Fabrication of functional polyester fibers by sputter deposition with stainless steel

Changliu Chu; Xinyu Liu; Yanxiao Bian; Chengwen Hu; Yanyan Sun

doi:10.1515/epoly-2022-0046

Article Open Access

Fabrication of functional polyester fibers by sputter deposition with stainless steel

Changliu Chu , Xinyu Liu , Yanxiao Bian , Chengwen Hu and Yanyan Sun

Published/Copyright: May 10, 2022

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From the journal e-Polymers Volume 22 Issue 1

Abstract

The effects of sputtering technological parameters (sputtering power, pressure, and time) on properties of stainless steel (SS)-sputtered polyester (PET) fiber were investigated. The variations in properties such as surface morphology, tensile strength, abrasion resistance, and electromagnetic shielding effectiveness of the prepared PET fiber sputtered under various parameters were discussed. The results indicated that the uniformity and denseness of the sputtered SS film were positively dependent upon the predetermined sputtering variables. The properties such as the breaking strength and abrasion resistance of SS-sputtered PET were remarkably enhanced as compared to the pristine one. It was found that the disorientation of macromolecules in fiber was mainly responsible for the deteriorated strength following wet and/or dry heating. In addition, a woven fabric composed of SS-sputtered fiber exhibited electromagnetic shielding capability. This research indicates that the metal deposition onto textile surfaces using magnetron sputtering is a straightforward approach for potential use in multifunctional materials.

Keywords: magnetron sputtering; surface metallization; metallic film; commercial polyester fiber; multifunctional textiles

1 Introduction

The investigation and applications of textile fiber materials are closely related to the daily life of the public and the further development of the relevant advanced manufacturing industry. However, the conventional and/or commercial fibers and the resulting fiber products cannot meet the requirements of modern society (1). The rapid growth of functional fibers (e.g., conductive, flame retardant, antibacterial, and photochromic) has stimulated the development of functional textiles for broad application (2,3).

Polyester (PET) fiber, one of the most widely used synthetic polymers, has advantages of wrinkle resistance, shape retention, and excellent tensile strength. However, the innately inert surface of such synthesis polymeric fibers is often not ideal (4). For example, it has poor moisture absorption, it can easily accumulate static electricity, etc. For these reasons, a lot of work has been done to prepare PET fiber-based functional materials, such as hydrophilic group grafting, copolymerization, and profiled section fiber, both domestically and abroad. It is evident that the improvement of surface characteristics of textile materials can be reached by the optimization of the preparation conditions (5); thereby, the final properties of materials change accordingly.

Currently, a variety of surface modification techniques have been employed to build the functional surfaces of textile materials, such as coating/spraying (6,7), chemical modification (8), plasma treatment (9,10,11,12,13), and magnetron sputtering. Among them, magnetron sputtering has been a widely useful technique having high deposition rates, uniformity over large areas of the substrates, and easy control over the composition of the sputtered films (14). For example, a cotton fabric first modified with a continuous polyvinyl alcohol thin film using the padding method and then coated with copper, stainless steel (SS), and titanium, respectively, using magnetron sputtering was prepared by Jiang et al. (15). The excellent properties of the as-prepared coated cotton fabric mean that it is a promising electroconductive and multi-shielding textile for smart applications. Baghriche et al. prepared functional PETs deposited on nanoparticulate Ag-thin films using direct current (DC) and pulse DC-magnetron sputtering, and the fibers have excellent antibacterial properties (16). A silver-coated PET fabric was prepared by Jiang et al. (17), and the as-prepared fabric exhibits excellent protection from ultraviolet (UV) radiation, excellent hydrophobicity, and good antibacterial performance. A copper-coated PET fabric pretreated with a laser using magnetron sputtering has excellent electrical conductive property, hydrophobicity, UV blocking, and heat generation properties, as reported by Peng et al. (18). The adhesion strength between the copper film and fibers is improved after laser treatment. Yuan et al. reported PET fabrics coated with nano-Ag/TiO₂ composite films using magnetron sputtering (19), and they pointed out that the colorfastness, mechanical behavior, and comfort were not significantly changed, whereas antistatic, anti-ultraviolet, and antibacterial properties were enhanced compared with the original PET fabrics. Kudzin et al. prepared PET knitwear fibers deposited with copper using magnetron sputtering (20), and such materials possess antimicrobial capability. Wang et al. performed deposition of polytetrafluoroethylene nanoparticles on graphene oxide/PET fabrics (21), and the results indicated that the prepared fabric showed the outstanding hydrophobic property, a remarkable capacity for adsorbing various organic solvents and oils from wastewater. Zhang et al. prepared a PET fabric deposited with copper films of 220 nm using magnetron sputtering, and the prepared Cu-coated fabric was further treated using a solution of benzotriazole to improve the stability of copper films in synthetic perspiration (22).

However, to the best of our knowledge, little work has been performed to modify the surface of a commercial PET fiber deposited with SS film, and there is a dearth of literature on the stability analysis of sputtered fiber strength following wet and/or dry heating. To this end, in this work, SS thin film was sputtered onto the surface of a commercial PET fiber using magnetron sputtering, and the effects of sputtering technological parameters (e.g., sputtering power, pressure, and time) on the structural morphology, tensile strength, and abrasion resistance performances were systematically investigated. In addition, the stability of tensile strength of sputtered PET fiber samples following wet and/or dry heating was also examined. Finally, the electromagnetic interference effectiveness (EMSE) of the SS-sputtered PET fiber fabric was measured. Such fundamental work can open new possibilities in the modification of polymer textiles, thereby improving their functionality in an eco-friendly, straightforward, and scalable manner.

2 Experimental

2.1 Raw materials

A white commercial PET fiber of 50 D/24F (purchased from Fujian Zhaosen Environmental Technology Co., Ltd., China) was used as the substance. Prior to the deposition, the fiber was ultrasonically cleaned in an alcohol bath, and then, it was repeatedly washed with deionized water and finally dried in an oven at 60°C. A sputtering SS target (99.99% pure) with a size of Φ 60 mm × 5 mm was used.

2.2 Fabrication of SS-sputtered PET fibers

Figure 1a graphically illustrates the schematic of the preparation of SS-sputtered PET fibers. As shown in the figure, SS film was sputtered onto PET fiber surface by using a magnetron sputtering system (JGP-450A; Sky Technology Development Co., Ltd., Chinese Academy of Sciences). The SS target was mounted on the bottom of the vacuum chamber (Figure 1b), and the PET fiber was just placed against the target. The distance from the SS target to the PET substrate in the experiment was 60 mm. Prior to the deposition, the pure argon gas, with a constant flow rate of 15 SCCM, that is, standard cubic centimeter per minute, was entered for 10 min to remove the impurities of the target surface, and the sputtering chamber was evacuated to achieve a base pressure of 5 × 10⁻⁴ Pa. Under the action of the electric field E, electrons collide with argon atoms during the flying to the substance, causing them to ionize to produce Ar-positive ions and new electrons. The Ar ion accelerates to the cathode target under the action of an electric field and bombards the surface of the SS target with high energy to cause the target to be sputtered. Finally, the SS atoms are deposited onto the PET surface to form a SS film. In order to improve the uniformity of SS film, the substrate holder was rotated at a speed of 100 rpm.

Figure 1

(a) Schematic and (b) the experimental setup of the preparation of SS-sputtered PET fiber; (c) the detailed deposition parameters.

The processing variables of magnetron sputtering play an essential role in determining the final properties of the SS-sputtered PET fiber. The detailed deposition parameters are summarized in Figure 1c. Three variables, such as sputtering time (15, 20, and 25 min), sputtering power (30, 40, and 50 W), and sputtering pressure (3, 5, and 7 Pa), were selected. The effects of the above three parameters on the final properties of PET were investigated using individual factor experiments.

2.3 Characterization

2.3.1 Surface morphology observation

Surface morphologies of SS-sputtered PET fiber samples under different treatment events were observed using scanning electron microscopy (SEM; Hitachi S-4800). Energy-dispersive X-ray spectroscopy (EDS) combined with SEM was further used to investigate the element distribution and the element content of each PET fiber surface.

2.3.2 Tensile behavior

Tensile behavior of the SS-sputtered PET fiber samples was measured using a YG(B)021DL tensile tester. Forty replicates, at a gauge length of 500 mm, a test speed of 500 mm·min⁻¹, and a preload of 0.5 cN‧tex⁻¹, were measured per sample as specified in Chinese standard GB/T 3916-2013. Finally, two indices, that is, tensile tenacity and the coefficient variation (CV/%), were calculated for further analysis.

Furthermore, box-and-whisker plots, which can provide some important information such as central tendency, dispersion, and skewness, were used to characterize the variation of tensile strength of SS-sputtered PET fiber samples under different treatment conditions.

In addition, to evaluate the stability of magnetron sputtering treatment, tensile behavior of SS-sputtered fiber samples under wet and dry heating events, that is, soaked in hot water of 100°C for 30 min and placed in an oven at 100°C for 30 min, was performed.

2.3.3 Abrasion resistance test

A Y731 cohesive force tester was used to assess the abrasion resistance of PET fiber samples with different technological variables at a testing speed of 60 times‧min⁻¹. At least 20 replicates were tested for each fiber sample.

2.3.4 Measurement of electromagnetic shielding effectiveness

The EMSE of PET fiber fabrics was measured using an anti-electromagnetic radiation tester (FY800; Nantong Sansi Textile Instrument Co., Ltd., China) over a frequency range of 30–3,000 MHz as specified in the standard ASTM D4935-10. Note that three woven fabrics composed of SS-sputtered PET fiber samples – (5 Pa, 30 W, 15 min), (5 Pa, 40 W, 15 min), and (5 Pa, 50 W, 15 min) – respectively, were carefully prepared in a handloom. A plain weave was made with a count of 380 ends/10 cm × 280 picks/10 cm, respectively. In addition, a reference woven fabric composed of pristine PET fiber was also prepared for comparison.

3 Results and discussion

3.1 Morphological structure and EDS analysis

3.1.1 Effect of technological parameters on surface morphology

Fiber structure has a decisive impact on the final properties of fibers and the subsequent products; a study on structural analysis gives an overall understanding of SS deposition onto fiber surface. Herein, the effects of three important technological variables, namely, sputtering power, sputtering time, and sputtering pressure, on the surface morphologies of the resultant treated fiber samples are presented in Figure 2. As shown in Figure 2a, the surface of pristine PET fiber is relatively smooth, and there are also some randomly arranged projections on its surface, which may be generated during the fabrication process. Upon comparing with Figure 2b and c, we found that with an increase in sputtering power from 30 to 50 W, a relatively compact SS film was deposited onto the surface of PET fiber. However, some interior parts of PET fiber were not sputtered with SS, primarily due to the multifilament form of PET. Similarly, compared with Figure 2d and e, as observed, at lower sputtering pressure, there are some defects present in the internal part of the PET multifilament. By increasing the sputtering pressure, more SS metal atoms had opportunities to collide with each other, thereby creating a more uniform and denser SS film. Moreover, as shown in Figure 2f and g, as expected, the SS film was fully covered with PET with an increase in sputtering time, indicating that the fiber surface became denser after being sputtered. Moreover, the individual fiber in PET multifilament was sputtered with SS film, irrespective of the internal and external considered. In short, the SS film can be successfully deposited onto the PET fiber surface by magnetron sputtering.

Figure 2

(a) The pristine PET fiber; effects of technological parameters, i.e., (b and c) sputtering power, (d and e) sputtering pressure, and (f and g) sputtering time on surface morphologies of fibers.

3.1.2 EDS analysis

Figure 3 exhibits the EDS spectra of SS-sputtered PET fiber samples deposited under various sputtering conditions. As can be seen, three elements (i.e., C, O, and Fe), and the varying proportions of the three elements can be found on the fiber surface, irrespective of the sputtering condition considered. As shown in Figure 3a–c, as the sputtering power increased from 30 to 50 W by keeping the other deposition conditions such as sputtering pressure of 5 Pa and sputtering time of 15 min as constant, the proportion of the Fe element was drastically increased from 4.28% to 13.23%, respectively. Why does an increasing trend exhibit? The following explanation can be interpreted: As is known to all, the major element in SS is Fe. It is considered that the high sputtering power in the magnetron sputtering system energizes argon gas to provide sufficient kinetic energy to adatoms. The enhanced surface diffusion of adatoms is somehow responsible for the growth of Fe in the SS film of PET fiber.

Figure 3

EDS spectra of SS-sputtered PET fibers deposited under various sputtering conditions: (a) 5 Pa, 30 W, 15 min; (b) 5 Pa, 40 W, 15 min; (c) 5 Pa, 50 W, 15 min; and (d) 3 Pa, 50 W, 15 min.

Further, compared with Figure 3c and d, a higher proportion of Fe (from 6.15% to 13.23%) was found with an increase of sputtering pressure from 3 to 5 Pa. With an increase in sputtering pressure, SS film was more crowded onto the PET fabric surface (which is already confirmed from the SEM shown in Figure 2d and e).

3.2 Tensile behavior and its stability analysis

3.2.1 Effect of technological parameters on tensile behavior

Herein, the effects of technological parameters on the tensile response of SS-sputtered fiber samples were systematically studied. Figure 4a and b presents the breaking tenacity and CV values of the as-prepared sputtered PET. Compared with the pristine PET fiber, the breaking tenacity of SS-sputtered fiber samples gradually increased, irrespective of the technological conditions considered. The weakest link theory can be used to interpret the change of fiber strength before and after magnetron sputtering treatments, since the randomly existing defects in PET fiber were filled with SS particles (Figure 4d). Specifically, the strength of pristine PET was 3.04 cN‧dtex⁻¹. The strength progressively increases with increasing sputtering power, reaching 4.21 cN‧dtex⁻¹ at 50 W (with a growing rate of strength of about 38.5%). As noted earlier, the sufficient kinetic energy to adatoms with high sputter pressure is responsible for the growth of SS film deposited on the fiber surface, which, in turn, leads to enhanced tensile strength. Furthermore, a sputtering pressure-enhanced effect was observed. The decreased density of the existing defects by increasing sputtering pressure can be employed to explain the enhanced fiber strength. Meanwhile, more SS particles were crowded onto the PET fiber surface with an increase in sputtering time, thereby resulting in an improvement of the tensile strength. In addition, we found that among the three predetermined technological parameters, the sputtering time seems to have a higher influence on the final fiber strength, followed by sputtering pressure and sputtering power.

Figure 4

Effects of technological parameters on (a) tensile tenacity and (b) CV% of SS-sputtered PET fibers; (c) boxplots for quantifying tensile strength; and (d) strength reinforcing mechanism.

With respect to Figure 4b, the CV values of tensile strength of all the prepared SS-sputtered PET fibers were less than 8%, indicating that all the breaking tenacities of fibers were stable and thus met the requirement of the actual production. The possible reason was given: there are some flaws existing on the surface of a pristine PET fiber, more or less. However, these flaws may be disappeared or reduced with the deposition of SS onto the fiber surface, since the SS nanoparticles may fill these flaws. As a result, the CV values of tensile strength of the sputtered fibers were reduced.

Furthermore, Figure 4c presents the box-and-whisker plots for tensile strength of SS-sputtered PET fiber samples before and after treatments (5 Pa, 40 W, and 15 min). As can be seen, the strength variation of the pristine fiber is higher than the sputtered one, demonstrating that the potential flaws within the pristine fiber were reduced or eliminated after magnetron sputtering treatment. Furthermore, the boxplot for the pristine group is positively skewed, whereas it looks a bit symmetric for the sputtered group.

3.2.2 Stability analysis of PET fibers for different treatment events

Furthermore, the stability of fiber strength was studied under wet and dry heating events, i.e., soaked in hot water of 100°C for 30 min, placed in an oven at 100°C for 30 min, respectively. Note that, the heat treatment experiments of PET fibers were carried out in a relaxed state.

The results given in Figure 5a shows that both wet and dry heating had caused an amount of damage and decreased the breaking tenacity of PET samples, irrespective of whether the fiber was sputtered or not. For example, the tensile strength of sputtered PET fiber (5 Pa, 40 W, and 15 min) is 3.98 cN‧dtex⁻¹, and the strength loss rate was 9.29% and 10.55% for the wet and dry heating, respectively. In addition, Figure 5b and c plots the variation of tensile strength of the pristine and sputtered fiber samples, respectively.

Figure 5

(a) Tensile data of PET fibers under different treatment conditions; (b and c) comparison of the pristine PET and sputtered PET fiber samples for different events, respectively.

Why the tensile strength of PET fiber under its relaxed state deteriorates following heat treatments? The possible reasons were presented as follows: On the one hand, the flexibility of molecular chains in relaxed fiber enhances following heat treatments. On the other hand, the fiber would undergo partial hydrolysis and a decrease in orientation. Consequently, the tensile strength of fiber decreases after wet and/or dry heating. Furthermore, comparing the fiber of wet and dry heating, we found that fiber strength in wet heating was relatively higher than that of dry heating at the same temperature. The existing alcoholic hydroxyl groups within the two ends of a PET fiber will bond with the water molecules in the wetting environment, producing certain intermolecular forces, which, in turn, results in a higher tensile strength of fiber following wet heating than that of dry heating.

3.3 Abrasion resistance of SS-sputtered PET fibers

Figure 6a shows that the abrasion-resistant number of SS-sputtered fiber samples drastically increased, irrespective of various sputtering variables considered. For example, the abrasion-resistant number of the pristine PET fiber was about 5,800, whereas the maximum number reached about 7,500 following the sputtering treatment. A uniform and denser SS film sputtered onto the surface of PET fiber (which will also cause a heavier PET fiber sample compared with the pristine one) may be responsible for the improvement of abrasion-resistant behavior of SS-sputtered PET. Furthermore, Figure 6b presents the consecutive SEM images of sputtered fiber at different abrasion times (e.g., 0, 500, and 1,000). It is evident that a uniform SS-sputtered layer on the fiber surface is observed without abrasion (i.e., 0 cycles). With an increase in the abrasion number, the sputtered layer is gradually worn out. Further increasing abrasion number may lead to a complete break of individual fiber around the PET surface, and then, the inner part of PET fiber will undergo wear (e.g., 1,000 cycles).

Figure 6

(a) Comparison of abrasion resistance of PET fibers under different sputtering conditions; (b) the consecutive SEM photographs of SS-sputtered PET fiber following different abrasion cycles.

3.4 EMSE of SS-sputtered PET fiber fabrics

The as-prepared SS-sputtered PET fiber fabrics have shown broad application potential in electromagnetic shielding field, owing to the excellent electrical conductivity of the sputtered PET fiber. As graphically illustrated in Figure 7a, the measurement consisted of a circular waveguide, working as a sample holder, with the input and output antennas connected to a vector network analyzer. Figure 7b shows the graphical representation of electromagnetic waves passing through the SS-sputtered PET fabrics. When the electromagnetic waves incidence on and encounter the surface of the fabric, that is, the SS layer, a part of the incident waves reflect, the others that are not being reflected will enter the interior part of the fabric, and finally, a few waves will pass through the thickness direction of PET fabric.

Figure 7

(a) Sketch of electromagnetic shielding testing system; (b) schematic of electromagnetic waves on passing through SS-sputtered PET fabric; and (c) EMSE under different sputtering treatments.

Figure 7c presents the effect of the sputtering power on the EMSE of as-prepared SS-sputtered PET fiber fabrics. As shown, the EMSE capability of PET fabrics increased when the sputtering power was increased from 30 to 50 W. Possible factors which were contributed to the considerable increase of high EMSE of sputtered fabrics at high sputtering power are considered to be an improvement of the density of the sputtered film. On the other hand, the lower value of EMSE at lower sputtering power is attributed to structural defects such as the incomplete sputter coating due to the relatively lower surface mobility. This is already confirmed from SEM images (Figure 2b and c). Furthermore, the EMSE over lower frequency ranges (e.g., 600–1,000 MHz) was higher than that over higher frequency ranges. This result reveals that the EMSE capability of SS-sputtered PET fabrics for lower-frequency, longer waves is relatively higher than for higher-frequency, shorter waves. In addition, the value of EMSE of reference fabric composed of the pristine PET fiber was less than 5 dB because the PET fiber is an electrical insulator and thus transparent to the electromagnetic interference radiation. In short, magnetron sputtering is a straightforward and eco-friendly surface deposition method, and it has better productivity in the rapid fabrication of electromagnetic shielding textile materials.

4 Conclusion

Herein, a SS film was successfully deposited on a commercial PET fiber by using the magnetron sputtering technique. Various analyses were executed to investigate the effects of sputtering technological parameters (power, pressure, and time) on the properties of SS-sputtered PET fiber samples.

The SEM–EDS results revealed that the uniformity and compactness of the sputtered SS film onto the fiber surface were positively dependent upon the given sputtering variables, and the content of each element (C, O, and Fe) varied under different sputtering conditions. A relatively uniform and dense SS film can be obtained with proper sputtering treatment. The properties such as the breaking strength and abrasion resistance performances of the sputtered PET fiber samples were enhanced as compared to the pristine fiber. The underlying mechanism can be revealed based on the weakest link theory since the existing randomly oriented defects in PET fiber were filled with the SS nanoparticles, which, in turn, results in the strengthening properties. Furthermore, the disorientation of macromolecules in a PET fiber under its relaxed state was primarily responsible for the weakened fiber strength following wet and/or dry heating. More importantly, a woven fabric consisting of the SS-sputtered PET fiber samples exhibits acceptable electromagnetic shielding capability, with the EMSE value reaching about 45 dB within the lower frequency range. This work provides a straightforward and scalable approach for the surface metallization of polymers, which is essential for potential use in multifunctional materials.

Funding information: This work was financially supported by the Open Project Program of Anhui Engineering and Technology Research Center of Textile, Anhui Province College Key Laboratory of Textile Fabrics (2021AETKL05), National College Student Innovation and Entrepreneurship Training Program (202110363051), Anhui Provincial College Student Innovation and Entrepreneurship Training Program (S202010363223), and the Key R&D project of Anhui Province (202004f06020038).
Author contributions: Changliu Chu: conceptualization, methodology, writing – original draft, project administration, funding acquisition; Xinyu Liu: investigation, writing – original draft; Yanxiao Bian: investigation; Chengwen Hu: investigation; Yanyan Sun: writing – review and editing, supervision. The authors applied the SDC approach for the sequence of authors.
Conflict of interest: Authors state no conflict of interest.
Data availability statement: The data sets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

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Received: 2022-03-16

Revised: 2022-04-12

Accepted: 2022-04-19

Published Online: 2022-05-10

This work is licensed under the Creative Commons Attribution 4.0 International License.

Articles in the same Issue

https://doi.org/10.1515/epoly-2022-0046

Keywords for this article

magnetron sputtering; surface metallization; metallic film; commercial polyester fiber; multifunctional textiles

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