| Cite this article as: |
Wencan Chen, Chao Li, Yehan Tao, Jie Lu, Jian Du, and Haisong Wang, Chitosan-based triboelectric materials for self-powered sensing at high temperatures, Int. J. Miner. Metall. Mater., 31(2024), No. 11, pp.2518-2527. https://dx.doi.org/10.1007/s12613-024-2839-2
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Flexible wearable sensor devices have attracted increasing attention in the last few decades [1]. In the healthcare field, sensor devices can be used to monitor body temperature, skin humidity, pulse vibration, and human movement to understand the human state further. Humans can adjust their conditions in time on the basis of electrical signal feedback to maintain good health levels. In particular, workers who work in high-temperature environments for a long time (e.g., steel workers and outdoor workers during summer) are prone to suffering from heat stroke and other diseases, which seriously endanger people’s health [2–4]. Therefore, developing rapid, sensitive, and stable sensors for recording the physiological parameters of workers in real time is important [5]. Conventional sensors often require battery power; however, battery lifespan and safety are degraded under long-term high-temperature conditions, resulting in fire damage [6]. Therefore, designing and developing self-powered sensors that can continue to work safely under hot conditions is important.
Triboelectric nanogenerators (TENGs) have been demonstrated as a new sustainable energy-harvesting technology that converts low-frequency, high-entropy mechanical energy into electrical energy since they were first proposed by Weng et al. in 2012 [7]. TENG prototypes have been employed as self-powered sensor devices due to their advantages of light mass, small size, wide material selection, and high-efficiency power generation at low frequencies. At the same time, these characteristics are exactly in line with the current boom in the Internet of Things (IOT), big data, artificial intelligence, and other technologies with disorderly and distributed characteristics [8–9]. Synthetic polymers are commonly utilized to construct TENGs. They include fluorinated ethylene propylene (FEP), poly(methyl methacrylate), Kapton, polydimethylsiloxane, dimethylsiloxane (PDMS), polyvinylidene fluoride (PVDF), polyethylene terephthalate (PET), polyurethane (PU), polyimide (PI), and polytetrafluoroethylene (PTFE) [10]. However, the high manufacturing costs, complex processes, nonbiocompatibility, and nonbiodedgradability after disposal of these polymers limit the practical application of TENGs. Our films were made from natural materials and did not generate any waste during preparation. Therefore, biodegradable materials have attracted increasing attention.
The use of various biodegradable materials, such as cellulose and its derivatives, collagen, silk fibroin, rice paper, seaweed, chitosan, and silk, as triboelectric layers has been demonstrated [11]. Chitosan (CS) derived from the deacetylation of natural chitin possesses a similar molecular skeleton as cellulose [12], except that a single-bond NH2 group replaces the single-bond OH group at the C-2 position. As a result of the electron-donating capacity of the abundant –OH groups and NH2 groups on CS [13], CS can be employed as tribopositive layers in TENGs [14–16]. However, triboelectric charges usually suffer from volatilization at high temperatures, thus severely reducing output stability and practical application.
Lignin is the most dominant aromatic polymer in terrestrial biomasses, with a content of 15wt%–40wt% [17]. A large amount of lignin (~50 million tons) is annually generated as a by-product by the pulp and paper-making industries. The lignin skeleton is an excellent building block for reinforcing the structural characteristics of composite films because of its unique aromatic rings. In the last few years, lignin has often been utilized as nanofillers to boost the triboelectric performances of TENGs [18–20]. Montmorillonite (MMT), the main component of bentonite, is a completely environmentally friendly filler. It also serves as a highly dielectric inorganic clay material that can considerably improve the output performances of TENGs when added in small amounts [21–23]. Recently, Gao et al. [24] revealed that the strengthened intermolecular interactions in matrices contribute to the dense structure of composite films as well as the stable output performances of TENGs under conditions of high temperature and humidity. Theoretically, the strong intermolecular interaction forces among lignin, CS, and MMT can make composite films form dense structures [25–27], inhibiting the volatilization of electrons and achieving a stable high output at high temperatures. To the best of our knowledge, research on preparing CS-based triboelectric materials via MMT doping and applying lignin to reduce the loss of charges at high temperatures has rarely been conducted.
In this work, we propose an advanced CS/MMT/lignin (CML) triboelectric material prepared through a facile strategy. The influence of MMT and lignin dosage on the microstructures, mechanical behaviors, light transmittance, and triboelectric process of the CS-based composite films were systematically investigated. The fabricated CML triboelectric film was assembled into TENGs, and the CML-TENGs were applied at high temperatures. This work provides an easy method for designing and fabricating green and advanced triboelectric materials that are suitable as healthcare sensors for workers exposed to hot conditions, such as outdoor venues during summer.
Sodium lignosulfonate (SL), acetic acid, CS, MMT (K-10), and glycerol were supplied by Aladdin, Shanghai, China. All chemicals were of analytical grade and used without further purification.
In brief, 2 g of CS was dissolved in 100 g of 2wt% acetic acid solution and successively added with MMT and SL [28]. Subsequently, the film solution was stirred at 45°C for 12 h to form a homogeneous solution. A total of 70 mL of the film solution was poured into a glass Petri dish with a diameter of 15 cm and dried in an oven at 45°C overnight. The fabricated composite films were denoted as CMxLy, where x and y represent the mass percentage of MMT and lignin in CS (%), respectively.
The fabricated CML composite films were employed as tribopositive layers in CS-based TENGs. In detail, pieces of PVDF film and CS-based film with the size of 4 cm × 4 cm were stuck on the glue side of Ag tape. TENGs were constructed in a typical vertical contact–separation mode by using the above electrodes.
The microstructures and surface morphology of the composite films were observed by using a scanning electron microscope (SEM, JSM7800F, JEOL, Japan) at an accelerating voltage of 5 kV. Prior to measurements, the composite films were sprayed with a thin Au layer. For the observation of cross-sectional morphologies, the composite films were quenched with liquid nitrogen.
Chemical structures were identified through Fourier transform infrared spectroscopy (FTIR, Spectrum Two, PerkinElmer, USA) with a scanning interval of 450–4000 cm−1 and resolution in transmission mode of 1 cm−1.
The output signals of TENGs were measured in contact–separation mode. Open-circuit voltage (Voc), short-circuit current (Isc), open-circuit charge (Qsc), and maximum instantaneous output power density were detected by using Keithley 6514 equipped with a data acquisition card, as shown in the supplementary information (Fig. S1 and Vedio S1). The maximum instantaneous output power was measured by connecting various resistances from 1 kΩ to 100 MΩ. A commercial linear mechanical motor (LinMot) was employed to provide external force and control contact frequency. The output performances of TENGs were measured at room temperature (~25°C, ~30% RH).
Mechanical strength was tested by using an electronic universal material tester (Instron 5965, Boston Instron Co., Ltd., USA). Laminated film was cut into strips of 2 cm × 8 cm (width × length). The travel distance and stretching rate between the two jigs were 40 mm and 10 mm/min, respectively.
Thermal stability was measured at 25–700°C through thermogravimetric analysis (TGA, Q500, TA, USA) under nitrogen atmosphere. Chalcogenometric scanning calorimetry (DSC) was performed by using the DSC instrument Q2000 (Q2000, TA, USA) with nitrogen flow rate of 50 mL/min.
Optical properties were observed with a double-beam UV–vis spectrophotometer (UH5300, Hitachi, Japan). Transmittance was calculated as the average of five measurements.
The dielectric constants of the fabricated composite films (with thickness of ~138 µm) were measured by using an Agilent LCR meter (4990A) at room temperature with frequency of 100 Hz to 1 MHz.
Composite films with the dimensions of 2 cm × 5 cm (width × length) were adhered to various parts of the human body with the assistance of double-sided adhesive. Electrical signals were collected by using a signal acquisition card. A handheld thermometer (HM-TPH21Pro-3AQF, China) was applied to measure temperature.
Fig. 1(a) depicts the detailed manufacture of CMxLy triboelectric films via a facile physical mixing process. The fabricated CM5L3 composite film appeared faint yellow, as shown in Fig. 1(b), and possessed good mechanical behaviors and flexibility. Such merits are the preconditions for application as flexible sensors. The abundant amino and hydroxyl groups on CS formed numerous hydrogen bonds with the oxygen-containing functional groups on lignin and coordination bonds with metal ions on MMT. Long-chain CS can tightly wrap MMT nanoparticles, which can conduct stress through interfacial interaction between MMT and CS when subjected to external force. Moreover, the reinforced interconnection between biopolymers and fillers is conducive to the suppression of electron dissipation from the surface of triboelectric layers under hot conditions. Therefore, the fabricated triboelectric materials are suitable for the construction of TENGs that can be employed in self-powered human health sensors for workers exposed to high-temperature conditions (Fig. 1(c)).
The intermolecular interactions between biopolymers and nanofillers were investigated by using FTIR. As shown in Fig. 2(a), typical characteristic peaks associated with CS, MMT, and lignin were observed at 1631, 1087, and 650 cm−1, respectively [29–30]. No new peaks were detected in CM5L0 and CM5L3, implying that the composite films are mainly linked through physical interaction. The mechanical behaviors of the composite films determine their practical applications as triboelectric materials. The typical tensile stress–strain curves of the fabricated CMxL0 and CM5Ly, are shown in Fig. 2(b) and (c), respectively. By incorporating MMT into CS (<5%), tensile stress was considerably enhanced, and CM5L0 achieved the maximum tensile stress of 22.62 MPa due to the reinforcement of interfacial interactions between MMT and CS. The tensile strain was restrained due to the rigid nature of MMT [31]. However, when the MMT content further increased (>5%), tensile stress and strain reduced due to the aggregation of MMT. Moreover, when lignin was introduced into the CM5L0 matrix, the mechanical behaviors of CM5Ly displayed similar trends as those of CMxL0 because the abundant oxygen-containing groups on lignin can bind with oxygen atoms on CS and MMT to form numerous hydrogen bonds, resulting in a dense structure. High lignin dosages would deteriorate the mechanical properties of the CML composite film due to lignin aggregation [32–33]. A dense network is beneficial for impeding the volatilization of charges, thereby boosting the output performances of TENGs at high temperatures. Moreover, when MMT was introduced into CS, light transmittance within 200–400 nm gradually decreased because of the opaque nature of MMT, as shown in Fig. 2(d). In particular, the light transmittance of CM5L20 almost reached zero, implying that the UV-blocking performance of the composite film was reinforced (Fig. 2(e)) [34]. Such UV-shielding behavior can protect the skin from damage when the film is employed as a component in wearable devices. As shown in Fig. 2(f), the TGA curves of pristine CS, CM5L0, and CM5L3 were compared to evaluate the influence of MMT and lignin on the thermal stability of the CML composite films. The weight losses at stage I (below 150°C) and stage II (150–300°C) were attributed to water evaporation and polymer chain depolymerization and decomposition via glycosidic bond cleavage, respectively [29]. The residual weight of the composite films gradually increased as MMT and lignin were introduced due to the inorganic nature of MMT and the reinforcement of interfacial interaction between the biopolymer and nanofillers. This result confirmed that the thermal stability of CM5L3 had enhanced compared with that of pristine CS and matched previously reported findings well [35–36]. Fig. 2(g)–(k) shows the photographs of the synthesized CM5L3 composite films, which presented good flexibility and structurally robust properties, such as bending, stretching, twisting, and load-bearing (20 g and 2 kg) properties. The water contact angle (WCA) test was conducted to test the wettability of the composite films. As shown in Fig. S2, the WCA of the CM5L3 film (105.02°) became higher than that of the pristine CH film (93.67°) upon the introduction of MMT and lignin. This increase is an important indicator of the reduction in surface wettability due to the occupation of the polar groups on polymers to form numerous hydrogen bonds and corresponded with previously reported results [37]. The reinforced hydrophobicity and moisture resistance of the composite film are beneficial for application in wearable sensors.
The microstructures and elemental distribution of the CS and CML composite films were characterized through SEM and EDS, respectively. The low- and high-magnification SEM images of the surface and cross-sectional nanostructures of the triboelectric layer before and after MMT/SL doping are displayed in Figs. 3 and S3. The pristine CS film displayed a smooth surface and dense structure, as shown in Fig. S3(a) and (d). Phase separation, cracks, and gaps were not observed when MMT and SL were successively introduced into the CS matrix, implying that CS exhibits excellent compatibility with MMT and SL through hydrogen bonding, as shown in Fig. 3(a)–(c). Moreover, the CM5L0 and CM5L3 composite films possessed dense structures, which are beneficial for reducing the volatilization of triboelectric charges at high temperatures. The cross-sectional SEM images in Fig. 3(d)–(f) illustrates that the triboelectric films possessed almost the same thickness of 137 μm. Furthermore, the elemental distribution images of Mg, Ca, Si, Al, and S (Fig. 3(g)) confirmed that MMT and lignin were homogeneously dispersed within the CS matrix. This result provides direct evidence for the good compatibility of MMT and lignin in CS.
The electrical signals of the CML-TENGs were investigated in vertical contact–separation mode. As shown in Fig. 4, the electrical signals can be generated in four stages. In stage I, an external motor drove the triboelectric electric layers to come into contact with each other. As a result of differences in electron-binding abilities, opposite charges can form with equal amounts on the surfaces of triboelectric layers after contact. Moreover, electrons were transferred from CML to PVDF because of the strong electron-withdrawing ability of PVDF. Therefore, CML and PVDF were positively and negatively charged, respectively. The potential difference between the two electrodes was gradually established when the electrodes were separated from each other in stage II, driving induced electrons to flow to the electrostatic equilibrium in stage III. In stage IV, when the electrode was pressed again, the induced electrons flowed back, thus generating an electrical signal in the opposite direction, completing an operation cycle. On the basis of this principle [38–40], electrical signals can be generated during one cycle, as shown in Fig. S4, and periodic output performances can be obtained by repeating contact/separation.
The Voc, Isc, Qsc, and maximum instantaneous output power density were tested to investigate the specific effects of fillers (e.g., MMT and SL) on CS-based TENGs. As shown in Fig. 5(a)–(c), Voc, Isc, and Qsc first increased and then decreased. The maximum Voc of 169.94 V, Isc of 9.23 μA, and Qsc of 61.06 nC were achieved at the MMT concentration of 5%. The Voc, Isc, and Qsc curves all increased and then decreased as a function of lignin dosage with the continued addition of SL to the CM5L0 composite membrane (Fig. 5(d)–(f)). The maximum Voc of 262.35 V, Isc of 14.76 μA, and Qsc of 162.64 nC can be obtained at the lignin concentration of 3%. Various resistors were loaded into the external circuit. Power density can be calculated on the basis of the current through resistors by using the formula P = U2/(RS) (where P, U, R, and S represent the power density, measured voltage of the load resistance, external load resistance, and contact area, respectively) [41], as shown in Fig. 5(g)–(i). With increasing resistance, the Voc of the TENGs based on three triboelectric layers gradually increased and reached the maximum value at 100 MΩ, which corresponded to the minimum Isc. Isc gradually decreased with increasing resistance, and the maximum Isc was obtained at 1000 Ω resistance, where Voc was minimal. The maximum power density at 10 MΩ of CM5L3-TENG was 429.83 mW/m2, which was larger than that of pristine CS-TENG (64.64 mW/m2) and CM5L0-TENG (93.39 mW/m2). The mechanism underlying the enhancement in triboelectric performances is discussed in the following section. Moreover, in terms of Voc, Isc, output power, and durability, the output performances at high temperatures of the fabricated CM5L3-TENG are comparable to those of cutting-edge TENGs, as presented in Table S1.
As shown in Fig. 6(a)–(c), the Voc, Isc, and Qsc of CM5L3 TENG demonstrated stable output behaviors as contact frequency increased, implying that contact frequency had a negligible influence on the output performances of TENG. Moreover, the output stability of TENGs plays a crucial role in practical applications. Figs. 6(d) and S5 depict that CM5L3-TENG exhibited stable Isc without discernible current attenuation during 10000 cycles at room temperature and 70°C, confirming the good long-term durability of the triboelectric materials. The underlying mechanism of this characteristic can be attributed to the compact structure of the composite film; such a structure is beneficial for dissipating external energy and endows the triboelectric layer with robust structural stability while avoiding breakage [42]. In accordance with the signal generation mechanism, the output signal of TENG is an alternating current (AC), which could not be directly used as the supply power. The signal is transformed into direct current (DC) before capacitor charging. As shown in Fig. 6(e), the capacitor of 1.1 μF can be quickly charged to 2.48 V within 20 s. Linear charging behaviors were observed when TENG was operated under quasi-short-circuit conditions by loading large capacitors. The charging time relies on capacitances analogous to those of a typical resistor–capacitor (RC) charging circuit [23]. The dielectric properties of the materials at different impact frequencies were characterized, as shown in Fig. 6(f), to further explore the reasons for the enhancement in output performance. Among the tested materials, pure CS had the lowest dielectric constant, which corresponded with its worst TENG performance. The dielectric constant increased with the addition of MMT. This trend persisted with the further addition of lignin and matched the TENG performances of the composite films well. Thus, the enhanced output performances of CML-based TENGs could be attributed to enhanced dielectric behaviors, which are beneficial for the long-term maintenance of triboelectric charges.
The output performances of CM5L3-TENG at different temperatures are illustrated in Fig. 7. As shown in Fig. 7(a) and (c), the Voc of CH-TENG drastically reduced by 61% from 87.57 to 34.83 V as the temperature increased from 25 (room temperature) to 70°C. However, CM5L3-TENG showed a suppressed reduction in Voc at high temperatures, and its Voc reduced by approximately 34% (from 234.55 to 155.91 V), as shown in Fig. 7(b) and (d). This is because the formation of additional hydrogen bonds within polymers and nanofillers contributed to the formation of a dense structure that prevented the volatilization of electrons at high temperatures. Therefore, the triboelectric charges at high temperatures can be well maintained, and the TENG still delivers high output performance [24].
A ring sensor based on TENG was constructed by using PVDF and CM5L3 as the tribonegative and tribopositive layers, respectively, as illustrated in Fig. 8(a). The use of a flexible support material with a certain stiffness can prevent PVDF from bonding with CM5L3 when the sensor was in a free state. When this sensor was attached to the human body, contact–separation behavior between PVDF and CM5L3 can be achieved through the deformation caused by human body movement, thereby converting biomechanical energy into electrical signals [24]. Human activity at room temperature (30°C) and high temperature (50°C) was monitored to verify the performance of CM5L3-TENG in practical applications. In this work, the temperatures ranged from 25 to 70°C. These temperatures are sufficient for wearable applications because the core human body temperature is between 36 and 38°C when at rest and can reach 41°C during exercise [43]. As shown in Figs. 8(b)–(h) and S6, regular waveforms were obtained as each part of the body underwent regular motion. The electrical signal generated by CM5L3-TENG varied with the degree of finger flexion because during low flexion, only one joint was active, and a limited area of the electrodes in CM5L3-TENG was subjected to friction when the electrodes were in contact with each other; CM5L3-TENG followed the finger’s violent bending, wherein the electrodes touched each other to produce a large area and friction force. This phenomenon is reflected by the difference in electrical signals (Fig. 8(e)–(f)). When the composite film was applied to other parts of the body and followed the movement of different parts, it also exhibited distinctive electrical signals. The electrical signals differed for the same reason that they differed when fingers were bent by different levels. The above experiments demonstrated that the monitoring signal is sensitive and can accurately respond to the movement of various human body parts. At high temperatures, electrical signal intensity decreased, and the characteristic peaks of each movement can be clearly identified, indicating that the TENG has good stability during motion at high temperatures.
We fabricated a novel CML triboelectric material with dense structures for self-powered motion sensing at high temperatures. The strong interfacial interaction among CS, MMT, and SL through hydrogen bonds resulted in dense structure and reinforced mechanical behaviors. Moreover, the presence of amino groups in CS boosted the tribopositive electrical signals and resistance to environmental disturbances of CML-TENG. Pristine CS-TENG retained only 39% of its initial Voc at 70°C, whereas the optimized CM5L3-TENG retained 66% of its initial Voc, verifying the reliability of CM5L3 as an advanced triboelectric material for application at high temperatures. This work proposed a facile strategy for developing functional triboelectric materials for use as self-powered sensing systems for workers exposed to harsh atmospheric conditions.
The authors are grateful for the financial support from the National Natural Science Foundation of China (Nos. 22208038, 22278047, and 22208040), the Liaoning Revitalization Talent Program, China (No. XLYC2002024), and the Fundamental Research Funds for the Universities of Liaoning Province, China (No. LJBKY2024055).
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
The online version contains supplementary material available at https://doi.org/10.1007/s12613-024-2839-2.
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