Polymers

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17 pages, 5614 KiB

Open AccessArticle

Revealing the Calcium Assisted Partial Catalytic Graphitization of Lignin-Derived Hard Carbon Anode and Its Electrochemical Behaviors in Sodium Ion Batteries

by Jungpil Kim, Sang-Hyun Lee and Junghoon Yang

Polymers 2025, 17(4), 540; https://doi.org/10.3390/polym17040540 - 19 Feb 2025

Cited by 2 | Viewed by 595

Abstract

Among the various contenders for next-generation sodium-ion battery anodes, hard carbons stand out for their notable reversible capacity, extended cycle life, and cost-effectiveness. Their economic advantage can be further enhanced by using inexpensive precursors, such as biomass waste. Lignin, one of the most [...] Read more.

Among the various contenders for next-generation sodium-ion battery anodes, hard carbons stand out for their notable reversible capacity, extended cycle life, and cost-effectiveness. Their economic advantage can be further enhanced by using inexpensive precursors, such as biomass waste. Lignin, one of the most abundant natural biopolymers on Earth, which can be readily obtained from wood, possesses a three-dimensional amorphous polymeric structure, making it a suitable candidate for producing carbonaceous materials through appropriate carbonization processes for energy storage applications. In this work, we synthesized hard carbon using lignin containing CaSO₄ to facilitate partial catalytic graphitization to improve the microstructural features, such as interlayer spacing, degree of disorder, and surface defects. Partial catalytic graphitization enables hard carbon to develop an ordered structure compared with hard carbon carbonized without CaSO₄ as analyzed by X-ray diffraction, Raman spectroscopy, scanning/transmission electron microscopy, and X-ray photoelectron spectroscopy. The CaSO₄-aided partially catalytic graphitized hard carbon (CCG-HC) exhibited improved electrochemical performance, showing a larger portion of the low-voltage plateau—an indicator typically associated with a highly ordered structure—compared to simply carbonized hard carbon (HC). Notably, CCG-HC delivered a reversible capacity of 237 mAh g⁻¹, retained 95.6% of its capacity over 100 cycles at 50 mA g⁻¹, and exhibited 127 mAh g⁻¹ at 1.0 A g⁻¹. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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15 pages, 3464 KiB

Open AccessArticle

Sterically Induced Enhancement in the Electrochemical Stability of Salen-Type Cathode Materials

by Julia V. Novoselova, Evgenii V. Beletskii, Daniil A. Lukyanov, Sofia S. Filippova, Uliana M. Rodionova, Vladimir V. Sizov, Elena V. Alekseeva and Oleg V. Levin

Polymers 2025, 17(2), 178; https://doi.org/10.3390/polym17020178 - 13 Jan 2025

Viewed by 666

Abstract

This study investigates the electrochemical degradation mechanisms of nickel–salen (NiSalen) polymers, with a focus on improving the material’s stability in supercapacitor applications. We analyzed the effects of steric hindrance near the nickel center by incorporating different bulky substituents into NiSalen complexes, aiming to [...] Read more.

This study investigates the electrochemical degradation mechanisms of nickel–salen (NiSalen) polymers, with a focus on improving the material’s stability in supercapacitor applications. We analyzed the effects of steric hindrance near the nickel center by incorporating different bulky substituents into NiSalen complexes, aiming to mitigate water-induced degradation. Electrochemical performance was assessed using cyclic voltammetry, operando conductance, and impedance measurements, while X-ray photoelectron spectroscopy (XPS) provided insights into molecular degradation pathways. The results revealed that increased steric hindrance from methyl groups significantly reduced the degradation rate, particularly in water-containing electrolytes, by hindering water coordination to the Ni center. Among the studied polymers, the highly substituted poly[Ni(Saltmen)] exhibited superior stability with minimal capacity loss. Density functional theory (DFT) calculations further supported that steric protection around the Ni atom effectively lowers the probability of water coordination. These findings suggest that sterically enhanced NiSalen polymers may offer a promising path toward durable supercapacitor electrodes, highlighting the route of molecular engineering to enhance material stability. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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14 pages, 9057 KiB

Open AccessArticle

Solution Casting Effect of PMMA-Based Polymer Electrolyte on the Performances of Solid-State Electrochromic Devices

by Abdelrahman Hamed Ebrahem Abdelhamed, Gregory Soon How Thien, Chu-Liang Lee, Benedict Wen-Cheun Au, Kar Ban Tan, H. C. Ananda Murthy and Kah-Yoong Chan

Polymers 2025, 17(1), 99; https://doi.org/10.3390/polym17010099 - 2 Jan 2025

Viewed by 1371

Abstract

Electrochromic devices (ECDs) are devices that change their optical properties in response to a low applied voltage. These devices typically consist of an electrochromic layer, a transparent conducting substrate, and an electrolyte. The advancement in solid-state ECDs has been driven by the need [...] Read more.

Electrochromic devices (ECDs) are devices that change their optical properties in response to a low applied voltage. These devices typically consist of an electrochromic layer, a transparent conducting substrate, and an electrolyte. The advancement in solid-state ECDs has been driven by the need for improved durability, optical performance, and energy efficiency. In this study, we investigate varying the temperature to the casting solution for polymethylmethacrylate (PMMA)-based electrolytes for solid-state ECDs with a structure of glass/ITO/WO₃/PMMA electrolyte/ITO/glass. The electrochromic layer, composed of WO₃, was deposited using the sol-gel method, while the electrolyte, comprising lithium perchlorate (LiClO₄) in propylene carbonate (PC) with PMMA, was prepared via solution casting. Various electrolyte samples were heated at different temperatures of 25, 40, 60, 80, and 100 °C to analyze the impact on the devices’ performance. Our findings indicate that the devices with electrolytes at 25 °C exhibited superior anodic and cathodic diffusion. An increase in heating temperature corresponded with an increase in switching time. Notably, the sample heated at higher temperatures (60, 80, and 100 °C) demonstrated exceptional cycle stability. Nevertheless, samples with higher temperatures displayed a decrease in optical modulation. Additionally, the 100 °C sample exhibited the highest coloration efficiency compared to other samples at lower temperatures. This research highlights the potential of varying the temperature of solution casting on PMMA-based electrolytes in optimizing the performance of solid-state ECDs, particularly regarding coloration efficiency and durability. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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15 pages, 4602 KiB

Open AccessArticle

Electrochemical Sensing of Metribuzin Utilizing the Synergistic Effects of Cationic and Anionic Bio-Polymers with Hetero-Doped Carbon

by Thirukumaran Periyasamy, Shakila Parveen Asrafali, Seong-Cheol Kim and Jaewoong Lee

Polymers 2025, 17(1), 39; https://doi.org/10.3390/polym17010039 - 27 Dec 2024

Cited by 1 | Viewed by 634

Abstract

The development of innovative, cost effective, and biocompatible sensor materials for rapid and efficient practical applications is a key area of focus in electroanalytical chemistry. In this research, we report on a novel biocompatible sensor, made using a unique polybenzoxazine-based carbon combined with [...] Read more.

The development of innovative, cost effective, and biocompatible sensor materials for rapid and efficient practical applications is a key area of focus in electroanalytical chemistry. In this research, we report on a novel biocompatible sensor, made using a unique polybenzoxazine-based carbon combined with amino cellulose and hyaluronic acid to produce a bio-polymer complex (PBC-ACH) (polybenzoxazine-based carbon with amino cellulose and hyaluronic acid). This sensor material is fabricated for the first time to enable the electroreduction of the herbicide, metribuzin (MTZ). The PBC-ACH sensor presents multiple advantages, including ease of fabrication, excellent biocompatibility, and low-cost production, making it suitable for various applications. In optimized experimental conditions, the sensor was fabricated by modifying a glassy carbon electrode (GCE) with the PBC-ACH complex, resulting in the creation of a GCE/PBC-ACH electrode. This modified electrode demonstrated the ability to detect MTZ at nanomolar levels, with an LoD of 13.04 nM, showcasing a high sensitivity of 1.40 µA µM⁻¹ cm⁻². Moreover, the GCE/PBC-ACH sensor exhibited remarkable selectivity, stability, and reproducibility in terms of its electrochemical performance, which are essential features for reliable sensing applications. The potential mechanism behind the detection of MTZ using the GCE/PBC-ACH sensor was investigated thoroughly, providing insights into its sensing behavior. Additionally, tests on real samples validated the sensor’s practicality and efficiency in detecting specific analytes. These findings emphasize the potential of the GCE/PBC-ACH sensor as a highly effective electrochemical sensor, with promising applications in environmental monitoring and other fields requiring precise analyte detection. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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11 pages, 3608 KiB

Open AccessArticle

Investigation of Solid-State Thermal Decomposition of Ammonia Borane Mix with Sulphonated Poly(ellagic Acid) for Hydrogen Release

by Carmela Astorino, Eugenio De Nardo, Stefania Lettieri, Giuseppe Ferraro, Mattia Bartoli, Marco Etzi, Angelica Monica Chiodoni, Candido Fabrizio Pirri and Sergio Bocchini

Polymers 2024, 16(24), 3471; https://doi.org/10.3390/polym16243471 - 12 Dec 2024

Cited by 1 | Viewed by 873

Abstract

The utilization of hydrogen in safety conditions is crucial for the development of a hydrogen-based economy. Among all methodologies, solid-state hydrogen release from ammonia borane through thermal stimuli is very promising due to the high theoretical hydrogen release. Generally, carbonaceous or inorganic matrices [...] Read more.

The utilization of hydrogen in safety conditions is crucial for the development of a hydrogen-based economy. Among all methodologies, solid-state hydrogen release from ammonia borane through thermal stimuli is very promising due to the high theoretical hydrogen release. Generally, carbonaceous or inorganic matrices have been used to tune the reactivity of ammonia borane. Nevertheless, these solutions lack chemical tunability, and they do not allow one to properly tune the complex chemical pathway of hydrogen release from ammonia borane. In this study, we investigated the effect of a bioderived multifunctional polymeric matrix on hydrogen release from ammonia borane, reaching pure hydrogen release of 1.2 wt.% at 94 °C. We also describe new chemical pathways involving the formation of anchored intermediates, namely BxNy species. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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13 pages, 1654 KiB

Open AccessArticle

When a Side Reaction Is a Benefit: A Catalyst-Free Route to Obtain High-Molecular Cobaltocenium-Functionalized Polysiloxanes by Hydroamination

by Anastasia N. Kocheva, Konstantin V. Deriabin, Igor Perevyazko, Nadezhda A. Bokach, Vadim P. Boyarskiy and Regina M. Islamova

Polymers 2024, 16(20), 2887; https://doi.org/10.3390/polym16202887 - 14 Oct 2024

Viewed by 963

Abstract

Cobaltocenium-containing (co)polysiloxanes (Cc-PDMSs) with terminal and side groups were synthesized by the reaction of catalyst-free hydroamination between ethynylcobaltocenium hexafluorophosphate and polysiloxanes comprising amino moieties as terminal and side groups. The conversion of NH₂ groups in the polymers reaches 85%. The obtained (co)polysiloxanes [...] Read more.

Cobaltocenium-containing (co)polysiloxanes (Cc-PDMSs) with terminal and side groups were synthesized by the reaction of catalyst-free hydroamination between ethynylcobaltocenium hexafluorophosphate and polysiloxanes comprising amino moieties as terminal and side groups. The conversion of NH₂ groups in the polymers reaches 85%. The obtained (co)polysiloxanes “gelate” due to an increase in their molecular weight by approx. 30 times, when stored at room temperature over one week. “Gelated” Cc-PDMSs remain soluble in most polar solvents. The structure of Cc-PDMSs and the mechanism of “gelation” were established by ¹H, ¹³C{¹H}, ²⁹Si{¹H}, ¹⁹F{¹H}, ³¹P{¹H} nuclear magnetic resonance, infrared, ultraviolet–visible, and X-ray photoelectron spectroscopies. As determined by cyclic voltammetry, Cc-PDMSs possess redox properties (Co^II/Co^III transitions at E_1/2 = −1.8 and −1.3 V before and after “gelation”, respectively). This synthetic approach allows to increase the molecular weights of the synthesized polysiloxanes functionalized with cobaltocenium groups easily, leading to their higher film-forming ability, which is desirable for some electronic applications. Cc-PDMSs can be utilized as redox-active polymer films in modified electrodes, electrochromic devices, redox-active coatings, and components for batteries. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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11 pages, 3398 KiB

Open AccessArticle

Sequential Cascade Doping of Conjugated-Polymer-Wrapped Carbon Nanotubes for Highly Electrically Conductive Platforms

by Da Young Lee, Da Eun Choi, Yejin Ahn, Hyojin Kye, Min Seon Kim and Bong-Gi Kim

Polymers 2024, 16(13), 1884; https://doi.org/10.3390/polym16131884 - 1 Jul 2024

Viewed by 1409

Abstract

To explore a highly conductive flexible platform, this study develops PIDF-BT@SWCNT by wrapping single-walled carbon nanotubes (SWCNTs) with a conjugated polymer, PIDF-BT, known for its effective doping properties. By evaluating the doping behaviors of various dopants on PIDF-BT, appropriate dopant combinations for cascade [...] Read more.

To explore a highly conductive flexible platform, this study develops PIDF-BT@SWCNT by wrapping single-walled carbon nanotubes (SWCNTs) with a conjugated polymer, PIDF-BT, known for its effective doping properties. By evaluating the doping behaviors of various dopants on PIDF-BT, appropriate dopant combinations for cascade doping are selected to improve the doping efficiency of PIDF-BT@SWCNT. Specifically, using F4TCNQ or F6TCNNQ as the first dopant, followed by AuCl₃ as the second dopant, demonstrates remarkable doping efficiency, surpassing that of the individual dopants and yielding an exceptional electrical conductivity exceeding 6000 S/cm. Characterization using X-ray photoelectron spectroscopy and Raman spectroscopy elucidates the doping mechanism, revealing an increase in the proportion of electron-donating atoms and the ratio of quinoid structures upon F4TCNQ/AuCl₃ cascade doping. These findings offer insights into optimizing dopant combinations for cascade doping, showcasing its advantages in enhancing doping efficiency and resulting electrical conductivity compared with single dopant processes. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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12 pages, 2444 KiB

Open AccessArticle

Mechanistic Insights into Anion-Induced Electrochromism of Ru(II)-Based Metallo-Supramolecular Polymer

by Xiaofang Fu, Zhuohui Zhang, Zhenhu Cao, Alexandr Alexandrovich Rogachev, Maxim Anatolievich Yarmolenko, Tao Chen, Hongtao Cao and Hongliang Zhang

Polymers 2023, 15(24), 4735; https://doi.org/10.3390/polym15244735 - 18 Dec 2023

Viewed by 1630

Abstract

The metallo-supramolecular polymer (MSP) is considered one of the most promising electrodes for electrochromic devices due to its intrinsically stable redox properties. Nevertheless, despite extensive work focusing on improving the electrochromic and electrochemical properties of MSPs, little experimental evidence exists from in-depth investigations [...] Read more.

The metallo-supramolecular polymer (MSP) is considered one of the most promising electrodes for electrochromic devices due to its intrinsically stable redox properties. Nevertheless, despite extensive work focusing on improving the electrochromic and electrochemical properties of MSPs, little experimental evidence exists from in-depth investigations on the anion-induced electrochromism of MSPs. Herein, Ru-based metallo-supramolecular polymer (polyRu) films with excellent electrochromic performance were fabricated through a novel electrochemical deposition method, and the electrochromic mechanism was further understood. The polyRu films possess fast reaction kinetics with a short switching time of 4.0 s (colored) and 2.8 s (bleached) and highly reversible redox properties due to the resulting impacts on the capacitive behaviors (containing surface, near-surface and intercalation pseudo-capacitance) of the perchlorate ions in the electrochromic process. Moreover, the electrochromic degradation of the polyRu films is considered to stem from the numerous nanopores in the film induced by ClO₄⁻ transport and the exchange of counter anions from Cl⁻ to ClO₄⁻. In addition, a physical model, revealing the transport of conduction ions and the evolution of the structure and properties of the polyRu film during the electrochromic process, is presented. It is observed that the charge balance of Ru³⁺ and Ru²⁺, achieved through the adsorption/desorption of ClO₄⁻ on the film, provides electrochromic and electrochemical reversibility to the polyRu film under positive/negative bias. Correspondingly, a transformation from polyRu·(Cl⁻)_2n to polyRu·(ClO₄⁻)_x(Cl⁻)_2n−x in the polyRu film is induced by a counter anion exchange from Cl⁻ to ClO₄⁻. Revealing the detailed perchlorate ion transfer kinetics and electrochromic mechanism in this film can offer new insights into the application of metallo-supramolecular polymers in electrochromic devices. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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18 pages, 9635 KiB

Open AccessArticle

In Situ Redox Synthesis of Highly Stable Au/Electroactive Polyimide Composite and Its Application on 4-Nitrophenol Reduction

by Yi-Sheng Chen, Wei-Zhong Shi, Kun-Hao Luo, Jui-Ming Yeh and Mei-Hui Tsai

Polymers 2023, 15(12), 2664; https://doi.org/10.3390/polym15122664 - 13 Jun 2023

Cited by 6 | Viewed by 2762

Abstract

In this study, we developed a series of Au/electroactive polyimide (Au/EPI-5) composite for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) using NaBH₄ as a reducing agent at room temperature. The electroactive polyimide (EPI-5) synthesis was performed by chemical imidization of its [...] Read more.

In this study, we developed a series of Au/electroactive polyimide (Au/EPI-5) composite for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) using NaBH₄ as a reducing agent at room temperature. The electroactive polyimide (EPI-5) synthesis was performed by chemical imidization of its 4,4′-(4.4′-isopropylidene-diphenoxy) bis (phthalic anhydride) (BSAA) and amino-capped aniline pentamer (ACAP). In addition, prepare different concentrations of Au ions through the in-situ redox reaction of EPI-5 to obtain Au nanoparticles (AuNPs) and anchored on the surface of EPI-5 to form series of Au/EPI-5 composite. Using SEM and HR-TEM confirm the particle size (23–113 nm) of the reduced AuNPs increases with the increase of the concentration. Based on CV studies, the redox capability of as-prepared electroactive materials was found to show an increase trend: 1Au/EPI-5 < 3Au/EPI-5 < 5Au/EPI-5. The series of Au/EPI-5 composites showed good stability and catalytic activity for the reaction of 4-NP to 4-AP. Especially, the 5Au/EPI-5 composite shows the highest catalytic activity when applied for the reduction of 4-NP to 4-AP within 17 min. The rate constant and kinetic activity energy were calculated to be 1.1 × 10⁻³ s⁻¹ and 38.9 kJ/mol, respectively. Following a reusability test repeated 10 times, the 5Au/EPI-5 composite maintained a conversion rate higher than 95%. Finally, this study elaborates the mechanism of the catalytic reduction of 4-NP to 4-AP. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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13 pages, 4940 KiB

Open AccessArticle

Developing Transparent and Conductive PolyHEMA Gels Using Deep Eutectic Solvents

by Tai-Yu Chen, Yi-Jie Jiang and Hsiu-Wen Chien

Polymers 2023, 15(12), 2605; https://doi.org/10.3390/polym15122605 - 8 Jun 2023

Cited by 5 | Viewed by 2755

Abstract

Poly(2-hydroxyethyl methacrylate) (polyHEMA) hydrogels are commonly used in biomaterials such as contact lenses. However, water evaporation from these hydrogels can cause discomfort to wearers, and the bulk polymerization method used to synthesize them often results in heterogeneous microstructures, reducing their optical properties and [...] Read more.

Poly(2-hydroxyethyl methacrylate) (polyHEMA) hydrogels are commonly used in biomaterials such as contact lenses. However, water evaporation from these hydrogels can cause discomfort to wearers, and the bulk polymerization method used to synthesize them often results in heterogeneous microstructures, reducing their optical properties and elasticity. In this study, we synthesized polyHEMA gels using a deep eutectic solvent (DES) instead of water and compared their properties to traditional hydrogels. Fourier-transform infrared spectroscopy (FTIR) showed that HEMA conversion in DES was faster than in water. DES gels also demonstrated higher transparency, toughness, and conductivity, along with lower dehydration, than hydrogels. The compressive and tensile modulus values of DES gels increased with HEMA concentration. A DES gel with 45% HEMA showed excellent compression–relaxation cycles and had the highest strain at break value in the tensile test. Our findings suggest that DES is a promising alternative to water for synthesizing contact lenses with improved optical and mechanical properties. Furthermore, DES gels’ conduction properties may enable their application in biosensors. This study presents an innovative approach to synthesizing polyHEMA gels and provides insights into their potential applications in the biomaterials field. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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15 pages, 2467 KiB

Open AccessArticle

Comparative Studies on Carbon Paste Electrode Modified with Electroactive Polyamic Acid and Corresponding Polyimide without/with Attached Sulfonated Group for Electrochemical Sensing of Ascorbic Acid

by Jiunn-Jer Hwang, Aamna Bibi, Yu-Ci Chen, Kun-Hao Luo, Hsiang-Yuan Huang and Jui-Ming Yeh

Polymers 2022, 14(17), 3487; https://doi.org/10.3390/polym14173487 - 25 Aug 2022

Cited by 5 | Viewed by 2137

Abstract

In this study, electroactive poly (amic acid) (EPAA) and corresponding polyimide (EPI) without or with a sulfonated group (i.e., S-EPAA, and S-EPI) were prepared and applied in electrochemical sensing of ascorbic acid (AA). The electroactive polymers (EAPs) containing EPAA/EPI and S-EPAA/S-EPI were synthesized [...] Read more.

In this study, electroactive poly (amic acid) (EPAA) and corresponding polyimide (EPI) without or with a sulfonated group (i.e., S-EPAA, and S-EPI) were prepared and applied in electrochemical sensing of ascorbic acid (AA). The electroactive polymers (EAPs) containing EPAA/EPI and S-EPAA/S-EPI were synthesized by using an amine-capped aniline trimer (ACAT) and sulfonated amine-capped aniline trimer (S-ACAT) as an electroactive segment that controlled the redox capability and influenced the degree of sensitivity of the EAPs towards AA. Characterization of the as-prepared EAPs was identified by FTIR spectra. The redox capability of the EAPs was investigated by electrochemical cyclic voltammetric studies. It should be noted that the redox capability of the EAPs was found to show the following trend: S-EPAA > S-EPI > EPAA > EPI. For the electrochemical sensing studies, a sensor constructed from an S-EPAA-modified carbon paste electrode (CPE) demonstrated 2-fold, 1.27-fold, and 1.35-fold higher electro-catalytic activity towards the oxidation of AA, compared to those constructed using a bare CPE, S-EPI-, and EPI/EPAA-modified CPE, respectively. The higher redox capability of S-EPAA-modified CPE exhibited a good electrochemical response towards AA at a low oxidative potential, with good stability and selectivity. Moreover, an electrochemical sensor constructed from S-EPAA-modified CPE was found to reveal better selectivity for a tertiary mixture of AA/DA/UA, as compared to that of EPI-modified, EPAA-modified and S-EPI-modified CPE, based on a series of differential pulse voltammograms. Full article

(This article belongs to the Special Issue Synthesis, Characterization and Applications of Electroactive Polymers: 2nd Edition)

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