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Keywords = TGA-DSC analysis

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25 pages, 17212 KiB  
Article
Three-Dimensional Printing of Personalized Carbamazepine Tablets Using Hydrophilic Polymers: An Investigation of Correlation Between Dissolution Kinetics and Printing Parameters
by Lianghao Huang, Xingyue Zhang, Qichen Huang, Minqing Zhu, Tiantian Yang and Jiaxiang Zhang
Polymers 2025, 17(15), 2126; https://doi.org/10.3390/polym17152126 (registering DOI) - 1 Aug 2025
Abstract
Background: Precision medicine refers to the formulation of personalized drug regimens according to the individual characteristics of patients to achieve optimal efficacy and minimize adverse reactions. Additive manufacturing (AM), also known as three-dimensional (3D) printing, has emerged as an optimal solution for precision [...] Read more.
Background: Precision medicine refers to the formulation of personalized drug regimens according to the individual characteristics of patients to achieve optimal efficacy and minimize adverse reactions. Additive manufacturing (AM), also known as three-dimensional (3D) printing, has emerged as an optimal solution for precision drug delivery, enabling customizable and the fabrication of multifunctional structures with precise control over morphology and release behavior in pharmaceutics. However, the influence of 3D printing parameters on the printed tablets, especially regarding in vitro and in vivo performance, remains poorly understood, limiting the optimization of manufacturing processes for controlled-release profiles. Objective: To establish the fabrication process of 3D-printed controlled-release tablets via comprehensively understanding the printing parameters using fused deposition modeling (FDM) combined with hot-melt extrusion (HME) technologies. HPMC-AS/HPC-EF was used as the drug delivery matrix and carbamazepine (CBZ) was used as a model drug to investigate the in vitro drug delivery performance of the printed tablets. Methodology: Thermogravimetric analysis (TGA) was employed to assess the thermal compatibility of CBZ with HPMC-AS/HPC-EF excipients up to 230 °C, surpassing typical processing temperatures (160–200 °C). The formation of stable amorphous solid dispersions (ASDs) was validated using differential scanning calorimetry (DSC), hot-stage polarized light microscopy (PLM), and powder X-ray diffraction (PXRD). A 15-group full factorial design was then used to evaluate the effects of the fan speed (20–100%), platform temperature (40–80 °C), and printing speed (20–100 mm/s) on the tablet properties. Response surface modeling (RSM) with inverse square-root transformation was applied to analyze the dissolution kinetics, specifically t50% (time for 50% drug release) and Q4h (drug released at 4 h). Results: TGA confirmed the thermal compatibility of CBZ with HPMC-AS/HPC-EF, enabling stable ASD formation validated by DSC, PLM, and PXRD. The full factorial design revealed that printing speed was the dominant parameter governing dissolution behavior, with high speeds accelerating release and low speeds prolonging release through porosity-modulated diffusion control. RSM quadratic models showed optimal fits for t50% (R2 = 0.9936) and Q4h (R2 = 0.9019), highlighting the predictability of release kinetics via process parameter tuning. This work demonstrates the adaptability of polymer composite AM for tailoring drug release profiles, balancing mechanical integrity, release kinetics, and manufacturing scalability to advance multifunctional 3D-printed drug delivery devices in pharmaceutics. Full article
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16 pages, 5071 KiB  
Article
Effect of Diatomite Content in a Ceramic Paste for Additive Manufacturing
by Pilar Astrid Ramos Casas, Andres Felipe Rubiano-Navarrete, Yolanda Torres-Perez and Edwin Yesid Gomez-Pachon
Ceramics 2025, 8(3), 96; https://doi.org/10.3390/ceramics8030096 (registering DOI) - 31 Jul 2025
Abstract
Ceramic pastes used in additive manufacturing offer several advantages, including low production costs due to the availability of raw materials and efficient processing methods, as well as a reduced environmental footprint through minimized material waste, optimized resource use, and the inclusion of recyclable [...] Read more.
Ceramic pastes used in additive manufacturing offer several advantages, including low production costs due to the availability of raw materials and efficient processing methods, as well as a reduced environmental footprint through minimized material waste, optimized resource use, and the inclusion of recyclable or sustainably sourced components. This study evaluates the effect of diatomite content in a ceramic paste composed of carboxymethyl cellulose, kaolinite, and feldspar on its extrusion behavior and thermal conductivity, with additional analysis of its implications for microstructure, mechanical properties, and thermal performance. Four ceramic pastes were prepared with diatomite additions of 0, 10, 30, and 60% by weight. Thermal conductivity, extrusion behavior, morphology, and distribution were examined using scanning electron microscopy (SEM), while thermal degradation was assessed through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results show that increasing diatomite content leads to a reduction in thermal conductivity, which ranged from 0.719 W/(m·°C) for the control sample to 0.515 W/(m·°C) for the 60% diatomite sample, as well as an improvement in extrusion behavior. The ceramic paste demonstrated adequate extrusion performance for 3D printing at diatomite contents above 30%. These findings lay the groundwork for future research and optimization in the development of functional ceramic pastes for advanced manufacturing applications. Full article
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18 pages, 7413 KiB  
Article
Thermal Degradation of Carboxymethyl Cellulose (CMC) in Saline Solution for Applications in Petroleum Industry Fluids
by Mirele Costa da Silva Farias, Waleska Rodrigues Pontes da Costa, Karine Castro Nóbrega, Victória Bezerra Romualdo, Anna Carolina Amorim Costa, Renalle Cristina Alves de Medeiros Nascimento and Luciana Viana Amorim
Polymers 2025, 17(15), 2085; https://doi.org/10.3390/polym17152085 - 30 Jul 2025
Viewed by 204
Abstract
This work aims to evaluate the thermal degradation of carboxymethyl cellulose (CMC) in solution in the presence of salt, as well as to study the correlation of the rheological behavior of these solutions with exposure to temperature. Step 1 involved characterizing powdered low- [...] Read more.
This work aims to evaluate the thermal degradation of carboxymethyl cellulose (CMC) in solution in the presence of salt, as well as to study the correlation of the rheological behavior of these solutions with exposure to temperature. Step 1 involved characterizing powdered low- and high-viscosity CMC using SEM, FTIR, TGA/DrTGA, and DSC. In step 2, CMC solutions in fresh and saline water were characterized by TGA/DrTGA and viscosity tests. Step 3 exposed saline solutions to 70–150 °C for varying times, followed by TGA/DrTGA and viscosity analyses. There were no significant differences in the thermal degradation of LV and HV CMC, nor in terms of the physical state of the polymer. The results demonstrate that the use of CMC necessitates a combined analysis of thermal degradation and rheological behavior. Full article
(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose: 2nd Edition)
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28 pages, 14491 KiB  
Article
Catalytically Active Oxidized PtOx Species on SnO2 Supports Synthesized via Anion Exchange Reaction for 4-Nitrophenol Reduction
by Izabela Ðurasović, Robert Peter, Goran Dražić, Fabio Faraguna, Rafael Anelić, Marijan Marciuš, Tanja Jurkin, Vlasta Mohaček Grošev, Maria Gracheva, Zoltán Klencsár, Mile Ivanda, Goran Štefanić and Marijan Gotić
Nanomaterials 2025, 15(15), 1159; https://doi.org/10.3390/nano15151159 - 28 Jul 2025
Viewed by 252
Abstract
An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO2 supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO2 supports, namely SnA (synthesized almost at room [...] Read more.
An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO2 supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO2 supports, namely SnA (synthesized almost at room temperature), SnB (hydrothermally treated at 180 °C), and SnC (annealed at 600 °C), are systematically investigated, all loaded with 1 mol% Pt from H2PtCl6 under identical mild conditions. The chloride ions from the SnCl4 precursors were efficiently removed via a strong-base anion exchange reaction, resulting in highly dispersed, crystalline ~5 nm cassiterite SnO2 particles. All Pt/SnO2 composites displayed mesoporous structures with type IVa isotherms and H2-type hysteresis, with SP1a (Pt on SnA) exhibiting the largest surface area (122.6 m2/g) and the smallest pores (~3.5 nm). STEM-HAADF imaging revealed well-dispersed PtOx domains (~0.85 nm), while XPS confirmed the dominant Pt4+ and Pt2+ species, with ~25% Pt0 likely resulting from photoreduction and/or interactions with Sn–OH surface groups. Raman spectroscopy revealed three new bands (260–360 cm−1) that were clearly visible in the sample with 10 mol% Pt and were due to the vibrational modes of the PtOx species and Pt-Cl bonds introduced due the addition and hydrolysis of H2PtCl6 precursor. TGA/DSC analysis revealed the highest mass loss for SP1a (~7.3%), confirming the strong hydration of the PtOx domains. Despite the predominance of oxidized PtOx species, SP1a exhibited the highest catalytic activity (kapp = 1.27 × 10−2 s−1) and retained 84.5% activity for the reduction of 4-NP to 4-AP after 10 cycles. This chloride-free low-temperature synthesis route offers a promising and generalizable strategy for the preparation of noble metal-based nanocatalysts on oxide supports with high catalytic activity and reusability. Full article
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16 pages, 2206 KiB  
Article
Turning Waste into Wealth: Sustainable Amorphous Silica from Moroccan Oil Shale Ash
by Anas Krime, Sanaâ Saoiabi, Mouhaydine Tlemcani, Ahmed Saoiabi, Elisabete P. Carreiro and Manuela Ribeiro Carrott
Recycling 2025, 10(4), 143; https://doi.org/10.3390/recycling10040143 - 20 Jul 2025
Viewed by 266
Abstract
Moroccan oil shale ash (MOSA) represents an underutilized industrial by-product, particularly in the Rif region, where its high mineral content has often led to its neglect in value-added applications. This study highlights the successful conversion of MOSA into amorphous mesoporous silica (AS-Si) using [...] Read more.
Moroccan oil shale ash (MOSA) represents an underutilized industrial by-product, particularly in the Rif region, where its high mineral content has often led to its neglect in value-added applications. This study highlights the successful conversion of MOSA into amorphous mesoporous silica (AS-Si) using a sol–gel process assisted by polyethylene glycol (PEG-6000) as a soft template. The resulting AS-Si material was extensively characterized to confirm its potential for environmental remediation. FTIR analysis revealed characteristic vibrational bands corresponding to Si–OH and Si–O–Si bonds, while XRD confirmed its amorphous nature with a broad diffraction peak at 2θ ≈ 22.5°. SEM imaging revealed a highly porous, sponge-like morphology composed of aggregated nanoscale particles, consistent with the nitrogen adsorption–desorption isotherm. The material exhibited a specific surface area of 68 m2/g, a maximum in the pore size distribution at a pore diameter of 2.4 nm, and a cumulative pore volume of 0.11 cm3/g for pores up to 78 nm. DLS analysis indicated an average hydrodynamic diameter of 779 nm with moderate polydispersity (PDI = 0.48), while a zeta potential of –34.10 mV confirmed good colloidal stability. Furthermore, thermogravimetric analysis (TGA) and DSC suggested the thermal stability of our amorphous silica. The adsorption performance of AS-Si was evaluated using methylene blue (MB) and ciprofloxacin (Cipro) as model pollutants. Kinetic data were best fitted by the pseudo-second-order model, while isotherm studies favored the Langmuir model, suggesting monolayer adsorption. AS-Si could be used four times for the removal of MB and Cipro. These results collectively demonstrate that AS-Si is a promising, low-cost, and sustainable adsorbent derived from Moroccan oil shale ash for the effective removal of organic contaminants from aqueous media. Full article
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14 pages, 2050 KiB  
Article
Electrospun PANI/PEO-Luffa Cellulose/TiO2 Nanofibers: A Sustainable Biocomposite for Conductive Applications
by Gözde Konuk Ege, Merve Bahar Okuyucu and Özge Akay Sefer
Polymers 2025, 17(14), 1989; https://doi.org/10.3390/polym17141989 - 20 Jul 2025
Viewed by 472
Abstract
Herein, electrospun nanofibers composed of polyaniline (PANI), polyethylene oxide (PEO), and Luffa cylindrica (LC) cellulose, reinforced with titanium dioxide (TiO2) nanoparticles, were synthesized via electrospinning to investigate the effect of TiO2 nanoparticles on PANI/PEO/LC nanocomposites and the effect of conductivity [...] Read more.
Herein, electrospun nanofibers composed of polyaniline (PANI), polyethylene oxide (PEO), and Luffa cylindrica (LC) cellulose, reinforced with titanium dioxide (TiO2) nanoparticles, were synthesized via electrospinning to investigate the effect of TiO2 nanoparticles on PANI/PEO/LC nanocomposites and the effect of conductivity on nanofiber morphology. Cellulose extracted from luffa was added to the PANI/PEO copolymer solution, and two different ratios of TiO2 were mixed into the PANI/PEO/LC biocomposite. The morphological, vibrational, and thermal characteristics of biocomposites were systematically investigated using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). As anticipated, the presence of TiO2 enhanced the electrical conductivity of biocomposites, while the addition of Luffa cellulose further improved the conductivity of the cellulose-based nanofibers. FTIR analysis confirmed chemical interactions between Luffa cellulose and PANI/PEO matrix, as evidenced by the broadening of the hydroxyl (OH) absorption band at 3500–3200 cm−1. Additionally, the emergence of characteristic peaks within the 400–1000 cm−1 range in the PANI/PEO/LC/TiO2 spectra signified Ti–O–Ti and Ti–O–C vibrations, confirming the incorporation of TiO2 into the biocomposite. SEM images of the biocomposites reveal that the thickness of nanofibers decreases by adding Luffa to PANI/PEO nanofibers because of the nanofibers branching. In addition, when blending TiO2 nanoparticles with the PANI/PEO/LC biocomposite, this increment continued and obtained thinner and smother nanofibers. Furthermore, the incorporation of cellulose slightly improved the crystallinity of the nanofibers, while TiO2 contributed to the enhanced crystallinity of the biocomposite according to the XRD and DCS results. Similarly, the TGA results supported the DSC results regarding the increasing thermal stability of the biocomposite nanofibers with TiO2 nanoparticles. These findings demonstrate the potential of PANI/PEO/LC/TiO2 nanofibers for advanced applications requiring conductive and structurally optimized biomaterials, e.g., for use in humidity or volatile organic compound (VOC) sensors, especially where flexibility and environmental sustainability are required. Full article
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21 pages, 6746 KiB  
Article
Harnessing Wild Jackfruit Extract for Chitosan Production by Aspergillus versicolor AD07: Application in Antibacterial Biodegradable Sheets
by Adhithya Sankar Santhosh and Mridul Umesh
Appl. Microbiol. 2025, 5(3), 71; https://doi.org/10.3390/applmicrobiol5030071 - 20 Jul 2025
Viewed by 368
Abstract
A fungal strain with comparably high chitosan yield was isolated from the Shivaganga hills and identified as Aspergillus versicolor AD07 through molecular characterization. Later, the strain was cultivated on Sabouraud Dextrose Broth (SDB) and wild jackfruit-based media to evaluate its potential for chitosan [...] Read more.
A fungal strain with comparably high chitosan yield was isolated from the Shivaganga hills and identified as Aspergillus versicolor AD07 through molecular characterization. Later, the strain was cultivated on Sabouraud Dextrose Broth (SDB) and wild jackfruit-based media to evaluate its potential for chitosan production. Among the various media formulations, the highest chitosan yield (178.40 ± 1.76 mg/L) was obtained from the jackfruit extract medium with added peptone and dextrose. The extracted chitosan was characterized through FTIR, XRD (reported a crystallinity index of 55%), TGA/DTG, and DSC analysis, confirming the presence of key functional groups and high thermal resistance. The extracted chitosan was fabricated into a sheet incorporated with 1% lemongrass oil; the sheet exhibited strong antibacterial activity against Escherichia coli (30 mm) and Bacillus megaterium (48 mm). The biodegradation studies reported a weight loss of 38.93 ± 0.51% after 50 days of soil burial. Further, the chitosan film was tested as a packaging material for paneer, demonstrating better preservation by maintaining nutritional quality and reducing microbial load over a 14-day storage period. These findings highlight the potential of A. versicolor AD07-derived chitosan, cultivated on a waste substrate medium, as a sustainable biopolymer for food packaging applications. Full article
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18 pages, 3500 KiB  
Article
Cellulose Acetate–PHB Biocomposite from Saccharum officinarum for Ni (II) Adsorption: Equilibrium and Kinetics
by Candelaria Tejada-Tovar, Ángel Villabona-Ortíz, Oscar Toro-Madrid, Rodrigo Ortega-Toro and Humberto Bonilla Mancilla
J. Compos. Sci. 2025, 9(7), 376; https://doi.org/10.3390/jcs9070376 - 18 Jul 2025
Viewed by 518
Abstract
This research work focused on the development of an adsorbent biocomposite material based on polyhydroxybutyrate (PHB) and cellulose acetate derived from sugarcane (Saccharum officinarum) fibre, through cellulose acetylation. The resulting material represents both an accessible and effective alternative for the treatment [...] Read more.
This research work focused on the development of an adsorbent biocomposite material based on polyhydroxybutyrate (PHB) and cellulose acetate derived from sugarcane (Saccharum officinarum) fibre, through cellulose acetylation. The resulting material represents both an accessible and effective alternative for the treatment and remediation of water contaminated with heavy metals, such as Ni (II). The biocomposite was prepared by blending cellulose acetate (CA) with the biopolymer PHB using the solvent-casting method. The resulting biocomposite exhibited a point of zero charge (pHpzc) of 5.6. The material was characterised by FTIR, TGA-DSC, and SEM analyses. The results revealed that the interaction between Ni (II) ions and the biocomposite is favoured by the presence of functional groups, such as –OH, C=O, and N–H, which act as active adsorption sites on the material’s surface, enabling efficient interaction with the metal ions. Adsorption kinetics studies revealed that the biocomposite achieved an optimal adsorption capacity of 5.042 mg/g at pH 6 and an initial Ni (II) concentration of 35 mg/L, corresponding to a removal efficiency of 86.44%. Finally, an analysis of the kinetic and isotherm models indicated that the experimental data best fit the pseudo-second-order kinetic model and the Freundlich isotherm. Full article
(This article belongs to the Special Issue Sustainable Biocomposites, 3rd Edition)
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22 pages, 4234 KiB  
Article
Furan–Urethane Monomers for Self-Healing Polyurethanes
by Polina Ponomareva, Zalina Lokiaeva, Daria Zakharova, Ilya Tretyakov, Elena Platonova, Aleksey Shapagin, Olga Alexeeva, Evgenia Antoshkina, Vitaliy Solodilov, Gleb Yurkov and Alexandr Berlin
Polymers 2025, 17(14), 1951; https://doi.org/10.3390/polym17141951 - 16 Jul 2025
Viewed by 239
Abstract
The repair efficiency of various self-healing materials often depends on the ability of the prepolymer and curing agent to form mixtures. This paper presents a synthesis and study of the properties of modified self-healing polyurethanes using the Diels–Alder reaction (DA reaction), obtained from [...] Read more.
The repair efficiency of various self-healing materials often depends on the ability of the prepolymer and curing agent to form mixtures. This paper presents a synthesis and study of the properties of modified self-healing polyurethanes using the Diels–Alder reaction (DA reaction), obtained from a maleimide-terminated preform and a series of furan–urethane curing agents. The most commonly used isocyanates (4,4′-methylene diphenyl diisocyanate (MDI), 2,4-tolylene diisocyanate (TDI), and hexamethylene diisocyanate (HDI)) and furan derivatives (furfurylamine, difurfurylamine, and furfuryl alcohol) were used as initial reagents for the synthesis of curing agents. For comparative analysis, polyurethanes were also obtained using the well-known “traditional” approach—from furan-terminated prepolymers based on mono- and difurfurylamine, as well as furfuryl alcohol and the often-used bismaleimide curing agent 1,10-(methylenedi-1,4-phenylene)bismaleimide (BMI). The structure and composition of all polymers were studied using spectroscopic methods. Molecular mass was determined using gel permeation chromatography (GPC). Thermal properties were studied using TGA, DSC, and TMA methods. The mechanical and self-healing properties of the materials were investigated via a uniaxial tensile test. Visual assessment of the completeness of damage restoration after the self-healing cycle was carried out using a scanning electron microscope. It was shown that the proposed modified approach helps obtain more durable polyurethanes with a high degree of self-healing of mechanical properties after damage. Full article
(This article belongs to the Special Issue Advances in Fracture and Failure of Polymers)
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16 pages, 4299 KiB  
Article
Gas Barrier Properties of Organoclay-Reinforced Polyamide 6 Nanocomposite Liners for Type IV Hydrogen Storage Vessels
by Dávid István Kis, Pál Hansághy, Attila Bata, Nándor Nemestóthy, Péter Gerse, Ferenc Tajti and Eszter Kókai
Nanomaterials 2025, 15(14), 1101; https://doi.org/10.3390/nano15141101 - 16 Jul 2025
Viewed by 266
Abstract
This study investigates the hydrogen permeability of injection-molded polyamide 6 (PA6) nanocomposites reinforced with organo-modified montmorillonite (OMMT) at varying concentrations (1, 2.5, 5, and 10 wt. %) for potential use as Type IV composite-overwrapped pressure vessel (COPV) liners. While previous work examined their [...] Read more.
This study investigates the hydrogen permeability of injection-molded polyamide 6 (PA6) nanocomposites reinforced with organo-modified montmorillonite (OMMT) at varying concentrations (1, 2.5, 5, and 10 wt. %) for potential use as Type IV composite-overwrapped pressure vessel (COPV) liners. While previous work examined their mechanical properties, this study focuses on their crystallinity, morphology, and gas barrier performance. The precise inorganic content was determined using thermal gravimetry analysis (TGA), while differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), and scanning electron microscopy (SEM) were used to characterize the structural and morphological changes induced by varying filler content. The results showed that generally higher OMMT concentrations promoted γ-phase formation but also led to increased agglomeration and reduced crystallinity. The PA6/OMMT-1 wt. % sample stood out with higher crystallinity, well-dispersed clay, and low hydrogen permeability. In contrast, the PA6/OMMT-2.5 and -5 wt. % samples showed increased permeability, which corresponded to WAXD and SEM evidence of agglomeration and DSC results indicating a lower degree of crystallinity. PA6/OMMT-10 wt. % showed the most-reduced hydrogen permeability compared to all other samples. This improvement, however, is attributed to a tortuous path effect created by the high filler loading rather than optimal crystallinity or dispersion. SEM images revealed significant OMMT agglomeration, and DSC analysis confirmed reduced crystallinity, indicating that despite the excellent barrier performance, the compromised microstructure may negatively impact mechanical reliability, showing PA6/OMMT-1 wt. % to be the most balanced candidate combining both mechanical integrity and hydrogen impermeability for Type IV COPV liners. Full article
(This article belongs to the Section Nanocomposite Materials)
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15 pages, 3491 KiB  
Article
Development and Characterization of Composite Films of Potato Starch and Carboxymethylcellulose/Poly(ethylene oxide) Nanofibers
by Yenny Paola Cruz Moreno, Andres Felipe Rubiano-Navarrete, Erika Rocio Cely Rincón, Adriana Elizabeth Lara Sandoval, Alfredo Maciel Cerda, Edwin Yesid Gomez-Pachon and Ricardo Vera-Graziano
Eng 2025, 6(7), 160; https://doi.org/10.3390/eng6070160 - 15 Jul 2025
Viewed by 514
Abstract
This study aimed to develop and characterize biodegradable films based on potato starch reinforced with carboxymethylcellulose (CMC) and polyethylene oxide (PEO) nanofibers, with the goal of improving their mechanical and thermal properties for potential use in sustainable packaging. The films were prepared through [...] Read more.
This study aimed to develop and characterize biodegradable films based on potato starch reinforced with carboxymethylcellulose (CMC) and polyethylene oxide (PEO) nanofibers, with the goal of improving their mechanical and thermal properties for potential use in sustainable packaging. The films were prepared through the thermal gelatinization of starch extracted from tubers, combined with nanofibers obtained by electrospinning CMC synthesized from potato starch. Key electrospinning variables, including solution concentration, voltage, distance, and flow rate, were analyzed. The films were morphologically characterized using scanning electron microscopy (SEM) and chemically analyzed by Fourier Transform Infrared Spectroscopy (FTIR) and X-ray Diffraction (XRD), and their thermal properties were assessed by Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). The results indicated an increase in tensile strength to 14.1 MPa in the reinforced films, compared to 13.6 MPa for pure starch and 7.1 MPa for the fiber-free CMC blend. The nanofibers had an average diameter of 63.3 nm and a porosity of 32.78%. A reduction in crystallinity and more stable thermal behavior were also observed in the composite materials. These findings highlight the potential of using agricultural waste as a functional reinforcement in biopolymers, providing a viable and environmentally friendly alternative to synthetic polymers. Full article
(This article belongs to the Section Materials Engineering)
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20 pages, 3330 KiB  
Article
Impact of Multiple Mechanical Recycling Cycles via Semi-Industrial Twin-Screw Extrusion on the Properties of Polybutylene Succinate (PBS)
by Vito Gigante, Laura Aliotta, Luigi Botta, Irene Bavasso, Alessandro Guzzini, Serena Gabrielli, Fabrizio Sarasini, Jacopo Tirillò and Andrea Lazzeri
Polymers 2025, 17(14), 1918; https://doi.org/10.3390/polym17141918 - 11 Jul 2025
Viewed by 501
Abstract
This study investigates the effects of repeated mechanical recycling on the structural, thermal, mechanical, and aesthetic properties of poly(butylene succinate) (PBS), a commercially available bio-based and biodegradable aliphatic polyester. PBS production scraps were subjected to five consecutive recycling cycles through semi-industrial extrusion compounding [...] Read more.
This study investigates the effects of repeated mechanical recycling on the structural, thermal, mechanical, and aesthetic properties of poly(butylene succinate) (PBS), a commercially available bio-based and biodegradable aliphatic polyester. PBS production scraps were subjected to five consecutive recycling cycles through semi-industrial extrusion compounding followed by injection molding to simulate realistic mechanical reprocessing conditions. Melt mass-flow rate (MFR) analysis revealed a progressive increase in melt fluidity. Initially, the trend of viscosity followed the melt flow rate; however, increasing the reprocessing number (up to 5) resulted in a partial recovery of viscosity, which was caused by chain branching mechanisms. The phenomenon was also confirmed by data of molecular weight evaluation. Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) confirmed the thermal stability of the polymer, with minimal shifts in glass transition, crystallization, and degradation temperatures during the reprocessing cycles. Tensile tests revealed a slight reduction in strength and stiffness, but an increase in elongation at break, indicating improved ductility. Impact resistance declined moderately from 8.7 to 7.3 kJ/m2 upon reprocessing; however, it exhibited a pronounced reduction to 1.8 kJ/m2 at −50 °C, reflecting brittle behavior under sub-ambient conditions. Despite these variations, PBS maintained excellent color stability (ΔE < 1), ensuring aesthetic consistency while retaining good mechanical and thermal properties. Full article
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18 pages, 2582 KiB  
Article
Thermal Stability and Eutectic Point of Chloride-Based High-Temperature Molten Salt Energy Systems
by Sunghyun Yoo, Jihun Kim, Sungyeol Choi and Jeong Ik Lee
Energies 2025, 18(14), 3616; https://doi.org/10.3390/en18143616 - 9 Jul 2025
Viewed by 314
Abstract
In response to the growing impact of the climate crisis, many countries are accelerating efforts to develop sustainable and carbon-free energy solutions. This has led to increasing interest in advanced energy storage and conversion technologies, particularly the development of high-temperature molten salt energy [...] Read more.
In response to the growing impact of the climate crisis, many countries are accelerating efforts to develop sustainable and carbon-free energy solutions. This has led to increasing interest in advanced energy storage and conversion technologies, particularly the development of high-temperature molten salt energy systems. Among these, chloride salt-based molten salt systems, which offer excellent thermal properties such as high thermal conductivity, low melting points, and favorable chemical stability, are emerging as strong candidates for thermal energy storage and heat-transfer applications. This study focuses on deriving key thermophysical properties essential for selecting suitable molten salt heat-transfer fluids by examining their eutectic points and thermal stability with respect to various salt compositions. Three chloride mixtures—NaCl-MgCl2, NaCl-KCl-MgCl2, and NaCl-KCl-ZnCl2—were evaluated for potential use in high-temperature molten salt energy systems. Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were employed to measure the melting points and thermal stability of molten salts with various compositions near their eutectic regions. Experimental results were compared with predicted eutectic points to assess the thermal performance of each salt mixture. The findings indicate that the NaCl-KCl-MgCl2 mixture exhibits the most promising characteristics, including a low melting point below 400 °C and superior thermal stability, making it highly suitable as a heat-transfer fluid in high-temperature molten salt energy systems. In contrast, NaCl-KCl-ZnCl2 was found unsuitable for such applications due to its high hygroscopicity and poor thermal stability. This study provides essential data for selecting optimal molten salt compositions for the efficient and reliable operation of high-temperature molten salt energy systems. Full article
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24 pages, 3329 KiB  
Article
Heat-Sealing Process for Chañar Brea Gum Films
by María Fernanda Torres, Federico Becerra, Mauricio Filippa, Gisela Melo and Martin Masuelli
Processes 2025, 13(7), 2189; https://doi.org/10.3390/pr13072189 - 9 Jul 2025
Viewed by 326
Abstract
This work presents a comprehensive evaluation of the heat-sealability of films developed from chañar brea gum (CBG), a biopolymer with potential for packaging applications. Heat sealability is a critical property in the packaging industry, as it directly determines the integrity and functionality of [...] Read more.
This work presents a comprehensive evaluation of the heat-sealability of films developed from chañar brea gum (CBG), a biopolymer with potential for packaging applications. Heat sealability is a critical property in the packaging industry, as it directly determines the integrity and functionality of the final product. The films were prepared by the 10% casting method with the addition of glycerin, and heat sealing was performed at 140 °C using a heat sealer. Heat sealing was performed on 2 cm × 10 cm strips of chañar gum in the horizontal (CBG-H) and vertical (CBG-V) directions. This study employs a joint determination to explore the fundamental properties of the films, including proximate analysis, antioxidant capacity, FTIR, DSC, TGA-DTGA, XRD, mechanical testing, water vapor permeability, sorption, and biodegradability. By integrating the results of all these determinations, this study seeks to evaluate and explain the “intimate relationships”—i.e., the complex interconnections among the molecular structure, composition, thermal behavior, mechanical properties, and barrier properties of channier gum films—and how these fundamental properties dictate and control their heat sealability. The thermal stability of CBG is up to 200 °C, with a melting point of 152.48 °C. The interstrand spacing was very similar at 4.88 nm for CBG and 4.66 nm for CBG-H. The SEM images of the heat seal show rounded shapes on the surface, while in the cross section, it is homogeneous and almost without gaps. The WVP decreased from 1.7 to 0.37 for CBG and CBG-H, respectively. The Young’s modulus decreased from 132 MPa for CBG to 96.5 MPa for CBG-H. The heat sealability is 656 N/m, with a biodegradability of 4 days. This comprehensive approach is crucial for optimizing the sealing process and designing functional and efficient biodegradable packages. Full article
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19 pages, 2841 KiB  
Article
Next-Generation Sustainable Composites with Flax Fibre and Biobased Vitrimer Epoxy Polymer Matrix
by Hoang Thanh Tuyen Tran, Johannes Baur, Racim Radjef, Mostafa Nikzad, Robert Bjekovic, Stefan Carosella, Peter Middendorf and Bronwyn Fox
Polymers 2025, 17(14), 1891; https://doi.org/10.3390/polym17141891 - 8 Jul 2025
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Abstract
This work presents the development of two vanillin-based vitrimer epoxy flax fibre-reinforced composites, with both the VER1-1-FFRC (a vitrimer-to-epoxy ratio of 1:1) and VER1-2-FFRC (a vitrimer-to-epoxy ratio of 1:2), via a vacuum-assisted resin infusion. The thermal and mechanical properties of the resulting vitrimer [...] Read more.
This work presents the development of two vanillin-based vitrimer epoxy flax fibre-reinforced composites, with both the VER1-1-FFRC (a vitrimer-to-epoxy ratio of 1:1) and VER1-2-FFRC (a vitrimer-to-epoxy ratio of 1:2), via a vacuum-assisted resin infusion. The thermal and mechanical properties of the resulting vitrimer epoxy flax composites were characterised using thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and mechanical four-point bending tests, alongside studies of solvent resistance and chemical recyclability. Both the VER1-1-FFRC (degradation temperature Tdeg of 377.0 °C) and VER1-2-FFRC (Tdeg of 395.9 °C) exhibited relatively high thermal stability, which is comparable to the reference ER-FFRC (Tdeg of 396.7 °C). The VER1-1-FFRC, VER1-2-FFRC, and ER-FFRC demonstrated glass transition temperatures Tg of 54.1 °C, 68.8 °C, and 83.4 °C, respectively. The low Tg of the vitrimer composite is due to the low crosslink density in the vitrimer epoxy resin. Particularly, the crosslinked density of the VER1-1-FFRC was measured to be 319.5 mol·m−3, which is lower than that obtained from the VER1-2-FFRC (434.7 mol·m−3) and ER-FFRC (442.9 mol·m−3). Furthermore, the mechanical properties of these composites are also affected by the low crosslink density. Indeed, the flexural strength of the VER1-1-FFRC was found to be 76.7 MPa, which was significantly lower than the VER1-2-FFRC (116.2 MPa) and the ER-FFRC (138.3 MPa). Despite their lower thermal and mechanical performance, these vitrimer composites offer promising recyclability and contribute to advancing sustainable composite materials. Full article
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