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16 pages, 3807 KiB  
Article
A Study on the Effect of Conductive Particles on the Performance of Road-Suitable Barium Titanate/Polyvinylidene Fluoride Composite Materials
by Zhenhua Zhao, Rui Li, Chen Zhao and Jianzhong Pei
Materials 2025, 18(5), 1185; https://doi.org/10.3390/ma18051185 - 6 Mar 2025
Viewed by 159
Abstract
The design of piezoelectric roads is one of the future directions of smart roads. In order to ensure the environmentally friendly and long-lasting use of piezoelectric road materials, lead-free piezoelectric ceramics (barium titanate), polymer piezoelectric materials (polyvinylidene fluoride), and conductive particles (conductive carbon [...] Read more.
The design of piezoelectric roads is one of the future directions of smart roads. In order to ensure the environmentally friendly and long-lasting use of piezoelectric road materials, lead-free piezoelectric ceramics (barium titanate), polymer piezoelectric materials (polyvinylidene fluoride), and conductive particles (conductive carbon black and graphene) were used to prepare composite piezoelectric materials. The electrical performance was studied by the conductivity, dielectric properties, and piezoelectric properties of the composite materials. Then, the mechanical properties of the composite material were investigated by load compression tests. Finally, the microstructure of the composite materials was studied. The results showed that as the amount of conductive particles increased, the electrical performance was improved. However, further addition of conductive particles led to a decline in the electrical performance. The addition of conductive particles had a minimal effect on the mechanical properties of composite materials. The composite material met road use requirements. The overall structure of the composite materials was compact, with a clear wrapping effect of the polymer, and good interface compatibility. The addition of conductive carbon black and graphene had no significant impact on the structure of the composite materials. Full article
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Figure 1
<p>The particle size distribution, SEM, and XRD images of BaTiO3 made by hydrothermal synthesis: (<b>a</b>) particle size distribution; (<b>b</b>) SEM; (<b>c</b>) XRD.</p>
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<p>The preparation method of BaTiO<sub>3</sub>/PVDF composite materials.</p>
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<p>The electrical performance of BaTiO<sub>3</sub>/PVDF composite materials: (<b>a</b>) dielectric properties; (<b>b</b>) piezoelectric properties.</p>
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<p>The influence of conductive particles on the electrical conductivity of three-phase composite materials: (<b>a</b>) conductive carbon black; (<b>b</b>) graphene.</p>
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<p>The influence of conductive particles on the dielectric properties of three-phase composite materials: (<b>a</b>) conductive carbon black; (<b>b</b>) graphene.</p>
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<p>The frequency-dependent dielectric properties of BaTiO<sub>3</sub>/PVDF/conductive carbon black composite materials: (<b>a</b>) relative dielectric constant; (<b>b</b>) dielectric loss.</p>
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<p>The frequency-dependent dielectric properties of BaTiO<sub>3</sub>/PVDF/graphene composite materials: (<b>a</b>) relative dielectric constant; (<b>b</b>) dielectric loss.</p>
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<p>The influence of conductive particles on the piezoelectric properties of three-phase composite materials: (<b>a</b>) conductive carbon black; (<b>b</b>) graphene.</p>
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<p>The influence of conductive particles on the mechanical performance of three-phase composite materials.</p>
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<p>The microscopic morphology of three-phase composite materials: (<b>a</b>) BaTiO<sub>3</sub>/PVDF composite materials; (<b>b</b>) 1.2% conductive carbon black in BaTiO<sub>3</sub>/PVDF composite materials; (<b>c</b>) 0.5% graphene in BaTiO<sub>3</sub>/PVDF composite materials.</p>
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17 pages, 4555 KiB  
Article
Preliminary Study on Wearable Smart Socks with Hydrogel Electrodes for Surface Electromyography-Based Muscle Activity Assessment
by Gabriele Rescio, Elisa Sciurti, Lucia Giampetruzzi, Anna Maria Carluccio, Luca Francioso and Alessandro Leone
Sensors 2025, 25(5), 1618; https://doi.org/10.3390/s25051618 - 6 Mar 2025
Viewed by 155
Abstract
Surface electromyography (sEMG) is increasingly important for prevention, diagnosis, and rehabilitation in healthcare. The continuous monitoring of muscle electrical activity enables the detection of abnormal events, but existing sEMG systems often rely on disposable pre-gelled electrodes that can cause skin irritation and require [...] Read more.
Surface electromyography (sEMG) is increasingly important for prevention, diagnosis, and rehabilitation in healthcare. The continuous monitoring of muscle electrical activity enables the detection of abnormal events, but existing sEMG systems often rely on disposable pre-gelled electrodes that can cause skin irritation and require precise placement by trained personnel. Wearable sEMG systems integrating textile electrodes have been proposed to improve usability; however, they often suffer from poor skin–electrode coupling, leading to higher impedance, motion artifacts, and reduced signal quality. To address these limitations, we propose a preliminary model of smart socks, integrating biocompatible hybrid polymer electrodes positioned over the target muscles. Compared with commercial Ag/AgCl electrodes, these hybrid electrodes ensure lower the skin–electrode impedance, enhancing signal acquisition (19.2 ± 3.1 kΩ vs. 27.8 ± 4.5 kΩ for Ag/AgCl electrodes). Moreover, to the best of our knowledge, this is the first wearable system incorporating hydrogel-based electrodes in a sock specifically designed for the analysis of lower limb muscles, which are crucial for evaluating conditions such as sarcopenia, fall risk, and gait anomalies. The system incorporates a lightweight, wireless commercial module for data pre-processing and transmission. sEMG signals from the Gastrocnemius and Tibialis muscles were analyzed, demonstrating a strong correlation (R = 0.87) between signals acquired with the smart socks and those obtained using commercial Ag/AgCl electrodes. Future studies will further validate its long-term performance under real-world conditions and with a larger dataset. Full article
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<p>Overview of the hardware architecture.</p>
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<p>Overview of the socks. (<b>a</b>) External side of the socks: equipped with a pocket for the electronic device and the cables that connect the electronic device to the electrodes. (<b>b</b>) Internal side of the socks: equipped with five pockets for placing the TA, GL, and reference electrodes. (<b>c</b>) User wearing sock: correct placement of electrodes enables the measurement of the EMG signal from selected muscles.</p>
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<p>Acquisition protocol. Each volunteer performed the activities shown in the figure for the time indicated, where GL MVC and TA MVC are defined as the maximum voluntary contraction of the Gastrocnemius muscle and Tibialis muscle, respectively.</p>
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<p>(<b>a</b>) Schematic representation of hybrid polymer electrode (HPe) production. (<b>b</b>) Photographs of fabricated HP electrodes and their connection to a commercial snap-on cable.</p>
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<p>(<b>a</b>) LED test with HP hydrogel electrode; (<b>b</b>) impedance versus potential of HP hydrogel electrodes and commercial hydrogel electrodes; (<b>c</b>) impedance versus frequency of HP electrodes and commercial electrodes; (<b>d</b>) Nyquist plot and equivalent circuit model used for fitting. Dashed lines represent measured experimental data; solid lines represent the fitted curves.</p>
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<p>(<b>a</b>) Raw and (<b>b</b>) processed signals recorded with the commercial system; (<b>c</b>) raw and (<b>d</b>) processed signals captured using the in-house system; and (<b>e</b>) a comparison of the processed signal, measured using commercial electrodes and in-house-developed stockings during the execution of three repetitions of 5 s of MVC of the Tibialis Anterior muscle followed by 10 s of rest.</p>
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<p>Example of signal patterns captured from the Gastrocnemius and Tibialis muscles during walking and strong muscle contraction using (<b>a</b>) the commercial electrodes and (<b>b</b>) the sock system.</p>
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19 pages, 10502 KiB  
Article
Flexible and Washable Poly(3,4-ethylenedioxythiophene): Polystyrene Sulfonate/Polyvinyl Alcohol Fabric Dry Electrode for Long-Term Electroencephalography Signals Measurement
by Fangmeng Zeng, Guanghua Wang, Chenyi Sun, Jiayi Gao, Shanqun Ji and Quanxi Zhang
Polymers 2025, 17(5), 683; https://doi.org/10.3390/polym17050683 - 4 Mar 2025
Viewed by 171
Abstract
Recent advancements in smart textiles have facilitated their extensive application in wearable health monitoring, particularly in brain activity measurement. This study introduces a flexible and washable fabric dry electroencephalography (EEG) electrode designed for brain activity measurement. The fabric dry electrode is constructed from [...] Read more.
Recent advancements in smart textiles have facilitated their extensive application in wearable health monitoring, particularly in brain activity measurement. This study introduces a flexible and washable fabric dry electroencephalography (EEG) electrode designed for brain activity measurement. The fabric dry electrode is constructed from electrically conductive polyester fabric with a resistivity of 0.09 Ω·cm, achieved by applying a PEDOT: PSS/PVA conductive paste coating on the textile substrate. A comparative analysis of the tensile properties between the conductive and untreated polyester fabric was conducted. The SEM images demonstrated that the PEDOT: PSS/PVA conductive polymer composite resulted in a uniform coating on the fabric surface. When enveloped in elastic foam, the fabric dry electrode maintained a low and stable electrode–skin contact impedance during prolonged EEG monitoring. Additionally, the short circuit noise level of the fabric dry electrode exhibited superior performance compared to both Ag/AgCl wet and finger dry electrode. The EEG signals acquired from the fabric dry electrode were comparable to those recorded by the Ag/AgCl wet electrode. Moreover, the fabric electrode effectively captured clear and reliable EEG signals, even after undergoing 10 washing cycles. The fabric dry electrode indicates good sweat resistance and biocompatibility during prolonged monitoring. Full article
(This article belongs to the Section Smart and Functional Polymers)
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<p>(<b>a</b>) Schematic illustration of the preparation process for conductive fabric; (<b>b</b>) structural design of the PEDOT: PSS/PVA fabric dry electrode; (<b>c</b>) model design of the electrode shell and its 3D-printed shell; (<b>d</b>) the assembled electrode and its components.</p>
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<p>(<b>a</b>) Schematic illustration of the preparation process for conductive fabric; (<b>b</b>) structural design of the PEDOT: PSS/PVA fabric dry electrode; (<b>c</b>) model design of the electrode shell and its 3D-printed shell; (<b>d</b>) the assembled electrode and its components.</p>
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<p>The schematic illustration of the setup for measuring EEG signals.</p>
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<p>(<b>a</b>) SEM image of the polyester fabric (×65); (<b>b</b>) SEM image of the polyester fabric (×500); (<b>c</b>) SEM image of PEDOT: PSS/PVA-coated conductive fabric (×65); (<b>d</b>) SEM image of PEDOT: PSS/PVA-coated conductive fabric (×500); (<b>e</b>) SEM image of PEDOT: PSS/PVA-coated conductive fabric after 10 washing cycles (×65); (<b>f</b>) SEM image of PEDOT: PSS/PVA-coated conductive fabric after 10 washing cycles (×500); (<b>g</b>) FTIR spectra of the polyester fabric, PEDOT: PSS-coated conductive fabric, and PEDOT: PSS/PVA-coated conductive fabric; (<b>h</b>) The resistance of PEDOT: PSS/PVA-coated conductive fabrics after various washing cycles.</p>
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<p>(<b>a</b>) Schematic illustration of the setup for measuring electrode–skin contact impedance using the OpenBCI Cyton Board; (<b>b</b>) The electrode–skin contact impedances of EEG electrodes over time, including Ag/AgCl wet electrode, finger dry electrode, and PEDOT: PSS/PVA fabric dry electrode.</p>
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<p>Results of the short circuit noise test: (<b>a</b>) noise measured with Ag/AgCl wet electrodes; (<b>b</b>) noise measured with finger dry electrodes; (<b>c</b>) noise measured with PEDOT: PSS/PVA fabric dry electrodes; (<b>d</b>) number of noises measured with Ag/AgCl wet electrodes at varying amplitudes; (<b>e</b>) number of noises measured with finger dry electrodes at varying amplitudes; (<b>f</b>) number of noises measured with PEDOT: PSS/PVA fabric dry electrodes at varying amplitudes.</p>
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<p>EEG signals were recorded for 30 s using the Ag/AgCl wet electrode and the PEDOT: PSS/PVA fabric dry electrode placed on the forehead of 5 subjects during a resting state. (<b>a</b>) Fp1; (<b>b</b>) Fp2.</p>
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<p>EEG artifacts were recorded for 30 s using the Ag/AgCl wet electrode and the PEDOT: PSS/PVA fabric dry electrode at Fp1 from 5 subjects. (<b>a</b>) Eye blinks; (<b>b</b>) teeth clenching.</p>
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<p>Results of EEG signal recordings for 30 s using the Ag/Ag/Cl wet electrode and the PEDOT: PSS/PVA fabric dry electrode from hairy areas (O1) from 5 subjects with the eyes closed/opened; (<b>a</b>) EEG signals; (<b>b</b>) PSD of EEG signals.</p>
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<p>Results of EEG signal recordings for 30 s using the Ag/Ag/Cl wet electrode and the PEDOT: PSS/PVA fabric dry electrode from hairy areas (O1) from 5 subjects with the eyes closed/opened; (<b>a</b>) EEG signals; (<b>b</b>) PSD of EEG signals.</p>
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<p>SNRs of the Ag/AgCl wet electrode and the PEDOT: PSS/PVA fabric dry electrode at Fp1, Fp2, and O1.</p>
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<p>Results of EEG signal recordings for 30 s using the PEDOT: PSS/PVA fabric dry electrode after 5 and 10 washing cycles at Fp1.</p>
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<p>Result of EEG signal recordings for 30 s using the PEDOT: PSS/PVA fabric dry electrode simulating insensible perspiration and sensible perspiration at Fp1.</p>
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<p>The skin condition test of wearing the PEDOT: PSS/PVA fabric dry electrode for 4 h.</p>
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16 pages, 4921 KiB  
Article
Thin Cells of Polymer-Modified Liquid Crystals Described by Voronoi Diagrams
by Felicity Woolhouse and Ingo Dierking
Materials 2025, 18(5), 1106; https://doi.org/10.3390/ma18051106 - 28 Feb 2025
Viewed by 210
Abstract
We investigated patterns formed during the polymerization process of bifunctional monomers in a liquid crystal for both large polymer concentrations (polymer-dispersed liquid crystals, PDLC) and small concentrations (polymer-stabilized liquid crystals, PSLC). The resulting experimental patterns are reminiscent of Voronoi diagrams, so a reverse [...] Read more.
We investigated patterns formed during the polymerization process of bifunctional monomers in a liquid crystal for both large polymer concentrations (polymer-dispersed liquid crystals, PDLC) and small concentrations (polymer-stabilized liquid crystals, PSLC). The resulting experimental patterns are reminiscent of Voronoi diagrams, so a reverse Voronoi algorithm was developed that provides the seed locations of cells, thus allowing a computational reproduction of the experimental patterns. Several metrics were developed to quantify the commonality between the faithful experimental patterns and the idealized and generated ones. This led to descriptions of the experimental patterns with accuracies better than 90% and showed that the curvature or concavity of the cell edges was below 2%. Possible reasons for the discrepancies between the original and generated Voronoi diagrams are discussed. The introduced algorithm and quantification of the patterns could be transferred to many other experimental problems, for example, melting of thin polymer films, ultra-thin metal films, or bio-membranes. The discrepancies between the experimental and ideal Voronoi diagrams are quantified, which may be useful in the quality control of privacy windows, reflective displays, or smart glass. Full article
(This article belongs to the Special Issue The 15th Anniversary of Materials—Recent Advances in Soft Matter)
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Figure 1
<p>(<b>A</b>) Example of a PDLC structure with removed liquid crystal in the so-called Swiss cheese morphology. (<b>B</b>) Scattering off-state of the device, and (<b>C</b>) transparent on-state with index matching between ordinary refractive index of the liquid crystal and the polymer matrix. (Reproduced by permission after [<a href="#B10-materials-18-01106" class="html-bibr">10</a>]).</p>
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<p>(<b>A</b>) Morphology of the polymer network with the liquid crystal removed. (<b>B</b>) At zero voltage, the polymerisation of bifunctional monomers is induced via UV radiation with a network forming that templates the LC orientation leading to a transparent off-state. Application of voltage causes breakup of the liquid crystal director field, which leads to the light scattering on-state. After field removal, the network elastically drives the LC back to its original state. (<b>C</b>) Some prototype devices from 1996 in the off- and on-state. (Reproduced by permission after [<a href="#B11-materials-18-01106" class="html-bibr">11</a>]).</p>
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<p>A basic representation of a Voronoi diagram in 2D, showing the boundaries as solid lines and the seed as a red point. The degenerate vertices are denoted with a crossed circle and the dummy vertices with a plus. Smart vertices are left as intersections of three cell edges.</p>
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<p>Comparison between faithful Voronoi-like pattern (<b>left</b>) and idealized Voronoi pattern (<b>right</b>) where vertices are inevitably connected by straight lines.</p>
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<p>Schematic figures to illustrate the geometric conditions available for the calculation of seed points from a given Voronoi pattern. (<b>A</b>) Cell boundaries are mirror planes to seeds of neighboring cells. (<b>B</b>) Seeds of adjacent cells lie on a circle centred on their common vertex. (<b>C</b>) Voronoi construction with dummy vertexes.</p>
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<p>Gradient functions employed and respective equations: step (<b>left</b>), linear (<b>middle</b>), and Gaussian (<b>right</b>). In each case x is the normalised distance from the cell edge of the pixel. x = 0 corresponds to an edge pixel, and x = 1 to the centre.</p>
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<p>(<b>A</b>) Exemplary result of a calculated Voronoi pattern, providing the seed points of each cell (some are outside of the picture). (<b>B</b>) Comparison with the original Voronoi pattern via a (relative) heat map derived from the Sørensen–Dice coefficient. Red represents areas of highest matching and blue represents areas of lowest matching.</p>
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<p>(<b>A</b>) Venn diagram of the relationship between pixel intersections and classification. (<b>B</b>) Definitions of the different commonality coefficients that can be used to compare sets A and B. Form 1 is the classification form and Form 2 the probability form.</p>
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<p>Experimental sample [<a href="#B59-materials-18-01106" class="html-bibr">59</a>], faithful pattern, idealised representation, generated Voronoi pattern and comparative heat map for polymer dispersed liquid crystal samples (<b>A</b>) PDLC-1, (<b>B</b>) PDLC-2, and (<b>C</b>) PDLC-3.</p>
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<p>Experimental sample, faithful pattern, idealised representation, generated Voronoi pattern and comparative heat map for polymer stabilised liquid crystal samples (<b>A</b>) PSLC-1, (<b>B</b>) PSLC-2, (<b>C</b>) PSLC-3, and (<b>D</b>) PSLC-4.</p>
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<p>Comparison between <span class="html-italic">C<sub>GI</sub></span> and <span class="html-italic">M</span> for both PDLC (black squares) and PSLC (red circles) samples.</p>
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37 pages, 1214 KiB  
Review
Cyclodextrin–Hydrogel Hybrids in Advanced Drug Delivery
by Hossein Omidian, Arnavaz Akhzarmehr and Erma J. Gill
Gels 2025, 11(3), 177; https://doi.org/10.3390/gels11030177 - 28 Feb 2025
Viewed by 335
Abstract
Cyclodextrin (CD)–hydrogel hybrids have emerged as versatile and multifunctional drug delivery systems, offering enhanced solubility, controlled drug release, and improved bioavailability. By combining the inclusion complexation properties of CDs with the swelling and retention capabilities of hydrogels, these hybrid systems overcome key challenges [...] Read more.
Cyclodextrin (CD)–hydrogel hybrids have emerged as versatile and multifunctional drug delivery systems, offering enhanced solubility, controlled drug release, and improved bioavailability. By combining the inclusion complexation properties of CDs with the swelling and retention capabilities of hydrogels, these hybrid systems overcome key challenges in conventional drug formulations. This review explores CD composition, hydrogel polymer selection, fabrication techniques, key drug release factors, and real-world therapeutic applications. Additionally, the latest advancements in stimuli-responsive hydrogels, nanogels, and microneedle-based drug delivery are discussed. While CD–hydrogel systems demonstrate significant potential, scalability, regulatory hurdles, and clinical translation remain key challenges. Future research should focus on smart hydrogels, improved drug loading strategies, and enhanced clinical validation to bridge the gap between laboratory innovations and commercial applications. Full article
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<p>Illustration of preparation of γ-CD-based polypseudorotaxane hydrogels and topical delivery of FLB for treatment of anterior uveitis. Adopted with permission [<a href="#B64-gels-11-00177" class="html-bibr">64</a>].</p>
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<p>A graphical representation showing the following: (<b>a</b>) CAB-Na was combined with HP-β-CD to formulate a suitable tablet reservoir that dissolved rapidly and completely when situated atop a swollen HF-MAP. (<b>b</b>,<b>c</b>) Intradermal delivery of this anti-HIV therapeutic was achieved over 24 h in rats in vivo, and drug pharmacokinetics were studied over the following 28 days, revealing that the formulated HF-MAP device had a long-acting delivery profile. Adopted with permission [<a href="#B61-gels-11-00177" class="html-bibr">61</a>].</p>
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<p>An illustration of pHEMA/MMA/β-CD intraocular lens (IOL) with the capability of maintaining the sustained release of anti-inflammatory drugs like dexamethasone. Adopted with permission [<a href="#B57-gels-11-00177" class="html-bibr">57</a>].</p>
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104 pages, 13734 KiB  
Review
Advancing Textile Waste Recycling: Challenges and Opportunities Across Polymer and Non-Polymer Fiber Types
by Mehrdad Seifali Abbas-Abadi, Brecht Tomme, Bahman Goshayeshi, Oleksii Mynko, Yihan Wang, Sangram Roy, Rohit Kumar, Bhargav Baruah, Karen De Clerck, Steven De Meester, Dagmar R. D’hooge and Kevin M. Van Geem
Polymers 2025, 17(5), 628; https://doi.org/10.3390/polym17050628 - 26 Feb 2025
Viewed by 516
Abstract
The growing environmental impact of textile waste, fueled by the rapid rise in global fiber production, underscores the urgent need for sustainable end-of-life solutions. This review explores cutting-edge pathways for textile waste management, spotlighting innovations that reduce reliance on incineration and landfilling while [...] Read more.
The growing environmental impact of textile waste, fueled by the rapid rise in global fiber production, underscores the urgent need for sustainable end-of-life solutions. This review explores cutting-edge pathways for textile waste management, spotlighting innovations that reduce reliance on incineration and landfilling while driving material circularity. It highlights advancements in collection, sorting, and pretreatment technologies, as well as both established and emerging recycling methods. Smart collection systems utilizing tags and sensors show great promise in streamlining logistics by automating pick-up routes and transactions. For sorting, automated technologies like near-infrared and hyperspectral imaging lead the way in accurate and scalable fiber separation. Automated disassembly techniques are effective at removing problematic elements, though other pretreatments, such as color and finish removal, still need to be customized for specific waste streams. Mechanical fiber recycling is ideal for textiles with strong mechanical properties but has limitations, particularly with blended fabrics, and cannot be repeated endlessly. Polymer recycling—through melting or dissolving waste polymers—produces higher-quality recycled materials but comes with high energy and solvent demands. Chemical recycling, especially solvolysis and pyrolysis, excels at breaking down synthetic polymers like polyester, with the potential to yield virgin-quality monomers. Meanwhile, biological methods, though still in their infancy, show promise for recycling natural fibers like cotton and wool. When other methods are not viable, gasification can be used to convert waste into synthesis gas. The review concludes that the future of sustainable textile recycling hinges on integrating automated sorting systems and advancing solvent-based and chemical recycling technologies. These innovations, supported by eco-design principles, progressive policies, and industry collaboration, are essential to building a resilient, circular textile economy. Full article
(This article belongs to the Section Circular and Green Polymer Science)
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Graphical abstract

Graphical abstract
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<p>The textile manufacturing chain, from building block to end product.</p>
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<p>Fiber categories based on polymer and fiber types.</p>
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<p>Worldwide distribution of fiber extraction and production. Natural fibers represent 30% of the total, while man-made fibers represent 70% [<a href="#B17-polymers-17-00628" class="html-bibr">17</a>].</p>
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<p>The viscose production process [<a href="#B101-polymers-17-00628" class="html-bibr">101</a>,<a href="#B102-polymers-17-00628" class="html-bibr">102</a>].</p>
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<p>The lyocell production process [<a href="#B109-polymers-17-00628" class="html-bibr">109</a>].</p>
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<p>Overall reaction for important polymerizations. The targeted polymer is listed above the arrow for clarity [<a href="#B111-polymers-17-00628" class="html-bibr">111</a>,<a href="#B112-polymers-17-00628" class="html-bibr">112</a>,<a href="#B114-polymers-17-00628" class="html-bibr">114</a>].</p>
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<p>The industrial polymerization and structure of PET [<a href="#B130-polymers-17-00628" class="html-bibr">130</a>,<a href="#B131-polymers-17-00628" class="html-bibr">131</a>].</p>
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<p>PA6,6 vs. PA6.</p>
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<p>Waste hierarchy staircase for textile end-of-life options. Ideally, processes at the top are used until they no longer yield a product or secondary raw material of sufficient quality, in which case a process lower down should be used, except for incineration or landfill.</p>
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<p>Textile waste management in the U.S. (1960–2018) [<a href="#B197-polymers-17-00628" class="html-bibr">197</a>].</p>
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<p>Example of the attenuated total reflection–Fourier transform infrared (ATR-FTIR) spectra of common fibers [<a href="#B231-polymers-17-00628" class="html-bibr">231</a>,<a href="#B232-polymers-17-00628" class="html-bibr">232</a>,<a href="#B233-polymers-17-00628" class="html-bibr">233</a>,<a href="#B234-polymers-17-00628" class="html-bibr">234</a>].</p>
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<p>Tire textile recovery [<a href="#B247-polymers-17-00628" class="html-bibr">247</a>].</p>
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<p>Re-extrusion of fibers from PET bottle or textile waste.</p>
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<p>The chain extension of recycled PET using PMDA [<a href="#B338-polymers-17-00628" class="html-bibr">338</a>].</p>
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<p>Dissolution of cellulose in an ionic liquid using the anti-H<sub>2</sub> bonding mechanism [<a href="#B357-polymers-17-00628" class="html-bibr">357</a>].</p>
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<p>Thermogravimetric analysis curves for original, hydrolyzed, and man-made cotton fibers [<a href="#B348-polymers-17-00628" class="html-bibr">348</a>].</p>
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<p>Functional groups of six polymer types, with examples theoretically lumped into one chain for the compactness of the figure [<a href="#B392-polymers-17-00628" class="html-bibr">392</a>,<a href="#B393-polymers-17-00628" class="html-bibr">393</a>,<a href="#B394-polymers-17-00628" class="html-bibr">394</a>,<a href="#B395-polymers-17-00628" class="html-bibr">395</a>,<a href="#B396-polymers-17-00628" class="html-bibr">396</a>,<a href="#B397-polymers-17-00628" class="html-bibr">397</a>,<a href="#B398-polymers-17-00628" class="html-bibr">398</a>,<a href="#B399-polymers-17-00628" class="html-bibr">399</a>,<a href="#B400-polymers-17-00628" class="html-bibr">400</a>,<a href="#B401-polymers-17-00628" class="html-bibr">401</a>,<a href="#B402-polymers-17-00628" class="html-bibr">402</a>,<a href="#B403-polymers-17-00628" class="html-bibr">403</a>,<a href="#B404-polymers-17-00628" class="html-bibr">404</a>,<a href="#B405-polymers-17-00628" class="html-bibr">405</a>,<a href="#B406-polymers-17-00628" class="html-bibr">406</a>,<a href="#B407-polymers-17-00628" class="html-bibr">407</a>].</p>
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<p>The thermal degradation process of PVC [<a href="#B408-polymers-17-00628" class="html-bibr">408</a>].</p>
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<p>Thermogravimetric analysis graphs of different polymers according to <a href="#polymers-17-00628-f017" class="html-fig">Figure 17</a> [<a href="#B392-polymers-17-00628" class="html-bibr">392</a>,<a href="#B393-polymers-17-00628" class="html-bibr">393</a>,<a href="#B394-polymers-17-00628" class="html-bibr">394</a>,<a href="#B395-polymers-17-00628" class="html-bibr">395</a>,<a href="#B396-polymers-17-00628" class="html-bibr">396</a>,<a href="#B397-polymers-17-00628" class="html-bibr">397</a>,<a href="#B398-polymers-17-00628" class="html-bibr">398</a>,<a href="#B399-polymers-17-00628" class="html-bibr">399</a>,<a href="#B400-polymers-17-00628" class="html-bibr">400</a>,<a href="#B401-polymers-17-00628" class="html-bibr">401</a>,<a href="#B402-polymers-17-00628" class="html-bibr">402</a>,<a href="#B403-polymers-17-00628" class="html-bibr">403</a>,<a href="#B404-polymers-17-00628" class="html-bibr">404</a>,<a href="#B405-polymers-17-00628" class="html-bibr">405</a>,<a href="#B406-polymers-17-00628" class="html-bibr">406</a>,<a href="#B417-polymers-17-00628" class="html-bibr">417</a>].</p>
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<p>The yields of PE pyrolysis products vs. temperature (adapted from [<a href="#B442-polymers-17-00628" class="html-bibr">442</a>]). PNA stands for polynuclear aromatics [<a href="#B442-polymers-17-00628" class="html-bibr">442</a>].</p>
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<p>Diagram illustrating PVC degradation and the subsequent reactions with light olefins during the pyrolysis of waste polyolefins [<a href="#B441-polymers-17-00628" class="html-bibr">441</a>].</p>
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<p>The proposed mechanism of PET degradation at elevated temperatures [<a href="#B411-polymers-17-00628" class="html-bibr">411</a>,<a href="#B452-polymers-17-00628" class="html-bibr">452</a>,<a href="#B453-polymers-17-00628" class="html-bibr">453</a>].</p>
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<p>Examples of PET depolymerization via solvolysis.</p>
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<p>Catalytic hydrogenation of PET via Ru(II) PNN pincer complexes [<a href="#B528-polymers-17-00628" class="html-bibr">528</a>].</p>
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<p>Reductive dechlorination of PVC to PE with the iridium catalyst/Et<sub>3</sub>SiH [<a href="#B565-polymers-17-00628" class="html-bibr">565</a>].</p>
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<p>Carbon footprint ranges of state-of-the-art virgin and recycled fiber production. v-PET = virgin PET; r-PET = recycled PET via methanolysis pathway [<a href="#B571-polymers-17-00628" class="html-bibr">571</a>]; r-PET, hydrolysis = PET recycled via the alkaline hydrolysis pathway [<a href="#B542-polymers-17-00628" class="html-bibr">542</a>]; v-Cotton and v-Viscose = virgin fibers; r-Viscose, CCA = cellulose carbamate fiber derived from waste cotton [<a href="#B573-polymers-17-00628" class="html-bibr">573</a>].</p>
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32 pages, 9267 KiB  
Article
On the Structural and Biological Effects of Hydroxyapatite and Gold Nano-Scale Particles in Poly(Vinylidene Fluoride) Smart Scaffolds for Bone and Neural Tissue Engineering
by Angelika Zaszczyńska, Marzena Zychowicz, Dorota Kołbuk, Piotr Denis, Arkadiusz Gradys and Paweł Ł. Sajkiewicz
Molecules 2025, 30(5), 1041; https://doi.org/10.3390/molecules30051041 - 25 Feb 2025
Viewed by 381
Abstract
Piezoelectric materials, due to their ability to generate an electric charge in response to mechanical deformation, are becoming increasingly attractive in the engineering of bone and neural tissues. This manuscript reports the effects of the addition of nanohydroxyapatite (nHA), introduction of gold nanoparticles [...] Read more.
Piezoelectric materials, due to their ability to generate an electric charge in response to mechanical deformation, are becoming increasingly attractive in the engineering of bone and neural tissues. This manuscript reports the effects of the addition of nanohydroxyapatite (nHA), introduction of gold nanoparticles (AuNPs) via sonochemical coating, and collector rotation speed on the formation of electroactive phases and biological properties in electrospun nanofiber scaffolds consisting of poly(vinylidene fluoride) (PVDF). FTIR, WAXS, DSC, and SEM results indicate that introduction of nHA increases the content of electroactive phases and fiber alignment. The collector rotational speed increases not only the fiber alignment but also the content of electroactive phases in PVDF and PVDF/nHA fibers. Increased fiber orientation and introduction of each of additives resulted in increased SFE and water uptake. In vitro tests conducted on MG-63 and hiPSC-NSC cells showed increased adhesion and cell proliferation. The results indicate that PVDF-based composites with nHA and AuNPs are promising candidates for the development of advanced scaffolds for bone and neural tissue engineering applications, combining electrical functionality and biological activity to support tissue regeneration. Full article
(This article belongs to the Special Issue Bio-Based Polymers for Sustainable Future)
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Figure 1

Figure 1
<p>Schematic illustration of electroactive biomaterials for bone and neural tissue regeneration.</p>
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<p>SEM micrographs of (<b>A</b>) PVDF_R, (<b>B</b>) PVDF_A, (<b>C</b>) PVDF/nHA_R, and (<b>D</b>) PVDF/nHA_A, (<b>E</b>) PVDF/AU_R, (<b>F</b>) PVDF/AU_A nanofibrous scaffolds.</p>
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<p>Diameter distributions approximated with Gaussian function of nanofibrous scaffolds (<b>A</b>) PVDF_R, (<b>B</b>) PVDF_A, (<b>C</b>) PVDF/nHA_R, and (<b>D</b>) PVDF/nHA_A, (<b>E</b>) PVDF/AU_R (<b>F</b>) PVDF/AU_A.</p>
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<p>Orientation distributions and anisotropy index α of all nanofibrous scaffolds (<b>A</b>) PVDF_R, (<b>B</b>) PVDF_A, (<b>C</b>) PVDF/nHA_R, and (<b>D</b>) PVDF/nHA_A, (<b>E</b>) PVDF/AU_R (<b>F</b>) PVDF/AU_A.</p>
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<p>Contact angle measurements for all nanofibrous scaffolds (“*” means <span class="html-italic">p</span>-value ≤ 0.05).</p>
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<p>Water uptake of all piezoelectric scaffolds calculated from Equation (8).</p>
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<p>(<b>A</b>) FTIR spectra of hydroxyapatite powder and PVDF samples with nHA addition in random and aligned fiber orientation; (<b>B</b>) FTIR spectra of AuNPs and PVDF samples with AuNPs addition in random and aligned fiber orientation.</p>
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<p>FTIR spectra of PVDF samples with nHA and AuNPs addition in random and aligned samples (<b>A</b>) with focus on 760 cm<sup>−1</sup> to 880 cm<sup>−1</sup> region (<b>B</b>), and 3200 cm<sup>−1</sup> to 2800 cm<sup>−1</sup> region (<b>C</b>). The graph shows the occurrence of piezoelectric β and γ phases, omitting the bands of non-piezoelectric α phase.</p>
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<p>Phase content from FTIR analysis.</p>
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<p>(<b>A</b>) The relation between fiber alignment (expressed as FWHM values), average fiber di-ameter, and piezoelectric phases content. (<b>B</b>) The relation between average fiber diameter, porosity, and piezoelectric phases con-tent.</p>
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<p>WAXS profiles registered for the scaffolds. Profiles for PVDF pellet melt-crystallized at 10 K/min and for pure nHA, provided for comparison, were used during the peak deconvolution analysis. Profiles registered at room temperature.</p>
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<p>Phases content results obtained from WAXS analysis.</p>
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<p>DSC scans registered during the 1st heating shown as the apparent heat capacity. The curves were shifted for clarity.</p>
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<p>Characteristics of the peaks P1, P2 and P3 determined after deconvolution of the DSC scans (see <a href="#molecules-30-01041-f013" class="html-fig">Figure 13</a>): maximum of the peak temperature, <span class="html-italic">Tp</span>, (left axis), and the cumulative melting enthalpies normalized to the PVDF content, Δ<span class="html-italic">H</span> (J/g<sub>PVDF</sub>) (right axis).</p>
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<p>Cell viability of MG-63 cells cultured on pristine and with nHA and AuNPs addition PVDF nanofibrous scaffolds as the rate of TCP (Tissue Culture Plastic, 100%). Statistical significance: * <span class="html-italic">p</span> &lt; 0.05.</p>
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<p>The relation between porosity, piezoelectric phase content, and MG-63 viability after day 5.</p>
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<p>FM images of stained MG-63 directly cultured on the specimen substrate for 3 days. Samples PVDF_R, PVDF_A, PVDF/nHA_R, PVDF/nHA_A, PVDF/AU_R and PVDF/AU_A in comparison to TCP.</p>
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<p>FM images of stained MG-63 directly cultured on the specimen substrate for 5 days. Samples PVDF_R, PVDF_A, PVDF/nHA_R, PVDF/nHA_A, PVDF/AU_R and PVDF/AU_A in comparison to TCP.</p>
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<p>Immunocytochemical analysis of hiPSC-derived NSC cultured for 5 days on the PVDF scaffolds. After 5 days of culture, cells were stained for a neuronal marker (β-tubulin III, red) or mechanotransduction mediating factors YAP/TAZ (green) together with f-actin staining (Alexa546-conjugated Phalloidin, red). Extracellular matrix-coated (diluted geltrex) glass coverslips served as 2D control. Cell nuclei are contra-stained with Hoechst (blue).</p>
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69 pages, 15463 KiB  
Review
Review of Shape-Memory Polymer Nanocomposites and Their Applications
by Rafiqul Islam, Sugandika Maparathne, Pailinrut Chinwangso and T. Randall Lee
Appl. Sci. 2025, 15(5), 2419; https://doi.org/10.3390/app15052419 - 24 Feb 2025
Viewed by 352
Abstract
Shape-memory polymer nanocomposites (SMPNCs) have emerged as a transformative class of smart materials, combining the versatility of shape-memory polymers (SMPs) with the enhanced properties imparted by nanostructures. Integrating these nanofillers, this review explores the pivotal role of SMPNCs in addressing critical limitations of [...] Read more.
Shape-memory polymer nanocomposites (SMPNCs) have emerged as a transformative class of smart materials, combining the versatility of shape-memory polymers (SMPs) with the enhanced properties imparted by nanostructures. Integrating these nanofillers, this review explores the pivotal role of SMPNCs in addressing critical limitations of traditional SMPs, including low tensile strength, restricted actuation modes, and limited recovery stress. It comprehensively examines the integration of nanofillers, such as nanoparticles, nanotubes, and nanofibers, which augment mechanical robustness, thermal conductivity, and shape-recovery performance. It also consolidates foundational knowledge of SMPNCs, covering the principles of the shape-memory phenomenon, fabrication techniques, shape-recovery mechanisms, modeling approaches, and actuation methods, with an emphasis on the structural parameters of nanofillers and their interactions with polymer matrices. Additionally, the transformative real-world applications of SMPNCs are also highlighted, including their roles in minimally invasive medical devices, adaptive automotive systems, 4D printing, wearable electronics, and soft robotics. By providing a systematic overview of SMPNC development and applications, this review aims to serve as a comprehensive resource for scientists, engineers, and practitioners, offering a detailed roadmap for advancing smart materials and unlocking the vast potential of SMPNCs across various industries in the future. Full article
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<p>Schematic representation of SMPNCs, including types of nanofillers, activation methods, and applications.</p>
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<p>Schematic presentation of shape-memory cycle.</p>
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<p>Schematic illustration of the molecular architecture of SMPs, composed of various types of netpoints and switching segments.</p>
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<p>(<b>a</b>) Illustration of the structure of Fe<sub>3</sub>O<sub>4</sub> NPs embedded in V-fa/ECO copolymers and object pushing actuation under a magnetic field using 5 wt.% NPs. Reproduced with permission from ref. [<a href="#B51-applsci-15-02419" class="html-bibr">51</a>]. Copyright 2023 Kingfa Scientific and Technological Co. Ltd. (<b>b</b>) Schematic of the manufacturing procedure for the composites used in 3D printing and the magneto-responsive shape-memory process of a honeycomb structure. Reproduced with permission from ref. [<a href="#B67-applsci-15-02419" class="html-bibr">67</a>]. Copyright 2022 Elsevier.</p>
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<p>(<b>a</b>) Schematic diagrams illustrating the chemical composition of EC-g-PCL/Fe<sub>3</sub>O<sub>4</sub> composites, stress-strain curves, the cyclic photothermal conversion process, and self-tightening knots of the composites. Reproduced with permission from ref. [<a href="#B75-applsci-15-02419" class="html-bibr">75</a>]. Copyright 2022 Elsevier. (<b>b</b>) Shape-memory behavior transitioning from a “bud” to a “blooming flower” of laser-triggered PHU-Fe<sub>3</sub>O<sub>4</sub> nanocomposites containing 30 wt.% of PDOMA-grafted Fe<sub>3</sub>O<sub>4</sub>. Reproduced with permission from ref. [<a href="#B76-applsci-15-02419" class="html-bibr">76</a>]. Copyright 2021 Elsevier. (<b>c</b>) NIR-triggered shape recovery of a rectangular specimen. Reproduced with permission from ref. [<a href="#B77-applsci-15-02419" class="html-bibr">77</a>]. Copyright 2023 Elsevier.</p>
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<p>(<b>a</b>) Schematic diagram illustrating the synthesis of AuNP-RGO nanohybrids; (<b>b</b>) diagrams depicting the photothermal effect (left) and the ability of PCL/AuNP and PCL/AuNP-RGO to lift a 10 g weight under NIR light (right). Reproduced with permission from ref. [<a href="#B85-applsci-15-02419" class="html-bibr">85</a>]. Copyright 2019 Elsevier.</p>
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<p>(<b>a</b>) SEM images using backscattered electrons and 2D SAXS detector images displaying the arrangement of AuNPs in the samples at various stages: before stretching, during stretching, and after shape recovery. Reproduced with permission from ref. [<a href="#B93-applsci-15-02419" class="html-bibr">93</a>]. Copyright 2021 American Chemical Society. (<b>b</b>) Graphs showing the temperature changes in response to varying NIR-light intensities and different AuNR concentrations, accompanied by sequential photos depicting the stages of the shape-recovery process for the PLCL-AuNR/PEG-2 nanocomposite. Reproduced with permission from ref. [<a href="#B80-applsci-15-02419" class="html-bibr">80</a>]. Copyright 2023 American Chemical Society.</p>
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<p>(<b>a</b>) Diagram illustrating the 3D printing strategy used for fabricating the composite materials, shape recovery, and fixity over five loading cycles, and the thermal response curve during and after NIR-light exposure. Reproduced with permission from ref. [<a href="#B100-applsci-15-02419" class="html-bibr">100</a>]. Copyright 2022 John Wiley and Sons. (<b>b</b>) Transmission Electron Microscopy (TEM) images displaying the structural details of AuNRs and AuNSs, alongside photographs that illustrate the wavelength-specific actuation of the composites, demonstrating controlled bending and straightening actions. Reproduced with permission from ref. [<a href="#B102-applsci-15-02419" class="html-bibr">102</a>]. Copyright 2018 American Chemical Society.</p>
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<p>(<b>a</b>) Diagram illustrating the preparation process of PAF alongside images of its fractured surface. (<b>b</b>) Graph depicting PAF’s recovery time and rate under various applied voltages. (<b>c</b>) Digital photos and infrared thermal images showing the electric/moisture actuation process and its recovery, with corresponding infrared images (left) and digital photos demonstrating the 10-s recovery process of PAF at 2 V (right). Reproduced with permission from ref. [<a href="#B44-applsci-15-02419" class="html-bibr">44</a>]. Copyright 2020 Elsevier.</p>
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<p>(<b>a</b>) Illustration of the network formation in the PmBz-PCL-Ag nanocomposite using SS-PCL modified AgNPs, along with photographs depicting the shape recovery of PmBz-PCL (1), PmBz-PCL-Ag0.001 (2), PmBz-PCL-Ag0.01 (3), PmBz-PCL-Ag0.1 (4), and PmBz-PCL-Ag0.3 (5) upon light activation. Reproduced with permission from ref. [<a href="#B57-applsci-15-02419" class="html-bibr">57</a>]. Copyright 2020 Elsevier. (<b>b</b>) UV−vis spectra of CNC-ad-AgNPs and CNC-g-AgNPs. Reproduced with permission from ref. [<a href="#B32-applsci-15-02419" class="html-bibr">32</a>]. Copyright 2018 American Chemical Society.</p>
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<p>(<b>a</b>) Diagram illustrating the conventional preparation methods for SMP surfaces with microcone arrays; (<b>b</b>) the transfer of droplets without any loss during both the “captured” and “detached” stages. Reproduced with permission from ref. [<a href="#B121-applsci-15-02419" class="html-bibr">121</a>]. Copyright 2020 American Chemical Society.</p>
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<p>(<b>a</b>) Illustration of cross-linked networks in the PEDGA/OEG-W<sub>18</sub>O<sub>49</sub> composite synthesis; (<b>b</b>) temperature vs. time plots for UV and NIR light irradiation at different wavelengths. Reproduced with permission from ref. [<a href="#B72-applsci-15-02419" class="html-bibr">72</a>]. Copyright 2019 John Wiley and Sons.</p>
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<p>(<b>a</b>) Schematic of the PCL-TiO<sub>2</sub> synthesis process; (<b>b</b>) visual demonstration of shape-memory behavior (left) and shape fixity (R<sub>f</sub>) and shape-recovery (R<sub>r</sub>) ratios of the polymer composites (right). Reproduced with permission from ref. [<a href="#B126-applsci-15-02419" class="html-bibr">126</a>]. Copyright 2023 Elsevier.</p>
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<p>(<b>a</b>) FESEM images of MgO NPs with MgO-loaded electrospun fibers containing 0.1, 0.5, 1, and 3 wt.% MgO. Reproduced with permission from ref. [<a href="#B131-applsci-15-02419" class="html-bibr">131</a>]. Copyright 2022 MDPI. (<b>b</b>) Photographs depicting the shape recovery of a “box”, as well as the processes of “Jump” and “Cross Obstacle” for a SMPU-PB material under 808 nm NIR light exposure. Reproduced with permission from ref. [<a href="#B132-applsci-15-02419" class="html-bibr">132</a>]. Copyright 2023 American Chemical Society.</p>
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<p>(<b>a</b>) Illustration of step-by-step network formation through maleimide-furan Diels-Alder addition; (<b>b</b>) shape-memory cycles of PCL-CAN, measured by DMA, starting from panels A to D; and (<b>c</b>) standard and infrared images illustrating the electroactive shape-memory recovery process driven by the Joule effect. Reproduced with permission from ref. [<a href="#B55-applsci-15-02419" class="html-bibr">55</a>]. Copyright 2023 Elsevier.</p>
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<p>(<b>a</b>) Images depict the production process of CPU@CNT using hot compression, with photos of a pure polymer film and a nanocomposite film before and after bending, along with SEM images of the cross-sectional and surface views of CPU@CNT1.0; (<b>b</b>) illustration of the scratch-healing process under NIR light; and (<b>c</b>) images of shape recovery for CPU@CNT and pure CPU. Reproduced with permission from ref. [<a href="#B152-applsci-15-02419" class="html-bibr">152</a>]. Copyright 2022 Elsevier.</p>
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<p>(<b>a</b>) Synthesis of CNT/EVA composites (i), locally reversible actuation demonstrated using a bird model (ii), and light-triggered reversible actuation of the composite (iii). Reproduced with permission from ref. [<a href="#B158-applsci-15-02419" class="html-bibr">158</a>]. Copyright 2023 American Chemical Society. (<b>b</b>) Electro-active shape-recovery images showing 10CNT at 5.5 V and 5CNT at 25 V. Reproduced with permission from ref. [<a href="#B168-applsci-15-02419" class="html-bibr">168</a>]. Copyright 2023 Elsevier.</p>
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<p>(<b>a</b>) Diagrams illustrating the fabrication process of nanocomposites from SBS, PCL, and CNF, as well as the shape-recovery cycle. Reproduced with permission from ref. [<a href="#B174-applsci-15-02419" class="html-bibr">174</a>]. Copyright 2019 Elsevier. (<b>b</b>) Plots showing the shape-recovery ratio vs. time for two distinct compositions: POE/LA/CB (50/50/20) (left) and POE/LA/CB (50/50/10) (right), under various voltage conditions. Reproduced with permission from ref. [<a href="#B182-applsci-15-02419" class="html-bibr">182</a>]. Copyright 2018 Elsevier.</p>
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<p>(<b>a</b>) Schematic diagram illustrating the synergistic hydration process of the composite; (<b>b</b>) shape-memory responses to water for various tape-like CNP samples; and (<b>c</b>) double folding times of various composites. (WCNP and DCNP were produced from the homogenization of CNFs in water and dimethylacetamide, respectively). Reproduced with permission from ref. [<a href="#B54-applsci-15-02419" class="html-bibr">54</a>]. Copyright 2019 Elsevier.</p>
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<p>(<b>a</b>) Schematic diagram of the water-responsive mechanism, shape recover process, and lignin (LIG) content-dependent recovery time graph of the CA/LIG/PVA/CNF composite. Reproduced with permission from ref. [<a href="#B209-applsci-15-02419" class="html-bibr">209</a>]. Copyright 2022 Elsevier. (<b>b</b>) Shape recovery of a 3D-printed flower-like structure of CNFs embedded nanocomposite. Reproduced with permission from ref. [<a href="#B213-applsci-15-02419" class="html-bibr">213</a>]. Copyright 2023 Elsevier.</p>
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<p>(<b>a</b>) Depiction of a possible interaction between PCL and CNC; (<b>b</b>) relationship between CNC concentration and tensile strength at yield and break; and (<b>c</b>) images of grippers taken at room temperature, following mechanical stretching, and after being heated to 40 °C. Reproduced with permission from ref. [<a href="#B215-applsci-15-02419" class="html-bibr">215</a>]. Copyright 2022 Elsevier.</p>
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<p>(<b>a</b>) A proposed switchable multi-stimuli shape-memory mechanism and (<b>b</b>) shape-recovery process for manually deformed TPU/CB/CNC-5 (5 wt.% CNC) strips under various conditions: water (23.0 °C), ethanol (23.0 °C), acid (23.0 °C, pH = 2), alkali (23.0 °C, pH = 10), and heat (82.6 °C). Reproduced with permission from ref. [<a href="#B139-applsci-15-02419" class="html-bibr">139</a>]. Copyright 2022 Elsevier.</p>
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<p>(<b>a</b>) Self-healing dynamic cross-linking network design; and (<b>b</b>) electrical healing process of the conductive device with an LED bulb. Reproduced with permission from ref. [<a href="#B223-applsci-15-02419" class="html-bibr">223</a>]. Copyright 2021 Elsevier.</p>
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<p>(<b>a</b>) (i) Schematic depiction of chemically bonded DGEBA-f-GO/EDA/DGEBA photothermal cross-links and (ii) surface temperature changes with varying nanofiller content in the HBPU/EP composite during NIR irradiation. Reproduced with permission from ref. [<a href="#B230-applsci-15-02419" class="html-bibr">230</a>]. Copyright 2020 Elsevier. (<b>b</b>) Graphical illustration of (i,ii) mechanical properties, (iii) temperature change as a function of GO content (wt.%) in TCPI/rGO composites, and (iv) the process of shape recovery of the TCPI-0.3/rGO-1% composite with a fixed <span class="html-italic">π</span>-shape under NIR irradiation. Reproduced with permission from ref. [<a href="#B236-applsci-15-02419" class="html-bibr">236</a>]. Copyright 2022 John Wiley and Sons. (<b>c</b>) (i) Graphene-incorporated FE-SEM image of polyurethane (PU) + graphene (G) nanocomposite, (ii) graphical representation of temperature vs. time for various GO content nanocomposites, and (iii) time needed for complete shape recovery for PU + 3 wt.% G composite at 75 V. Reproduced with permission from ref. [<a href="#B238-applsci-15-02419" class="html-bibr">238</a>]. Copyright 2019 Elsevier.</p>
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<p>(<b>a</b>) TEM image of the clay-embedded polymer nanocomposite. Reproduced with permission from ref. [<a href="#B256-applsci-15-02419" class="html-bibr">256</a>]. Copyright 2022 John Wiley and Sons. (<b>b</b>) (i,ii) EDS images and (iii,iv) shape-memory cycle of PLA-TPU and PLA-TPU-5% NC, respectively. Reproduced with permission from ref. [<a href="#B253-applsci-15-02419" class="html-bibr">253</a>]. Copyright 2023 Elsevier. (<b>c</b>) (i) Two-step polymerization process, (ii) SEM images (scale bar ~10 μm), and (iii) illustration of comparative SMEs of pure HPL, HPL-Na, and HPL-15A. Reproduced with permission from ref. [<a href="#B258-applsci-15-02419" class="html-bibr">258</a>]. Copyright 2019 Elsevier.</p>
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<p>(<b>a</b>) (i) TEM image of PDANPS (scale bar: 1 μm), (ii) schematic of the chemical structure of PDANPs incorporated PCL-PDA polyurethane nanocomposite, (iii) NIR-responsive shape-recovery behavior of the nanocomposite, and (iv) recovery ratio variations for PCL–PDA with increasing irradiation time under 808 nm laser at intensities of 0.33, 0.66, and 1.00 W/cm<sup>2</sup>. Reproduced with permission from ref. [<a href="#B260-applsci-15-02419" class="html-bibr">260</a>]. Copyright 2022 American Chemical Society. (<b>b</b>) (i) Digital photographs and optical microscope images illustrating the appearance of the damaged and healed samples, (ii) illustrations showing the photo-induced shape-memory and self-healing mechanisms in EVA/PCL/PPy blend composites, and (iii) mechanical performance of the healed nanocomposite. Reproduced with permission from ref. [<a href="#B266-applsci-15-02419" class="html-bibr">266</a>]. Copyright 2021 Elsevier.</p>
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<p>(<b>a</b>) Schematic illustration of LAA with thrombi and the magnetic-induced 4D transformation process of transcatheter LAA closure (scale bar = 10 mm). Reproduced with permission from ref. [<a href="#B278-applsci-15-02419" class="html-bibr">278</a>]. Copyright 2021 American Chemical Society. (<b>b</b>) Magnetically activated shape-recovery process of 4D printed occlusion devices. Reproduced with permission from ref. [<a href="#B279-applsci-15-02419" class="html-bibr">279</a>]. Copyright 2019 John Wiley and Sons. (<b>c</b>) Illustration of NIR controlled shape-memory “double umbrella” structure atrial septal defect (ASD) occlusion device in an isolated pig heart. Reproduced with permission from ref. [<a href="#B80-applsci-15-02419" class="html-bibr">80</a>]. Copyright 2023 American Chemical Society. (<b>d</b>) 3D-printed stent showing shape recovery ex vivo within a porcine intestinal segment using NIR light irradiation. Reproduced with permission from ref. [<a href="#B100-applsci-15-02419" class="html-bibr">100</a>]. Copyright 2022 John Wiley and Sons. (<b>e</b>) Schematic representation of the direct writing printing technique and the shape-recovery process of the 4D intravascular stent controlled by a magnetic field. Reproduced with permission from ref. [<a href="#B281-applsci-15-02419" class="html-bibr">281</a>]. Copyright 2016 American Chemical Society. (<b>f</b>) Design and fabrication of bone tissue scaffolds using 4D printing technology. Reproduced with permission from ref. [<a href="#B285-applsci-15-02419" class="html-bibr">285</a>]. Copyright 2020 Elsevier. (<b>g</b>) Magnetic field-stimulated the shape-recovery process of scaffolds for bone repair. Reproduced with permission from ref. [<a href="#B286-applsci-15-02419" class="html-bibr">286</a>]. Copyright 2019 Elsevier.</p>
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<p>(<b>a</b>) Illustration of wearable touch, tape, and flex sensor using SMP:AgNWs composite. Reproduced with permission from ref. [<a href="#B292-applsci-15-02419" class="html-bibr">292</a>]. Copyright 2022 American Chemical Society. (<b>b</b>) The current signals and photos (inset) of the composite sensor while detecting finger bending. Reproduced with permission from ref. [<a href="#B297-applsci-15-02419" class="html-bibr">297</a>]. Copyright 2022 Elsevier. (<b>c</b>) 4D-printed tactile sensor (4DPS) tested through the application on both spherical dome and saddle surfaces. Reproduced with permission from ref. [<a href="#B183-applsci-15-02419" class="html-bibr">183</a>]. Copyright 2023 Elsevier. (<b>d</b>) Schematic and experimental demonstration of the application of the nanocomposite in high-temperature warning devices. Reproduced with permission from ref. [<a href="#B236-applsci-15-02419" class="html-bibr">236</a>]. Copyright 2022 John Wiley and Sons. (<b>e</b>) Optical image of the conductive SMPC tape circuit used to light an LED. Reproduced with permission from ref. [<a href="#B304-applsci-15-02419" class="html-bibr">304</a>]. Copyright 2021 Springer Nature. (<b>f</b>) Photographic illustration of unpressed and patterned CNC-SMP and GE-SMP for optical anti-counterfeiting. Reproduced with permission from ref. [<a href="#B306-applsci-15-02419" class="html-bibr">306</a>]. Copyright 2023 John Wiley and Sons.</p>
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<p>(<b>a</b>) Illustration of a DLP-printed gripper activated by light, serving as a soft robotic hand to grab objects. Reproduced with permission from ref. [<a href="#B89-applsci-15-02419" class="html-bibr">89</a>]. Copyright 2021 John Wiley and Sons. (<b>b</b>) Illustration of a 4D-printed soft robot folded by magnetic stimulation during hazardous chemical handling. Reproduced with permission from ref. [<a href="#B307-applsci-15-02419" class="html-bibr">307</a>]. Copyright 2023 Elsevier. (<b>c</b>) Schematic of a 3D-printing technique and photographs of thermos-responsive soft grippers. Reproduced with permission from ref. [<a href="#B213-applsci-15-02419" class="html-bibr">213</a>]. Copyright 2023 Elsevier. (<b>d</b>) Demonstration of a magnetically controlled micro-robot navigating and transporting an I-shaped cargo by rotating around it in response to pH changes. Reproduced with permission from ref. [<a href="#B31-applsci-15-02419" class="html-bibr">31</a>]. Copyright 2023 Springer Nature. (<b>e</b>) Schematic illustration of a crawling robot, inspired by leopard locomotion, walking on stairs according to steps 1–3 with IR light sequentially switched on and off. Reproduced with permission from ref. [<a href="#B311-applsci-15-02419" class="html-bibr">311</a>]. Copyright 2019 American Chemical Society. (<b>f</b>) Photographs of a low voltage-driven walking robot. Reproduced with permission from ref. [<a href="#B312-applsci-15-02419" class="html-bibr">312</a>]. Copyright 2021 American Chemical Society.</p>
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<p>(<b>a</b>) The antimicrobial properties of PLLA and PCL-TiO<sub>2</sub>/PLLA were tested against <span class="html-italic">B. subtilis</span>, <span class="html-italic">B. licheniformis</span>, and mold. Reproduced with permission from ref. [<a href="#B126-applsci-15-02419" class="html-bibr">126</a>]. Copyright 2023 Elsevier. (<b>b</b>) Photos of the 5f-t667 yarn sensor sewn onto silk fabric and a cotton glove, alongside relative resistance changes in the sensor when attached to a bending finger. Reproduced with permission from ref. [<a href="#B46-applsci-15-02419" class="html-bibr">46</a>]. Copyright 2023 Elsevier. (<b>c</b>) Illustration of rewritable photonic papers, along with optical and SEM images of a red photonic nanocomposite under 0%, 50%, and 100% tensile strain. Reproduced with permission from ref. [<a href="#B317-applsci-15-02419" class="html-bibr">317</a>]. Copyright 2018 John Wiley and Sons. (<b>d</b>) Fabrication of microcone arrays involved assembly procedures and showing the lossless transfer of droplets in both the “captured” and “detached” conditions. Reproduced with permission from ref. [<a href="#B121-applsci-15-02419" class="html-bibr">121</a>]. Copyright 2020 American Chemical Society. (<b>e</b>) Illustration of the shape-recovery procedure using several Morse codes based on different activation techniques. Reproduced with permission from ref. [<a href="#B320-applsci-15-02419" class="html-bibr">320</a>]. Copyright 2017 American Chemical Society.</p>
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<p>Illustration of the yearly quantity of scientific publications since 2000, obtained by employing the search phrases “shape-memory polymer”, “shape-memory polymer composites”, and “shape-memory polymer nanocomposites”. The data analysis was conducted with the Scopus search system on 29 January 2024.</p>
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9 pages, 5372 KiB  
Article
A Model of a “Smart” Thermoresponsive Composite with Convertible Surface Geometry Controlled by the Magnetocaloric Effect
by Abdulkarim A. Amirov, Maksim A. Koliushenkov, Dibir M. Yusupov, Eldar K. Murliev, Alisa M. Chirkova and Alexander P. Kamantsev
J. Compos. Sci. 2025, 9(3), 97; https://doi.org/10.3390/jcs9030097 - 21 Feb 2025
Viewed by 273
Abstract
A model of a “smart” composite based on a thermosensitive PNIPAM polymer deposited on a FeRh substrate with a modified periodic microstructure was proposed. The initial parameters of the model were determined from the properties of the actual composite sample and its components. [...] Read more.
A model of a “smart” composite based on a thermosensitive PNIPAM polymer deposited on a FeRh substrate with a modified periodic microstructure was proposed. The initial parameters of the model were determined from the properties of the actual composite sample and its components. Cooling of the sample using a magnetic field was shown by two independent methods, and at ~37 °C, it was −5.5 °C when a magnetic field of 1.8 T was applied. Based on experimental data, models of traditional and modified PNIPAM/FeRh composites were constructed. Calculations show that surface modification allows for an increase in the activation time for a polymer layer that is 20 µm thick from ~20 ms for a conventional composite to ~60 ms for a modified composite. Modification of the surface in the form of wells can be used to more effectively implement the idea of loading and releasing drugs for potential biomedical applications. Full article
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<p>Concept of the control PNIPAM properties by the magnetocaloric effect in the PNIPAM/FeRh smart composite: composite at dehydrated state at 37 °C and zero magnetic field (<b>a</b>) and composite is cooled down due inverse MCE at applied 2 T magnetic field, induced LCST in PNIPAM and transform it to hydrated state (<b>b</b>).</p>
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<p>SEM images of the FeRh sample and its composite modified by laser radiation: general image of modified sample (<b>a</b>), cross section of PNIPAM/FeRh sample (<b>b</b>) and images of hole -like structures (<b>c</b>,<b>d</b>).</p>
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<p>(<b>a</b>) Temperature dependence of magnetization for Fe<sub>49</sub>Rh<sub>51</sub> measured in a 1.8 T magnetic field at heating—red dots, left axis. Temperature dependence of dM/dT in a 1.8 T magnetic field—orange curve, right axis. (<b>b</b>) Magnetic field dependences of the adiabatic temperature change in the PNIPAM/FeRh sample as a result of the inverse MCE at magnetic fields up to 1.8 M measured at 37 °C.</p>
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<p>IR images obtained from MCE studies in PNIPAM/FeRh samples using a COX CG-640 IR camera at (<b>a</b>) zero and (<b>b</b>) 1.45 T applied magnetic field.</p>
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<p>A 3D model of a conventional (<b>a</b>) and modified (<b>b</b>) PNIPAM/FeRh composite.</p>
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<p>Time dependence of a normal and modified PNIPAM/FeRh composite.</p>
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<p>Three-dimensional maps of the temperature distribution in a sample at a selected time of modified PNIPAM/FeRh are presented when a 1.8 T magnetic field is used.</p>
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16 pages, 5102 KiB  
Article
Tröger’s Base Polyimide Membranes with Enhanced Mechanical Robustness for Gas Separation
by Xingfeng Lei, Zixiang Zhang, Yuyang Xiao, Qinyu Yu, Yewei Liu, Xiaohua Ma and Qiuyu Zhang
Polymers 2025, 17(4), 524; https://doi.org/10.3390/polym17040524 - 18 Feb 2025
Viewed by 443
Abstract
The rigid V-shaped Tröger’s base (TB) unit has been proven efficacious in creating microporosity, making TB-based polyimides (PIs) exhibiting significant advantages in simultaneously increasing gas permeability and selectivity for the separation industry. However, TB-based PIs commonly display undesired mechanical [...] Read more.
The rigid V-shaped Tröger’s base (TB) unit has been proven efficacious in creating microporosity, making TB-based polyimides (PIs) exhibiting significant advantages in simultaneously increasing gas permeability and selectivity for the separation industry. However, TB-based PIs commonly display undesired mechanical performance due to the low molecular weight resulting from the evident steric hindrance and low reactivity of TB-containing diamines. Herein, a novel diamine-containing bisimide linkage (BIDA) has been synthesized and then polymerized with paraformaldehyde via a moderate “TB polymerization” strategy to furnish polymers simultaneously, including imide linkages and TB units in the polymer main chains, namely, TB-PIs. This TB polymerization strategy avoids the direct polymerization of dianhydride with low-reactivity TB diamine. After incorporating a meta-methyl substituent into BIDA diamine, the m-MBIDA diamine-derived m-MTBPI ultimately exhibits a high molecular weight, good tensile strength (90.4 MPa) and an outstanding fracture toughness (45.1 MJ/m3). And more importantly, the m-MTBPI membrane displays an evidently enhanced gas separation ability in comparison with BIDA-derived TBPI, with overall separation properties much closer to the 1991 Robeson upper bound. Moreover, no sign of plasticization appears for the m-MTBPI membrane when separating a high-pressure CO2/CH4 mixture (v/v = 1/1) up to 20 bar, with the CO2/CH4 mixed-gas separation performance approaching the 2018 upper bound. Full article
(This article belongs to the Special Issue Advances in High-Performance Polymer Materials)
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<p>FT-IR spectra of (<b>a</b>) <span class="html-italic">m</span>-<b>MBIDA</b> diamine and (<b>b</b>) <span class="html-italic">m</span>-<b>MTBPI</b> polymer.</p>
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<p><sup>1</sup>H-NMR spectra of (<b>a</b>) <span class="html-italic">m</span>-<b>MBIDA</b> diamine and (<b>b</b>) <span class="html-italic">m</span>-<b>MTBPI</b> polymer in DMSO-<span class="html-italic">d</span><sub>6</sub>. The asterisk indicates solvent and moisture residuals or the <span class="html-italic">H</span>-grease signal.</p>
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<p>(<b>a</b>) TGA curves and (<b>b</b>) DMA curves of <b>TBPI</b> and <span class="html-italic">m</span>-<b>MTBPI</b> membranes. <span class="html-italic">Note:</span> the red dotted line in (<b>a</b>) indicates 95 w.t.% weight residuals.</p>
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<p>Tensile stress–strain curves of <span class="html-italic">m</span>-<b>MTBPI</b> membranes.</p>
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<p>WAXD patterns of <b>TBPI</b> and <span class="html-italic">m</span>-<b>MTBPI</b> membranes.</p>
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<p>(<b>a</b>) N<sub>2</sub> adsorption and desorption isotherms of the resulting polyimides tested at 77 K; (<b>b</b>) pore-size distribution of the resulting polyimides calculated by the H-K method according to N<sub>2</sub> sorption isotherms.</p>
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<p>Robeson plots relevant to the resulting polyimide membranes for the (<b>a</b>) CO<sub>2</sub>/CH<sub>4</sub> gas pair, (<b>b</b>) H<sub>2</sub>/CH<sub>4</sub> gas pair, (<b>c</b>) O<sub>2</sub>/N<sub>2</sub> gas pair and (<b>d</b>) H<sub>2</sub>/N<sub>2</sub> gas pair. The data points from the commercial polycarbonate, cellulose acetate, Matrimid 5218, polysulfones and several reported <b>TB-PI</b>s are shown for comparison. <span class="html-italic">Note</span>: The black line and red line, respectively, indicate the 1991 and 2008 Robeson upper bound.</p>
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<p>Comprehensive gas separation performance of the <span class="html-italic">m</span>-<b>MTBPI</b> membrane for the CO<sub>2</sub>/CH<sub>4</sub> mixed gas (50:50) relative to the 2018 upper bound. The results were obtained in the pressure range of 2–20 bar at 35 °C.</p>
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<p>CO<sub>2</sub>/CH<sub>4</sub> mixed-gas separation performance plotted with increasing upstream pressure for <span class="html-italic">m</span>-<b>MTBPI</b> membrane: (<b>a</b>) CO<sub>2</sub> permeability and (<b>b</b>) CO<sub>2</sub>/CH<sub>4</sub> gas pair selectivity.</p>
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<p>Reaction route for the synthesis of diamine monomers containing bisimide linkage.</p>
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<p>Reaction route for the preparation of TB-based polyimides.</p>
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49 pages, 3382 KiB  
Review
Recent Advances in the Fabrication of Intelligent Packaging for Food Preservation: A Review
by Tshamisane Mkhari, Jerry O. Adeyemi and Olaniyi A. Fawole
Processes 2025, 13(2), 539; https://doi.org/10.3390/pr13020539 - 14 Feb 2025
Viewed by 832
Abstract
The advancement of intelligent packaging technologies has emerged as a pivotal innovation in the food industry, significantly enhancing food safety and preservation. This review explores the latest developments in the fabrication of intelligent packaging, with a focus on applications in food preservation. Intelligent [...] Read more.
The advancement of intelligent packaging technologies has emerged as a pivotal innovation in the food industry, significantly enhancing food safety and preservation. This review explores the latest developments in the fabrication of intelligent packaging, with a focus on applications in food preservation. Intelligent packaging systems, which include sensors, indicators, and RFID technologies, offer the real-time monitoring of food quality and safety by detecting changes in environmental conditions and microbial activity. Innovations in nanotechnology, bio-based materials, and smart polymers have led to the development of eco-friendly and highly responsive packaging solutions. This review underscores the role of active and intelligent packaging components—such as oxygen scavengers, freshness indicators, and antimicrobial agents in extending shelf life and ensuring product integrity. Moreover, it highlights the transformative potential of intelligent packaging in food preservation through the examination of recent case studies. Finally, this review provides a comprehensive overview of current trends, challenges, and potential future directions in this rapidly evolving field. Full article
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<p>Classification of time–temperature indicators (TTIs) [<a href="#B47-processes-13-00539" class="html-bibr">47</a>]. Reproduced with permission from J Food Process Technol, under the terms of the Creative Commons Attribution License (Copyright, 2021).</p>
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<p>The uses of nanocomposites in food packaging [<a href="#B113-processes-13-00539" class="html-bibr">113</a>]. Reproduced with permission from Springer, copyright (2024).</p>
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<p>Potential uses of microfluidics in the field of food science as well as technology [<a href="#B152-processes-13-00539" class="html-bibr">152</a>]. Reproduced with permission from MDPI under the terms of the Creative Commons Attribution License (Copyright, 2022).</p>
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<p>Temperature-responsive polymers of (<b>A</b>) lemon essential oil [<a href="#B265-processes-13-00539" class="html-bibr">265</a>] and (<b>B</b>) cinnamon essential oil based on PNIPAm [<a href="#B266-processes-13-00539" class="html-bibr">266</a>]. Both figures are reproduced with permission from Elsevier (Copyright, 2024).</p>
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<p>Various types of pH indicators employed in intelligent packaging [<a href="#B267-processes-13-00539" class="html-bibr">267</a>]. Reproduced with permission from Taylor and Francis (Copyright, 2024).</p>
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11 pages, 9905 KiB  
Proceeding Paper
Production Parameters and Thermo-Mechanical Performance of Twisted and Coiled Artificial Muscles (TCAMs)
by Salvatore Garofalo, Chiara Morano, Leonardo Pagnotta and Luigi Bruno
Eng. Proc. 2025, 85(1), 1; https://doi.org/10.3390/engproc2025085001 - 13 Feb 2025
Viewed by 207
Abstract
High-strength polymer fibers such as nylon 6, nylon 6,6, and polyethylene are utilized to produce Twisted and Coiled Artificial Muscles (TCAMs) through the twisting of low-cost fibers. These artificial muscles exhibit high displacement and specific power, particularly under electrothermal actuation, which requires conductive [...] Read more.
High-strength polymer fibers such as nylon 6, nylon 6,6, and polyethylene are utilized to produce Twisted and Coiled Artificial Muscles (TCAMs) through the twisting of low-cost fibers. These artificial muscles exhibit high displacement and specific power, particularly under electrothermal actuation, which requires conductive elements. An experimental setup was developed to produce, thermally treat, and characterize commercially available nylon 6,6 fibers coated with silver. The results demonstrate that TCAMs can contract by over 15% and generate forces up to 2.5 N with minimal energy input. Key factors such as motor speed, applied load, and fiber geometry affect the overall performance. Full article
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<p>Manufacturing process of TCAM: twisting and coiling are necessary to create the structure of the artificial muscle; annealing and training allow to relax stress during the previous steps and set the geometry; plying is needed when multi-plies geometries are required.</p>
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<p>SEM analysis performed on the precursor fibers: (<b>a</b>) SEM image obtained of the Shieldex 235/36x4 HCB precursor fiber; (<b>b</b>) SEM magnification of (<b>a</b>).</p>
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<p>Micrographs taken of the precursor fibers and determination of their average diameters: (<b>a</b>) Shieldex 117/17x2 HCB; (<b>b</b>) Shieldex 235/36x2 HCB; (<b>c</b>) Shieldex 235/36x4 HCB.</p>
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<p>Schematic representation of the experimental setup (on the <b>left</b>) and its prototyping (on the <b>right</b>).</p>
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<p>Results of percentage displacement obtained for TCAMs made from the Shieldex 235/36x4 HCB fiber at the three rotational speeds during production: <span class="html-italic">ω</span> = 300 rpm (red curve); <span class="html-italic">ω</span> = 600 rpm (blue curve); <span class="html-italic">ω</span> = 900 rpm (black curve). The tests were conducted with a supply current of 0.6 A.</p>
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<p>Results of percentage displacement obtained for TCAMs made from the Shieldex 235/36x2 HCB fiber at the three rotational speeds during production: <span class="html-italic">ω</span> = 300 rpm (red curve); <span class="html-italic">ω</span> = 600 rpm (blue curve); <span class="html-italic">ω</span> = 900 rpm (black curve). The tests were conducted with a supply current of 0.35 A.</p>
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<p>Results of percentage displacement obtained for TCAMs made from the Shieldex 117/17x2 HCB fiber at the three rotational speeds during production: <span class="html-italic">ω</span> = 300 rpm (red curve); <span class="html-italic">ω</span> = 600 rpm (blue curve); <span class="html-italic">ω</span> = 900 rpm (black curve). The tests were conducted with a supply current of 0.15 A.</p>
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<p>Experimental results in terms of displacement obtained for TCAMs produced with a DC motor rotational speed of <span class="html-italic">ω</span> = 300 rpm, using increasing supply currents. The graphs refer to the following precursor fibers: (<b>a</b>) Shieldex 235/36x4 HCB; (<b>b</b>) Shieldex 235/36x2 HCB; (<b>c</b>) Shieldex 117/17x2 HCB.</p>
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15 pages, 3735 KiB  
Article
Development of Smart Material Identification Equipment for Sustainable Recycling in Future Smart Cities
by Gaku Manago, Tadao Tanabe, Kazuaki Okubo, Tetsuo Sasaki and Jeongsoo Yu
Polymers 2025, 17(4), 462; https://doi.org/10.3390/polym17040462 - 10 Feb 2025
Viewed by 605
Abstract
Waste recycling is critical for the development of smart cities. Local authorities are responsible for the disposal of waste plastics, but the extent of material recycling is insufficient, and much of the waste generated is incinerated. This conflicts with the trend of decarbonisation. [...] Read more.
Waste recycling is critical for the development of smart cities. Local authorities are responsible for the disposal of waste plastics, but the extent of material recycling is insufficient, and much of the waste generated is incinerated. This conflicts with the trend of decarbonisation. Of particular note are the effects of the COVID-19 pandemic, during and after which large quantities of waste plastics, such as plastic containers and packaging, were generated. In order to develop a sustainable smart city, we need an effective scheme where we can separate materials before they are taken to the local authorities and recyclers. In other words, if material identification can be performed at the place of disposal, the burden on recyclers can be reduced, and a smart city can be created. In this study, we developed and demonstrated smart material identification equipment for waste plastic materials made of PET, PS, PP, and PE using GaP THz and sub-THz wavelengths. As basic information, we used a GaP terahertz spectrometer to sweep frequencies from 0.5 THz to 7 THz and measure the spectrum, and the transmittance rate was measured using the sub-THz device. The sub-THz device used a specific frequency below 0.14 THz. This is a smaller, more carriable, and less expensive semiconductor electronic device than the GaP. Moreover, the sub-terahertz device used in the development of this equipment is compact, harmless to the human body, and can be used in public environments. As a result, smart equipment was developed and tested in places such as supermarkets, office entrances, and canteens. The identification of materials can facilitate material recycling. In this study, we found that measuring devices designed to identify the PET and PS components of transparent containers and packaging plastics, and the PP and PE components of PET bottle caps, could effectively identify molecular weights, demonstrating new possibilities for waste management and recycling systems in smart cities. With the ability to collect and analyse data, these devices can be powerful tools for pre-sorting. Full article
(This article belongs to the Special Issue Polymer Composites in Municipal Solid Waste Landfills)
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<p>Research background and methodology.</p>
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<p>Broadband terahertz spectroscopic equipment (the right picture was adopted from [<a href="#B30-polymers-17-00462" class="html-bibr">30</a>]).</p>
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<p>Terahertz spectra of polyethylene terephthalate (<b>a</b>) and polystyrene (<b>b</b>).</p>
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<p>Terahertz spectra from 0.5 THz to 5 THz of (<b>a</b>) a polypropylene plate, (<b>b</b>) a polyethylene plate, and (<b>c</b>) PE and PP bottle caps [<a href="#B15-polymers-17-00462" class="html-bibr">15</a>].</p>
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<p>Terahertz transmission distribution of PET and PS at frequencies of 0.1 THz and 0.075 THz.</p>
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<p>The z-scores for the transmittance rates of each sample.</p>
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<p>Bottle caps’ transmittance rates after being subjected to 0.14THz irradiation.</p>
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<p>The design of the smart identification equipment for identifying waste plastic containers used in the demonstration (<b>a</b>), and the implementation of the demonstration (<b>b</b>).</p>
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<p>The design of the smart identification equipment for identifying waste bottle caps used in the demonstration (<b>a</b>), and the implementation of the demonstration (<b>b</b>).</p>
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15 pages, 4052 KiB  
Article
Viscoelastic, Shape Memory, and Fracture Characteristics of 3D-Printed Photosensitive Epoxy-Based Resin Under the Effect of Hydrothermal Ageing
by Mohamad Alsaadi, Tamer A Sebaey, Eoin P. Hinchy, Conor T. McCarthy, Tielidy A. de M. de Lima, Alexandre Portela and Declan M. Devine
J. Manuf. Mater. Process. 2025, 9(2), 46; https://doi.org/10.3390/jmmp9020046 - 1 Feb 2025
Viewed by 807
Abstract
Using 3D-printed (3DPd) polymers and their composites as shape memory materials in various smart engineering applications has raised the demand for such functionally graded sustainable materials. This study aims to investigate the viscoelastic, shape memory, and fracture toughness properties of the epoxy-based ultraviolet [...] Read more.
Using 3D-printed (3DPd) polymers and their composites as shape memory materials in various smart engineering applications has raised the demand for such functionally graded sustainable materials. This study aims to investigate the viscoelastic, shape memory, and fracture toughness properties of the epoxy-based ultraviolet (UV)-curable resin. A UV-based DLP (Digital Light Processing) printer was employed for the 3D printing (3DPg) epoxy-based structures. The effect of the hydrothermal accelerated ageing on the various properties of the 3DPd components was examined. The viscoelastic performance in terms of glass transition temperature (Tg), storage modulus, and loss modulus was evaluated. The shape memory polymer (SMP) performance with respect to shape recovery and shape fixity (programming the shape) were calculated through dynamic mechanical thermal analysis (DMTA). DMTA is used to reveal the molecular mobility performance through three different regions, i.e., glass region, glass transition region, and rubbery region. The shape-changing region (within the glass transition region) between the Tg value from the loss modulus and the Tg value from the tan(δ) was analysed. The temperature memory behaviour was investigated for flat and circular 3DPd structures to achieve sequential deployment. The critical stress intensity factor values of the single-edge notch bending (SENB) specimens have been explored for different crack inclination angles to investigate mode I (opening) and mixed-mode I/III (opening and tearing) fracture toughness. This study can contribute to the development of highly complex shape memory 3DPd structures that can be reshaped several times with large deformation. Full article
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<p>Schematic diagram of the thermomechanical SMP cycle [<a href="#B4-jmmp-09-00046" class="html-bibr">4</a>].</p>
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<p>The programming/recovery process: (<b>a</b>) schematic diagram and (<b>b</b>) images of the 3DPd specimens under the programming/recovery process.</p>
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<p>Schematic diagram of the geometrical configuration of the SENB specimen.</p>
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<p>(<b>a</b>) DSC analysis before and after thermal post-curing; (<b>b</b>) the change in water uptake versus ageing time of the 3DP-Ep objects.</p>
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<p>Viscoelastic properties of the 3DP-Ep before and after the hydrothermal ageing: (<b>a</b>) <span class="html-italic">E’</span>, (<b>b</b>) (<span class="html-italic">tan(δ)</span>), and (<b>c</b>) <span class="html-italic">E</span>”.</p>
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<p>Thermomechanical SMP cycle of 3DPd samples using 4-step DMTA test, (<b>a</b>) Ep-135 °C, Ep-170 °C and Me-100 °C samples, (<b>b</b>) EP0h, EP600h, and EP1800 h samples.</p>
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<p>3DPd epoxy-based structures demonstrate temporary and recovery shapes.</p>
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<p>Mode I and mixed mode I/III critical stress intensity factors of the 3DP-Ep beams.</p>
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<p>(<b>i</b>) SENB specimens under test, and (<b>ii</b>) the samples and fracture surfaces of the (<b>a</b>) mode I θ = 90°, (<b>b</b>) mixed-mode I/III θ = 60°, and (<b>c</b>) mixed-mode I/III θ = 30°.</p>
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<p>SEM micrographs of the tensile test specimen fracture surface (red frame represents the location of the 50 µ image).</p>
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19 pages, 10271 KiB  
Article
Advanced Rheological, Dynamic Mechanical and Thermal Characterization of Phase-Separation Behavior of PLA/PCL Blends
by Evgeni Ivanov, Rumiana Kotsilkova, Vladimir Georgiev, Todor Batakliev and Verislav Angelov
J. Manuf. Mater. Process. 2025, 9(2), 35; https://doi.org/10.3390/jmmp9020035 - 27 Jan 2025
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Abstract
This research presents a comprehensive investigation of PLA/PCL polymer blends using advanced rheological characterization, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and dynamic mechanical, thermal analysis (DMTA) to evaluate phase-separation behavior and functional properties. Polymer composites with various PLA/PCL ratios were fabricated [...] Read more.
This research presents a comprehensive investigation of PLA/PCL polymer blends using advanced rheological characterization, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and dynamic mechanical, thermal analysis (DMTA) to evaluate phase-separation behavior and functional properties. Polymer composites with various PLA/PCL ratios were fabricated via melt extrusion, a sustainable and scalable approach. The rheological studies revealed significant insights into the blends’ viscoelastic behavior, while SEM analyses provided detailed observations of microstructural phase separation. Thermal transitions and crystallization behaviors were evaluated through DSC, and the dynamic mechanical properties were examined via DMTA. The results confirmed that the tailored PLA/PCL blends exhibit properties suitable for advanced additive manufacturing (AM) and shape memory applications, merging flexibility and environmental sustainability. This study emphasizes the novelty of integrating multidisciplinary characterization methods to unravel the structure–property relationships in PLA/PCL systems. By addressing modern demands for eco-friendly, high-performance materials, this work establishes a foundation for the development of innovative polymer composites with potential applications in smart and responsive technologies. Full article
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Figure 1

Figure 1
<p>Processing and characterization workflow of PLA/PCL polymer blends.</p>
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<p>SEM micrographs of blends with ratios of 95/5, 70/30, 60/40, and 30/70 <span class="html-italic">w</span>/<span class="html-italic">w</span> PLA/PCL at low and high magnifications of 20 µm and 5 µm. Arrows pointed to the PLA and the PCL phases.</p>
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<p>(<b>a</b>–<b>h</b>) Dynamic rheological characteristics, G′&amp;G″, and <b><span class="html-italic">η</span></b>* vs. angular frequency (ω) of melts at 190 °C: (<b>a</b>) PLA, (<b>b</b>) 95PLA/5PCL, (<b>c</b>) 70PLA/30PCL, (<b>d</b>) 60PLA/40PCL, (<b>e</b>) 30PLA/70PCL, (<b>f</b>) PCL, and (<b>g</b>,<b>h</b>) comparison of <b><span class="html-italic">η</span></b>* and G′&amp; G″ vs. (ω) for all samples at 190 °C.</p>
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<p>(<b>a</b>,<b>b</b>) Phase angle (δ) as a function of angular frequency (<b>a</b>) and Cole–Cole plots (<b>b</b>) for PCL/PLA blends at various weight ratios at 190 °C.</p>
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<p>(<b>a</b>–<b>g</b>) Storage and loss moduli (G′&amp;G″) vs. temperature (T) at heating rates of 3 °C/min and 5 °C/min under airflow of (<b>a</b>) PLA, (<b>b</b>) 95PLA/5PCL, (<b>c</b>) 70PLA/30PCL, (<b>d</b>) 60PLA/40PCL, (<b>e</b>) 30PLA/70PCL, (<b>f</b>) PCL, and (<b>f</b>,<b>g</b>) comparison of G′&amp;G″ vs. T at 3 °C/min and 5 °C/min, respectively.</p>
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<p>(<b>a</b>,<b>b</b>) Tan δ curves for the neat PLA and the PLA/PCL blends with increasing the PCL content from 5 to 70 wt.% at heating rates 3 °C/min (<b>a</b>) and 5 °C/min (<b>b</b>).</p>
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<p>Glass transition temperature (T<sub>g,PLA</sub>) determined from DMTA tests for PLA and its blends with varying PCL content at two different heating rates: 3 °C/min (black dots) and 5 °C/min (red dots).</p>
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<p>(<b>a</b>,<b>b</b>) DSC thermograms of PLA, PCL, and blends: (<b>a</b>) heating run and (<b>b</b>) cooling run at a ramp of 10 °C/min.</p>
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<p>The crystallinity of the PLA, PCL, and total crystallinity depending on the blend ratio.</p>
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<p>TGA thermograms of weight loss vs. temperature (<b>a</b>) and their first derivative (<b>b</b>) of the PLA/PCL blends.</p>
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<p>Temperatures corresponding to the 2% (dark green circle), 5% (red triangle), 10% (blue star), and 50% (light green square) weight loss vs. the PCL content in the PLA/PCL.</p>
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