A study of Cu sputtering on the polyphenylene sulfide fiber with plasma surface treatment | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article A study of Cu sputtering on the polyphenylene sulfide fiber with plasma surface treatment JeongJin Park, EunHye Kang, HyeonJi Kim, GyeongCheol Yu, SeungGoo Lee This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6155734/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract Sputtering is an effective technique for coating various substrates. However, the high energy involved can cause damage to polymers. In this study, polyphenylene sulfide, an engineering plastic known for its excellent thermal properties, was coated with Cu to impart electrical conductivity. To minimize polymer degradation during sputtering, oxygen plasma treatment was employed prior to deposition to investigate its effect on the process. The plasma treatment facilitated the attachment of oxygen species to the polyphenylene sulfide surface, which significantly enhanced the copper deposition rate. Notably, electrical conductivity increased by a factor of 10¹² during sputtering, with conductivity being 1.75 times greater after plasma treatment compared to untreated samples. Additionally, the thermal and mechanical properties of the polyphenylene sulfide were improved. These findings suggest that the plasma-assisted sputtering process not only enhances the electrical conductivity of polyphenylene sulfide but also has the potential to broaden its industrial applications. Composites Sputtering Metal coating Electric conductivity Engineering plastic Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 1. Introduction Polyphenylene sulfide (PPS) is an engineering plastic composed of aromatic rings linked by sulfide bonds, widely used in various industries for its excellent thermal stability, chemical resistance, and high mechanical strength [ 1 – 3 ]. With a glass transition temperature of 85°C and a melting temperature of 285°C, PPS is suitable for high-temperature industrial applications. Due to its exceptional properties, PPS is being studied for use in membranes [ 4 – 7 ], fiber reinforced resins [ 8 – 12 ], fiber fillers [ 13 ], and nonwovens [ 14 , 15 ]. PPS nonwovens, in particular, are employed as bag filters in industries that generate oxidizing substances, benefiting from their superior chemical stability [ 16 – 19 ]. However, their low electrical conductivity poses a risk of fire due to sparks or static electricity accumulation from dust-fiber friction. To mitigate this risk, conductive coatings are applied, and research is ongoing to modify surface conductivity to prevent damage caused by static charge [ 16 , 20 – 22 ]. Metal coatings on fiber surfaces provide various benefits, including increased electrical conductivity [ 23 ] , improved thermal and mechanical properties [ 24 , 25 ] , antimicrobial effects, and protection against electromagnetic interference [ 26 , 27 ]. Coating methods include electroplating[ 28 – 30 ], electroless plating[ 31 – 33 ], chemical vapor deposition[ 34 ], and sputtering [ 35 – 37 ]. However, the coating rate is often low due to the limited interaction between fibers and metals. Among these methods, sputtering has the advantage of forming strong, uniform, and adhesive bonds between metal atoms and the fiber matrix[ 38 – 40 ]. This technique allows for easy coating regardless of fiber type, but the high temperatures generated during sputtering can significantly damage the fibers. However, in the case of PPS, which has excellent thermal stability, the material is expected to withstand the heat produced during sputtering. In this study, high-energy sputtering was applied to PPS nonwoven. While increasing sputtering time can enhance deposition thickness, prolonged exposure to high temperatures can lead to fiber damage. Plasma treatment offers a simple method to attach desired elements to fiber surfaces by adjusting the gas composition, while etching increases surface roughness to promote stronger physical bonding during coating [ 41 ]. This pretreatment improves coating efficiency and shortens sputtering time, thereby reducing fiber damage. The resulting enhancement of electrical conductivity in PPS nonwovens is expected to broaden their potential applications in industrial settings. 2. Experimental 2.1. Materials The PPS nonwoven used in this study, provided by Huvis (Korea), has a core composed of PPS scrim. Prior to surface treatment, isopropyl alcohol (> 99.7%, DAEJUNG, Korea) was used to remove surface impurities of PPS nonwoven. Copper was selected as the sputtering target due to its excellent electrical conductivity and cost-effectiveness[ 42 ]. Additionally, copper's structural stability contributes to its flexibility, which is crucial for extending the service life of coated fibers particularly flexible materials such as nonwovens. Therefore, sputtering with Cu is expected to enhance the durability of PPS nonwovens when applied as bag filters. 2.2. Oxygen plasma process of PPS nonwoven The PPS nonwoven fabric was cut into 10 cm diameter circles for loading into the sputtering system. Samples were immersed in isopropyl alcohol for 1 h to remove impurities, followed by vacuum drying at 80°C for 4 h. Plasma surface treatment was conducted using a mini-plasma system (Plasmart, Korea). O₂ was chosen as the plasma gas due to its significant effect on the surface roughness of PPS [ 43 ]. The plasma process was performed at 100 W power and an O₂ flow rate of 10 mL/min for durations of 30, 60, 90, and 120 s to evaluate the impact of plasma treatment time on the surface. 2.3. Preparation of Cu coated PPS nonwoven fiber with sputtering system A high-purity Cu target (99.99%) was mounted on an RF sputtering system (DS-200, ADTECH, Korea), and pre-deposition of Cu was conducted on O₂ plasma-treated PPS nonwoven under an Argon atmosphere (99.99%) for 10 min to prevent oxidation. Sputtering was performed at a pressure of 3.0×10⁻³ Torr and a power of 100 W. To avoid under-deposition caused by the nonwoven fabric's 3D structure, the target tilt angle was set to 45°, and the substrate plate was rotated counterclockwise at 7.5 rpm during deposition. Cu sputtering was conducted for 10, 30, 60, and 90 min to assess the effect of sputtering time on the deposition process. 2.4. Analysis of the Cu coated PPS nonwoven Field emission scanning electron microscopy (FE-SEM, JSM-7610F, JEOL, Japan) was used to observe changes in the surface morphology of the fibers. The applied voltage was 15.0 kV, with measurements taken at ×1000 and ×3000 magnification. The presence of Cu deposition on the fiber surface after sputtering was confirmed by energy dispersive X-ray spectroscopy (EDS). Additionally, X-ray photoelectron spectroscopy (XPS, K-alpha, Thermo Fisher Scientific, USA) was used to analyze changes in surface chemical composition over different Cu deposition times. Electrical conductivity of Cu coated nonwoven was measured using the Four-Point Probe method [ 44 ]. The FPP measurements were conducted following established literature[ 45 ]. Specimens were cut into rectangles measuring 15 × 150 mm, and the thickness, w , was measured at 2.949 ± 0.020 mm. Electrical conductivity was assessed using a digital multimeter (2450 SourceMeter SMU, KEITHLEY, Ohio, USA), with a probe gap, S , of 1 mm. A constant current, I , of 0.1 µA was applied to measure the steady-state voltage, V . The electrical resistivity, ρ , was determined using the following equation. $$\:{\rho\:}=\frac{\pi\:}{\text{ln}2}w\left(\frac{V}{I}\right){F}_{1}{F}_{2}$$ Since electrical resistivity measurements are influenced by the specimen's geometry, corrections must be applied using the geometric correction factors F₁ and F₂. According to the literature [ 45 ], F₂ is 0.97, while F₁ is determined using the following equation. $$\:{\text{F}}_{1}=\:\frac{\text{ln}2}{\text{ln}[\text{sinh}(w/S)/\text{sinh}\left(w/2S\right)]}$$ Electrical conductivity, σ , was calculated as the reciprocal of electrical resistivity, ρ . Metal coatings with superior thermal properties alter the thermal characteristics of fibers [ 46 ]. Therefore, thermal properties after deposition were analyzed using thermogravimetric analysis (TGA, TGA4000, Perkin Elmer, USA) with a heating rate of 10℃/min, up to a maximum temperature of 700℃. To determine the thermal decomposition temperature, derivative thermogravimetry (DTG) was obtained by differentiating the TGA data. The mechanical properties of fibers improve when coated with metals that have higher strength and Young’s modulus compared to the fibers[ 47 ]. Accordingly, the mechanical properties were measured using a universal testing machine (UTM, AGS-X STD, Shimadzu, Japan), following ASTM D3822 for single filament tensile testing at a head speed of 1 mm/min. The results are reported as the average of 10 tests. 3. Results and Discussion 3.1. Characterization of PPS nonwoven after plasma treatment Figure 1 shows the surface of PPS nonwoven fabric before and after plasma treatment. In the untreated PPS (Fig. 1 a), a rough texture is visible on the fiber surface. After plasma treatment (Fig. 1 b-e), the surface becomes etched and cleaner. As the plasma treatment time increases, the surface smoothens, impurities are removed, and no significant fiber damage is observed. Figure 2 shows the XPS variation of PPS nonwoven during plasma treatment at different exposure times. In Fig. 2 a, the XPS data for S is presented. For untreated PPS (black line), peaks corresponding to C-S-C and C-S-S-C bonds are observed at 163.9 eV and 165.1 eV, respectively[ 48 ]. These peaks increase with short plasma treatment times (30 and 60 s), likely due to new bonding between neighboring copper and sulfur atoms as a result of the plasma energy. However, with prolonged plasma exposure, the peaks decrease, suggesting decomposition under sustained high-energy conditions. Additionally, new peaks at 167 eV and 169 eV appear, attributed to the formation of S = O and O = S = O bonds, indicating the introduction of sulfonyl groups through oxygen plasma treatment[ 49 – 51 ]. Figure 2 b displays the XPS data for C before and after plasma treatment. The C-C bond peak at 285 eV decreases as plasma time increases, indicating bond breakage due to plasma-induced high energy[ 52 ]. In Fig. 2 c, the oxide-related peak around 530.8 eV seen in the untreated specimen disappears after plasma treatment, likely due to the removal of surface impurity or material deposited during manufacturing[ 53 ]. Additionally, a small peak near 532.5 eV, attributed to oxygen bonded to carbon in the PPS[ 54 ], increases after plasma treatment, along with a peak at ~ 534 eV associated with carboxyl group formation[ 55 ]. A new peak around ~ 535 eV appears, which is due to the adsorption of reactive oxygen species introduced by the plasma, confirming the incorporation of oxygen species into the PPS surface. Table 1 Atomic percent of PPS nonwoven by plasma time. O plasma time (sec) Atomic percent (wt%) C O S Pristine PPS 84.94 10.63 4.43 30 74.96 19.75 5.29 60 69.87 21.18 8.94 90 66.1 23.92 9.98 120 59.41 33.38 7.21 3.2. Cu sputtering on PPS nonwoven Cu sputtering was performed on samples plasma-treated for 120 s, the time at which the highest concentration of sulfonyl groups was observed, as confirmed by post-plasma SEM and XPS analysis. Figure 3 presents SEM-EDS images of Cu-coated PPS nonwoven. Figure 3 a shows the SEM image of PPS nonwoven fiber without O₂ plasma treatment, while Fig. 3 b displays an SEM image of a PPS sample sputtered with Cu for 30 min, without prior plasma treatment. The surface appears smoother compared to the pristine PPS (Fig. 3 a), suggesting that sputtering, like plasma treatment, etches the surface. This trend is also observed in the sample sputtered for 10 min after plasma treatment (Fig. 3 c), where some particles are visible on the smoothed surface. In Fig. 3 d, the sample sputtered for 30 min after plasma treatment shows increased particle deposition on the surface. As sputtering time increases, the fiber surface becomes progressively rougher, with more particles accumulating. Notably, in Fig. 3 f, which represents the sample sputtered for 90 min, the particles on the PPS surface appears to have grown into rod-like structures. EDS analysis of the uncoated PPS nonwoven fiber (Fig. 3 g) reveals that the surface composition consists of 79.78 wt% C, 1.72 wt% O, and 18.5 wt% S. In contrast, Fig. 3 h shows the EDS results for the PPS nonwoven fiber after 90 min of Cu sputtering, with C, O, S, and Cu present at 15.14 wt%, 3.89 wt%, 5.77 wt%, and 75.2 wt%, respectively. The analysis indicates an increase in the proportions of O and S, alongside Cu, compared to the uncoated fiber. Additionally, the particles observed on Cu-sputtered sample are confirmed to be composed of Cu. Table 2 Change in diameter and atomic percent with sputtering time of EDS analysis Cu sputtering time (min) Diameter of fiber (µm) Atomic percent (wt%) C O S Cu Pristine PPS 14.502 ± 0.083 79.78 1.72 18.5 - 10 14.748 ± 0.235 53.38 3.02 30.03 13.56 30 (Plasma untreated) 15.324 ± 0.753 48.27 3.65 19.29 28.79 30 15.898 ± 0.334 23.64 3.92 12.07 60.36 60 15.282 ± 0.012 20.51 4.32 8.52 66.65 90 14.937 ± 0.129 15.14 3.89 5.77 75.2 The Cu sputtered PPS nonwoven fibers were characterized by XPS to analyze changes in surface chemical composition, as shown in Fig. 4 . Figure 4 a presents the XPS results for oxygen, indicating a decrease in the peak at 532.5 eV, associated with carbon oxygen bonds in PPS, following Cu coating. Additionally, the peak around 530.8 eV, which had decreased after plasma treatment, increases significantly again, suggesting that oxygen species were either displaced by sputtering energy or bonded with Cu to form oxides. Figure 4 b shows the XPS results for copper element. After 10 min of sputtering, a peak at 933 eV indicates the presence of copper oxide. Peaks at 935 eV and 955 eV correspond to C-O bonds, which likely formed between oxygen adsorbed on the PPS surface and copper during the initial stages of coating. As sputtering time increases, the peaks at 931.8 eV and 952.48 eV, corresponding to Cu 2P1/2 and 2P3/2, respectively, increase, confirming the deposition of pure copper[ 56 ]. Simultaneously, the oxide-related peaks also increase, as indicated by the growing satellite peaks around 940 eV and 960 eV, signifying the presence of copper oxides[ 57 ]. Table 3 presents the atomic percentages from the XPS analysis. The atomic percentage of carbon decreases as sputtering time increases, which can be attributed to the reduced thickness of the fiber surface layer as copper is deposited. Since XPS has a detection depth in the nanometer range, this reduced surface layer becomes less [ 58 , 59 ]detectable. Conversely, the atomic percentage of oxygen increases, likely due to the formation of copper oxide. After sputtering, XPS detects the carbon component of the fiber but not sulfur, in contrast to the EDS results. This difference arises because XPS has a much shallower detection depth (a few nanometers), while EDS detects to micrometer depths. The absence of sulfur in the XPS results suggest that sulfur was removed from the fiber surface during sputtering, which affects only the outermost few nanometers of the fiber. Table 3 Atomic fraction of PPS nonwovens as a function of sputtering time obtained by XPS analysis. Cu sputtering time (min) Atomic percent (wt%) C O Cu S Plasma treated PPS 84.94 4.43 - 10.63 10 69.85 24.02 6.13 - 30 73.34 21.14 5.53 - 60 59.11 29.69 11.2 - 90 36.9 46.85 16.25 - The graph illustrates the electrical conductivity of Cu-coated PPS nonwoven measured using the Four-Point Probe method, with detailed values provided in Table 4 . For PPS without Cu coating, the electrical conductivity was 2×10⁻¹⁶ S/cm. After 90 min of Cu coating, the conductivity increased by approximately 10¹² times to 1.42×10⁻⁴ S/cm. This demonstrates a significant improvement in conductivity through Cu sputtering. However, the electrical conductivity remained lower than that of pure copper, likely due to the nonwoven structure’s lack of continuity and the formation of non-conductive oxides, as indicated by the XPS analysis. To assess the impact of plasma treatment on conductivity, a non-plasma-treated PPS sample was sputtered under identical conditions for 30 min. Plasma treatment led to 1.75 times increase in conductivity compared to the untreated sample, confirming that plasma treatment significantly enhances Cu coating efficiency[ 60 ]. Table 4 Electrical conductivity of Cu coated PPS nonwoven by sputtering time Cu sputtering time (min) Electrical conductivity (S/cm) 0 (Plasma treated PPS) 2.0 − 16 10 2.52 − 10 30 (Plasma untreated) 8.09 − 09 30 1.42 − 08 60 1.80 − 05 90 1.42 − 04 Figure 6 shows the thermograms of TGA and DTG for PPS nonwoven before and after Cu coating, illustrating the thermal properties. The thermal degradation initial temperature (T di ), degradation finish temperature (T df ), and peak temperature (T p ) are listed in Table 5 . As sputtering time increases, the overall thermal degradation time is extended. This effect is attributed to the metal coating on the fiber surface, as the metal’s higher thermal conductivity facilitates heat dissipation, thereby delaying the thermal degradation process. Table 5 Degradation initial, degradation final and peak temperature of Cu coated PPS nonwoven fibers by sputtering time. Sputtering time (min) T di (℃) T df (℃) T p (℃) 0 427.5 655.6 557.1 10 427.9 653 559 30 430.3 670.5 559.8 60 441.3 665.3 560.5 90 454.8 665.3 559.3 Figure 7 illustrates the variation in tensile properties of PPS with increasing Cu sputtering time. The tensile strength and elongation increase up to 30 min of sputtering, after which they begin to decrease. Notably, even after just 10 min of sputtering, there is a measurable increase in tensile strength and elongation. The increase in strength is attributed to the deposition of the higher-strength metal, while the increase in elongation is likely due to fiber etching caused by sputtering. However, beyond 30 min of sputtering, both strength and elongation begin to decline. In contrast, Young’s modulus consistently increases with sputtering time, which is attributed to the increased stiffness of the fibers resulting from the coating of the high-modulus metal. 4. Conclusions In this study, Cu was coated on PPS nonwoven fibers using sputtering to enhance the electrical conductivity of this otherwise non-conductive material. The effect of O₂ plasma treatment on the sputtering process was thoroughly investigated. XPS analysis indicated that O₂ plasma disrupted carbon-sulfur bonds in the PPS nonwoven fibers, leading to the formation of new bonds with oxygen. The electrical conductivity of the Cu-coated PPS nonwoven increased by up to 10¹² times, demonstrating metal-like conductivity, with further enhancements observed in plasma-treated samples. Additionally, the effects of sputtering time on the fiber properties were evaluated. TGA analysis revealed that the metal coating delayed the thermal degradation of PPS nonwoven fibers. In terms of mechanical properties, both tensile strength and elongation improved at shorter sputtering times, but prolonged sputtering led to fiber degradation due to excessive energy input, reducing the mechanical performance. Since mechanical properties directly impact the durability and usability of the fibers in applications, it is critical to carefully balance sputtering time to optimize both mechanical strength and electrical conductivity. This study confirmed that Cu can be successfully coated onto PPS, despite their relatively low bonding affinity, using sputtering. The substantial increase in electrical properties due to the Cu coating suggests that PPS can be utilized in a wide range of applications. However, challenges remain, including the reduction in mechanical properties with prolonged sputtering and the unevenness of the coating. Addressing these issues will be critical for future improvements in the process. Declarations Acknowledge: This work was supported by a research fund from Chungnam National University (2022-0762-01). Data Availability declaration : The data are available from the authors upon reasonable request. Contributions : P.JJ wrote the main manuscript text, design of methodology and prepared figures; K.EH, K.HJ and Y.GC contributed to the preparation of experiment samples; L.SG contributed to the supervision and critical review. All authors reviewed the manuscript. Competing Interests : The authors declare no competing interests. References Hill, H.W., Brady, D.G.: Properties, environmental stability, and molding characteristics of polyphenylene sulfide. Polym. Eng. 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E-Polymers. 21 , 140–150 (2021). https://doi.org/10.1515/epoly-2021-0020 Primc, G., Mozetič, M.: Surface Modification of Polymers by Plasma Treatment. for Appropriate Adhesion of Coatings (2024) Velicu, I.L., Ianoş, G.T., Porosnicu, C., Mihăilă, I., Burducea, I., Velea, A., Cristea, D., Munteanu, D., Tiron, V.: Energy-enhanced deposition of copper thin films by bipolar high power impulse magnetron sputtering. Surf. Coat. Technol. 359 , 97–107 (2019). https://doi.org/10.1016/j.surfcoat.2018.12.079 Inagaki, N., Narushima, K., Morita, M.: Plasma surface modification of poly(phenylene sulfide) films for copper metallization. J. Adhes. Sci. Technol. 20 , 917–938 (2006). https://doi.org/10.1163/156856106777657797 Park, M., Park, J.H., Yang, B.J., Cho, J., Kim, S.Y., Jung, I.: Enhanced interfacial, electrical, and flexural properties of polyphenylene sulfide composites filled with carbon fibers modified by electrophoretic surface deposition of multi-walled carbon nanotubes. Compos. Part. Appl. Sci. Manuf. 109 , 124–130 (2018). https://doi.org/10.1016/j.compositesa.2018.03.005 Mironov, V.S., Kim, J.K., Park, M., Lim, S., Cho, W.K.: Comparison of electrical conductivity data obtained by four-electrode and four-point probe methods for graphite-based polymer composites. Polym. Test. 26 , 547–555 (2007). https://doi.org/10.1016/j.polymertesting.2007.02.003 Bard, S., Schönl, F., Demleitner, M., Altstädt, V.: Copper and nickel coating of carbon fiber for thermally and electrically conductive fiber reinforced composites. Polym. (Basel). 11 (2019). https://doi.org/10.3390/polym11050823 Okokpujie, I.P., Tartibu, L.K., Musa-Basheer, H.O., Adeoye, A.O.M.: Effect of Coatings on Mechanical, Corrosion and Tribological Properties of Industrial Materials. A Comprehensive Review (2024) Wang, N., Yang, Z., Wang, Y., Thummavichai, K., Xia, Y., Ghita, O., Zhu, Y.: Interface and properties of inorganic fullerene tungsten sulphide nanoparticle reinforced poly (ether ether ketone) nanocomposites. Results Phys. 7 , 2417–2424 (2017). https://doi.org/10.1016/j.rinp.2017.07.018 Liu, Y., Wang, W., Wang, A., Jin, Z., Zhao, H., Yang, Y.: N-doped carbyne polysulfide as cathode material for lithium/sulfur batteries. Electrochim. Acta. 232 , 142–149 (2017). https://doi.org/10.1016/j.electacta.2017.02.137 Ishida, T., Choi, N., Mizutani, W., Tokumoto, H., Kojima, I., Azehara, H., Hokari, H., Akiba, U., Fujihira, M.: High-resolution X-ray photoelectron spectra of organosulfur monolayers on Au(111): S(2p) spectral dependence on molecular species. Langmuir. 15 , 6799–6806 (1999). https://doi.org/10.1021/la9810307 Duwez, A.S.: Exploiting electron spectroscopies to probe the structure and organization of self-assembled monolayers: A review. J. Electron. Spectros Relat. Phenom. 134 , 97–138 (2004). https://doi.org/10.1016/j.elspec.2003.10.005 Lee, W.H., Lee, J.G., Reucroft, P.J.: XPS study of carbon fiber surfaces treated by thermal oxidation in a gas mixture of O2/(O2 + N2). Appl. Surf. Sci. 171 , 136–142 (2001). https://doi.org/10.1016/S0169-4332(00)00558-4 Kim, B.J., Oh, C., Bin, Lee, J.E., Lee, M.Y.: Effects of the Simultaneous Strengthening of the Glass Fiber Surface and Polyamide-6 Matrix by Plasma Treatment and Nanoclay Addition on the Mechanical Properties of Multiscale Hybrid Composites. J. Compos. Sci. 7 (2023). https://doi.org/10.3390/jcs7050176 Idriss, H.: On the wrong assignment of the XPS O1s signal at 531–532 eV attributed to oxygen vacancies in photo- and electro-catalysts for water splitting and other materials applications. Surf. Sci. 712 (2021). https://doi.org/10.1016/j.susc.2021.121894 Primc, G., Mozetič, M.: Surface Modification of Polymers by Plasma Treatment. for Appropriate Adhesion of Coatings (2024) Kumar, M., Bhatt, V., Nayal, O.S., Sharma, S., Kumar, V., Thakur, M.S., Kumar, N., Bal, R., Singh, B., Sharma, U.: CuI nanoparticles as recyclable heterogeneous catalysts for C-N bond formation reactions. Catal. Sci. Technol. 7 , 2857–2864 (2017). https://doi.org/10.1039/c7cy00832e Mulla, R., Rabinal, M.K.: CuO/CuxS composites fabrication and their thermoelectric properties. Mater. Renew. Sustain. Energy. 10 (2021). https://doi.org/10.1007/s40243-021-00189-7 Kumari, P., Bahadur, N., O’Dell, L.A., Kong, L., Sadek, A., Merenda, A., Dumée, L.F.: Nanoscale 2D semi-conductors – Impact of structural properties on light propagation depth and photocatalytic performance. Sep. Purif. Technol. 258 (2021). https://doi.org/10.1016/j.seppur.2020.118011 Gupta, B.D., Semwal, V., Pathak, A.: Nanotechnology-based fiber-optic chemical and biosensors. In: Nano-Optics, pp. 163–195. Elsevier (2020) Nishan Thilawala, K.G., Kim, J.K., Lee, J.M.: Improvement of conductivity of graphene-silver nanowire hybrid through nitrogen doping using low power plasma treatment. J. Alloys Compd. 773 , 1009–1017 (2019). https://doi.org/10.1016/j.jallcom.2018.09.272 Additional Declarations No competing interests reported. Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6155734","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":425000512,"identity":"482dcb24-81ab-4325-add7-72ef63ee6d21","order_by":0,"name":"JeongJin Park","email":"","orcid":"","institution":"Shinshu University","correspondingAuthor":false,"prefix":"","firstName":"JeongJin","middleName":"","lastName":"Park","suffix":""},{"id":425000513,"identity":"39bc4ca8-4b07-46db-82fe-aca41a4a0cfd","order_by":1,"name":"EunHye Kang","email":"","orcid":"","institution":"Chungnam National University","correspondingAuthor":false,"prefix":"","firstName":"EunHye","middleName":"","lastName":"Kang","suffix":""},{"id":425000514,"identity":"cb9b5933-231b-4dbe-b317-84227aec43ee","order_by":2,"name":"HyeonJi Kim","email":"","orcid":"","institution":"Chungnam National University","correspondingAuthor":false,"prefix":"","firstName":"HyeonJi","middleName":"","lastName":"Kim","suffix":""},{"id":425000515,"identity":"f7ddbe34-e0b2-4068-8d29-af7e8ba07748","order_by":3,"name":"GyeongCheol Yu","email":"","orcid":"","institution":"Chungnam National University","correspondingAuthor":false,"prefix":"","firstName":"GyeongCheol","middleName":"","lastName":"Yu","suffix":""},{"id":425000516,"identity":"f007906a-0672-41ce-b0de-7424a63aabe4","order_by":4,"name":"SeungGoo Lee","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAtElEQVRIiWNgGAWjYBACPjBZAeMeIEILG5g8Q7IWxjaStPAfv/jg4zy7PIMDzA8/MJy5R4QWiZxiw5nbkosNDrAZSzDcKCZGC0+aNO+2A4kbDjCYMTB8SCDGYWeAWuaAtLB/I1ILQ/oxad4GkBYeoC03iNEikcNsOONYcuLMwzzFEglniNDCz3/84YMPNXaJfcfbN374cIwILQwMPAYQmhmIidLAwMD+gDh1o2AUjIJRMHIBAKppN7gSxmx/AAAAAElFTkSuQmCC","orcid":"","institution":"Chungnam National University","correspondingAuthor":true,"prefix":"","firstName":"SeungGoo","middleName":"","lastName":"Lee","suffix":""}],"badges":[],"createdAt":"2025-03-04 15:53:22","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6155734/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6155734/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":78149131,"identity":"ae789007-e2ad-4970-b994-399367aff0ea","added_by":"auto","created_at":"2025-03-10 11:29:31","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":433359,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of (a) PPS nonwoven and (b-e) plasma treated PPS nonwoven by plasma time for 30,60,90 and 120 s\u003c/p\u003e","description":"","filename":"floatimage120.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/52c861493d3a55a42f197ed9.png"},{"id":78149133,"identity":"ec2cee8f-19ba-4aa6-bbbd-9c69ab958fee","added_by":"auto","created_at":"2025-03-10 11:29:32","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":243840,"visible":true,"origin":"","legend":"\u003cp\u003eXPS graphs of Oxygen plasma treated PPS nonwovens by plasma time; element of (a) sulfur, (b) carbon and (c) oxygen\u003c/p\u003e","description":"","filename":"floatimage29.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/81c990da224435141f90d482.png"},{"id":78149132,"identity":"a126e91d-b17a-43e0-9978-4c956e9807fe","added_by":"auto","created_at":"2025-03-10 11:29:32","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":1298847,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of (a) pristine PPS nonwoven fiber, Cu coated PPS nonwoven fibers (b) without plasma treatment and (c-f) with plasma treatment by sputtering time; 10, 30, 60, and 90 min. EDS images of PPS nonwoven fibers; (g) before Cu sputtering and (h) after 90 min Cu sputtering\u003c/p\u003e","description":"","filename":"floatimage310.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/d3fc4a34439e0e6062411b24.png"},{"id":78147869,"identity":"56e63d68-88a0-461a-822d-c6a31ba0c922","added_by":"auto","created_at":"2025-03-10 11:21:32","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":178706,"visible":true,"origin":"","legend":"\u003cp\u003eXPS graphs of Cu sputtered PPS nonwovens by sputtering time; element of (a) oxygen and (b) copper.\u003c/p\u003e","description":"","filename":"floatimage45.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/9a9e7f52e17c5afbde653ba3.png"},{"id":78147866,"identity":"155793a9-e726-4751-9a9d-722c5bd6866b","added_by":"auto","created_at":"2025-03-10 11:21:31","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":81347,"visible":true,"origin":"","legend":"\u003cp\u003eGraph of electrical conductivity of Cu coated PPS nonwoven fiber. (The pentagram symbol indicates plasma untreated specimen)\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/4f1a7107fd5d84d2e5c2a532.png"},{"id":78147872,"identity":"8890a4b8-9179-4468-99ed-aa76dcf768c9","added_by":"auto","created_at":"2025-03-10 11:21:32","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":113424,"visible":true,"origin":"","legend":"\u003cp\u003eTGA and DTG thermograph of Cu coated PPS nonwovens by sputtering time.\u003c/p\u003e","description":"","filename":"floatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/d72d0525ad1248db0bba097f.png"},{"id":78149410,"identity":"cbc85bc9-7189-419f-b8a4-ddd151087e09","added_by":"auto","created_at":"2025-03-10 11:37:32","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":171904,"visible":true,"origin":"","legend":"\u003cp\u003eMechanical properties of Cu-coated PPS nonwoven by sputtering time\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/57aba533e9ec71900b6759b5.png"},{"id":78256178,"identity":"1a9b80ce-cfe1-4997-8e5b-1c616c7d89eb","added_by":"auto","created_at":"2025-03-11 10:46:58","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":3392743,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6155734/v1/eb9af611-527c-4dab-b58e-13243b3390a8.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"A study of Cu sputtering on the polyphenylene sulfide fiber with plasma surface treatment","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003ePolyphenylene sulfide (PPS) is an engineering plastic composed of aromatic rings linked by sulfide bonds, widely used in various industries for its excellent thermal stability, chemical resistance, and high mechanical strength [\u003cspan additionalcitationids=\"CR2\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. With a glass transition temperature of 85\u0026deg;C and a melting temperature of 285\u0026deg;C, PPS is suitable for high-temperature industrial applications. Due to its exceptional properties, PPS is being studied for use in membranes [\u003cspan additionalcitationids=\"CR5 CR6\" citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e], fiber reinforced resins [\u003cspan additionalcitationids=\"CR9 CR10 CR11\" citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e], fiber fillers [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e], and nonwovens [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. PPS nonwovens, in particular, are employed as bag filters in industries that generate oxidizing substances, benefiting from their superior chemical stability [\u003cspan additionalcitationids=\"CR17 CR18\" citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. However, their low electrical conductivity poses a risk of fire due to sparks or static electricity accumulation from dust-fiber friction. To mitigate this risk, conductive coatings are applied, and research is ongoing to modify surface conductivity to prevent damage caused by static charge [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e, \u003cspan additionalcitationids=\"CR21\" citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eMetal coatings on fiber surfaces provide various benefits, including increased electrical conductivity [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e] , improved thermal and mechanical properties [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e, \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e] , antimicrobial effects, and protection against electromagnetic interference [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. Coating methods include electroplating[\u003cspan additionalcitationids=\"CR29\" citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e], electroless plating[\u003cspan additionalcitationids=\"CR32\" citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e], chemical vapor deposition[\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e], and sputtering [\u003cspan additionalcitationids=\"CR36\" citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e]. However, the coating rate is often low due to the limited interaction between fibers and metals. Among these methods, sputtering has the advantage of forming strong, uniform, and adhesive bonds between metal atoms and the fiber matrix[\u003cspan additionalcitationids=\"CR39\" citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]. This technique allows for easy coating regardless of fiber type, but the high temperatures generated during sputtering can significantly damage the fibers. However, in the case of PPS, which has excellent thermal stability, the material is expected to withstand the heat produced during sputtering.\u003c/p\u003e \u003cp\u003eIn this study, high-energy sputtering was applied to PPS nonwoven. While increasing sputtering time can enhance deposition thickness, prolonged exposure to high temperatures can lead to fiber damage. Plasma treatment offers a simple method to attach desired elements to fiber surfaces by adjusting the gas composition, while etching increases surface roughness to promote stronger physical bonding during coating [\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e]. This pretreatment improves coating efficiency and shortens sputtering time, thereby reducing fiber damage. The resulting enhancement of electrical conductivity in PPS nonwovens is expected to broaden their potential applications in industrial settings.\u003c/p\u003e"},{"header":"2. Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1. Materials\u003c/h2\u003e \u003cp\u003eThe PPS nonwoven used in this study, provided by Huvis (Korea), has a core composed of PPS scrim. Prior to surface treatment, isopropyl alcohol (\u0026gt;\u0026thinsp;99.7%, DAEJUNG, Korea) was used to remove surface impurities of PPS nonwoven.\u003c/p\u003e \u003cp\u003eCopper was selected as the sputtering target due to its excellent electrical conductivity and cost-effectiveness[\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e]. Additionally, copper's structural stability contributes to its flexibility, which is crucial for extending the service life of coated fibers particularly flexible materials such as nonwovens. Therefore, sputtering with Cu is expected to enhance the durability of PPS nonwovens when applied as bag filters.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2. Oxygen plasma process of PPS nonwoven\u003c/h2\u003e \u003cp\u003eThe PPS nonwoven fabric was cut into 10 cm diameter circles for loading into the sputtering system. Samples were immersed in isopropyl alcohol for 1 h to remove impurities, followed by vacuum drying at 80\u0026deg;C for 4 h. Plasma surface treatment was conducted using a mini-plasma system (Plasmart, Korea). O₂ was chosen as the plasma gas due to its significant effect on the surface roughness of PPS [\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. The plasma process was performed at 100 W power and an O₂ flow rate of 10 mL/min for durations of 30, 60, 90, and 120 s to evaluate the impact of plasma treatment time on the surface.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3. Preparation of Cu coated PPS nonwoven fiber with sputtering system\u003c/h2\u003e \u003cp\u003eA high-purity Cu target (99.99%) was mounted on an RF sputtering system (DS-200, ADTECH, Korea), and pre-deposition of Cu was conducted on O₂ plasma-treated PPS nonwoven under an Argon atmosphere (99.99%) for 10 min to prevent oxidation. Sputtering was performed at a pressure of 3.0\u0026times;10⁻\u0026sup3; Torr and a power of 100 W. To avoid under-deposition caused by the nonwoven fabric's 3D structure, the target tilt angle was set to 45\u0026deg;, and the substrate plate was rotated counterclockwise at 7.5 rpm during deposition. Cu sputtering was conducted for 10, 30, 60, and 90 min to assess the effect of sputtering time on the deposition process.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4. Analysis of the Cu coated PPS nonwoven\u003c/h2\u003e \u003cp\u003eField emission scanning electron microscopy (FE-SEM, JSM-7610F, JEOL, Japan) was used to observe changes in the surface morphology of the fibers. The applied voltage was 15.0 kV, with measurements taken at \u0026times;1000 and \u0026times;3000 magnification. The presence of Cu deposition on the fiber surface after sputtering was confirmed by energy dispersive X-ray spectroscopy (EDS). Additionally, X-ray photoelectron spectroscopy (XPS, K-alpha, Thermo Fisher Scientific, USA) was used to analyze changes in surface chemical composition over different Cu deposition times.\u003c/p\u003e \u003cp\u003eElectrical conductivity of Cu coated nonwoven was measured using the Four-Point Probe method [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e]. The FPP measurements were conducted following established literature[\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e]. Specimens were cut into rectangles measuring 15 \u0026times; 150 mm, and the thickness, \u003cem\u003ew\u003c/em\u003e, was measured at 2.949\u0026thinsp;\u0026plusmn;\u0026thinsp;0.020 mm. Electrical conductivity was assessed using a digital multimeter (2450 SourceMeter SMU, KEITHLEY, Ohio, USA), with a probe gap, \u003cem\u003eS\u003c/em\u003e, of 1 mm. A constant current, \u003cem\u003eI\u003c/em\u003e, of 0.1 \u0026micro;A was applied to measure the steady-state voltage, \u003cem\u003eV\u003c/em\u003e. The electrical resistivity, \u003cem\u003eρ\u003c/em\u003e, was determined using the following equation.\u003cdiv id=\"Equa\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equa\" name=\"EquationSource\"\u003e\n$$\\:{\\rho\\:}=\\frac{\\pi\\:}{\\text{ln}2}w\\left(\\frac{V}{I}\\right){F}_{1}{F}_{2}$$\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eSince electrical resistivity measurements are influenced by the specimen's geometry, corrections must be applied using the geometric correction factors F₁ and F₂. According to the literature [\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e], F₂ is 0.97, while F₁ is determined using the following equation.\u003cdiv id=\"Equb\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equb\" name=\"EquationSource\"\u003e\n$$\\:{\\text{F}}_{1}=\\:\\frac{\\text{ln}2}{\\text{ln}[\\text{sinh}(w/S)/\\text{sinh}\\left(w/2S\\right)]}$$\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eElectrical conductivity, \u003cem\u003eσ\u003c/em\u003e, was calculated as the reciprocal of electrical resistivity, \u003cem\u003eρ\u003c/em\u003e.\u003c/p\u003e \u003cp\u003eMetal coatings with superior thermal properties alter the thermal characteristics of fibers [\u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e]. Therefore, thermal properties after deposition were analyzed using thermogravimetric analysis (TGA, TGA4000, Perkin Elmer, USA) with a heating rate of 10℃/min, up to a maximum temperature of 700℃. To determine the thermal decomposition temperature, derivative thermogravimetry (DTG) was obtained by differentiating the TGA data.\u003c/p\u003e \u003cp\u003eThe mechanical properties of fibers improve when coated with metals that have higher strength and Young\u0026rsquo;s modulus compared to the fibers[\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e]. Accordingly, the mechanical properties were measured using a universal testing machine (UTM, AGS-X STD, Shimadzu, Japan), following ASTM D3822 for single filament tensile testing at a head speed of 1 mm/min. The results are reported as the average of 10 tests.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results and Discussion","content":"\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003e3.1. Characterization of PPS nonwoven after plasma treatment\u003c/h2\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e shows the surface of PPS nonwoven fabric before and after plasma treatment. In the untreated PPS (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea), a rough texture is visible on the fiber surface. After plasma treatment (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb-e), the surface becomes etched and cleaner. As the plasma treatment time increases, the surface smoothens, impurities are removed, and no significant fiber damage is observed.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e shows the XPS variation of PPS nonwoven during plasma treatment at different exposure times. In Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea, the XPS data for S is presented. For untreated PPS (black line), peaks corresponding to C-S-C and C-S-S-C bonds are observed at 163.9 eV and 165.1 eV, respectively[\u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e]. These peaks increase with short plasma treatment times (30 and 60 s), likely due to new bonding between neighboring copper and sulfur atoms as a result of the plasma energy. However, with prolonged plasma exposure, the peaks decrease, suggesting decomposition under sustained high-energy conditions. Additionally, new peaks at 167 eV and 169 eV appear, attributed to the formation of S\u0026thinsp;=\u0026thinsp;O and O\u0026thinsp;=\u0026thinsp;S\u0026thinsp;=\u0026thinsp;O bonds, indicating the introduction of sulfonyl groups through oxygen plasma treatment[\u003cspan additionalcitationids=\"CR50\" citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e51\u003c/span\u003e]. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb displays the XPS data for C before and after plasma treatment. The C-C bond peak at 285 eV decreases as plasma time increases, indicating bond breakage due to plasma-induced high energy[\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e]. In Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ec, the oxide-related peak around 530.8 eV seen in the untreated specimen disappears after plasma treatment, likely due to the removal of surface impurity or material deposited during manufacturing[\u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e53\u003c/span\u003e]. Additionally, a small peak near 532.5 eV, attributed to oxygen bonded to carbon in the PPS[\u003cspan citationid=\"CR54\" class=\"CitationRef\"\u003e54\u003c/span\u003e], increases after plasma treatment, along with a peak at ~\u0026thinsp;534 eV associated with carboxyl group formation[\u003cspan citationid=\"CR55\" class=\"CitationRef\"\u003e55\u003c/span\u003e]. A new peak around ~\u0026thinsp;535 eV appears, which is due to the adsorption of reactive oxygen species introduced by the plasma, confirming the incorporation of oxygen species into the PPS surface.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eAtomic percent of PPS nonwoven by plasma time.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"4\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eO plasma time (sec)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"3\" nameend=\"c4\" namest=\"c2\"\u003e \u003cp\u003eAtomic percent (wt%)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eC\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eS\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePristine PPS\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e84.94\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e10.63\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e4.43\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e74.96\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e19.75\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e5.29\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e69.87\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e21.18\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e8.94\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e66.1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e23.92\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e9.98\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e120\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e59.41\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e33.38\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e7.21\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e3.2. Cu sputtering on PPS nonwoven\u003c/h2\u003e \u003cp\u003eCu sputtering was performed on samples plasma-treated for 120 s, the time at which the highest concentration of sulfonyl groups was observed, as confirmed by post-plasma SEM and XPS analysis. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e presents SEM-EDS images of Cu-coated PPS nonwoven. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea shows the SEM image of PPS nonwoven fiber without O₂ plasma treatment, while Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb displays an SEM image of a PPS sample sputtered with Cu for 30 min, without prior plasma treatment. The surface appears smoother compared to the pristine PPS (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea), suggesting that sputtering, like plasma treatment, etches the surface. This trend is also observed in the sample sputtered for 10 min after plasma treatment (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ec), where some particles are visible on the smoothed surface. In Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ed, the sample sputtered for 30 min after plasma treatment shows increased particle deposition on the surface. As sputtering time increases, the fiber surface becomes progressively rougher, with more particles accumulating. Notably, in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ef, which represents the sample sputtered for 90 min, the particles on the PPS surface appears to have grown into rod-like structures.\u003c/p\u003e \u003cp\u003eEDS analysis of the uncoated PPS nonwoven fiber (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eg) reveals that the surface composition consists of 79.78 wt% C, 1.72 wt% O, and 18.5 wt% S. In contrast, Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eh shows the EDS results for the PPS nonwoven fiber after 90 min of Cu sputtering, with C, O, S, and Cu present at 15.14 wt%, 3.89 wt%, 5.77 wt%, and 75.2 wt%, respectively. The analysis indicates an increase in the proportions of O and S, alongside Cu, compared to the uncoated fiber. Additionally, the particles observed on Cu-sputtered sample are confirmed to be composed of Cu.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eChange in diameter and atomic percent with sputtering time of EDS analysis\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"6\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\"\u0026plusmn;\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eCu sputtering time (min)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eDiameter of fiber (\u0026micro;m)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"4\" nameend=\"c6\" namest=\"c3\"\u003e \u003cp\u003eAtomic percent (wt%)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eC\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003eCu\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePristine PPS\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026plusmn;\" colname=\"c2\"\u003e \u003cp\u003e14.502\u0026thinsp;\u0026plusmn;\u0026thinsp;0.083\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e79.78\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e1.72\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e18.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026plusmn;\" colname=\"c2\"\u003e \u003cp\u003e14.748\u0026thinsp;\u0026plusmn;\u0026thinsp;0.235\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e53.38\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e3.02\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e30.03\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e13.56\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30 (Plasma untreated)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026plusmn;\" colname=\"c2\"\u003e \u003cp\u003e15.324\u0026thinsp;\u0026plusmn;\u0026thinsp;0.753\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e48.27\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e3.65\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e19.29\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e28.79\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026plusmn;\" colname=\"c2\"\u003e \u003cp\u003e15.898\u0026thinsp;\u0026plusmn;\u0026thinsp;0.334\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e23.64\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e3.92\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e12.07\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e60.36\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026plusmn;\" colname=\"c2\"\u003e \u003cp\u003e15.282\u0026thinsp;\u0026plusmn;\u0026thinsp;0.012\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e20.51\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e4.32\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e8.52\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e66.65\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026plusmn;\" colname=\"c2\"\u003e \u003cp\u003e14.937\u0026thinsp;\u0026plusmn;\u0026thinsp;0.129\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e15.14\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e3.89\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e5.77\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e75.2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eThe Cu sputtered PPS nonwoven fibers were characterized by XPS to analyze changes in surface chemical composition, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea presents the XPS results for oxygen, indicating a decrease in the peak at 532.5 eV, associated with carbon oxygen bonds in PPS, following Cu coating. Additionally, the peak around 530.8 eV, which had decreased after plasma treatment, increases significantly again, suggesting that oxygen species were either displaced by sputtering energy or bonded with Cu to form oxides. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb shows the XPS results for copper element. After 10 min of sputtering, a peak at 933 eV indicates the presence of copper oxide. Peaks at 935 eV and 955 eV correspond to C-O bonds, which likely formed between oxygen adsorbed on the PPS surface and copper during the initial stages of coating. As sputtering time increases, the peaks at 931.8 eV and 952.48 eV, corresponding to Cu 2P1/2 and 2P3/2, respectively, increase, confirming the deposition of pure copper[\u003cspan citationid=\"CR56\" class=\"CitationRef\"\u003e56\u003c/span\u003e]. Simultaneously, the oxide-related peaks also increase, as indicated by the growing satellite peaks around 940 eV and 960 eV, signifying the presence of copper oxides[\u003cspan citationid=\"CR57\" class=\"CitationRef\"\u003e57\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eTable\u0026nbsp;\u003cspan refid=\"Tab3\" class=\"InternalRef\"\u003e3\u003c/span\u003e presents the atomic percentages from the XPS analysis. The atomic percentage of carbon decreases as sputtering time increases, which can be attributed to the reduced thickness of the fiber surface layer as copper is deposited. Since XPS has a detection depth in the nanometer range, this reduced surface layer becomes less [\u003cspan citationid=\"CR58\" class=\"CitationRef\"\u003e58\u003c/span\u003e, \u003cspan citationid=\"CR59\" class=\"CitationRef\"\u003e59\u003c/span\u003e]detectable. Conversely, the atomic percentage of oxygen increases, likely due to the formation of copper oxide. After sputtering, XPS detects the carbon component of the fiber but not sulfur, in contrast to the EDS results. This difference arises because XPS has a much shallower detection depth (a few nanometers), while EDS detects to micrometer depths. The absence of sulfur in the XPS results suggest that sulfur was removed from the fiber surface during sputtering, which affects only the outermost few nanometers of the fiber.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab3\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 3\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eAtomic fraction of PPS nonwovens as a function of sputtering time obtained by XPS analysis.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eCu sputtering time (min)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"4\" nameend=\"c5\" namest=\"c2\"\u003e \u003cp\u003eAtomic percent (wt%)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eC\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eCu\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePlasma treated PPS\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e84.94\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e4.43\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e10.63\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e69.85\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e24.02\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6.13\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e73.34\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e21.14\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e5.53\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e59.11\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e29.69\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e11.2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e36.9\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e46.85\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e16.25\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eThe graph illustrates the electrical conductivity of Cu-coated PPS nonwoven measured using the Four-Point Probe method, with detailed values provided in Table\u0026nbsp;\u003cspan refid=\"Tab4\" class=\"InternalRef\"\u003e4\u003c/span\u003e. For PPS without Cu coating, the electrical conductivity was 2\u0026times;10⁻\u0026sup1;⁶ S/cm. After 90 min of Cu coating, the conductivity increased by approximately 10\u0026sup1;\u0026sup2; times to 1.42\u0026times;10⁻⁴ S/cm. This demonstrates a significant improvement in conductivity through Cu sputtering. However, the electrical conductivity remained lower than that of pure copper, likely due to the nonwoven structure\u0026rsquo;s lack of continuity and the formation of non-conductive oxides, as indicated by the XPS analysis. To assess the impact of plasma treatment on conductivity, a non-plasma-treated PPS sample was sputtered under identical conditions for 30 min. Plasma treatment led to 1.75 times increase in conductivity compared to the untreated sample, confirming that plasma treatment significantly enhances Cu coating efficiency[\u003cspan citationid=\"CR60\" class=\"CitationRef\"\u003e60\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab4\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 4\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eElectrical conductivity of Cu coated PPS nonwoven by sputtering time\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"2\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eCu sputtering time (min)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eElectrical conductivity (S/cm)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e0 (Plasma treated PPS)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026minus;\" colname=\"c2\"\u003e \u003cp\u003e2.0\u003csup\u003e\u0026minus;\u0026thinsp;16\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026minus;\" colname=\"c2\"\u003e \u003cp\u003e2.52\u003csup\u003e\u0026minus;\u0026thinsp;10\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30 (Plasma untreated)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026minus;\" colname=\"c2\"\u003e \u003cp\u003e8.09\u003csup\u003e\u0026minus;\u0026thinsp;09\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026minus;\" colname=\"c2\"\u003e \u003cp\u003e1.42\u003csup\u003e\u0026minus;\u0026thinsp;08\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026minus;\" colname=\"c2\"\u003e \u003cp\u003e1.80\u003csup\u003e\u0026minus;\u0026thinsp;05\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\"\u0026minus;\" colname=\"c2\"\u003e \u003cp\u003e1.42\u003csup\u003e\u0026minus;\u0026thinsp;04\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e shows the thermograms of TGA and DTG for PPS nonwoven before and after Cu coating, illustrating the thermal properties. The thermal degradation initial temperature (T\u003csub\u003edi\u003c/sub\u003e), degradation finish temperature (T\u003csub\u003edf\u003c/sub\u003e), and peak temperature (T\u003csub\u003ep\u003c/sub\u003e) are listed in Table\u0026nbsp;\u003cspan refid=\"Tab5\" class=\"InternalRef\"\u003e5\u003c/span\u003e. As sputtering time increases, the overall thermal degradation time is extended. This effect is attributed to the metal coating on the fiber surface, as the metal\u0026rsquo;s higher thermal conductivity facilitates heat dissipation, thereby delaying the thermal degradation process.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab5\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 5\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eDegradation initial, degradation final and peak temperature of Cu coated PPS nonwoven fibers by sputtering time.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"4\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSputtering time (min)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eT\u003csub\u003edi\u003c/sub\u003e (℃)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eT\u003csub\u003edf\u003c/sub\u003e (℃)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eT\u003csub\u003ep\u003c/sub\u003e (℃)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e427.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e655.6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e557.1\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e427.9\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e653\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e559\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e430.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e670.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e559.8\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e441.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e665.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e560.5\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e454.8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e665.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e559.3\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e illustrates the variation in tensile properties of PPS with increasing Cu sputtering time. The tensile strength and elongation increase up to 30 min of sputtering, after which they begin to decrease. Notably, even after just 10 min of sputtering, there is a measurable increase in tensile strength and elongation. The increase in strength is attributed to the deposition of the higher-strength metal, while the increase in elongation is likely due to fiber etching caused by sputtering. However, beyond 30 min of sputtering, both strength and elongation begin to decline. In contrast, Young\u0026rsquo;s modulus consistently increases with sputtering time, which is attributed to the increased stiffness of the fibers resulting from the coating of the high-modulus metal.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eIn this study, Cu was coated on PPS nonwoven fibers using sputtering to enhance the electrical conductivity of this otherwise non-conductive material. The effect of O₂ plasma treatment on the sputtering process was thoroughly investigated. XPS analysis indicated that O₂ plasma disrupted carbon-sulfur bonds in the PPS nonwoven fibers, leading to the formation of new bonds with oxygen. The electrical conductivity of the Cu-coated PPS nonwoven increased by up to 10\u0026sup1;\u0026sup2; times, demonstrating metal-like conductivity, with further enhancements observed in plasma-treated samples. Additionally, the effects of sputtering time on the fiber properties were evaluated. TGA analysis revealed that the metal coating delayed the thermal degradation of PPS nonwoven fibers. In terms of mechanical properties, both tensile strength and elongation improved at shorter sputtering times, but prolonged sputtering led to fiber degradation due to excessive energy input, reducing the mechanical performance. Since mechanical properties directly impact the durability and usability of the fibers in applications, it is critical to carefully balance sputtering time to optimize both mechanical strength and electrical conductivity.\u003c/p\u003e \u003cp\u003eThis study confirmed that Cu can be successfully coated onto PPS, despite their relatively low bonding affinity, using sputtering. The substantial increase in electrical properties due to the Cu coating suggests that PPS can be utilized in a wide range of applications. However, challenges remain, including the reduction in mechanical properties with prolonged sputtering and the unevenness of the coating. Addressing these issues will be critical for future improvements in the process.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledge:\u003c/strong\u003e\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eThis work was supported by a research fund from Chungnam National University (2022-0762-01).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData Availability declaration :\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe data are available from the authors upon reasonable request.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eContributions :\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eP.JJ wrote the main manuscript text, design of methodology and prepared figures; K.EH, K.HJ and Y.GC \u0026nbsp; contributed to the preparation of experiment samples; L.SG contributed to the supervision and critical review. All authors reviewed the manuscript.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCompeting Interests :\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare no competing interests.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eHill, H.W., Brady, D.G.: Properties, environmental stability, and molding characteristics of polyphenylene sulfide. Polym. Eng. 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Alloys Compd. \u003cb\u003e773\u003c/b\u003e, 1009\u0026ndash;1017 (2019). \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.jallcom.2018.09.272\u003c/span\u003e\u003cspan address=\"10.1016/j.jallcom.2018.09.272\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"
[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Composites, Sputtering, Metal coating, Electric conductivity, Engineering plastic","lastPublishedDoi":"10.21203/rs.3.rs-6155734/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6155734/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eSputtering is an effective technique for coating various substrates. However, the high energy involved can cause damage to polymers. In this study, polyphenylene sulfide, an engineering plastic known for its excellent thermal properties, was coated with Cu to impart electrical conductivity. To minimize polymer degradation during sputtering, oxygen plasma treatment was employed prior to deposition to investigate its effect on the process. The plasma treatment facilitated the attachment of oxygen species to the polyphenylene sulfide surface, which significantly enhanced the copper deposition rate. Notably, electrical conductivity increased by a factor of 10¹² during sputtering, with conductivity being 1.75 times greater after plasma treatment compared to untreated samples. Additionally, the thermal and mechanical properties of the polyphenylene sulfide were improved. These findings suggest that the plasma-assisted sputtering process not only enhances the electrical conductivity of polyphenylene sulfide but also has the potential to broaden its industrial applications.\u003c/p\u003e","manuscriptTitle":"A study of Cu sputtering on the polyphenylene sulfide fiber with plasma surface treatment","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-03-10 11:21:27","doi":"10.21203/rs.3.rs-6155734/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"
[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"351ab3da-67ea-4f31-8903-32a75199bc0b","owner":[],"postedDate":"March 10th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2025-03-11T10:38:39+00:00","versionOfRecord":[],"versionCreatedAt":"2025-03-10 11:21:27","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-6155734","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6155734","identity":"rs-6155734","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}
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