhay Chandak, Roxana Mariuca Gavriloaia, Ancuța Cătălina Fița, Denisa Teodora Nită and Mirela Adriana Mitu
Materials 2026, 19(7), 1336; https://doi.org/10.3390/ma19071336 - 27 Mar 2026
Abstract
The present study investigates the co-crystallization process of rivaroxaban (RIV), a poorly water-soluble potent oral anticoagulant, with niacinamide (NIA), a highly soluble and pharmaceutically acceptable co-crystal former, in two different molar ratios (1:1 and 1:2). The aim was to enhance the physicochemical and [...] Read more.
The present study investigates the co-crystallization process of rivaroxaban (RIV), a poorly water-soluble potent oral anticoagulant, with niacinamide (NIA), a highly soluble and pharmaceutically acceptable co-crystal former, in two different molar ratios (1:1 and 1:2). The aim was to enhance the physicochemical and biopharmaceutical properties of rivaroxaban such as dissolution rate and aqueous solubility, by forming stable co-crystals through a solvent evaporation technique. The resulting co-crystals (RIV-NIA, 1:1 co-crystallization compound, F1 and RIV-NIA, 1:2 co-crystallization compound, F3) were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), powder X-ray diffraction (XRD) and thermal analysis, which confirmed the formation of a new rivaroxaban–niacinamide co-crystalline phase. In vitro dissolution studies confirmed a significant enhancement in the dissolution rate of the two obtained co-crystals. These findings suggest that stoichiometric variation plays an important role in co-crystal performance and in improving solubility compared with the pure drug. Also, the obtained results suggest that niacinamide is an effective coformer for improving the dissolution and physicochemical properties of rivaroxaban. Full article
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