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Search Results (1,574)

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Keywords = biocomposite

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16 pages, 4447 KiB  
Article
Innovative Hemp Shive-Based Bio-Composites, Part II: The Effect of the Phase Change Material (PCM) Additive on Characteristics of Modified Potato Starch Binders
by Laura Vitola, Ina Pundiene, Jolanta Pranckevičienė and Diana Bajare
Materials 2025, 18(4), 891; https://doi.org/10.3390/ma18040891 - 18 Feb 2025
Viewed by 255
Abstract
This study investigates the effect of phase change materials (PCM) on the properties of modified potato starch binders and hemp shive-based bio-composites, emphasizing their potential for sustainable construction applications. PCM-modified binders have shown reduced viscosity during gelatinization, enhancing their workability and uniformity during [...] Read more.
This study investigates the effect of phase change materials (PCM) on the properties of modified potato starch binders and hemp shive-based bio-composites, emphasizing their potential for sustainable construction applications. PCM-modified binders have shown reduced viscosity during gelatinization, enhancing their workability and uniformity during processing. A microstructural analysis reveals that PCM addition results in a denser and more cohesive binder network, leading to improved adhesion and reduced porosity. A thermal analysis demonstrates a shift to higher decomposition temperatures and a linear increase in specific heat capacity within the PCM phase-change range (20–30 °C), significantly enhancing the thermal storage capacity of the bio-composites. PCM addition improves compressive strength by up to twice, with optimal performance achieved at 8% PCM additive content. The prolonged cooling time, up to three times longer in bio-composites with PCM additive, highlights their effectiveness in thermal regulation. Additionally, bio-composites with a PCM additive exhibits increased bulk density and reduced water swelling, improving dimensional stability. These findings underline the dual benefits of enhanced thermal and mechanical performance in bio-composites with a PCM additive, making them a viable alternative to conventional building materials. Full article
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<p>Preparation scheme of studied binders and bio-composites.</p>
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<p>Viscosity of obtained potato starch binder.</p>
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<p>Micro-structure of B-0 and B-32.</p>
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<p>FTIR of obtained potato starch binders.</p>
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<p>TGA/DSC of obtained potato starch binder.</p>
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<p>Obtained bio-composites.</p>
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<p>Microstructure of BC-0 and BC-32.</p>
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<p>The index of the material density of the obtained bio-composites depending on the PCM amount in the composition.</p>
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<p>The index of swelling of the obtained bio-composites depending on the PCM amount in the composition (pale purple area—region indicating improved swelling performance compared to the reference sample BC-0).</p>
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<p>The index of the compressive strength of the bio-composite samples depending on the PCM amount in the composition (pale purple area—region indicating improved compressive strength performance compared to the reference sample BC-0).</p>
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<p>Heat capacity and thermal conductivity of obtained bio-composites.</p>
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<p>The cool-down time of the obtained bio-composites.</p>
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18 pages, 3008 KiB  
Article
Influence of Cooling Rate on the Flexural and Impact Properties of Compression Molded Non-Woven Flax/PLA Biocomposites
by Anurag Pisupati, Marco Curto, Thomas Laurent, Benoit Cosson, Chung Hae Park and Hom Nath Dhakal
Polymers 2025, 17(4), 493; https://doi.org/10.3390/polym17040493 - 13 Feb 2025
Viewed by 333
Abstract
This work investigates the influence of crystallinity on the mechanical properties of needle-punched non-woven flax/polylactic acid (PLA) biocomposites with different flax fiber contents. Biocomposites were fabricated by a compression molding adopting different cooling rates to understand the mechanism of crystallinity and their contribution [...] Read more.
This work investigates the influence of crystallinity on the mechanical properties of needle-punched non-woven flax/polylactic acid (PLA) biocomposites with different flax fiber contents. Biocomposites were fabricated by a compression molding adopting different cooling rates to understand the mechanism of crystallinity and their contribution to the mechanical properties. Image-based analysis of the fiber distribution in non-woven preform indicates the probable origins of the residual porosities and the potential nucleation sites for crystal formation within the composites. The improvement of 25% and 100% in flexural modulus is observed for the composites with 40% and 50% of flax fiber mass fractions, respectively, when subjected to a lower cooling rate, which implies the significant influence of the void content on the brittleness of composites. The impact properties of the composites decrease from 11% to 18% according to the flax fiber mass fraction when the cooling rate decreases to 1 °C/min, and the composites become more brittle. The induced impact and flexural properties of the composites are compared with those of other composites in the literature to emphasize their applicability to semi-structural applications. Full article
(This article belongs to the Topic Advanced Composites Manufacturing and Plastics Processing)
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<p>Schematic representation of the carding process.</p>
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<p>Stepped consolidation cycle in compression molding.</p>
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<p>Contour plots of fiber distributions in different flax/PLA non-wovens.</p>
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<p>Nonisothermal crystallization kinetics of flax/PLA non-woven composites.</p>
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<p>Thermal behavior of flax/PLA composites.</p>
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<p>Residual void content and crystallinity of flax/PLA composites.</p>
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<p>Experimental setups for mechanical characterization: flexural tests (<b>left</b>) and impact tests (<b>right</b>).</p>
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<p>Flexural properties of flax/PLA composites subjected to different cooling rates.</p>
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<p>Impact properties of flax/PLA composites subjected to different cooling rates.</p>
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29 pages, 10857 KiB  
Article
Improved Mechanical and Thermal Properties of Date Palm Microfiber-Reinforced PCL Biocomposites for Rigid Packaging
by Sakib Hossain Khan, Hom N. Dhakal, Abu Saifullah and Zhongyi Zhang
Molecules 2025, 30(4), 857; https://doi.org/10.3390/molecules30040857 - 13 Feb 2025
Viewed by 565
Abstract
To increase the use of agricultural residues, such as date palm fibers, for the sustainable reinforcement of biocomposites, this study investigated the incorporation of varying weight percentages of date palm microfibers (DPMF) ranging from 0 wt.% to 10 wt.% into polycaprolactone (PCL) matrix. [...] Read more.
To increase the use of agricultural residues, such as date palm fibers, for the sustainable reinforcement of biocomposites, this study investigated the incorporation of varying weight percentages of date palm microfibers (DPMF) ranging from 0 wt.% to 10 wt.% into polycaprolactone (PCL) matrix. Biocomposites were fabricated using a combination of compression molding and dry blending techniques with and without sodium hydroxide (NaOH) alkali treatment. The surface modification was found to increase the surface roughness of the fibers, removing impurities such as lignin, hemicellulose, and wax, while improving crystallinity, as evidenced by FTIR, XRD, TGA, and particle size analyses. Among the different biocomposites investigated, the results for 5 wt.% DPMF content biocomposites exhibited the highest tensile properties: approximately 20% increase in tensile strength and 164% increase in Young’s Modulus in comparison to neat PCL. The crystallinity of the matrix exhibited an increasing trend from approximately 39% for neat PCL to 43% for the 5 wt.% DPMF biocomposites. Furthermore, treated biocomposites demonstrated higher water-repellency behavior and improved thermal properties. Dynamic mechanical analysis (DMA) results indicated enhanced storage moduli for alkali-treated composites; at 35 °C, the storage modulus showed approximately 22% increase compared to the untreated DPMF biocomposites, reflecting improved stiffness and thermomechanical performances. This study highlights the potential of DPMF as an efficient, eco-friendly alternative to fossil-based conventional reinforcement for biocomposite materials’ potential for sustainable rigid packaging applications. Full article
(This article belongs to the Topic Biomass for Energy, Chemicals and Materials)
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Graphical abstract

Graphical abstract
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<p>Steps involved in extraction of cellulosic materials from agricultural residues.</p>
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<p>Suitability of DPMFs and PCL in packaging application.</p>
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<p>Dry blending–compression molding benefits.</p>
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<p>Fiber-grinding process: (<b>a</b>) date palm leaf fibers; (<b>b</b>) RETSCH Ultra Centrifugal Mill ZM 300; (<b>c</b>) date palm micro-fibers.</p>
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<p>Description of dry-blending process used for biocomposites fabrication: (<b>a</b>) polymer grinding; (<b>b</b>) shear mixing of fibers and polymer; (<b>c</b>) compression molding; (<b>d</b>) final biocomposites plates.</p>
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<p>The neat PCL and different concentrations of DPMF composites where the samples became darker with the increase in micro-fiber content compared to the neat PCL.</p>
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<p>FTIR spectra for untreated and treated DP microfibers.</p>
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<p>X-ray diffraction (XRD) spectra of untreated and treated DP microfibers.</p>
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<p>Crystallinity index versus NaOH concentration for agave fibers [<a href="#B44-molecules-30-00857" class="html-bibr">44</a>] (Copyright License number: 5956470259977).</p>
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<p>Thermogravimetric Analysis (TGA): (<b>a</b>) weight loss versus temperature traces; (<b>b</b>) derivative thermogravimetric (DTG) of untreated and alkali-treated date palm microfibers.</p>
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<p>Cumulative distribution of the particle size of the untreated and treated date palm micro-fibers.</p>
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<p>Optical microscopy images (<b>a</b>,<b>b</b>) untreated microfiber; (<b>c</b>,<b>d</b>) treated micro-fiber.</p>
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<p>(<b>a</b>) Tensile strength and (<b>b</b>) Young’s Modulus of the untreated and treated date palm–PCL biocomposites.</p>
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<p>(<b>a</b>) Flexural strength and (<b>b</b>) flexural modulus of the untreated and treated date palm microfiber–PCL biocomposites.</p>
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<p>X-ray μCT micrographs of (<b>a</b>) 2.5 wt.%, (<b>b</b>) 5 wt.%, and (<b>c</b>) 10 wt.% date palm microfiber-reinforced PCL composites.</p>
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<p>Moisture absorption curves (<b>a</b>) for 10% and 5% with respect to time; (<b>b</b>) moisture absorption of all samples.</p>
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<p>DSC heating curves (<b>a</b>) for neat PCL with 5 and 10% DPF-PCL composite samples (<b>b</b>) for treated and untreated DPMF composite samples.</p>
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<p>(<b>a</b>) Storage modulus curve for neat PCL and different DPMF composites; (<b>b</b>) storage modulus for treated and untreated DPMF composites.</p>
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<p>(<b>a</b>) Viscosity with respect to frequency; (<b>b</b>) viscosity with respect to shear rate; (<b>c</b>) storage modulus; (<b>d</b>) loss modulus with respect to frequency.</p>
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<p>Curves of viscosity versus shear rate for alkali-treated DPF and untreated DPF.</p>
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<p>TGA of 5% and 10% treated DPMF-PCL biocomposites.</p>
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<p>SEM images of fractured region; (<b>a</b>,<b>b</b>) untreated date palm fiber composites; (<b>c</b>–<b>f</b>) treated date palm fiber composites.</p>
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30 pages, 1693 KiB  
Article
Greener Packaging Solutions: The Social Impact of Biocomposite Lids in Colombia
by Lady-Joana Rodríguez, Juan D. Galvis-Nieto and Carlos E. Orrego
Sustainability 2025, 17(4), 1426; https://doi.org/10.3390/su17041426 - 10 Feb 2025
Viewed by 495
Abstract
Biocomposite materials respond to market trends and regulatory pressures for environmentally friendly packaging. Few studies have assessed the social life cycle assessment (SLCA) using stakeholder indicators across the entire supply chain. The objective of this study is to provide reliable indicators and data [...] Read more.
Biocomposite materials respond to market trends and regulatory pressures for environmentally friendly packaging. Few studies have assessed the social life cycle assessment (SLCA) using stakeholder indicators across the entire supply chain. The objective of this study is to provide reliable indicators and data to compare the SLCA of jar lid biocomposites filled with post-harvest banana fibers (BFs) in Colombia. Methodologies from the United Nations Environment Programme, the relevant literature, and Colombian regulations were used to select indicators. A comprehensive survey involved all stakeholders in the supply chain and consumer responsibility during the use phase. The data collected were integrated, scored, and weighted. This approach aimed to reduce uncertainty in comparing different scenarios and contribute to the standardization and integration of SLCA methods. The study highlights the significant benefits of incorporating banana fibers (BFs) into jar lids. Lids composed of 40% BFs provide notable social advantages, particularly within the agricultural sector. They contribute to improving the economic income and quality of life for farmers, transporters, and intermediaries while promoting equity among them. Additionally, these lids help preserve cultural heritage in local communities. From a corporate perspective, beyond financial gains, companies enhance their sustainability visibility by offering a product that is environmentally friendly, naturally sourced, and directly connected to farmers. Furthermore, these lids strengthen the overall social impact of the supply chain and business sector by utilizing renewable and locally available resources. Full article
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<p>General methodology for the SLCA study. Figure designed by the authors based on Refs. [<a href="#B29-sustainability-17-01426" class="html-bibr">29</a>,<a href="#B30-sustainability-17-01426" class="html-bibr">30</a>]. Only by contextualizing the social and legal aspects for each product can the methodology used to be applied to other case studies.</p>
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<p>Scenarios evaluated for the social life cycle assessment. Scenario (<b>A</b>) without fiber, Scenarios (<b>B1</b>) and (<b>B2</b>) with 10% and 40% fiber, respectively.</p>
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<p>SLCA scenario performance scores per subcategories. Scenario (<b>A</b>) without fiber, Scenarios (<b>B1</b>) and (<b>B2</b>) with 10% and 40% fiber, respectively.</p>
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13 pages, 3415 KiB  
Article
Effects of Infill Patterns on the Mechanical and Tribological Behaviour of 3D-Printed Polylactic Acid/Bamboo Biocomposites for Structural Applications
by Devarajan Balaji, Balasubramanian Arulmurugan and Venkateswaran Bhuvaneswari
Polymers 2025, 17(4), 448; https://doi.org/10.3390/polym17040448 - 8 Feb 2025
Viewed by 396
Abstract
Composite materials are gaining attention owing to their exemplary characteristics and, if the materials are eco-friendly, they attract much more. One such composite of poly lactic acid (PLA) combined with bamboo fiber in the ratio of 80:20 is selected for this study. The [...] Read more.
Composite materials are gaining attention owing to their exemplary characteristics and, if the materials are eco-friendly, they attract much more. One such composite of poly lactic acid (PLA) combined with bamboo fiber in the ratio of 80:20 is selected for this study. The composites are manufactured using additive manufacturing, or the 3D-printing technique. In this article, a novel approach of infilling a honeycomb with around 12 infill patterns has been made, and all the 3D-printed specimens were tested for their mechanical and tribological properties. The 3D-printed composites were characterized using Fourier Transform InfraRed spectroscopy (FTIR) and X-Ray Diffraction (XRD) to evaluate their chemical composition and crystallite size (CS), respectively. Based on the results, the cross infill pattern outperforms irregular geometries like the Gyroid in terms of impact strength owing to its efficient stress distribution and superior interlayer bonding. By utilizing bidirectional reinforcement and distributing loads uniformly, the grid infill was able to attain the Shore D maximum hardness due to its strong 3D lattice structure; the Octet infill is very resistant to wear, which improves energy absorption and decreases material loss. Such honeycomb-filled 3D-printed composites can act as high-mechanical-strength components and find their applications in aerospace applications like drones and their allied structures. Full article
(This article belongs to the Section Polymer Composites and Nanocomposites)
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<p>PLA/bamboo filament.</p>
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<p>3D printing parameters.</p>
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<p>FTIR peaks for PLA/bamboo composite filament.</p>
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<p>Impact specimen of cross infill honeycomb after test.</p>
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<p>Morphology of PLA/bamboo specimen after impact failure.</p>
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<p>Hardness specimen of grid infill honeycomb after test.</p>
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20 pages, 4464 KiB  
Review
Recycling Water Hyacinth as Supplementary Cementitious Material, Admixture, and Fiber in Mortar and Concrete: Current Trends and Research Gaps
by Gilberto García, René Cabrera, Julio Rolón and Roberto Pichardo
Recycling 2025, 10(1), 18; https://doi.org/10.3390/recycling10010018 - 4 Feb 2025
Viewed by 858
Abstract
This review explores the potential of water hyacinth (WH) as a sustainable material in cement-based applications, focusing on its use as an addition, admixture, and fiber reinforcement. WH’s unique physical and chemical properties, such as high cellulose content and pozzolanic potential, make it [...] Read more.
This review explores the potential of water hyacinth (WH) as a sustainable material in cement-based applications, focusing on its use as an addition, admixture, and fiber reinforcement. WH’s unique physical and chemical properties, such as high cellulose content and pozzolanic potential, make it suitable for bio-composites and eco-friendly concrete formulations. The present study highlights several promising findings, including the enhancement of the resulting mechanical properties and the reduction in their environmental impact when the WH is incorporated in controlled quantities. Challenges such as workability and durability issues at higher dosages are discussed. This review aims to bridge knowledge gaps and support WH’s adoption in sustainable construction practices. Full article
(This article belongs to the Topic Sustainable Building Materials)
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<p>WH visual aspect.</p>
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<p>Water absorption and sorptivity of mortars with WHA. Adapted from: [<a href="#B76-recycling-10-00018" class="html-bibr">76</a>].</p>
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<p>WH microstructure: WH microfibrils at 500× (<b>a</b>) and internal structure of WH at 2000× (<b>b</b>). Retrieved from: [<a href="#B90-recycling-10-00018" class="html-bibr">90</a>].</p>
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<p>WHF stem structure at 100× (<b>a</b>) and at 500× (<b>b</b>). Retrieved from: [<a href="#B50-recycling-10-00018" class="html-bibr">50</a>].</p>
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<p>Untreated (<b>a</b>) and alkaline treated (<b>b</b>) WHF; untreated (<b>c</b>) and heated treated (<b>d</b>). Retrieved from: [<a href="#B89-recycling-10-00018" class="html-bibr">89</a>,<a href="#B94-recycling-10-00018" class="html-bibr">94</a>].</p>
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<p>SEM images of WH powder particles at different magnifications (<b>a</b>–<b>c</b>) and WHA particles at different magnifications (<b>d</b>–<b>f</b>). Retrieved from: [<a href="#B95-recycling-10-00018" class="html-bibr">95</a>].</p>
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22 pages, 5276 KiB  
Article
Development of Doum Palm Fiber-Based Building Insulation Composites with Citric Acid/Glycerol Eco-Friendly Binder
by Hicham Elmoudnia, Younoussa Millogo, Paulina Faria, Rachid Jalal, Mohamed Waqif and Latifa Saâdi
J. Compos. Sci. 2025, 9(2), 67; https://doi.org/10.3390/jcs9020067 - 2 Feb 2025
Viewed by 935
Abstract
This study focuses on the development of an insulation biocomposite using Doum palm (Chamaerops humilis) fibers reinforced with a natural binder based on citric acid and glycerol. The main objective is to optimize the thermal conductivity and mechanical properties of the biocomposite as [...] Read more.
This study focuses on the development of an insulation biocomposite using Doum palm (Chamaerops humilis) fibers reinforced with a natural binder based on citric acid and glycerol. The main objective is to optimize the thermal conductivity and mechanical properties of the biocomposite as a function of fiber preparation (short or powdered fibers) and binder content (20%, 30% and 40%), and relate them to the bonding of the fibers and the binder. The obtained results suggest that the addition of the binder greatly enhances the density, compressive strength and Young’s modulus of biocomposites. More specifically, the addition of 20% by weight of the citric acid/glycerol binder improves the bond between fibers, whether they are short fibers or powders. This leads to an increase in the mechanical properties, with Young’s modulus reaching (212.1) MPa and compressive strength at (24.3) MPa. On the other hand, the results show that these biocomposites also have acceptable thermal insulation performance, achieving a thermal conductivity of (0.102) W/(m·K), making them suitable for a variety of applications in sustainable buildings and for refurbishment. Full article
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<p>Binder preparation protocol with glycerol, citric acid, water and catalyst, with thermal treatments.</p>
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<p>Preparation of the fibers: (<b>a</b>) Chamaerops humilis; (<b>b</b>) chopped fibers; (<b>c</b>) cut fibers; (<b>d</b>) mill used to prepare the fibers; (<b>e</b>) short and (<b>f</b>) powdered fibers.</p>
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<p>Composite specimens and thermal and mechanical experimental tests carried out.</p>
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<p>SEM EDX analysis of DPfs.</p>
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<p>FTIR spectra of DPfs in the raw state.</p>
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<p>X-ray diffractogram of DPfs in the raw state.</p>
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<p>ATG-ATD curves of raw DPfs.</p>
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<p>SEM observation of untreated DPfs.</p>
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<p>Infrared spectrum of the biosourced binder synthesized based on CA-GLY.</p>
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<p>Reactions involving both citric acid and glycerol molecules in condensation.</p>
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<p>Mechanical properties of DPf-based specimens at different sizes with b-average and standard deviation: (<b>a</b>): compressive strength; (<b>b</b>): Young’s modulus.</p>
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<p>Thermal conductivity of Doum fiber-based test pieces at various sizes.</p>
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18 pages, 2993 KiB  
Article
New Insights into Antiviral Natural Formulations: Biopolymeric Films for the Prevention and Treatment of a Wide Gamma of Viral Infections
by Victoria Belén Ayala-Peña, Ana Karen Jaimes, Ana Lucía Conesa, Cybele Carina García, Claudia Soledad Sepulveda, Fernando Gaspar Dellatorre, Ezequiel Latour, Nora Marta Andrea Ponce, Vera Alejandra Álvarez and Verónica Leticia Lassalle
Viruses 2025, 17(2), 216; https://doi.org/10.3390/v17020216 - 1 Feb 2025
Viewed by 458
Abstract
Viral infections remain a major concern, as existing treatments often yield inadequate responses or lead to the development of antiviral resistance in some cases. Fucoidan extracted from Undaria pinnatifida (F) is a natural sulphated polysaccharide that exhibits antiviral action. Despite its potential, the [...] Read more.
Viral infections remain a major concern, as existing treatments often yield inadequate responses or lead to the development of antiviral resistance in some cases. Fucoidan extracted from Undaria pinnatifida (F) is a natural sulphated polysaccharide that exhibits antiviral action. Despite its potential, the biomedical application of F is limited due to its difficult administration through trans-mucosal, skin, or oral ingestion. The most effective way to solve these problems is to propose novel methods of administration aiming to ensure better contact between the biopolymers and pathogens, leading to their inactivation. In this work, the synthesis of films based on chitosan (Ch)-coupled F is reported, aiming to generate a synergic effect between both biopolymers in terms of their antiviral and antioxidant capability. Biocomposites were prepared by a sonochemical method. They were characterized to infer structural properties, functionality, and possible F-Ch interactions by using Zeta potential, FTIR, and XRD techniques. The biocomposites showed excellent film-forming ability. They also exhibited improved antioxidant activity with respect to F and Ch individually and proved to be non-cytotoxic. These results demonstrate, for the first time, the antiviral activity of F:Ch biocomposites against bovine coronavirus and human viruses (adenovirus, poliovirus, herpes simplex, and respiratory syncytial virus), which could be applied in film form to prevent or treat viral infections. Full article
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<p>(<b>a</b>) Chemical structure of biopolymers. (<b>b</b>) Images of the obtained biomaterials as an aqueous dispersion and film biocomposites.</p>
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<p>(<b>a</b>) FTIR spectra of biomaterials and raw polymers. (<b>b</b>) X-ray diffractogram of biomaterials and raw polymers. Arbitrary units (A.U.).</p>
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<p>(<b>a</b>) Cell viability dose–response curve (blue lines) and antiviral assay for fucoidan (F) and chitosan (Ch) against BCoV (black bars) or HSV-1 (grey bars). (<b>b</b>) Virucidal assay of F (100 µg/mL) or Ch (300 µg/mL). (<b>c</b>) Cells infected under different treatment conditions in the presence of F (100 µg/mL) or Ch (300 µg/mL). Results are expressed as the mean ± SD of data from at least three separate experiments; each condition was processed in duplicate. * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01, <sup>&amp;</sup> <span class="html-italic">p</span> &lt; 0.05 respect to to 10 µg/mL of F, <sup>#</sup> <span class="html-italic">p</span> &lt; 0.05 with respect to 15 µg/mL of Ch.</p>
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<p>(<b>a</b>) HSV-1 Kos titer reduction in a virucidal (green) and cell viability (blue) assay. Means and SD are shown from three separate experiments. Each condition was processed in duplicate. * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01 vs. vehicle. (<b>b</b>) Representative TEM micrographs of HSV-1 Kos exposed to biocomposites. Orange arrows indicate the viral capsid, and yellow arrows indicate the viral envelope of HSV-1 exposed to formulations. Scale bar: 200 nm.</p>
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<p>Virucidal activity of F:Ch biocomposites (1:1 or 1:2). Results are expressed as the mean ± SD of data from at least three separate experiments. Each condition was processed in duplicate. * <span class="html-italic">p</span> &lt; 0.05 vs. each indicated treatment.</p>
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<p>Scavenging effects on DPPH radicals by F, Ch, F:Ch biocomposites (1:1; 1:2; 2:1) and AA (ascorbic acid). Values represent the mean from three independent tests. * <span class="html-italic">p</span> &lt; 0.05 vs. each indicated treatment.</p>
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42 pages, 2870 KiB  
Systematic Review
Exploring Advancements in Bio-Based Composites for Thermal Insulation: A Systematic Review
by Daria Pawłosik, Krzysztof Cebrat and Marcin Brzezicki
Sustainability 2025, 17(3), 1143; https://doi.org/10.3390/su17031143 - 30 Jan 2025
Viewed by 838
Abstract
The growing need to mitigate the environmental impact of human activities has underscored the importance of biomaterials in sustainable architecture and construction. In this systematic review, advancements in bio-composite materials are consolidated and critically evaluated, emphasizing their thermal insulation properties and broader applications [...] Read more.
The growing need to mitigate the environmental impact of human activities has underscored the importance of biomaterials in sustainable architecture and construction. In this systematic review, advancements in bio-composite materials are consolidated and critically evaluated, emphasizing their thermal insulation properties and broader applications in sustainable building practices. Key aspects analyzed included morphology, internal structure, and thermal performance, along with supplementary insights into mechanical properties when available. The review focused on studies published between January and October 2024, sourced from the Scopus database and adhering to PRISMA guidelines. A keyword meta-analysis using VOSviewer (version 1.6.20) illustrated keyword co-occurrence trends. Methods for assessing bias included evaluating study design, data collection processes, and potential conflicts of interest, aligned with PRISMA standards. Significant findings revealed bio-composites achieving thermal conductivity values as low as 0.016 W/m·K, surpassing many traditional materials in insulation performance. Data from 48 studies, analysing 50 bio-composite materials, showed that 44% were optimized for thermal insulation and 40% for sub-structural applications. These materials also exhibit biodegradability and recyclability, critical attributes for sustainable construction. However, challenges such as scalability and durability remain as the key barriers to widespread adoption. In this review, the viability of bio-composites as sustainable alternatives to traditional materials is highlighted and research priorities are identified, particularly in scaling production technologies and enhancing durability testing methods, to advance their application in sustainable building practices. Full article
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<p>The systematic search process: an initial pool of 6475 publications was narrowed to 2965 through thematic filtering. Further refinement, including applying inclusion criteria and manual reviews, resulted in the final selection of 48 studies covering 50 bio-composite materials.</p>
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<p>(a) A traditional classification of engineering materials. This review is restricted to materials categorized as composites. (<b>b</b>) A schematic representation of the phase classification of selected composites based on the organic origin of the raw materials. This review focuses on composites containing at least one organic or semi-organic phase.</p>
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<p>Classification of raw materials based on biological origin. This review emphasizes composites with at least one bio-phase derived from plant or animal sources. Materials are included if no more than one phase is inorganic and meets the criterion of natural origin.</p>
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<p>Network visualisation of keyword co-occurrences from analysed papers. Node size indicates term frequency, and connecting lines represent co-occurrence relationships. Colour-coded clusters highlight thematic groups, with larger nodes showing greater importance. Created using VOSviewer, December 2024.</p>
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<p>Hierarchy of composite materials: An overview of the structural classification of composites, highlighting reinforcement types (particle, fibre, and layer) and their subdivisions, as well as the matrix materials that bind them. The fundamental components of the composite are marked with a yellow border. According to the definition, a composite should contain at least two phases but may also include various additives. However, these additives are not essential for classifying the material as a composite.</p>
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<p>A schematic, scale-free 3D axonometric section of a building illustrating potential locations where conventional materials could be replaced with the bio-composites reviewed in this study. The materials are coded using serial numbers corresponding to those in the tables, with thermal insulation materials highlighted in yellow. <a href="#app1-sustainability-17-01143" class="html-app">Table S4</a>, included in the <a href="#app1-sustainability-17-01143" class="html-app">Supplementary Materials</a>, compares conventional materials and their equivalent bio-based alternatives.</p>
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<p>Comparison of thermal conductivity (<span class="html-italic">λ</span>) values [W/m·K] for bio-composites with EPS (shown in blue). Materials are coded using serial numbers corresponding to those in the <a href="#sustainability-17-01143-t003" class="html-table">Table 3</a>, <a href="#sustainability-17-01143-t004" class="html-table">Table 4</a>, <a href="#sustainability-17-01143-t005" class="html-table">Table 5</a>, <a href="#sustainability-17-01143-t006" class="html-table">Table 6</a>, <a href="#sustainability-17-01143-t007" class="html-table">Table 7</a> and <a href="#sustainability-17-01143-t008" class="html-table">Table 8</a>. * values are estimated by analogy to similar commercial materials, as the original authors provide no specific thermal conductivity measurements.</p>
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<p>Comparison of flexural strength (<span class="html-italic">σ<sub>f</sub></span>) [MPa] of load-bearing bio-composites with steel (shown in blue). Materials are coded using serial numbers corresponding to those in the <a href="#sustainability-17-01143-t003" class="html-table">Table 3</a>, <a href="#sustainability-17-01143-t004" class="html-table">Table 4</a>, <a href="#sustainability-17-01143-t005" class="html-table">Table 5</a>, <a href="#sustainability-17-01143-t006" class="html-table">Table 6</a>, <a href="#sustainability-17-01143-t007" class="html-table">Table 7</a> and <a href="#sustainability-17-01143-t008" class="html-table">Table 8</a>.</p>
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<p>Comparison of mechanical properties: (<b>a</b>) tensile strength (<span class="html-italic">σ<sub>t</sub></span>) [MPa] of load-bearing bio-composites with steel; (<b>b</b>) compressive strength (<span class="html-italic">σ<sub>t</sub></span>) [MPa] of load-bearing bio-composites with concrete. Materials are coded using serial numbers corresponding to those in the <a href="#sustainability-17-01143-t003" class="html-table">Table 3</a>, <a href="#sustainability-17-01143-t004" class="html-table">Table 4</a>, <a href="#sustainability-17-01143-t005" class="html-table">Table 5</a>, <a href="#sustainability-17-01143-t006" class="html-table">Table 6</a>, <a href="#sustainability-17-01143-t007" class="html-table">Table 7</a> and <a href="#sustainability-17-01143-t008" class="html-table">Table 8</a>.</p>
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<p>(<b>a</b>) Distribution of bio-based composite materials based on their functional applications in buildings; (<b>b</b>) analysis of materials further categorised by their origin.</p>
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<p>(<b>a</b>) Reinforcement types in bio-based composite materials show the prevalence of particle-based reinforcement (large particles and dispersion strengthening); (<b>b</b>) the matrix composition is primarily polymers, with ceramics as a secondary component.</p>
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<p>(<b>a</b>) Overview of biodegradability, compostability, and recyclability; (<b>b</b>) recycled waste in producing the reviewed bio-based composites.</p>
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23 pages, 17284 KiB  
Article
Preparation and Study of Physicochemical and Adsorption Properties of Alginate Composites
by Małgorzata Wasilewska, Sylwia Gubernat and Paulina Gil-Kulik
Materials 2025, 18(3), 629; https://doi.org/10.3390/ma18030629 - 30 Jan 2025
Viewed by 504
Abstract
This paper presents the preparation and study of the properties of alginate materials, which were obtained on the basis of sodium alginate, activated carbon, cellulose, and calcium chloride. Alginate–carbon (AlgCa + C) and alginate–cellulose (AlgCa + Cel) composites, as well as pure calcium [...] Read more.
This paper presents the preparation and study of the properties of alginate materials, which were obtained on the basis of sodium alginate, activated carbon, cellulose, and calcium chloride. Alginate–carbon (AlgCa + C) and alginate–cellulose (AlgCa + Cel) composites, as well as pure calcium alginate (AlgCa) for comparative purposes, were obtained. Their textural (nitrogen adsorption/desorption isotherms), morphological (scanning electron microscopy), thermal (thermal analysis), and acid–base (pH drift method) properties, as well as the swelling index, were investigated. Additionally, to determine the adsorption properties, comprehensive equilibrium and kinetic studies of the adsorption of sodium salts of ibuprofen (IBP), diclofenac (D), and naproxen (NPX) from aqueous solutions on biocomposities were carried out. Adsorption isotherms were fitted using the Marczewski–Jaroniec isotherm equation (R2 = 0.941–0.988). Data on the adsorption rate were analyzed using simple kinetic equations, of which the best quality of fit was obtained using the multi-exponential equation (R2 − 1 = (3.9 × 10−4)–(6.9 × 10−4)). The highest obtained adsorption values were reached in systems with alginate–carbon composite and were 1.23 mmol/g for NPX, 0.81 mmol/g for D, and 0.43 mmol/g for IBP. The AlgCa + C material was characterized by a large specific surface area (1151 m2/g), a high degree of swelling (300%) and high resistance to high temperatures. Full article
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<p>Nitrogen adsorption/desorption isotherms of C (<b>a</b>), AlgCa + C (<b>a</b>), Cel (<b>a</b>,<b>b</b>), and AlgCa + Cel (<b>a</b>,<b>b</b>).</p>
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<p>SEM micrographs of ALGCa [magnifications: 100—(<b>a</b>); 500—(<b>b</b>); 1000—(<b>c</b>); 5000—(<b>d</b>)], Cel [magnifications: 100—(<b>e</b>); 500—(<b>f</b>); 1000—(<b>g</b>); 5000—(<b>h</b>)], AlgCa + Cel [magnifications: 50—(<b>i</b>); 500—(<b>j</b>); 1000—(<b>k</b>); 5000—(<b>l</b>)], C [magnifications: 100—(<b>m</b>); 500—(<b>n</b>); 1000—(<b>o</b>); 5000—(<b>p</b>)], and AlgCa + C [magnifications: 50—(<b>r</b>); 500—(<b>s</b>); 1000—(<b>t</b>); 5000—(<b>u</b>)].</p>
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<p>SEM micrographs of ALGCa [magnifications: 100—(<b>a</b>); 500—(<b>b</b>); 1000—(<b>c</b>); 5000—(<b>d</b>)], Cel [magnifications: 100—(<b>e</b>); 500—(<b>f</b>); 1000—(<b>g</b>); 5000—(<b>h</b>)], AlgCa + Cel [magnifications: 50—(<b>i</b>); 500—(<b>j</b>); 1000—(<b>k</b>); 5000—(<b>l</b>)], C [magnifications: 100—(<b>m</b>); 500—(<b>n</b>); 1000—(<b>o</b>); 5000—(<b>p</b>)], and AlgCa + C [magnifications: 50—(<b>r</b>); 500—(<b>s</b>); 1000—(<b>t</b>); 5000—(<b>u</b>)].</p>
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<p>XPS survey spectra of AlgNa (<b>a</b>,<b>b</b>), AlgCa (<b>a</b>,<b>b</b>), Cel (<b>a</b>), C (<b>b</b>,<b>c</b>), AlgCa + Cel (<b>a</b>), and AlgCa + C (<b>b</b>).</p>
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<p>XPS survey spectra of AlgNa (<b>a</b>,<b>b</b>), AlgCa (<b>a</b>,<b>b</b>), Cel (<b>a</b>), C (<b>b</b>,<b>c</b>), AlgCa + Cel (<b>a</b>), and AlgCa + C (<b>b</b>).</p>
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<p>Comparison of TG (<b>a</b>), DTG (<b>b</b>), and DSC (<b>c</b>) curves of AlgNa, AlgCa, Cel, C, AlgCa + Cel, and AlgCa + C.</p>
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<p>Point of zero charge for AlgCa + Cel and AlgCa + C.</p>
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<p>Dependence of swelling index on incubation time in redistilled water for AlgCa, AlgCa + Cel, and AlgCa + C.</p>
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<p>The adsorption isotherms for IBP, D, and NPX on AlgCa + Cel (<b>a</b>) and AlgCa + C (<b>b</b>).</p>
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<p>The adsorption kinetics for IBP, D, and NPX on AlgCa + C shown as changes in concentration (<b>a</b>) and adsorption (<b>b</b>) over time.</p>
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<p>The adsorption kinetics for IBP, D, and NPX on AlgCa + C shown as changes in concentration (<b>a</b>) and adsorption (<b>b</b>) over time.</p>
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17 pages, 6511 KiB  
Article
Development of Bio-Composites from Milkweed Fibers Using Air-Laid Spike Process for Automobile Dashboard Applications
by Deborah Lupescu, Patrice Cousin, Mathieu Robert and Said Elkoun
Materials 2025, 18(3), 618; https://doi.org/10.3390/ma18030618 - 29 Jan 2025
Viewed by 722
Abstract
This study focused on examining the reinforcement of milkweed fibers in polylactic acid (PLA) bio-composites used for dashboards in car interiors. Milkweed fiber is a natural fiber with a hollow structure that provides tremendous thermal insulation and noise resistance properties. Firstly, the milkweed [...] Read more.
This study focused on examining the reinforcement of milkweed fibers in polylactic acid (PLA) bio-composites used for dashboards in car interiors. Milkweed fiber is a natural fiber with a hollow structure that provides tremendous thermal insulation and noise resistance properties. Firstly, the milkweed fibers were blended with PLA fibers in a weight ratio of 75:25 using an air-laying process. Then, several layers of nonwoven material were compressed in a hydraulic press to obtain bio-composites. Finally, three bio-composites were obtained with different numbers of layers. The density, microstructure, thermal conductivity, sound transmission loss (STL), mechanical properties, dynamic mechanical analysis (DMA), and contact angles of the bio-composites were evaluated. The microstructure analysis revealed that some milkweed fibers collapsed due to the high-pressure molding process, which does not affect the bio-composite properties. The bio-composite with a higher number of nonwoven layers presented a poor interface between PLA and milkweed fibers, thus making it less homogeneous. This bio-composite showed a decrease of 5% in thermal conductivity values and a 19% increase in STL values. In addition, it exhibited a 160% increase in specific flexural strength and a 335% increase in specific flexural modulus compared to samples with a lower number of nonwoven layers. Therefore, it offers the best mechanical-property-to-density ratio, with values that conform to the specifications required for automotive dashboards. Full article
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<p>Manufacturing process of (<b>a</b>) the nonwovens and (<b>b</b>) the bio-composites using air laying.</p>
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<p>SEM images of (<b>a</b>) milkweed fiber and (<b>b</b>) milkweed fiber from C1, (<b>c</b>) milkweed fiber from C2, and (<b>d</b>) milkweed fiber from C3. Dispersion of the fibers in (<b>e</b>) C1, (<b>f</b>) C2, and (<b>g</b>) C3.</p>
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<p>Weight loss curves for (<b>a</b>) C1, (<b>b</b>) C2, and (<b>c</b>) C3.</p>
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<p>Weight loss curves for (<b>a</b>) C1, (<b>b</b>) C2, and (<b>c</b>) C3.</p>
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<p>Thermal conductivity values versus Ma.</p>
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<p>Thermal conductivity values at average temperatures of −4 °C, 5 °C, and 29 °C.</p>
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<p>STL values versus frequency.</p>
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<p>The tensile properties of STC1, STC2, and STC3 are represented in (<b>a</b>) bar graphs of tensile strength and specific tensile strength and (<b>b</b>) bar graphs of modulus and specific tensile modulus.</p>
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<p>The flexural properties of SFC1, SFC2, and SFC3 are represented in (<b>a</b>) bar graphs of flexural strength and specific flexural strength and (<b>b</b>) bar graphs of modulus and specific flexural modulus.</p>
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22 pages, 8208 KiB  
Article
Elastomeric Biocomposites of Natural Rubber Containing Biosynthesized Zinc Oxide
by Anna Sowińska-Baranowska and Magdalena Maciejewska
Int. J. Mol. Sci. 2025, 26(3), 1101; https://doi.org/10.3390/ijms26031101 - 27 Jan 2025
Viewed by 417
Abstract
Zinc oxide (ZnO) particles were successfully synthesized through the green method using aloe vera extract and zinc nitrate (1:1). The structure, morphology and properties of the biosynthesized ZnO (bioZnO) particles were analyzed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), time of [...] Read more.
Zinc oxide (ZnO) particles were successfully synthesized through the green method using aloe vera extract and zinc nitrate (1:1). The structure, morphology and properties of the biosynthesized ZnO (bioZnO) particles were analyzed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), time of flight secondary ion mass spectrometry (TOF-SIMS) and thermogravimetry (TG). The morphology and the size of ZnO particles were elucidated by scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS). Then, the ability of bioZnO to activate sulfur curing of natural rubber (NR) was tested and compared to commercial ZnO traditionally used as vulcanization activator. The bioZnO showed similar activity in the vulcanization process to commercial ZnO. NR composites containing bioZnO were pro-ecological in nature and exhibited better mechanical characteristics and durability against thermo-oxidative aging than NR with commonly used micrometric ZnO. Moreover, NR vulcanizates containing bioZnO showed good mechanical properties in dynamic conditions and satisfactory thermal stability. The present research is new and in addition to the analysis of biosynthesized ZnO particles, the effect of the activator in the vulcanization process of the NR elastomer and its influence on the properties of the final products were additionally discussed. Full article
(This article belongs to the Section Materials Science)
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<p>Mechanism of bio-ZnO nanoparticle formation using aloe vera extract.</p>
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<p>Thermogravimetric (TG) curve of bioZnO powder.</p>
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<p>FTIR spectra of ZnO powders.</p>
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<p>Diffraction pattern for bioZnO.</p>
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<p>Time-of-flight secondary ion mass spectrometry (TOF-SIMS) spectra for commercial ZnO: (<b>a</b>) negative ions; (<b>b</b>) positive ions.</p>
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<p>TOF-SIMS spectra for bioZnO: (<b>a</b>) negative ions; (<b>b</b>) positive ions.</p>
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<p>Scanning electron microscopy (SEM) (<b>a</b>) with energy-dispersive X-ray spectroscopy (EDS) (<b>b</b>) analysis for pure commercial ZnO.</p>
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<p>SEM (<b>a</b>) with EDS (<b>b</b>) analysis for bioZnO.</p>
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<p>Distribution of curatives in NR composite with commercial ZnO: (<b>a</b>) SEM image; (<b>b</b>) EDS spectrum.</p>
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<p>Distribution of curatives in NR composite with bioZnO: (<b>a</b>) SEM image; (<b>b</b>) EDS spectrum.</p>
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<p>Differential scanning calorimetry (DSC) curves of NR compounds containing commercial and bioZnO.</p>
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<p>Loss factor (tan δ) graphs against temperature for NR vulcanizates with commercial and bioZnO.</p>
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<p>Changes in the properties of NR vulcanizates due to thermo-oxidative aging: (<b>a</b>) crosslink density; (<b>b</b>) stress at 300% elongation; (<b>c</b>) tensile strength; (<b>d</b>) elongation at break; (<b>e</b>) hardness.</p>
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<p>Thermal stability of NR vulcanizates: (<b>a</b>) TG curves, (<b>b</b>) DTG curves.</p>
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<p>The scheme of biosynthesis method used in this study.</p>
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12 pages, 2148 KiB  
Article
A New Means to Generate Liposomes by Rehydrating Engineered Lipid Nanoconstructs
by Yuqi Huang, Ziqian Xu, Umit Celik, Christopher F. Carnahan, Roland Faller, Atul N. Parikh and Gang-yu Liu
Micromachines 2025, 16(2), 138; https://doi.org/10.3390/mi16020138 - 25 Jan 2025
Viewed by 538
Abstract
The concept and feasibility of producing liposomes by rehydrating engineered lipid nanoconstructs are demonstrated in this study. Nanoconstructs of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC) were produced using a microfluidic delivery probe integrated with an atomic force microscope. The subsequent rehydration of these POPC constructs led to [...] Read more.
The concept and feasibility of producing liposomes by rehydrating engineered lipid nanoconstructs are demonstrated in this study. Nanoconstructs of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC) were produced using a microfluidic delivery probe integrated with an atomic force microscope. The subsequent rehydration of these POPC constructs led to the formation of liposomes, most of which remained adhered to the surface. The size (e.g., diameter) of the liposomes could be tuned by varying the lateral dimension of the lipid constructs. Hierarchical liposomal structures, such as pentagons containing five liposomes at the corners, could also be designed and produced by depositing lipid constructs to designated locations on the surfaces, followed by rehydration. This new means allows for regulating liposomal sizes, distributions, and compositions. The outcomes benefit applications of liposomes as delivery vehicles, sensors, and building blocks in biomaterials design. The ability to produce hierarchical liposomal structures benefits numerous applications such as proto-cell development, multiplexed bio-composite materials, and the engineering of local bio-environments. Full article
(This article belongs to the Collection Women in Micromachines)
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<p>(<b>A</b>) Schematic diagram of an AFM combined with a microfluidic delivery. (<b>B</b>) Schematic diagram illustrating the key steps, following the delivery in (<b>A</b>), in forming liposomes via the rehydration of lipid nanostructures.</p>
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<p>(<b>A</b>) A 3D display of an AFM topographic image of a 5 × 5 array of POPC constructs formed under a delivery pressure of −250 mbar. The AFM scan speed was set at 16.48 µm/s. (<b>B</b>) A 2D confocal scan of the POPC constructs array before rehydration, taken at z = 0.8 µm above the glass surface. (<b>C</b>) A 2D confocal scan of the liposome array 24 min after rehydration, taken at z = 0.8 µm above the glass surface. Scale bars = 5 µm.</p>
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<p>(<b>A</b>) A 3D display of an AFM topographic image of a 5 × 5 array of POPC constructs under a delivery pressure of 0 mbar. The AFM scan speed was set at 16.48 µm/s. (<b>B</b>) A 2D confocal scan of the liposome array 13 min after rehydration, taken at z = 0.8 µm above the glass surface. (<b>C</b>) A 2D confocal scan of the liposome array 18 min after rehydration, taken at z = 0.8 µm above the glass surface. Scale bars = 5 µm.</p>
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<p>Top row, (<b>A</b>,<b>C</b>,<b>E</b>,<b>G</b>,<b>I</b>) are 3D displays of AFM topographs of five POPC constructs selected from the five representative experiments. The AFM scan speeds were set at 16.48, 23.96, 23.96, 16.00, and 24.00 µm/s, respectively, from left to right. Bottom row, (<b>B</b>,<b>D</b>,<b>F</b>,<b>H</b>,<b>J</b>) are the LSCM images of the liposomes formed by rehydrating the POPC construct shown in the image above. The LSCM scans were taken at the central plane of the vertical dimensions of each individual liposome. Scale bars = 5 µm.</p>
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<p>(<b>A</b>) Plotting of the liposome diameter against the lateral dimension and height of the POPC constructs. (<b>B</b>) Correlation between the liposome diameter and the lateral dimension of the POPC constructs, overlayed with the outcome of the linear regression. (<b>C</b>) Correlation between the liposome diameter and the height of the POPC constructs. The 3D plot shown in (<b>A</b>) was prepared using OriginPro 2025.</p>
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<p>(<b>A</b>) AFM topographic image of five POPC constructs positioned at the vertices of a pentagon designed with side lengths of 2.0 µm. (<b>B</b>) Confocal scan of the liposome array 1 min after rehydrating the POPC constructs in (<b>A</b>), taken at z = 0.5 µm above the glass surface. The dotted circles indicate the original locations of each POPC construct. Scale bars = 1 µm.</p>
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27 pages, 2737 KiB  
Article
Thermal Decomposition of Date Seed/Polypropylene Homopolymer: Machine Learning CDNN, Kinetics, and Thermodynamics
by Zaid Abdulhamid Alhulaybi Albin Zaid and Abdulrazak Jinadu Otaru
Polymers 2025, 17(3), 307; https://doi.org/10.3390/polym17030307 - 23 Jan 2025
Viewed by 1086
Abstract
The buildup of abandoned plastics in the environment and the need to optimize agricultural waste utilization have garnered scrutiny from environmental organizations and policymakers globally. This study presents an assessment of the thermal decomposition of date seeds (DS), polypropylene homopolymer (PP), and their [...] Read more.
The buildup of abandoned plastics in the environment and the need to optimize agricultural waste utilization have garnered scrutiny from environmental organizations and policymakers globally. This study presents an assessment of the thermal decomposition of date seeds (DS), polypropylene homopolymer (PP), and their composites (DS/PP) through experimental measurements, machine learning convolutional deep neural networks (CDNN), and kinetic and thermodynamic analyses. The experimental measurements involved the pyrolysis and co-pyrolysis of these materials in a nitrogen-filled thermogravimetric analyzer (TGA), investigating degradation temperatures between 25 and 600 °C with heating rates of 10, 20, and 40 °C.min−1. These measurements revealed a two-stage process for the bio-composites and a decrease in the thermal stability of pure PP due to the moisture, hemicellulose, and cellulose content of the DS material. By utilizing machine learning CDNN, algorithms and frameworks were developed, providing responses that closely matched (R2~0.942) the experimental data. After various modelling modifications, adjustments, and regularization techniques, a framework comprising four hidden neurons was determined to be most effective. Furthermore, the analysis revealed that temperature was the most influential parameter affecting the thermal decomposition process. Kinetic and thermodynamic analyses were performed using the Coats–Redfern and general Arrhenius model-fitting methods, as well as the Flynn–Wall–Ozawa and Kissinger–Akahira–Sunose model-free approaches. The first-order reaction mechanism was identified as the most appropriate compared to the second and third order F-Series solid-state reaction mechanisms. The overall activation energy values were estimated at 51.471, 51.221, 156.080, and 153.767 kJ·mol−1 for the respective kinetic models. Additionally, the kinetic compensation effect showed an exponential increase in the pre-exponential factor with increasing activation energy values, and the estimated thermodynamic parameters indicated that the process is endothermic, non-spontaneous, and less disordered. Full article
(This article belongs to the Section Biobased and Biodegradable Polymers)
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<p>Plots depicting experimental TGA-DTG data against degradation temperature [°C] for (<b>a</b>) pure polypropylene [PP], (<b>b</b>) pure date seed [DS], (<b>c</b>) composites composed of DS/PP under condition of constant heating rate, and (<b>d</b>) composites subjected to varied heating rates.</p>
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<p>Illustration of a machine learning deep neural network (DNN) framework displaying the standard configuration of input, hidden, and output layers, each composed of 10 hidden neurons, denoted as 10 HNs (see <a href="#app1-polymers-17-00307" class="html-app">Supplementary Information</a>).</p>
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<p>Computed data from deep neural network (DNN) modelling reveals (<b>a</b>) plots depicting the true error against epochs for 10, 8, 6, and 4 hidden neuron layers (HNS), and (<b>b</b>) plots illustrating the DNN-computed weight percentages compared to the corresponding experimental data percentages.</p>
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<p>An illustration depicting the utilization of convolutional deep neural networks (CDNN) in the filtration and training processes of specific experimental datasets.</p>
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<p>Plots of real and convoluted (CNN) weight fraction [-] against reduced degradation temperature [-] for the pure DS, PP, and composites for (<b>a</b>) a constant heating rate of 10 °C.min<sup>−1</sup> and (<b>b</b>) constant material composition. Data from CDNN and DNN modelling showing (<b>c</b>) plots of true error against epochs computed for 10, 8, 6, and 4 HNS and (<b>d</b>) plots of experimental and CDNN computed weight [%] against CNN—reduced temperature [-] for the DS-10 sample at selected stages of computational trainings.</p>
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<p>Plots illustrating the experimental and CDNN computed weight [%] against CNN degradation temperature [°C] for (<b>a</b>) DS and PP at 10 °C.min<sup>−1</sup> of heating rate, and (<b>b</b>,<b>c</b>) DSP, DP and blends at obtained different heating rates.</p>
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<p>Plots of (<b>a</b>) Coats–Redfern’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </semantics></math> at different reaction orders against inverse of conversion temperature [K<sup>−1</sup>], (<b>b</b>) Arrhenius’ <math display="inline"><semantics> <mrow> <mrow> <mrow> <mi mathvariant="normal">ln</mi> </mrow> <mo>⁡</mo> <mrow> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </mrow> </mrow> </semantics></math> at different reaction orders against inverse of conversion temperature [K<sup>−1</sup>], (<b>c</b>) Coats–Redfern’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </semantics></math> at different heating rates against inverse of conversion temperature [K<sup>−1</sup>], (<b>d</b>) Coats–Redfern’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </semantics></math> at varied PD/PP compositions against inverse of conversion temperature [K<sup>−1</sup>], (<b>e</b>) activation energy, and (<b>f</b>) energies [kJ.mol<sup>−1</sup>] against percentage composition of DS in the composites.</p>
Full article ">Figure 7 Cont.
<p>Plots of (<b>a</b>) Coats–Redfern’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </semantics></math> at different reaction orders against inverse of conversion temperature [K<sup>−1</sup>], (<b>b</b>) Arrhenius’ <math display="inline"><semantics> <mrow> <mrow> <mrow> <mi mathvariant="normal">ln</mi> </mrow> <mo>⁡</mo> <mrow> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </mrow> </mrow> </semantics></math> at different reaction orders against inverse of conversion temperature [K<sup>−1</sup>], (<b>c</b>) Coats–Redfern’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </semantics></math> at different heating rates against inverse of conversion temperature [K<sup>−1</sup>], (<b>d</b>) Coats–Redfern’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mo>(</mo> <msub> <mrow> <mi mathvariant="normal">F</mi> </mrow> <mrow> <mi mathvariant="normal">i</mi> </mrow> </msub> <mo>)</mo> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </semantics></math> at varied PD/PP compositions against inverse of conversion temperature [K<sup>−1</sup>], (<b>e</b>) activation energy, and (<b>f</b>) energies [kJ.mol<sup>−1</sup>] against percentage composition of DS in the composites.</p>
Full article ">Figure 8
<p>The kinetic compensation effect is illustrated by the plots of <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced separators="|"> <mrow> <mi>A</mi> </mrow> </mfenced> </mrow> </semantics></math> against <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mfenced separators="|"> <mrow> <msub> <mrow> <mi>E</mi> </mrow> <mrow> <mi>A</mi> </mrow> </msub> </mrow> </mfenced> </mrow> </semantics></math>.</p>
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<p>Plots of (<b>a</b>) FWO’s <math display="inline"><semantics> <mrow> <mi>l</mi> <mi>n</mi> <mi>Q</mi> </mrow> </semantics></math> against the inverse of conversion temperature T<sup>−1</sup> [K<sup>−1</sup>] for a 20% constant conversion and varied material compositions, (<b>b</b>) KAS’ <math display="inline"><semantics> <mrow> <mrow> <mrow> <mi mathvariant="normal">ln</mi> </mrow> <mo>⁡</mo> <mrow> <mfenced open="[" close="]" separators="|"> <mrow> <mstyle scriptlevel="0" displaystyle="true"> <mfrac> <mrow> <mi mathvariant="normal">Q</mi> </mrow> <mrow> <msup> <mrow> <mi>T</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msup> </mrow> </mfrac> </mstyle> </mrow> </mfenced> </mrow> </mrow> </mrow> </semantics></math> against the inverse of conversion temperature T<sup>−1</sup> [K<sup>−1</sup>] for a 20% constant conversion and varied material compositions, (<b>c</b>) FWO’s <math display="inline"><semantics> <mrow> <mi mathvariant="normal">l</mi> <mi mathvariant="normal">n</mi> <mi mathvariant="normal">Q</mi> </mrow> </semantics></math> against the inverse of conversion temperature T<sup>−1</sup> [K<sup>−1</sup>] for a 25% constant sample composition and varied conversions, and (<b>d</b>) overall activation energy [kJ.mol<sup>−1</sup>] against percentage composition of DS in the composites.</p>
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19 pages, 4900 KiB  
Article
ι-Carrageenan Manganese Oxide Bionanocomposites as a Promising Solution to Agricultural Challenges
by Spartak S. Khutsishvili, Nino Gagelidze, Astghik S. Tsokolakyan, Mkrtich A. Yeranosyan, Eteri Tkesheliadze, Vardan A. Sargsyan, Darejan Dughashvili, Natela Dzebisashvili, Keso Aronia, Archil Benashvili, Dali Dzanashvili, Irine Gurgenidze, Grigor Tatishvili and Paula Fraga-García
Materials 2025, 18(3), 495; https://doi.org/10.3390/ma18030495 - 22 Jan 2025
Viewed by 794
Abstract
Agriculture faces numerous challenges: infectious diseases through phytopathogens and soil nutrient deficiencies hinder plant growth, reducing crop yields. Biopolymer nanocomposites offer promising solutions to these challenges. In this work, we synthesize and characterize novel bionanocomposites (ι-CG-Mn) of manganese (hydr)oxide nanoparticles (approx. [...] Read more.
Agriculture faces numerous challenges: infectious diseases through phytopathogens and soil nutrient deficiencies hinder plant growth, reducing crop yields. Biopolymer nanocomposites offer promising solutions to these challenges. In this work, we synthesize and characterize novel bionanocomposites (ι-CG-Mn) of manganese (hydr)oxide nanoparticles (approx. 3 to 11 nm) embedded in the matrix of the natural polysaccharide ι-carrageenan (ι-CG). Using spectroscopic methods we verify the presence of the nanoparticles in the polymer matrix while leaving the polysaccharide structural characteristics unaffected. Elemental analysis determines the mass content of metal ions in the ι-CG-Mn to be approx. 1 wt%. Electron microscopy techniques show the supramolecular organization of the ι-CG-Mn and the homogeneous nanoparticle distribution in the polymer matrix, while thermal analysis reveals that the bionanocomposite maintains high thermal stability. Moreover, the co-incubation of the phytopathogen Clavibacter sepedonicus with ι-CG-Mn inhibits the pathogen growth by 67% compared to the control. Our bionanocomposites demonstrate (1) strong bactericidal activity and (2) potential as microfertilizers that stimulate agricultural plant growth through the dosage of metal ions. These properties arise from the bioactivity of the widely available, naturally sulfated polysaccharide biopolymer matrix, combined with the antimicrobial effects of manganese (hydr)oxide nanoparticles, which together enhance the efficacy of the biocomposite. The non-toxic, biocompatible, and biodegradable nature of this biopolymer satisfies the high environmental demands for future biotechnological and agricultural technologies. Full article
(This article belongs to the Special Issue Advances in Bio-Polymer and Polymer Composites)
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Figure 1

Figure 1
<p>Obtaining of pure cultures of (<b>A</b>) <span class="html-italic">Cms</span> NCPPB 2137, (<b>B</b>) the bacterial lawn culture on the surface of GPY agar Petri dish, (<b>C</b>) and Gram-stained culture.</p>
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<p>FTIR spectra of the original <span class="html-italic">ι</span>-CG (1) and the nanocomposite <span class="html-italic">ι</span>-CG-Mn (2).</p>
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<p>Raman spectra of the original <span class="html-italic">ι</span>-CG (1) and the nanocomposite <span class="html-italic">ι</span>-CG-Mn (2).</p>
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<p>The UV-vis spectra of the original <span class="html-italic">ι</span>-CG (1) and the nanocomposite <span class="html-italic">ι</span>-CG-Mn (2).</p>
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<p>The EPR spectrum of the nanocomposite <span class="html-italic">ι</span>-CG-Mn.</p>
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<p>Curves of mass loss (green) and heat effects (blue) of the thermostability of the nanocomposite <span class="html-italic">ι</span>-CG-Mn (<b>A</b>) and the original <span class="html-italic">ι</span>-CG (<b>B</b>).</p>
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<p>The SEM images of the original <span class="html-italic">ι</span>-CG (<b>A</b>) and the nanocomposite <span class="html-italic">ι</span>-CG-Mn (<b>B</b>).</p>
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<p>The TEM micrographs and size distribution of nanoparticles of <span class="html-italic">ι</span>-CG-Mn. The scale bar size is 100 nm.</p>
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<p>The bactericidal impact of an aqueous solution of <span class="html-italic">ι</span>-CG-Mn compared to the pure <span class="html-italic">ι</span>-CG and the control on <span class="html-italic">Cms</span> in agar plates; 1—control, 2—<span class="html-italic">ι</span>-CG, 3—<span class="html-italic">ι</span>-CG-Mn.</p>
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<p>The bactericidal impact of an aqueous solution of <span class="html-italic">ι</span>-CG-Mn compared to the pure <span class="html-italic">ι</span>-CG and the control on <span class="html-italic">K. pneumoniae</span> (<b>A</b>) and <span class="html-italic">E. coli</span> (<b>B</b>) in agar plates; 1—control, 2—<span class="html-italic">ι</span>-CG, 3—<span class="html-italic">ι</span>-CG-Mn.</p>
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<p>Determination of the optical turbidity (D<sub>595</sub> nm) of the bacterial suspension and effect of <span class="html-italic">ι</span>-CG-Mn treatment in volume on growth of <span class="html-italic">Cms</span> pathogen; 1—control, 2—<span class="html-italic">ι</span>-CG, 3—<span class="html-italic">ι</span>-CG-Mn; * <span class="html-italic">p</span> ≤ 0.01 compared to the control according to the Mann–Whitney test.</p>
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