Fabrication and performance of the wide-band highly shielded polyvinylidene fluoride film

The white weathering layer materials that can effectively block the entire solar light band is of great importance for improving the service life, safety, and reliability of the materials. In this work, CsxWO₃@PDA was prepared by in situ polymerization to achieve high absorption in the full spectral range and increase the compatibility between CsxWO₃ particles and polyvinylidene fluoride (PVDF). PVDF composite films with different particle contents were prepared through compounding with titanium dioxide (TiO₂) and CsxWO₃@PDA. The prepared composite films were characterized by FT-IR, field emission scanning electron microscopy, universal material testing machine, whiteness meter, and ultraviolet visible spectroscopy. The results showed that the CsPVDF composite films with CsxWO₃@PDA and TiO₂ exhibited a whiteness level higher than 74, a transmittance of less than 5% in the wavelength range of 200–2500 nm, and a transmittance close to zero in the range below 1750 nm, demonstrating excellent shielding effect. The xenon lamp aging test also confirmed that the composite films had excellent weather resistance after aging 500 h. At the same time, adding a certain amount of CsxWO₃@PDA could improve the tensile strength of PVDF.

1 Introduction

The importance of lightweight, high-performance materials across multiple industries is increasing with the rapid advancement of technology. These materials play crucial roles in fields such as aerospace, construction, transportation, and energy (Mountasir et al., 2015; Lv et al., 2022). They can not only enhance the performance of structures but also expand the boundaries of design, enabling the realization of more efficient and sustainable solutions (Ali and Andriyana, 2020; Jiang et al., 2016). Flexible fiber-reinforced composite materials, a specialized class of lightweight materials with a multi-layer structure, are widely utilized in applications such as aerostats, flexible structures, and inflatable construction. The lightweight and high-strength properties of these materials render them ideal candidates for the implementation of high-performance structures (Kang et al., 2006; Meng et al., 2017). The properties of flexible fiber-reinforced durability, weatherability, and adaptability to environmental changes, directly influence the reliability and service life of the entire structure. In aerospace, the lightweight and high-strength properties of flexible fiber-reinforced composite materials are critical for increasing the floating height and payload of aerostats (Meng et al., 2016). In architecture, they provide designers with the capability to create flexible, deformable spaces. Furthermore, the applications of flexible fiber-reinforced composite materials are also expanding in the transportation and energy sectors, such as movable structures and temporary facilities. To meet these diverse application requirements, flexible fiber-reinforced composite materials are generally composed of a lightweight and high-strength polymer multilayer, in which the structures are weather-resistant layer/barrier layer/intermediate layer/load-bearing fabric/heat sealing layer from the exterior to the interior. Among these, the weather-resistant layer, as an extremely important functional layer in the composite material, is usually white and directly related to the safety and stability of the aerostats (Lv et al., 2021).

Fluoropolymers are utilized in a wide range of fields due to their excellent weathering and chemical resistance (Améduri, 2023; Puts et al., 2019). The Tedlar, PVF series of composite films of DuPont’s are well known for their excellent effective aging resistance with its polyvinyl fluoride as the base resin and inorganic fillers with UV-visible light-blocking capabilities in the current market (Kim et al., 2012). However, there are processing challenges for polyvinyl fluoride due to its insolubility in most solvents and has a decomposition temperature similar to the melting temperature, limiting some of the applications (Alaaeddin et al., 2019). In contrast, polyvinylidene fluoride (PVDF) exhibits favorable aging resistance, abrasion resistance, and excellent mechanical properties (Dallaev et al., 2022). The processing performance of PVDF is also superior. However, it is inherently transparent, with high transmittance to UV and visible light, and cannot be utilized as a weathering layer to protect inner layers from radiation (Liu et al., 2020; Dong et al., 2018). To achieve a high shielding effect in the broad band, researchers have investigated various methods, such as blocking UV light by incorporating UV absorbers such as TiO₂ and benzophenone into the weathering layer (Deng et al., 2019; Jiang et al., 2021). Nevertheless, the shielding performance of these materials usually refers to the visible light region, and the covering ability for the near-infrared light region is even less effective (Muzata et al., 2023; Wu et al., 2019; Silva et al., 2023). Li et al. improved the opacity of PVDF composite films by adding TiO₂ and an extremely small amount of carbon black (Li et al., 2016). However, there was no information about the solar shielding properties. Although the carbon-based nanofiller and metal oxide (such as CuS) could also serve as light-shielding agents through reasonable regulation (Huang and Ruan, 2017; Yang et al., 2024; Yuan et al., 2020; Xu et al., 2017), the strong absorbance of sunlight and the complex preparation process of metal oxide, as well as the high cost, limit the applications in the fields such as aerostat and pneumatic architecture, which needs the materials with high whiteness and low transmittance as much as possible. Therefore, the development of white weathering layer materials that can effectively block the entire solar light band is of great importance for improving the service life, safety, and reliability of the materials. In this regard, novel materials and technologies are being explored. Among them, cesium tungsten bronze powder (Cs_xWO₃) has garnered considerable attention as an energy-saving coating additive, which can absorb more than 90% of near-infrared (NIR) light but not affect the performance in the visible light region (Nakakura et al., 2024; Nakakura et al., 2019; Zhang et al., 2024). Enhanced sunlight shielding can be achieved by compounding it with TiO₂. However, there is still a challenge for the dispersion of Cs_xWO₃ in the resin matrix.

Thus, in this study, dopamine, which is compatible with the resin, was utilized to modify Cs_xWO₃ through coating and compounded with TiO₂ to achieve effective shielding in broad wavelength bands and improved mechanical properties. This research can provide insights for the design of weathering layers for aerostat envelope materials and inflatable building materials.

2 Experimental section

2.1 Materials

Rutile TiO₂ with an average particle size of approximately 300 nm and CsxWO₃ with an average particle size of approximately 30 nm were supplied by DuPont’s and Yingcheng New Materials Co., Ltd., respectively. Dopamine hydrochloride with a purity of 98% and tris(hydroxymethyl)aminomethane solution (Tris) with a purity ≥99.9% were purchased from Energy Chemical and Aladdin Reagent Co., Ltd., respectively. The PVDF (SolefVR 6010) resin was obtained from Solvay Solexis Co., Ltd. N′, N′-dimethylformamide (DMF) was brought from Beijing Chemical Factory.

2.2 Preparation of CsxWO₃@PDA

As shown in Figure 1, 0.5 g/L CsxWO₃ dispersion was obtained first under the assistance of a cell disruptor. Then, a certain amount of dopamine hydrochloride was added and stirred to dissolve. Subsequently, a measured amount of the Tris buffer solution was mixed into the above dispersion to adjust the pH of the system to 8.5. Finally, the dispersion was washed and centrifuged with deionized water for 6∼10 times after reacting 6 h at room temperature to obtain CsxWO₃@PDA particles, which were dried for later use.

Figure 1

Figure 1. Fabrication process of PVDF composite films.

2.3 Preparation of the CsxWO₃@PDA/PVDF film

The composite films were prepared by solution casting. Initially, the PVDF solution with the fraction of 10.0 wt% and 0.1 g/L CsxWO₃@PDA dispersion in DMF were prepared for use. Soon afterward, a certain amount of TiO₂ and CsxWO₃@PDA were dispersed into the PVDF solution and stirred at a speed of 1,000 rpm for 2 h at room temperature. Then, the films were fabricated by pouring the suspension onto a glass substrate, which was kept in a horizontal level and coated with a casting stick and dried at 80°C to obtain a film with a thickness of approximately 50 μm. The samples were named in sequence as CPVDF-1, CPVDF-2, CPVDF-3, and CPVDF-4, where the total amount of CsxWO₃@PDA and TiO₂ was always controlled at 20.0 wt%. For comparison, samples containing 20.0 wt% TiO₂ and 18.0 wt% TiO₂ +2.0% CsxWO₃ were prepared and named TPVDF and CsPVDF, respectively. The composition of samples is listed in Table 1.

Table 1

Table 1. Composition of samples.

2.4 Characterization

The structure of CsxWO₃@PDA composite particles and composite film was characterized by X-ray photoelectron spectroscopy (XPS, Thermo ESCALAB250 X, Thermo Scientific Company, United States) with Al-Kα radiation and Fourier transform infrared spectroscopy (FT-IR, INVENIO-R, Bruker, Germany) over the wavenumber range of 400–4,000 cm⁻¹.

The morphology of inorganic fillers and the resulting films were characterized using a field-emission scanning electron microscope (FESEM, XL-30, FEI company, United States) with an acceleration voltage of 10 kV and a transmission electron microscope (TEM, JOEL-1400, Japan) under an acceleration voltage of 120 kV, respectively. The cross section of the composite film was obtained by quenching in liquid nitrogen, and the samples were sputter-coated with gold before testing.

Ultraviolet-visible near-infrared absorption performance was evaluated using a UV3600 spectrometer (Shimadzu, Japan) with a scanning interval of 2 nm/s and a scanning range of 200–2,500 nm.

The whiteness test of the material was conducted on a whiteness meter (Lichen, LC-WSB-2Y), which was calibrated using a standard whiteboard, which was the average value calculated of at least five points.

The composite films were cut into dumbbell-shaped strips and placed in a xenon lamp aging chamber for 500 h, followed by testing of mechanical properties at a stretching rate of 200 mm/min. At least 5 strips were tested, and the average value was calculated.

3 Results and discussions

3.1 Structural characterization of CsxWO₃@PDA

Figure 2 shows the TEM images of CsxWO₃ and CsxWO₃@PDA particles. It can be seen that CsxWO₃ was in an irregular rectangular shape, and an obvious circle appeared in CsxWO₃@PDA, which indicated the successful cladding of PDA.

Figure 2

Figure 2. TEM images of (A) CsxWO₃ and (B, C) CsxWO₃@PDA; the scale bar is 50 nm.

Figure 3A shows the FT-IR and XPS spectra of CsxWO₃ and CsxWO₃@PDA particles. It can be seen that after being coated with PDA, the characteristic absorption peaks of the stretching vibrations of phenolic hydroxyl and amine, imine N-H bonds appeared at 3,100–3,600 cm⁻¹. The peak at 1,600 cm⁻¹ corresponded to the stretching vibrations of the benzene ring C=C and the bending vibrations of N-H, and the shear vibration peak of N-H appeared at 1,510 cm⁻¹, which also indicated the successful preparation of CsxWO₃@PDA. At the same time, for the XPS peaks (Figures 3B, C), a characteristic peak of N1s appeared at 402 eV after being coated with PDA, which also implied the successful synthesis of CsxWO₃@PDA composite particles.

Figure 3

Figure 3. (A) FT-IR and (B, C) XPS spectra of CsxWO₃ and CsxWO₃@PDA particles.

3.2 Structural characterization of PVDF composite films

It can be seen from Figure 4 that there was no new characteristic peak appearing after compounding with TiO₂, CsxWO₃, or CsxWO₃@PDA particles, indicating that there was only a physical interaction between PVDF and the inorganic fillers, and no chemical bonding has occurred. However, the characteristic absorption peaks of CPVDF-4 among 3,300–3,400 cm⁻¹ were stronger than those of CsPVDF and TPVDF, which meant there were hydrogen bonds among PVDF and CsxWO₃@PDA (Figure 4B). The existence of −NH₂ and −OH groups could form strong hydrogen bonding with the F atom in the C-F bond.

Figure 4

Figure 4. (A) FT-IR spectra of PVDF composite films and (B) hydrogen bonding among PVDF and CsxWO₃@PDA.

3.3 Microscopic morphology of PVDF composite films

Figure 5 shows the morphologies of TiO₂, CsxWO₃@PDA, and PVDF composite films. It can be observed from the figure that TiO₂ and CsxWO₃@PDA were uniformly distributed in the resin matrix without any significant aggregation. In contrast, obvious aggregation of TiO₂ and CsxWO₃ particles was observed in the matrix (Figure 5F). The uniform dispersion was attributed to the modification of PDA, where −OH and −NH₂ could form hydrogen bonds with C-F bonds. In addition, CsxWO₃@PDA served as a diluent to a certain extent, which spaced the TiO₂ apart, resulting in more evenly dispersion of particles.

Figure 5

Figure 5. SEM images of (A) CsxWO₃@PDA, (B) TiO₂, (C) PVDF, (D) TPVDF, (E) CPVDF-4, and (F) CsPVDF.

3.4 Whiteness and light shielding properties of PVDF composite films

Whiteness was tested to study the influence of CsxWO₃ and TiO₂ on the composite film. The whiteness of TPVDF and CsPVDF was 81.4 and 76.2, respectively. With the increase in CsxWO₃@PDA, the whiteness of samples decreased from 80.3 to 74.7, owing to the induction of PDA. Even so, the whiteness of CPVDF was still maintained higher than that of carbon-based and commercial Tedlar.

To verify the light-shielding properties of the composite films, ultraviolet-visible near-infrared (UV-Vis-NIR) transmission tests were conducted, and the results are shown in Figure 6. The PVDF film had a transmittance close to 90% in the wavelength range of 240–2,500 nm. The transmittance of TPVDF with an addition of 20 wt% TiO₂ was close to zero in the wavelength range below 400 nm because of the excellent ultraviolet absorption properties of rutile TiO₂. In the visible and near-infrared regions above 400 nm, the transmittance of TPVDF increased with the increase in wavelength in the range of 400–2,500 nm and reached 25% at approximately 2,100 nm. The transmittance of CPVDF in the wavelength range above 500 nm decreased significantly with the addition of a small amount of CsxWO₃@PDA. Among them, CPVDF-4 with 2.0 wt% CsxWO₃@PDA had a transmittance of less than 5% throughout the entire spectrum, where the transmittance was close to zero in the range below 1750 nm. It is the multiple absorption of light at the interface of the core-shell structure for CsxWO₃@PDA that contributes to the excellent wide-band shielding properties. However, the transmittance across the entire spectrum of CsPVDF with CsxWO₃ and TiO₂ was much higher than that of CPVDF-4, especially in the regions of 400–800 nm and 1,500–2,500 nm. This was mainly because that CsxWO₃ has superior absorption performance in the 900–1,500-nm region but higher transmittance in the visible light region, which can also confirm that this is the effective combination of CsxWO₃ and PDA. Additionally, except for the pure PVDF film, the transmittance of the ultraviolet region for the other samples was close to zero, indicating that the materials had excellent UV shielding capabilities.

Figure 6

Figure 6. UV-Vis-NIR transmission spectra (A) and amplified spectra (B) of PVDF composite films.

3.5 Thermal stability test

Thermal stability is an important property for practical applications, which was tested in a nitrogen atmosphere, and the resulting curves are shown in Figure 7 and Table 2. The initial decomposition temperature and temperature at 5 wt% loss of the pure PVDF membrane were 392.7°C and 428.1°C, respectively. The thermal decomposition temperature reduced for TPVDF with TiO₂ and CsxWO₃, whose temperature at 5 wt% loss was 342.2°C and 346.9°C, respectively, which was speculated that addition of fillers may reduce the activation energy for thermal decomposition. With the increase in dopamine-modified CsxWO₃, the 5 wt% loss temperature of the composite films gradually decreased with the increase in CsxWO₃@PDA from CPVDF-1 to CPVDF-4, which was 358.6°C, 358.1°C, 354.2°C, and 351.8°C, respectively. The reason was that the interface interaction between CsxWO₃@PDA and PVDF had changed, which affected the crystallinity of PVDF and thereby affected the thermal stability of the composite films.

Figure 7

Figure 7. (A) TGA and (B) DTA curves of PVDF composite films.

Table 2

Table 2. TGA data on CsxWO₃@PDA/PVDF in nitrogen.

3.6 Contact angle measurement

Through the water contact angle experiment, it can be observed that the water contact angle of pure PVDF was 115.5°, showing good hydrophobicity (Figure 8). The TPVDF showed reduced water contact angle to 98.7° due to the polar functional groups such as hydroxyl on TiO₂, which could increase the surface energy and decrease the water contact angle. Owing to the presence of phenolic hydroxyl and amino groups in dopamine of CsxWO₃@PDA, the hydrophilicity of CPVDF-1 to CPVDF-4 was enhanced; thus, the water contact angle of the material decreased with the increase in CsxWO₃@PDA from 98.7 to 88.1°. In contrast, the addition of the CsxWO₃ powder did not significantly increase the surface energy like CsxWO₃@PDA. The reduction in the water contact angle is more conducive to adhesive bonding or heat sealing between PVDF composite films with other functional layers, which is vital for laminated structures.

Figure 8

Figure 8. Water contact angle of the PVDF composite films.

3.7 Aging performance of PVDF composite films

The aging resistance of the material could be assessed by comparing the mechanical properties of PVDF films before and after aging. Furthermore, the results are shown in Figure 9 and Table 3. The mechanical strength of the PVDF film slightly decreased from 59.3 ± 1.2 MPa to 55.3 ± 2.1 MPa after the addition of 20 wt% TiO₂, which may be due to the large addition fraction of TiO₂ and the lack of special surface treatment, resulting in a slightly poor interfacial bonding strength between TiO₂ and PVDF and led to stress concentration under load. The tensile strength of the sample further decreased to 53.2 ± 2.1 MPa after addition of untreated CsxWO₃, where CsxWO₃ dispersed poorly in the system, leading to stress concentration. Interestingly, on the basis of TPVDF, the fracture strength of the material increased to some extent with the increase in CsxWO₃@PDA content, especially when the addition amount is 2.0 wt%, the tensile strength of CPVDF-4 reached 63.5 ± 1.7 MPa, which was 14.8% higher than the pure PVDF of 55.3 ± 1.9 MPa. This was mainly because the coating of PDA contributed to the formation of a good interface transition between CsxWO₃ and PVDF through hydrogen bonding, which maximized the reinforcing effect. The strong hydrogen interaction rendered CsxWO₃@PDA as physical crosslinkers, which could serve as the dissipative unit to transfer the force to surrounding segments and particles rapidly. At the same time, 2.0 wt% CsxWO₃@PDA also acted as a spacer agent to dilute the dispersion of TiO₂ in the matrix and decrease the aggregates, as shown in Figure 4, improving the incompatibility between the matrix and the filler, ultimately making the material’s mechanical properties superior to pure PVDF. Moreover, after 500 h of xenon lamp aging, the mechanical properties of the film changed little, indicating that the material has excellent weather resistance.

Figure 9

Figure 9. Comparison of the fracture strength of PVDF films before and after aging.

Table 3

Table 3. Mechanical properties of PVDF composite films.

4 Conclusion

In this work, CsxWO₃ was modified by dopamine in situ polymerization, and a series of light-shielding PVDF composite films with TiO₂ and CsxWO₃@PDA were prepared through solution casting. Results showed that CsxWO₃@PDA and TiO₂ synergically achieved the high whiteness level above 74 and an absorption in the full spectral range and increased the compatibility between CsxWO₃ and PVDF, where CPVDF-4 with 18.0 wt% TiO₂ and 2.0 wt% CsxWO₃@PDA exhibited a transmittance close to zero in the range below 1750 nm, achieving excellent light shielding over a wide spectral range. Correspondingly, the prepared films showed excellent light aging properties, which were no slight changes after 500 h xenon lamp aging. Furthermore, PDA modification improved the interfacial compatibility between nanoparticles and PVDF, promoted the uniform dispersion of nanoparticles in the matrix, and thereby enhanced the mechanical properties of the composite film, especially the tensile strength reached 63.5 ± 1.7 MPa, which was notably higher than that of pure PVDF. In addition, the hydrophilicity of composite films was enhanced, which could contribute to the adhesive bonding or heat sealing among PVDF composite films with other functional layers.

Data availability statement

The original contributions presented in the study are included in the article/supplementary material; further inquiries can be directed to the corresponding authors.

Author contributions

LF: conceptualization, methodology, and writing–original draft. JH: writing–original draft. PL: writing–original draft. DX: writing–original draft, data curation, and investigation. WH: writing–original draft, methodology, and resources. LC: writing–original draft. YZ: writing–review and editing, conceptualization, and funding acquisition. XZ: writing–review and editing and writing–original draft. DY: resources and writing–review and editing. XJ: writing–original draft.

Funding

The author(s) declare that financial support was received for the research, authorship, and/or publication of this article. Talent Project - Youth Growth Technology Project of Jilin Province (20240602112RC).

Acknowledgments

The authors gratefully acknowledge the financial support from the Talent Project - Youth Growth Technology Project of Jilin Province (20240602112RC).

Conflict of interest

Author LF was employed by Pipe China Storage and Transportation Technology Company. Authors JH, DX, and LC were employed by Pipe China West Pipeline Company. Author PL was employed by the Production Department of Pipe China. Author WH was employed by Pipe China Gansu Pipeline Company. Author XJ was employed by Lianyungang Jingwei Composite New Materials Co., Ltd.

The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

The reviewer LL declared a shared affiliation with the authors YZ and XZ at the time of review.

Generative AI statement

The author(s) declare that no Generative AI was used in the creation of this manuscript.

Publisher’s note

All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations, or those of the publisher, the editors and the reviewers. Any product that may be evaluated in this article, or claim that may be made by its manufacturer, is not guaranteed or endorsed by the publisher.

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