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Research Article  |  Open Access  |  8 Jan 2024

A facile in-situ reaction method for preparing flexible Sb2Te3 thermoelectric thin films

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Soft Sci 2024;4:3.
10.20517/ss.2023.34 |  © The Author(s) 2024.
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Abstract

Inorganic p-type Sb2Te3 flexible thin films (f-TFs) with eco-friendly and high thermoelectric performance have attracted wide research interest and potential for commercial applications. This study employs a facile in-situ reaction method to prepare flexible Sb2Te3 thin films by rationally adjusting the synthesized temperature. The prepared thin films show good crystallinity, which enhances the electrical conductivity of ~1,440 S·cm-1 due to the weakened carrier scattering. Simultaneously, the optimized carrier concentration, through adjusting the synthesis temperature, causes the intermediate Seebeck coefficient. Consequently, a high-power factor (16.0 μW·cm-1·K-2 at 300 K) is achieved for Sb2Te3 f-TFs prepared at 623 K. Besides, the f-TFs also exhibit good flexibility due to the slight change in resistance after bending. This study specifies that the in-situ reaction method is an effective route to prepare Sb2Te3 f-TFs with high thermoelectric performance.

Keywords

Thermoelectric, Sb2Te3, flexible thin film, thermal diffusion

INTRODUCTION

Thermoelectric (TE) technology can achieve direct conversion between thermal energy and electrical energy, which has significant applications in power generation and refrigeration[1-5]. With an increasing demand for micro-electromechanical systems of chip-sensors, wearable electronics, and implantable electronic devices, the TE flexible thin films (f-TFs) have attracted extensive interest due to their high adaptability to various conditions with high TE performance[6-10]. The TE performance of f-TFs can be accessed via power factor (S2σ)[11], where σ and S represent the electric conductivity and Seebeck coefficient, respectively. Herein, σ is defined as σ = nheμ, where nh, e, and μ represent carrier concentration, elementary charge, and carrier mobility, respectively[12,13]. The S can be evaluated by Mott formula[14,15]. The increase of S can be achieved by the decreased nh and increased effective mass (m*). However, it is a significant challenge to simultaneously increase the S and σ due to their coupled relationship. Typically, f-TFs are composed of organic f-TFs and inorganic f-TFs[16,17]. For typical organic f-TFs, such as 3-hexylthiophene-2, 5-diyl (FeCl3-doped P3HT, S2σ = ~0.2 μW·cm-1·K-2 at 340 K)[18], carbon nanotubes/polyaniline (CNTs/PANI, S2σ = ~4.07 μW·cm-1·K-2 at room temperature)[19], and poly (3,4-ethyl enedioxythiophene) polystyrene sulfonate (PEDOT/PSS, S2σ = ~3.34 μW·cm-1·K-2 at room temperature)[20], a room temperature S2σ is lower than 5.0 μW·cm-1·K-2. Inorganic f-TFs, such as Ag2Se (S2σ = ~18.6 μW·cm-1·K-2 at room temperature)[21], SnSe (S2σ = ~3.5 μW·cm-1·K-2 at 300 K)[22], Cu2Se (S2σ = ~11.12 μW·cm-1·K-2 at 549 K)[23], n-type Bi2Te3(S2σ = ~14.65 μW·cm-1·K-2 at room temperature)[24], p-type Sb2Te3 (S2σ = ~21.0 μW·cm-1·K-2 at room temperature)[25], have been attracted great attention from the TE research community. It is evident that inorganic f-TFs approaches exhibited higher S2σ than that of the organic f-TFs, depicting good potential for commercial applications.

Among inorganic TE f-TFs, p-type Sb2Te3 f-TFs with a narrow bandgap of ~0.3 eV possess good TE performance at near room temperature[26]. So far, numerous methods have been employed to synthesize p-type Sb2Te3 f-TFs[27-32], such as thermal evaporation[29], magnetron sputtering[30], solution printing[31], and thermal diffusion[32]. Vieira et al. realized a high σ of ~320 S·cm-1 and S2σ of ~12.0 μW·cm-1·K-2 at 298 K for Sb2Te3 f-TFs prepared by thermal evaporation[29]. Shang et al. successfully prepared (00l)-preferential orientation p-type Sb2Te3 f-TFs by magnetron sputtering methods and approached the σ of ~740 S·cm-1 and S2σ of ~12.4 μW·cm-1·K-2 at 300 K. Sb2Te3 f-TFs prepared by screen-printing technology can approach σ of ~250 S·cm-1 and S2σ of ~14.3 μW·cm-1·K-2 at room temperature[30,31]. It is concluded that the σ of Sb2Te3 f-TFs prepared by most of the preparation methods is lower than 1,000 S·cm-1 due to poor crystal growth. Consequently, the carrier transport properties were suppressed, and the corresponding TE performance of Sb2Te3 f-TFs is also limited.

In the present work, we employed a thermal diffusion method to prepare p-type Sb2Te3 f-TFs on a flexible polyimide (PI) substrate. The Sb and Te precursor films were deposited by thermal evaporation, as shown in Figure 1A. Pure Sb and Te f-TFs were obtained separately. The schematic diagram of the thermal diffusion process and the optical image of as-prepared Sb2Te3 f-TFs are shown in Figure 1B. The copper mold consists of a convex mold on the top and a concave mold placed below. Cu molds at both the top and bottom can enhance heat conduction and improve the uniformity of heat distribution during the thermal diffusion process. The Sb2Te3 f-TFs were synthesized by thermal diffusion methods using Te and Sb pure precursor films. The schematic diagram of the reaction process of Sb and Te during the thermal diffusion process is shown in Figure 1C. Through tuning the thermal diffusion temperature (Tdiff), the Sb2Te3 f-TFs with standard stoichiometric ratios were obtained. Moreover, the moderate Seebeck coefficient of > 95 μV·K-1 was achieved at room temperature. Simultaneously, the μ and σ increased with increasing Tdiff due to the weakened carrier scattering. Correspondingly, the highest value of S2σ of 16.0 μW·cm-1·K-2 at Tdiff = 623 K has been achieved. Besides, our prepared Sb2Te3 f-TFs approach good bending resistance.

A facile <i>in-situ</i> reaction method for preparing flexible Sb<sub>2</sub>Te<sub>3</sub> thermoelectric thin films

Figure 1. (A) The schematic diagram of the Sb and Te f-TFs prepared by thermal evaporation; (B) The schematic diagram of the thermal diffusion process. The Inset shows the optical image; (C) The schematic diagram of Sb2Te3 f-TF preparation through the thermal diffusion process. f-TFs: Flexible thin films.

EXPERIMENTAL

Sb2Te3 f-TF preparation process

The p-type Sb2Te3 f-TFs were prepared on a flexible PI substrate by a thermal diffusion method. First, Sb and Te films were deposited on PI substrates by using thermal evaporation. Te content is higher than a standard stoichiometric ratio of Sb:Te (2:3) due to the facile volatilization of Te induced by high saturation vapor pressure. The purity Sb (99.99 %) and Te (99.99 %) powders were weighed for 0.7025 and 1.5217 g, respectively. The Sb and Te evaporation parameters were as follows: the evaporation power of 18 and 20 W, the evaporation time of 13 and 16 min, and the evaporation pressure of 5 × 10-5 Torr, respectively, and the thickness of the Sb film and Te film were ~220 and ~520 nm. Secondly, the Te and Sb f-TFs were pressurized in the copper molds placed on heating equipment with a pressure of 1 N·mm-2. The Tdiff was set as 573, 603, 623, and 643 K, respectively. The corresponding heating and cooling rates are ~20 and 2 K/min, respectively. The sample was held at the target temperature for 30 min, and the pressurized sample was kept under vacuum for about 2 h to cool to room temperature. The as-prepared p-type Sb2Te3 f-TFs are shown in the inset of Figure 1B. The thickness of the as-prepared Sb2Te3 thin film is ~700 nm.

Characterization of the Sb2Te3 f-TFs

X-ray diffraction (XRD, D/max 2500 Rigaku Corporation, CuKα radiation) was employed to investigate crystal structures. Scanning electron microscopy (SEM) (Zeiss spra 55) and SEM with energy dispersive X-ray spectroscopy (SEM-EDS) (Bruker Quantax 200) were used to analyze the surface morphology and chemical composition of as-prepared Sb2Te3 f-TFs. Transmission electron microscopy (TEM) (FEI Tecnai G2 F20) and TEM-EDS (Bruker XFlash 5030) were also employed to study the crystal structure and chemical composition. X-ray photoelectron spectroscopy (XPS) was employed to measure the valence states of Sb and Te. The Geometric phase analysis (GPA) was further employed to analyze the lattice strains by the Strain++ software. A hall measurement system (HL5500PC, Nanometrics) was used to record the Hall performance. SBA458 (Nezsch) was used to measure the S and σ (error bars of 5% for S and 5% for σ).

RESULTS AND DISCUSSION

The crystal structure of Sb2Te3 f-TFs was investigated by XRD technology [Figure 2A]. All XRD peaks can be indexed to Sb2Te3 (PDF#15-0874), and no obvious impurity peaks were observed. The (015), (1010), and (110) diffraction peaks are the three main peaks. The highest peak is (015), indicating (015) preferred orientation of Sb2Te3 f-TFs. The enlarged (015) peaks are plotted in the inset I of Figure 2A, and the (015) peaks increased with increasing the Tdiff. Further, the corresponding calculated crystallinity increased with increasing Tdiff [Figure 2B]. Figure 2C depicts the calculated lattice parameters a and c, which clearly indicate the absence of any displacement in crystal structures. The valence states of Sb and Te in the Sb2Te3 films were investigated by XPS [Figure 2D-F]. Figure 2D-F presents the full XPS spectra and XPS spectra of Sb and Te, respectively. The presence of oxidized Sb2Te3 (indicated by peaks at 539.35 and 530.19 eV) and oxygen (evident in the O1s peak) is observed in Figure 2E due to the unencapsulated Sb2Te3 f-TFs used in an atmospheric environment. The binding energies at 528.46 and 537.77 eV were related to Sb 3d5/2 and Sb 3d3/2, respectively [Figure 2E], and the corresponding valance state of Sb was +3. The 3d core level of Te with two peaks at 586.54 and 576.99 eV was related to the oxidized Sb2Te3. Moreover, the binding energies at 583.03 and 572.82 eV are associated with Te 3d3/2 and Te 3d5/2, respectively [Figure 2F], and the corresponding valance state of Te is -2.

A facile <i>in-situ</i> reaction method for preparing flexible Sb<sub>2</sub>Te<sub>3</sub> thermoelectric thin films

Figure 2. (A) The XRD spectra of as-prepared Sb2Te3 f-TFs; (B) The enlarged (015) peaks and the corresponding calculated crystallinity; (C) The lattice parameters; (D) The full XPS spectra; (E) and (F) XPS spectra of Sb and Te, respectively. f-TFs: Flexible thin films; XPS: X-ray photoelectron spectroscopy; XRD: X-ray diffraction.

The crystal morphology and chemical composition of the as-prepared Sb2Te3 f-TFs were investigated through SEM and SEM-EDS technology [Figure 3]. Figure 3A shows the SEM surface morphology of Sb2Te3 f-TFs. All the films depict a morphology characterized by large particles, suggesting a typical dense polycrystalline structure. Figure 3B presents the EDS spectrum and atomic content of Sb2Te3 f-TFs prepared at Tdiff = 623 K. As can be seen, the chemical stoichiometry of Sb:Te was ~2.0:3.0. The corresponding EDS maps are shown in Figure 3C. Uniformly distributed Sb and Te elements were obtained, and no obvious enrichment in Te and Sb was detected. Figure 3C shows the atomic content of Sb2Te3 f-TFs, where the chemical stoichiometry of Sb:Te was closed to 2.0:3.0 for Sb2Te3 films prepared at Tdiff from 573 to 623 K. When the Tdiff reaches at 643 K, the chemical stoichiometry of Sb:Te was 2.0:2.8. It is suggested that the Te content slightly decreases due to the evaporation of Te at high temperatures.

A facile <i>in-situ</i> reaction method for preparing flexible Sb<sub>2</sub>Te<sub>3</sub> thermoelectric thin films

Figure 3. (A) SEM morphology of Sb2Te3 f-TFs prepared at Tdiff = 603, 623, and 643 K, respectively; (B) EDS spectrum and atomic content of Sb2Te3 f-TFs prepared at Tdiff = 623 K; (C) The corresponding SEM-BSE images and EDS maps; (D) The measured atomic contents of Sb2Te3 f-TFs. BSE: Backscattered electron; EDS: energy dispersive X-ray spectroscopy; f-TFs: flexible thin films; SEM: scanning electron microscopy.

To further study the changes in microstructure in detail, TEM was employed for the as-prepared Sb2Te3f-TFs [Figure 4]. The low-resolution [Figure 4A] and high-resolution images [Figure 4B] for Sb2Te3 prepared at Tdiff = 623 K show a neat arranged of lattices and the corresponding clear diffraction spots, which indicates good crystallinity of Sb2Te3 f-TFs. Figure 4C presents the enlarged image of the yellow square in Figure 4B. It can be seen that the measured value of the crystal spacing of ~3.2 Å can be indexed as the (015) plane of Sb2Te3, which was consistent with the XRD results. The lattice strains of Figure 4C are shown in Figure 4D and present no obvious lattice strain concentration along different directions due to the fewer lattice defects and lattice mismatches. In Figure 4E, the TEM-EDS maps depict that the Sb and Te are uniformly distributed throughout the Sb2Te3 nanoparticles. From the TEM-EDS [Figure 4F], it can be predicted that the chemical stoichiometry of Sb:Te is also close to 2.0:3.0 (at the nano-scale range).

A facile <i>in-situ</i> reaction method for preparing flexible Sb<sub>2</sub>Te<sub>3</sub> thermoelectric thin films

Figure 4. (A) Low-resolution TEM image of Sb2Te3 f-TF prepared at Tdiff = 623 K; (B) High-resolution TEM image taken from the yellow square in Figure 4A; (C) The enlarged TEM images of the yellow square in Figure 4B; (D) The corresponding lattice strains of Figure 4C along different directions; (E) The TEM-EDS maps of Sb and Te; (F) The corresponding TEM-EDS spectrum. EDS: Energy dispersive X-ray spectroscopy; f-TFs: flexible thin films; TEM: transmission electron microscopy.

As can be seen, Sb2Te3 thin films possess the highest S2σ near room temperature, as shown in Supplementary Figure 1. This work focuses on analyzing room-temperature TE performance as the core research topic. The TE performance of as-prepared Sb2Te3 f-TFs at room temperature is shown in Figure 5. The room temperature σ of Sb2Te3 f-TFs as a function of Tdiff is shown in Figure 5A. The room temperature σ increased with increasing Tdiff. Moreover, the highest value of σ reaches 1,440 S·cm-1 at Tdiff = 643 K. To further study the changes of σ, we measured the μ and nh of Sb2Te3 f-TFs at room temperature. Figure 5B compares the measured and calculated [based on single parabolic band (SPB)-model] μ as a function of nh[33]. The μ increases with increasing Tdiff, while the nh varies from around 1.1 × 1019 cm-3. It can be suggested that increasing μ is not mainly caused by the changes of nh. The μ is achieved from 63.4 cm2·V-1·s-1 at Tdiff = 573 K to a high value of 79.7 cm2·V-1·s-1 at Tdiff = 643 K. In addition, the deformation potential coefficient (Edef) calculated by the SPB model roughly decreases with increasing Tdiff. It is suggested that the enhanced crystallinity leads to the weakened carrier scattering, which is the main reason for the increased σ with increasing Tdiff. Figure 5C presents the room temperature S as a function of Tdiff. The positive values of S show the typical p-type semiconductor characteristics. Similar Seebeck coefficients are achieved due to all the films with a near standard stoichiometric ratio of 2:3. The S slightly increases and then decreases in the range of 95-110 μV·K-1 with increasing Tdiff. The maximum S of ~106 μV·K-1 is achieved at Tdiff = 623 K. The high Seebeck coefficient of as-prepared Sb2Te3 f-TFs is competitive with that of some bulk Sb2Te3[34]. Figure 5D shows the comparison between the measured and calculated S (based on the SPB model) as a function of nh. As can be seen, the measured room temperature nh remains nearly constant around 1.1 × 1020 cm-3 with increasing Tdiff. Furthermore, the m* calculated by the SPB model changed in the range from 1.26 to 1.37 m0. Besides, the m* increases and then decreases with increasing Tdiff. Correspondingly, the trend of S with increasing Tdiff is the same as the trend of m*. The changes of S can be attributed to the changes of m*. Figure 5E compares the measured S2σ and the calculated S2σ based on the SPB model at room temperature. All the S2σ value of Sb2Te3 f-TFs at room temperature is higher than 11 μW·cm-1·K-2. The maximum value of S2σ approaches as high as 16.0 μW·cm-1·K-2 at Tdiff = 623 K due to the high σ and moderate S. The high S2σ of our prepared Sb2Te3 f-TFs is competitive with that of the reported Sb2Te3 f-TFs [Supplementary Table 1]. Herein, the prepared Sb2Te3 f-TFs possess high bending resistance. The high bending resistance of Sb2Te3 thin film is mainly attributed to the PI flexible substrate and Nano-scale thickness Sb2Te3[35,36]. Both the resistance change (∆R/R0) and Seebeck coefficient change (∆S/S0) are lower than 10% under the bending cycles of 1,000 and bending radius of 18 mm [Figure 5F].

A facile <i>in-situ</i> reaction method for preparing flexible Sb<sub>2</sub>Te<sub>3</sub> thermoelectric thin films

Figure 5. (A) The measured room temperature σ as a function of Tdiff; (B) Comparison between the measured and SPB model calculated μ as a function of nh; (C) The measured room temperature S as a function of Tdiff; (D) Comparison between the measured and SPB model calculated S as a function of nh; (E) Comparison between the measured S2σ and the calculated S2σ based on the SPB model at room temperature; (F) The ∆R/R0 and ∆S/S0 changes of Sb2Te3 with bending cycles of 1,000 and a bending radius of 18 mm. SPB: Single parabolic band.

CONCLUSION

In this work, we successfully prepared Sb2Te3 f-TFs with high TE performance and bending resistance by the thermal diffusion method. Sb2Te3 f-TFs with standard stoichiometric ratios were achieved, which rationally tuned Tdiff and increased the crystallinity of Sb2Te3 f-TFs. With increasing Tdiff, tuning crystallinity increased σ and thus attenuated carrier scattering, achieving a high σ of ~1,440 S·cm-1 at Tdiff = 643 K. The moderate S larger than 95 μV·K-1 has been achieved due to standard stoichiometric ratios of Sb2Te3 f-TFs. Correspondingly, an excellent room temperature S2σ of 16.0 μW·cm-1·K-2 at Tdiff = 623 K has been achieved. Besides, a ΔR/R0 of < 10% is achieved after 1,000 bending cycles with a bending radius of 18 mm, indicating good bending resistance.

DECLARATIONS

Authors’ contributions

Made substantial contributions to the conceptualization and design of methodology and writing - original draft: Ao D, Wu B, Sun B, Yang D, Zhong Y

Performed data acquisition and technical work and provided supervision for writing - review and editing: Bushra J, Zheng Z

Availability of data and materials

Not applicable.

Financial support and sponsorship

This work was supported by Natural Science Foundation of China (12204355 and 52272210), Natural Science Fundations of Shandong Province (ZR2022QA018 and ZR2023ME001), the China Postdoctoral Science Foundation(2023M732609), and Doctoral Research Initiation Fund of Weifang University (2023BS01).

Conflicts of interest

All authors declared that there are no conflicts of interest.

Ethical approval and consent to participate

Not applicable.

Consent for publication

Not applicable.

Copyright

© The Author(s) 2024.

Supplementary Materials

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Ao D, Wu B, Bushra J, Sun B, Yang D, Zhong Y, Zheng Z. A facile in-situ reaction method for preparing flexible Sb2Te3 thermoelectric thin films. Soft Sci 2024;4:3. http://dx.doi.org/10.20517/ss.2023.34

AMA Style

Ao D, Wu B, Bushra J, Sun B, Yang D, Zhong Y, Zheng Z. A facile in-situ reaction method for preparing flexible Sb2Te3 thermoelectric thin films. Soft Science. 2024; 4(1): 3. http://dx.doi.org/10.20517/ss.2023.34

Chicago/Turabian Style

Ao, Dongwei, Bo Wu, Jabar Bushra, Bing Sun, Dong Yang, Yiming Zhong, Zhuanghao Zheng. 2024. "A facile in-situ reaction method for preparing flexible Sb2Te3 thermoelectric thin films" Soft Science. 4, no.1: 3. http://dx.doi.org/10.20517/ss.2023.34

ACS Style

Ao, D.; Wu B.; Bushra J.; Sun B.; Yang D.; Zhong Y.; Zheng Z. A facile in-situ reaction method for preparing flexible Sb2Te3 thermoelectric thin films. Soft. Sci. 2024, 4, 3. http://dx.doi.org/10.20517/ss.2023.34

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