Wood Anisotropic Compression-Induced Power Enhancement Aerogel Thermoelectric Generator Based on BC/PEDOT:PSS/SWCNT

doi:10.21203/rs.3.rs-2242962/v1

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Wood Anisotropic Compression-Induced Power Enhancement Aerogel Thermoelectric Generator Based on BC/PEDOT:PSS/SWCNT

https://doi.org/10.21203/rs.3.rs-2242962/v1

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published 27 Jan, 2023

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Aerogel is a solid material with a large specific surface area and ultra-high porosity, which is considered a promising candidate for thermoelectric (TE) devices due to its unique ultra-low thermal conductivity. Generally, aerogels prepared from common organic polymers usually have low mechanical strength. Bacterial cellulose (BC), a particular nanomaterial with good mechanical properties, can act as a significant component for preparing high-performance nanomaterials. This study prepared aerogel thermoelectric generator (TEG) based on BC, poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) (PEDOT:PSS), and single-walled carbon nanotubes (SWCNT). The aerogel exhibits excellent mechanical properties with stresses of up to 241 KPa at 90% compressive deformation, and the output performance can be easily tuned by temperature difference and compressive strain. Additionally, the TE device consisting of a single aerogel achieves an optimal output power of 84 nW at 30% strain and 50 K temperature difference. This work takes into account both the high mechanical properties and TE performance of cellulose aerogels and elucidates the strengthening effect of the layered ordered inner structure of lignoid on TEG. TE aerogels exhibit excellent heat harvesting capability under both vertical temperature difference and mechanical deformation, which provides good insight for future design and application of multifunctional self-powered sensors.

thermoelectric aerogel

directional freezing

bacterial cellulose

thermoelectric generator

high strength

Low-grade heat widely exists in the natural environment and industrial production process, which has been rarely used due to the lack of sustainable energy recovery technology(Jin et al. 2018; Kim et al. 2013; We et al. 2014; Yang et al. 2021). Thermoelectric materials, which can directly convert low-grade heat into electricity with high efficiency, have gained tremendous attention for collecting waste heat(Ding et al. 2019; Khan et al. 2016; Park et al. 2013; Ren et al. 2014; Wang et al. 2018a). Among these, organic polymers have been utilized to manufacture thermoelectric materials with outstanding properties for weakening the brittleness and high thermal conductivity of inorganic TE materials based on their super flexibility and highly ordered molecular structure(Okada et al. 2020; Wang et al. 2018b; Wang et al. 2019). However, low electrical conductivity limits their further applications. In this aspect, recombining organic polymers with low thermal conductivity and carbon nanomaterials with high electrical conductivity has been an attractive strategy to prepare conductive nanomaterials with high TE properties, based on the interfacial π-π conjugation between organic polymers and carbon nanomaterials(Li et al. 2021; Pillai et al. 2021; Wei et al. 2022a). Zhang and Chen et al. prepared thermoelectric composites which could achieve a maximum power factor of 182.7 ± 9.2 μWm^-1K^-2 at normal atmospheric temperature due to the high conductivity of SWCNT and the interfacial interactions by mixing PEDOT:PSS/SWCNT with ionic liquid (IL)(Deng et al. 2021b). Deng and Chen et al. disclosed that SWCNT loading significantly influences the electrical conductivity and Seebeck coefficient of the SWCNT/PEDOT:PSS composite(Wei et al. 2022b). In addition, the composites exhibit different temperature dependencies of TE performance as a function of SWCNT content. However, the nanocomposites prepared by conventional methods such as solution casting and vacuum filtration usually have low mechanical strength and high thermal conductivity due to a large amount of SWCNT.

As a natural renewable resource, BC has excellent mechanical properties, good thermal stability up to 250℃, and an especially rich three-dimensional network porous microstructure that can fabricate flexible thermoelectric devices with low thermal conductivity(Abol-Fotouh et al. 2019; Zhou et al. 2020). In addition, the hydrophilic functional groups (e.g., OH) of highly crystalline BC can interact with conducting polymers by hydrogen bonding and induce their ordered growth(Han et al. 2019; Han et al. 2017). Chen’s group et al. researched a foldable and flexible cellulose/PEDOT:PSS TE material with excellent mechanical and TE properties by dip-coating and drying(Deng et al. 2021a). PEDOT:PSS could be readily wrapped on the surfaces of cellulose fibers via hydrogen-bond interactions. Chen and Ji et al. prepared hybrid helical PEDOT/BC/SWCNT fiber, which has low thermal conductivity and good mechanical strength(Liang et al. 2022). Therefore, as a unique nanocellulose, BC can be firmly combined with conductive materials and assembled into TE generators along a planar structure to improve conductivity and mechanical properties. However, TE generators with a planar structure are unsuitable for vertical direction heat collection and hardly meet the requirement of efficient heat dissipation.

Compared with conventional thin film materials, aerogels have a large specific surface area and ultra-high porosity, which makes them unique in their lightweight and ultra-low thermal conductivity(Chen et al. 2021a; Chen et al. 2021b; Tan et al. 2017; Zhao et al. 2015). Thus, aerogels can use large-area heat sources fully and are a promising candidate for thermoelectric devices(Bryning et al. 2007). The aerogel prepared by the traditional freeze-drying method usually has poor mechanical strength, influencing its practical applications in many areas(Berglund and Burgert 2018; Bryning et al. 2007). In nature, woods exhibit distinct anisotropic and laminarly ordered internal structures owing to the orderly arrangement of structural units, leading to high elasticity and excellent mechanical strength(Chen et al. 2020a; Joseph et al. 2020; Zeng et al. 2019). Researchers have recently induced ice crystal growth through directional freezing techniques "bottom-up" to obtain cellulose lamella wood-like structure aerogels(Han et al. 2021; Qin et al. 2021; Wang et al. 2021a). In addition, mechanical deformation will cause a change in porosity, thus affecting the transmission channel of electrons and further influencing the TE properties of wood-like aerogels(Chen et al. 2020b; Li et al. 2022; Wang et al. 2021b). Thus, the influence mechanism of mechanical deformation on material properties needs to be studied urgently.

Inspired by the laminar-ordered internal structure of woods, this study assembled a wood-like TE aerogel for thermoelectric energy conversion at vertical temperature differences in a BC framework in a directed manner. First, PEDOT:PSS was uniformly coated on the BC surface induced by hydrogen bonding through simple physical mixing. Then SWCNTs were dispersed by ultrasonic, which formed a tightly connected charge transport network with PEDOT:PSS through interfacial π-π conjugation to enhance the electrical conductivity effectively. Subsequently, the directional freezing treatment promotes the directional arrangement of BC. Thus PEDOT:PSS and SWCNT are ordered in the cellulose framework. Finally, structure orderly aerogels with excellent mechanical and thermoelectric properties are fabricated. The aerogel has a stress of up to 241 Kpa at 90% compressive deformation, and the TE performance can be readily tuned by mechanical deformation and temperature variation. The TE device consisting of a single aerogel achieves a maximum output power of 84 nW at 50 K temperature difference and 30% mechanical deformation. TE aerogels have promising applications for heat harvesting under mechanical deformation and vertical heat sources.

2.1. Materials

Bacterial cellulose (BC) was solid content of 0.8 wt%, and purity was > 99%. The average length was 20 μm, and the diameter was 50-100 nm. Single-walled carbon nanotubes (SWCNTs) purity was 95%, length was 5-30 μm, and the average diameter was 1-2 nm. There were purchased from XianFeng Nano (Guangzhou, China). PEDOT:PSS was purchased from Heraeus Clevios (Anhui, China) and had a solid content of 1.3 wt%. All chemicals used in this study were used as received and were analytical grade.

2.2. Preparation of BC/PEDOT:PSS/SWCNT dispersion

BC and 3 ml PEDOT:PSS was added in 40 ml deionized water. After a uniform mixing well, 0.16 g SWCNT was added. Among them, the absolute dry quantity ratio of BC was 0.5 wt%. Subsequently, the dispersion solution was dispersed in the ultrasonic ice water bath for 30min, with the power of 800W. The absolute dry quantity of SWCNT and PEDOT:PSS was 0.5 wt%. Under the same experimental conditions, composite aerogels with different PEDOT:PSS/SWCNT weight fractions were prepared for comparison.

2.3. Fabrication of BC/PEDOT:PSS/SWCNT TE aerogel

The ultrasonic dispersion is poured into a Teflon mold, placed on a radiator platform, and the radiator plane is frozen by entering liquid nitrogen at a temperature of -200℃. The pressure is normal atmospheric pressure. The gel is then dried in a freeze-dryer for 56 hours to prepare the thermoelectric aerogel.

2.4. Characterization

The surface mapping and morphology of TE aerogels were observed by SEM system (Sigma 300, ZEISS, Germany) at an accelerating voltage of 3 KV. TEM image acquisition through transmission electron microscope system (Talos F200, FEI, USA). The Raman spectra were recorded on a Raman spectrometer (InVia, Renishaw, England) equipped with a laser diode irradiated at an excitation wavelength of 532 nm. An X-ray diffraction (XRD) system (D8 Advance, Bruker, Germany) with Cu-Ka radiation was used to characterize the crystal structure of the aerogel. Three-dimensional (3D) images of the aerogel interior were obtained using a multiscale X-ray nano-computed tomography (nano-CT) system (Skyscan 2211, Bruker, Germany). The thermal analysis of aerogels was obtained by a thermogravimetric analyzer system (TGAQ50, TA, USA) from 373 K to 1073 K at a heating rate of 10 K min^-1.

2.5. Measurements of mechanical and TE performances

The cyclic compressive stress-strain measurements were performed from 10% to 30% strain at 20 mm min^-1 using a tensile apparatus (TA.XT plusC, Stable Micro Systems, England). The conventional four-probe technique was used to measure the electrical conductivity of TE aerogels. The square sample's length, width and thickness were approximately 2 cm, 2 cm and 2 cm, respectively. The Seebeck coefficient is determined by the slope of the voltage versus temperature difference (ΔT) curve. A homemade instrument combined with a digital source meter measurement unit (2450, Keithley, USA) was used to collect output voltage and current data. The hot end heat source via heating platform (TM-2020, JF, China). Thin copper sheets were glued to both ends of the square sample with silver paste. Type K thermocouples measure the temperature difference between the two ends separately.

3.1. Synthesis and Characterization of BC/PEDOT:PSS/SWCNT TE aerogel

The preparation process of thermoelectric composite aerogel is shown in Fig. 1. Firstly, PEDOT:PSS was added to the BC solution under vigorous stirring to coat them uniformly on the BC surface by the action of hydrogen bonding. Subsequently, SWCNT was dispersed into the above solution assisted by ultrasonic stirring, which could form a tightly connected charge transfer network with PEDOT:PSS through interfacial interaction, thus preventing flocculation. Then, the mixture was poured into PTFE molds for directional freeze-drying. The thermoelectric materials in the dispersant can be assembled in an orderly manner from the bottom up, allowing PEDOT:PSS and SWCNT to assemble in the BC framework. Finally, ice crystals were removed by freeze-drying to form a woody aerogel with excellent thermoelectric and mechanical properties.

The SEM microscopic morphological characterization of the aerogel is shown in Fig. 2a-c. The pictures clearly show that the aerogel surface is loose and porous (Fig. 2a). PEDOT:PSS is wrapped on the BC surface via the interaction of hydrogen bonding, forming a conductive network between BC and SWCNT, which are uniformly dispersed in the BC network (Fig. 2b and 2c). Fig. 2d shows that the ultralight aerogel can be placed easily on the petals of the pink flowers without causing significant deformation. These structural characteristics help to decrease the thermal conductivity of TE materials. Subsequently, elemental mapping is used to analyze the presence and detailed spatial distribution of elements C, O, and S over a large area (Fig. 2e), where element S belongs to the characteristic elements of PEDOT:PSS. As shown in Fig. 2e, the distribution of element S is sufficient to prove that PEDOT:PSS is uniformly distributed inside the aerogel. Fig. 2f-g shows the TEM pictures of BC and BC/PEDOT:PSS/SWCNT dispersion, respectively. Fig. 2g indicates that the PEDOT:PSS layer is encased around the surface of BC fibers, and the SWCNT bundle is bound to BC fibers through PEDOT:PSS. In addition, the Tindal effect observed in the BC and BC/PEDOT:PSS/SWCNT dispersions reveals that these substances have been homogeneously mixed. As shown in Fig. 2h, aerogels with various shapes can be easily prepared by changing the mold, exhibiting good machinability.

Further, Nano-CT was utilized to reveal the internal structure of the aerogel and the fiber orientation. The distinct laminar orientation inside the aerogel after the directional freezing treatment was observed (Fig. 2i). Thus, the TE material can be encapsulated on the BC surface due to the laminar structure of aerogel and the role of hydrogen bonding, which were beneficial for improving the mechanical and thermoelectric properties of TE aerogels. Fig. 2i shows the apparent pattern, and the transverse patterns are shown in Fig. 2j and 2k, respectively.

The Raman spectra of SWCNT, PEDOT:PSS, and TE aerogels are shown in Fig. 3a. The interfacial π-π conjugation of PEDOT and SWCNT and the partial charge transfer are demonstrated by the typical peak of the original SWCNT (G band) at 1590 cm^-1 and the C-C stretching vibration peak of PEDOT:PSS at 1436 cm^-1 shifted to 1593 cm^-1 and 1433 cm^-1, respectively. The interaction between BC, PEDOT:PSS, and SWCNT can be further demonstrated from the XRD characterization plots in Fig. 3b. BC/PEDOT:PSS aerogels exhibit typical diffraction peaks at 2θ = 14.5°, 16.8°, and 22.6°, which are more robust than those of pure BC aerogels. In addition, the intensity of the characteristic diffraction peaks of PEDOT in BC/PEDOT:PSS/SWCNT aerogels became stronger after the addition of SWCNT, indicating that the orderliness of the PEDOT molecular structure is enhanced, which contributes to the charge transport in the composites. Fig. 3c-d shows the thermo-gravimetric pictures of aerogels with various PEDOT:PSS/SWCNT weight fractions, showing a temperature range of 200 ℃ to 300 ℃ for the thermal decomposition of cellulose and PEDOT:PSS., while the weight decay of SWCNT occurs when they reach about 500℃. Interestingly, the weight loss interval of the composites moved to 250℃~400℃ with the increase in the proportion of SWCNT, and the best thermal stability of the composites was achieved when the proportion of SWCNT was 80%, which proved that the interfacial interaction between PEDOT and SWCNT could interfere with the heat transfer and the thermal stability was improved.

3.2. Mechanical performance of the BC/PEDOT:PSS/SWCNT TE aerogel

Due to the directional freezing technique enables the orderly assembly of thermoelectric materials inside the aerogel, resulting in excellent mechanical properties. The compression data of the composite aerogel is shown in Fig. 4. Among these, Fig. 4a directly displays the demonstration of an aerogel undergoing compression-return to its native state after a single press of a finger. The cycling stability of aerogels with different SWCNT weight fractions under 30% compression deformation was shown in Fig. 4b-f, and the insets show the digital photos before and after compression. As the proportion of SWCNT increases, there is a significant increase in the compressive stress of the aerogels. Stress generated by the compression of the aerogel to 30% deformation is 6 KPa without SWCNT, while the stress increases to 15 KPa, 2.5 times than the former when the percentage of SWCNT is 100%. Although SWCNT can make the aerogel have excellent mechanical properties, it causes poor retention of fatigue intensity of the aerogel. As shown in Fig. 4d and 4f, the strength of aerogels with 50% and 100% SWCNT content showed a significant decline, with peak stresses of only 91% and 84% of the first compression after 100 cycles. In comparison, the strength of aerogels with 0% and 20% SWCNT content was retained at 92% and 94%. To our delight, the strength of the aerogel was retained at 97% when the percentage of SWCNT was 80%, indicating that the interfacial interaction between SWCNT and PEDOT can improve the fatigue strength of the aerogel, which is consistent with the former structural characterization. Thus, the rigidity of the aerogel increases significantly with the increase of the proportion of SWCNT. When the proportion of SWCNT is too high, the interfacial interaction between SWCNT and PEDOT is not available inside, resulting in increased SWCNT flocculation and decreased fatigue strength of the aerogel.

3.3. Thermoelectric performance of the BC/PEDOT:PSS/SWCNT TE aerogel

Fig. 5 shows the thermoelectric performance of the composited aerogel. The analog pictures of aerogel during thermoelectric transition and the schematic diagram of the electron transport between PEDOT:PSS and SWCNT inside the aerogel is shown in Fig. 5a. Firstly, PEDOT:PSS forms a tightly connected charge transport network with SWCNT dispersed between the BC, while the orientation treatment aligns the BC in the same direction, enhancing the carrier transport within the aerogel. Subsequently, the temperature difference causes the carriers to migrate from the hot end of the aerogel to the cold end. Eventually, a potential difference is created at the two ends of the aerogel.

The graph of the output voltage data of the aerogel with various SWCNT contents under different temperature differences is shown in Fig. 5b. It can be seen that the increase in aerogel output voltage is proportional to the SWCNT. The variation of the Seebeck coefficient for the five aerogels under different temperature difference conditions is shown in Fig. 5c. In addition, the Seebeck coefficients of the five aerogels reach their highest at a temperature difference of 10 K and then stabilize as the temperature difference increases. This phenomenon occurs because the temperature difference between PEDOT:PSS and SWCNT inside the aerogel are not established when the temperature difference at the hot end is low, and the heat dissipation is slow.

Fig. 5d shows the output voltage, current, and fitted power curves for the five aerogels at a temperature difference of 50 K. It can be seen that the overall thermoelectric properties of the aerogel reach a maximum at an SWCNT ratio of 80%, with an output power of 21 nW. In contrast, at 60% SWCNT ratio, the output power of the aerogel is only 6 nW due to its poor electrical conductivity. The effect of different SWCNT ratios on the electrical conductivity of aerogel and PF is shown in Fig. 5e. The conductivity of the aerogel can reach up to 80 S/m as the SWCNT ratio increases to 80%. Still, a decrease in conductivity occurs when the SWCNT ratio is further increased, owing to the large-scale flocculation of SWCNT, which hinders the conductive path. Meanwhile, the reduction of the PEDOT:PSS ratio deteriorates further the SWCNT conductive network dispersion, leading to a decrease in conductivity. Interestingly, the Seebeck coefficient increases in proportion to the SWCN, but the improvement is insignificant. Therefore, the highest PF value of the aerogel is achieved at 80% of SWCNT with 0.3 μWm^-1K^-2. Figure 5f shows the aerogel output voltage and current curves when the SWCNT ratio is 80% at different temperatures. The I-V curves at a constant temperature difference of 50 K in response to different strains is shown in Fig. 5g. It can be seen that the slope of the I-V curve changes while changing the strain, indicating that the internal resistance of the aerogel can be regulated by applying deformation. The power curves at different strains at a temperature difference of 50 K are shown in Fig. 5h. The output power of a single aerogel at 30% strain (84 nW) is four times higher than that (21 nW) of aerogel with 0% deformation. The applied deformation causes the cellulose sheet layers to grow directionally inside the aerogel to bend and contact each other, thus creating new conductive paths and increasing the aerogel output power.

3.4. Stability of the BC/PEDOT:PSS/SWCNT TE aerogel for practical applications

The continuous variation of the aerogel output voltage with an increasing temperature gradient is shown in Fig. 6a. The static output voltage response of the aerogel is measured for a constant ΔT increase from 0 to 30 K for a duration of 100 s. Fig. 6b shows the output voltage response of the aerogel at various ΔT. The aerogel undergoes three temperature loading and unloading cycles at different ΔT, each with a duration of 200 s, and the output voltage remains stable. Fig. 6c shows a schematic of the aerogel connected to the LED through the boost converter. When a temperature difference is built up at both ends of the TE aerogel, the carriers migrate from the hot end to the cold end of the aerogel, creating an electrical potential difference. Therefore, the TE aerogel can continuously harvest low-grade thermal energy and generate electricity. A simple self-powered lighting device was fabricated further to demonstrate the practical applications of the TE aerogel. The TE aerogel is connected to an LED with an operating voltage of about 2 V by paralleling it with a boost converter.

Fig. 6d shows the application of the TEG. First, the properties of the TEG were monitored in the absence of deformation, which provides no temperature difference during the first 10 s. No change in the thermoelectric device's output voltage and relative resistance was observed in this state. Then, one end of the thermoelectric device was brought into a temperature difference by employing finger contact, and the other end is kept at room temperature to produce a temperature difference across the device for the next 10 s. The output voltage is gradually increased to 0.1 mV. Still, there is no relative resistance change, and the voltage amplifier’s output voltage makes the aerogel light up the light-emitting diode. Finally, the temperature difference is kept constant by pressing the aerogel with a finger. Under pressure, the change in internal resistance is proportional to the deformation of the aerogel, causing the output current to increase in the same proportion. In contrast, the output voltage increases slightly, and the final output power increases significantly. As shown in video S1, the light-emitting diode becomes significantly brighter with the introduction of strain. This state has remained stable for the last 10 s, further demonstrating the potential of the thermoelectric device to collect heat under compressive strain and stable self-powered capability even under mechanical deformation.

Inspired by wood's laminar-ordered internal structure, this study prepared an elastic aerogel with BC, PEDOT:PSS, and SWCNT by a directed freezing technique for thermoelectric energy conversion in various environments. Raman spectroscopy and XRD characterization reveal internal interfacial interactions between PEDOT and SWCNT, which constructs a tightly connected charge transport network, significantly enhancing the thermoelectric device's electrical conductivity and Seebeck coefficient. Additionally, SWCNT enhances the mechanical properties of the TE aerogel. The maximum stress at 90% compressive strain is up to 241 KPa, the Seebeck coefficient is up to 28.6 μV/K, and the PF value is up to 0.3 μWm^-1K^-2. At a temperature difference of 50 K, the aerogel can provide 84 nW of output power at 30% strain. This work demonstrates the thermoelectric device's potential in heat harvesting under compressive strain. These will significantly facilitate the development of TE aerogels and TEG to broaden a wide range of application scenarios.

Authors’ contribution

Luzheng Chen: Conceptualization, Methodology, Writing-original draft, preparation, Writing-review & editing. Jiang Lou: Conceptualization, Supervision, Writing-review & editing. Yudong Zong: Conceptualization, Methodology, Visualization, Formal analysis, Data curation. Zhuqing Liu: Software. Yifei Jiang: Writing-review & editing. Wenjia Han: Conceptualization, Methodology, Visualization, Formal analysis, Data curation, Supervision, Writing-original draft, Writing-review & editing.

Acknowledgements

This work is supported by the Foundation of the Shandong Key R&D Program (No. 2021CXGC011002), the Natural Science Foundation of Shandong Province, China (No. ZR2021QB009 & No. ZR2020QB002), and the QUTJBZ Program (No. 2022JBZ01-05).

Funding

Not applicable.

Consent for publication

All authors approved the final manuscript and the submission to Cellulose.

Competing interests: 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.

Ethical approval and consent to participate: This article does not contain any studies with human participants or animals performed by any of the authors.

Availability of data and materials

All data generated or analyzed during this study are included in this published article and its supplementary information files.

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Wood Anisotropic Compression-Induced Power Enhancement Aerogel Thermoelectric Generator Based on BC/PEDOT:PSS/SWCNT

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