Article pubs.acs.org/IECR
Atmospheric Plasma Effect on Cotton Nonwovens Sudheer Jinka,†,‡ Uday Turaga,†,‡ Vinitkumar Singh,† Rachel L. Behrens,§ Cenk Gumeci,§ Carol Korzeniewski,§ Todd Anderson,⊥ Rory Wolf,∥ and Seshadri Ramkumar*,† †
Nonwovens & Advanced Materials Laboratory, §Department of Chemistry and Biochemistry, and ⊥Department of Environmental Toxicology, Texas Tech University, Lubbock, Texas 79409, United States ∥ Pillar Technologies, Hartland, Wisconsin 53029-0110, United States ABSTRACT: The possibility of using atmospheric pressure plasma treatment (APT) without any additional functionalizing chemicals as an environmentally friendly technique for processing cotton nonwovens has been investigated. The quantitative determination of waxes suggested that APT results in the removal of waxes from cotton nonwovens and consequently increases its hydrophilicity. Fourier transform infrared studies showed that APT was capable of removing wax covering individual layers of cotton fibers. Intense plasma treatment causes a decrease in the strength of cotton nonwovens. Results show that APT can be a viable alternative for caustic soda treatment for dewaxing cotton.
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INTRODUCTION Cotton is the most consumed natural fiber in the world.1,2 In today’s market, cotton is being used extensively in woven and knitted forms for a wide range of applications. Currently, it is penetrating into nonwovens and industrial textile sectors.3 The majority of applications of cotton in textiles, in both conventional and unconventional sectors such as wipes and absorbent products, require it to be hydrophilic and wettable because it enables the uptake of liquids during wiping and dyes and other chemicals during finishing stages. The noncellulosic components in cotton such as waxes and pectins impart hydrophobicity to raw cotton, often compromising its dye uptake and water-absorbent properties.4,5 Sodium hydroxide (NaOH) scouring is used in the removal of wax in cotton textiles to make it absorbent and hydrophilic. Nevertheless, chemical methods pose considerable energy and environmental challenges. Recently, new approaches such as environmentally friendly plasma for processing textiles are being investigated.4−6 Plasma treatment is an environmentally benign process that can be used to alter and functionalize the surface of textile materials without changing its bulk properties. The mode of action of plasma on a given substrate mainly depends on the type of plasma and the process gas involved and can be categorized as (1) fine cleaning, (2) surface activation, (3) etching, (4) crosslinking, and (5) chemical vapor deposition.7,8 The types of plasma can be broadly classified as thermal and nonthermal. Thermal plasma involves high temperatures and, hence, may not be suitable for textile applications.9 Nonthermal plasma, which includes both vacuum plasma and atmospheric pressure plasma, is used in textile applications. Some features of atmospheric pressure plasma that facilitate its usage in textile applications include (1) it could be optimized for use as a continuous process on the industrial scale and (2) the process is more efficient in that highly activated particle densities could be attained at low temperatures.10 Other advantages of atmospheric pressure plasma treatment (APT) over existing processing techniques such as NaOH scouring and desizing used in the textile industry include (1) shorter treatment times, © 2014 American Chemical Society
(2) minimal usage of chemicals, and (3) no water consumption.4−6 Previous researchers have reported that the effect of plasma treatment on textile fabrics depends not only on the plasma gases used but also on the textile substrate’s structure.11−13 Recently, researchers have attempted to critically study the effect of plasma on cellulosic materials such as cotton and paper at the molecular level.14−16 For example, superhydrophobic cotton fabrics were developed, and it was concluded that the various effects of plasma treatment on cotton could be attributed to the etching action and subsequent introduction of new functional groups on the surface of cotton.14,15 Balu et al.14 have observed that plasma treatment selectively removes the amorphous domains, thereby exposing the crystalline moieties in cellulose, which eventually roughens the surface of cotton. In another study, Caschera et al.15 have studied the effects of various processing gases used in plasma treatment and found that gases like argon and oxygen result in more etching. Furthermore, these authors have observed that the use of argon gas results in the breaking of covalent bonds and the subsequent detachment of low-molecular-weight species such as waxes. These chemical functionalizations and surface roughening induced by plasma treatment also play a critical role in changing the surface properties of cotton such as enhanced hydrophilicity. Furthermore, Cai et al.17 and Bhat et al.18 have reported the use of APT for desizing of bleached and greige cotton woven fabrics, respectively. These authors claim that APT could be a viable solution to replace traditional textile pretreatment processes such as desizing. Karahan et al.4 have successfully employed APT to increase the pilling resistance, thermal resistance, water vapor permeability, and surface friction coefficient of bleached cotton woven fabrics. In another study, APT was used as a pretreatment to impart wrinkleReceived: Revised: Accepted: Published: 12587
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resistant properties19 and antimicrobial functionalities20 to blends of cotton and polyester woven fabrics. Additionally, Sun and Stylios21 and Tian et al.22 have applied APT as a pretreatment to enhance scourability and dyeability of cotton and wool woven fabrics. A decrease in the contact angle between the fabric and liquid in a dyeing and scouring bath and a subsequent increase in the wicking length of 1% Remazol Brilliant Red dye leading to a 50% increase in the dyeability rate owing to an increase in the hydrophilicity were reported by Sun and Stylios.21 As is evident from the aforementioned studies, these authors have investigated the use of APT as a finishing treatment in conjunction with conventional textile pretreatment processes such as desizing, bleaching, and fabric finishing. It should be noted that fabrics used in the above-mentioned studies were preprocessed wherein natural impurities such as waxes and other foreign matter have already been removed, leading to increased hydrophilicity, unlike in our work wherein APT has been used as a standalone treatment to remove waxes from unprocessed raw cotton without any chemical treatment to investigate the effect of APT on the hydrophilicity and wettability of fabrics, which heretofore have not been reported, to our best knowledge. Furthermore, Tian et al.22 have reported that the ability of APT to impart hydrophilicity to knitted cotton substrates was enhanced when the waxes in cotton fabric were removed using a solvent-extraction procedure. However, these authors did not quantify the amount of waxes present in unprocessed and treated fabrics, which in the authors’ view is important in order to understand the role of waxes and APT treatment in the removal of waxes, thereby enhancing the hydrophilic property of the textile substrate. In addition, because none of the aforementioned studies reported the use of standalone APT to remove waxes, it is important to understand the quantitative (using an extraction procedure) and qualitative (chemical modifications) effects of APT in removing waxes, because processes such as NaOH scouring and bleaching also remove waxes and other foreign matter to enhance hydrophilicity. The present study investigates the potential of APT to enhance the processability of nonwoven cotton fabrics and replace some of the current wet-processing techniques. Furthermore, the study focused on quantifying the effect of APT on wax in raw cotton because it influences the hydrophilicity and wettability of cotton. To our knowledge, there have been no studies that have attempted to understand the influence of APT on the hydrophilicity and wettability of unprocessed cotton nonwoven fabrics. This study is important because cotton nonwoven fabrics are finding applications as consumer and industrial wipes. Therefore, in the authors’ view, such a study wherein a standalone treatment is used to remove waxes and enhance hydrophilicity, as well as quantitatively report the amount of waxes before and after treatment, is timely and useful.
Table 1. HVI Characteristics of Cotton micronaire
length (in.)
uniformity index (%)
strength (g/ tex)
elongation (%)
4.29 (0.02)
1.06 (0.02)
82.50 (0.30)
27.8 (0.78)
7.0 (0.42)
Values within parentheses indicate the standard deviation. For micronaire measurement, the following procedure was used: one repeat per cotton sample and three samples per cotton type. For the length, uniformity, strength, and elongation, the following procedure was used: two repeats per cotton sample and three samples per cotton type.
Table 2. AFIS Characteristics of Cotton fineness (mtex)
immature fiber content (%)
maturity ratio
161 (2.64)
7.8 (0.60)
0.85 (0.005)
Values within parentheses indicate the standard deviation. For the fineness, immature fiber content, and maturity ratio, the following testing procedure was used: one repeat per cotton sample and three samples per cotton type.
textile substrate’s are the most widely used and preferred form for developing wipes. Needle-punched cotton fabric [225 g/m2 (GSM)] was developed using H1 needle-punching technology at the Nonwovens and Advanced Materials Laboratory, Texas Tech University. Conical blade needles (model 5238916) were obtained from Foster Needle Company (Manitowoc, WI). Parameters that were maintained constant throughout the needle-punching process include the following: needle penetration depth, 7.1 mm; outlet speed, 2.2 m/min; punching speed, 805 strokes/min; advance per stroke, 2.9 mm. The punching intensity was calculated to be 706.35 punches/in.2.23
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EXPERIMENTAL SECTION APT of needle-punched cotton fabric was carried out at Enercon Industries Corp. (Menomonee Falls, WI). Cotton nonwoven fabric was subjected to two different types of treatments: (1) Plasma I and (2) Plasma II. The treatment conditions are summarized in Table 3. Argon was chosen as the Table 3. Plasma Process Parameters Plasma I web speed (ft/min) system frequency (kHz) electrode type electrode gap power (kW) watt density (W/ft2/min) pressure (torr) process gas gas flow (L/min)
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MATERIALS Texas Upland cotton was used in the study. The characteristics of cotton were measured using Uster High Volume Instrument (HVI) and Uster Advanced Fiber Information System (AFIS) at Texas Tech University’s Fiber and Biopolymer Research Institute (FBRI). HVI and AFIS characteristics of the cotton used are presented in Tables 1 and 2, respectively. Plasma treatment effects on fabric directly depend upon the type of textile substrate being treated.12,13 In this study, we exclusively focused on nonwoven fabrics because nonwoven
Plasma II
20 100−200 ceramic 0.04 4 16
20 100−200 ceramic 0.04 4 16
760 90% argon + 10% oxygen 40
760 90% argon + 10% oxygen 10
process gas because it was proven to result in more etching4,24 and partial decomposition of the hydrophobic layer in cotton substrates.22 Plasma II is more effective than Plasma I with the ability to develop homogeneous plasmas and eliminate boundary-layer air effects.25 Plasma II also uses less gas compared to Plasma I, as shown in Table 3. All of the samples were conditioned for 6 h at 21 ± 2 °C and at a relative humidity of 65 ± 3%. Wax Extraction. A modification of Conrad’s method26 that employs the technique of accelerated solvent extraction (ASE) 12588
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was used for the quantification of waxes in cotton fibers. It is a two-step process. The first step involves extraction of cotton samples with isopropyl alcohol using a Dionex ASE 150 system. The second step is a phase-separation process and involves the addition of chloroform and deionized water to the isopropyl alcohol extract obtained in the first step. In this step, waxes present in the isopropyl alcohol extract were transferred to the chloroform phase in the isopropyl alcohol−chloroform−water mixture. Finally, chloroform was evaporated to determine the amount of waxes in cotton on a gravimetric basis. Such a method was found to be very efficient and specific because the nonwax constituents in the initial extract end up in the isopropyl alcohol−water layer. Only the waxes are retained in the chloroform phase.26 Contact-Angle Measurement. Contact-angle measurements were performed using a Rame-Hart A-100 goniometer. A drop of distilled water was carefully placed on the specimen using a syringe, and the image of the drop was captured with a high-resolution optical lens. The angle between the solid− liquid interfaces was measured using Rame-Hart DROPimage software. Wicking Test. A vertical wicking test was performed using the AATCC test method 198-2011, wherein a 1:1 mixture of water and ethanol (surface tension: 30 dyn/cm) was used as a wicking liquid. The specimen was cut into 3 cm × 25 cm pieces and inserted into the wicking liquid up to a depth of 1 cm. The wicking height was measured after 5 min. Mechanical Properties. The effect of APT on the strength and abrasion resistance of cotton nonwoven fabrics was evaluated using the ASTM 5035-06 and ASTM D4966 methods, respectively. It is important to quantify the changes in the strength and abrasion resistance of the fabrics as they were subjected to electromagnetic forces during plasma treatment. The tensile strength of cotton fabrics was measured in machine and cross directions and reported in terms of breaking load (N) and elongation at break (mm). The abrasion resistance of cotton substrates is reported in percentage weight loss over 2500, 5000, and 7500 rubs. Fourier Transform Infrared Attenuated Total Reflectance (FTIR-ATR) Measurement. FTIR-ATR spectra were obtained using a Bruker Vertex 70 spectrophotometer (Bruker, Billerica, MA) equipped with a liquid-nitrogen-cooled MCT detector and a VeeMaxII ATR accessory from Pike Technology. The ATR spectra (128 scans and 4 cm−1 resolution) were recorded using a single-reflection 60° ZnSe ATR crystal at an incident angle of 40°. A 2 cm × 2 cm cotton sample was mounted on top of the ATR crystal and gently pressed with a clamp for FTIR analysis. Scanning Electron Microscopy (SEM) Measurement. The surface morphology of cotton samples was studied using a Hitachi S-4300 scanning electron microscope. Samples were mounted on an aluminum stub with a conductive carbon tape. The scanning electron microscope was operated at an accelerated voltage of 2 kV to minimize charging effects, and a magnification of 5000× was used in imaging samples in this study. Statistical Analysis. Statistical analysis of all of the results was performed using the R software (version 2.13.1, R Core Development Team, 2011). All experiments were performed in triplicate. The means were compared using the analysis of variance method followed by multiple comparisons using Tukey’s honest significant difference test. A confidence interval
of 95% (p = 0.05) was used to analyze the statistical difference in the means of variables.
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RESULTS AND DISCUSSION Effect of APT on the Amount of Wax in Cotton. The amount of wax extracted from untreated and plasma-treated nonwoven cotton samples is shown in Figure 1. It was observed
Figure 1. Effect of APT on cotton wax.
that both Plasma I and II treatments have resulted in a significant removal of wax from the cotton fabric, as is evident from the amount of wax extracted after plasma treatments (p < 0.05). This could be attributed to the phenomenon of ablation that usually results in the detachment of low-molecular-weight species such as waxes.7,15,16 The amount of wax after Plasma I and II treatments decreased by 47.9% and 85.5%, respectively, compared to untreated cotton fabric. Intense plasma treatment as in Plasma II resulted in a treated cotton sample having only 0.31% wax compared to untreated fabric with 2.15% wax. Table 4 summarizes the effect of APT on the physical properties of cotton nonwovens such as contact angle, wicking Table 4. Contact-Angle, Surface Free Energy, and Wicking Height Data of Cotton Nonwoven Fabrics sample ID
contact angle (deg)
surface free energy (mJ/ m2)
wicking height (cm)
untreated Plasma I Plasma II
113.9 (1.84) 89.08 (2.74) 87.03 (3.54)
13.82 (1.05) 27.2 (4.92) 28.13 (4.29)
1.93 (0.12) 2.8 (0.1) 3.1 (0.1)
Values within parentheses indicate standard deviation.
height, and surface free energy. The decrease in the amount of wax in cotton nonwoven samples after plasma treatments was substantiated with contact-angle, surface free energy, and vertical wicking height measurements. It was observed that both types of plasma treatment have resulted in a significant decrease in the contact angle of the substrates (p < 0.05). The decrease in the contact angle suggests that APT imparts hydrophilicity to nonwoven cotton fabrics. Furthermore, it was observed that both treatments have resulted in a significant increase in the wicking heights in fabrics (p < 0.05) because APT of cotton nonwoven fabric enhanced its hydrophilicity due to plasma oxidation via reactive oxygen species resulting in hydrophilic functional groups. Plasma treatment induces chemical functionalities and topographical changes that improve the hydrophilicity of cotton substrates.14−16 The etching effect of plasma increases the effective pore size in cotton substrates and reduces the capillary pressure, eventually resulting in an increase in the wicking ability and enhanced 12589
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wettability.15,16 Additionally, the physicochemical changes in cotton nonwovens induced by plasma treatment could be justified by a change in the surface free energy of the substrates. It was observed that both Plasma I and II significantly increased the surface free energy of cotton nonwovens, as shown in Table 4. Changes in the surface free energies of cotton nonwoven substrates after plasma treatment could be attributed to the presence of polar components on the surface of cotton after plasma treatment.15,16 These physiochemical changes have been further discussed in detail in the FTIR section. On the basis of the above results, it can be inferred that APT has significantly enhanced the hydrophilic and wettable properties of cotton nonwovens to develop next-generation environmentally friendly absorbent wipes. This may prove beneficial to the dyeing and finishing industries because solvent-free and environmentally benign processing treatments reduce the overall cost of manufacturing and conserve energy. FTIR-ATR Analysis. The FTIR-ATR technique is convenient to apply in the characterization of waxes present at the surface of cotton fibers because the limited penetration depth of radiation beyond the ATR crystal confines the infrared beam to the outermost few microns of a sample. Because the waxes are present at the surface of cotton fibers and are dominated by long alkyl chains, the main features attributed to the waxes appear in the region between 3000 and 2800 cm−1.27 This region is indicative of alkyl chains and contains bands associated with asymmetric and symmetric CH2 stretching modes near 2920 and 2850 cm−1, respectively, methyl group asymmetric C−H stretching around 2960 cm−1, and symmetric stretching near 2895 cm−1 (Figure 2B). It is within this region that the peaks were integrated to determine the percentage change in the wax content following plasma treatments. Relative to the sample prior to plasma treatment (black line), the integrated intensity is lower by 28% for the Plasma I treated sample (red line) and 33% for the Plasma II treated sample (blue line). This clearly suggests that APT causes a loss in wax constituents in the nonwoven cotton samples. Other spectral features that can be traced to waxes are present in the spectrum of the untreated sample (black line) shown in Figure 2A. Bands at 1610, 1513, and 1259 cm−1 can be assigned to the asymmetric COO− stretch, the aromatic ring stretch, and the C−O carboxylic acid stretch, respectively, present in waxes such as gossypol and 1-octacosanol. These features are greatly diminished in spectra of the Plasma I (red line) and Plasma II (blue line) treated samples. The strongest bands in Figure 2A, which are present in the region between 1160 and 887 cm−1,27,28 are characteristic of cellulose. The peaks include the asymmetric bridge C−O−C stretches between 1160 and 1106 cm−1, the asymmetric C−C ring stretch at 1054 cm−1, and the C−O stretches at 1029 and 1006 cm−1. Other cellulose bands include C−H wagging at 131527,29,30 and 1429 cm−1 and C−H bending at 1368 cm−1.27 These bands are present in all three samples analyzed (untreated and Plasma I and II treated). The three spectra also display a broad band centered near 3300 cm−1. The feature contains contributions from the stretching modes of hydrogenbonded OH groups, which can be present in both the cellulose material and waxes. The qualitative estimate of cotton waxes in three cotton nonwoven fabrics gives a clear idea that the plasma treatment certainly modifies the surface of the cotton fabric toward hydrophilic nature. It may also be inferred that APT results in the removal of wax covering each individual fiber to a considerable extent.
Figure 2. FTIR spectra of untreated (black line), Plasma I treated (red line), and Plasma II treated (blue line) cotton nonwoven fabrics in the regions of 1800−800 cm−1 (A, top) and 3500−2600 cm−1 (B, bottom).
SEM Analysis. The surface morphology of untreated and plasma-treated nonwoven cotton samples was evaluated using a scanning electron microscope (Figure 3). The untreated cotton sample was observed to have a relatively smooth surface (Figure 3A). Morphological changes such as cracks and grooves and roughening of the surface due to the etching effect of plasma treatment were evident in Plasma I and II treated cotton nonwoven samples. Our results corroborate with the findings of Balu et al.,14 wherein it was reported that plasma treatment selectively removes the amorphous domains, exposing the crystalline cellulose moieties and eventually resulting in roughening of the surface. The amorphous domains that encapsulate the crystalline cellulose moieties are susceptible to the etching effect of plasma. More importantly, Plasma II treatment resulted in a larger number of grooves and cracks compared to Plasma I treatment. This could be attributed to the intensity of Plasma II treatment. The elimination of boundary-layer effects in Plasma II treatment minimizes the possibility of the process gases being displaced by atmospheric air. This eventually translates into increased plasma densities in the case of Plasma II compared to that of Plasma I.31 Hence, 12590
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Figure 3. SEM images of untreated (A), Plasma I treated (B), and Plasma II treated (C−E) cotton nonwoven samples.
Plasma II is more intense and effective compared to Plasma I and has resulted in more surface modifications of treated samples. In addition, because of the improvements in the processing design of the Plasma II systems over Plasma I, it was evident that the gas flow of 10 L/min was optimum enough compared to 40 L/min in Plasma I (Table 3) to have a significant effect on the substrate, which indirectly relates to lower processing costs and energy conservation. Effect of APT on the Physical Properties. Strength is an important property for textiles because it relates to its performance and use. Hence, it is useful to understand the effect of APT on the mechanical properties of cotton nonwovens. The results of strip tests performed to evaluate the effect of APT on the tensile properties of cotton samples are presented in Figures 4 and 5. Figure 4 shows the effect of APT on the breaking load of the samples in machine and cross directions. It was observed that Plasma I has not resulted in a significant decrease in the load at break in the machine direction. However, Plasma II has resulted in a significant decrease in the load at break (p < 0.05) in the machine direction. The presence of a larger number of cracks and grooves in Plasma II treated cotton nonwovens compromises
Figure 4. Tensile strength of cotton nonwovens.
its strength. Such a result is consistent with other studies.32−34 Other reasons for the decrease in the strength of plasma-treated fabrics include stress concentration effect and chain scis12591
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FTIR analyses, respectively. Moreover, other researchers have observed that plasma treatment may increase32 or decrease4 the abrasion resistance of woven bleached cotton fabrics depending on the type of fabric and the nature of the plasma treatment. An increase in the abrasion resistance could be ascribed to the interfiber entanglement and an increase in the fiber-to-fiber friction after plasma treatment, as reported by Siavashani et al. in 2014.35
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CONCLUSIONS We have demonstrated that APT increases the hydrophilicity of cotton nonwovens because of the removal of waxes from cotton fibers. The removal of waxes up to 85% can be achieved depending on the intensity of the plasma treatment. FTIR analysis showed that APT is effective in removing waxes from the surface of individual cotton fibers. However, intense plasma treatments may compromise the strength of cotton nonwovens because they result in cracks and grooves on the surface of individual fibers. The decrease was predominantly observed only in the machine direction. The results show that APT could be used as an environmentally friendly technique in the processing of cotton nonwovens.
Figure 5. Tensile extension of cotton nonwovens.
sion.32−34 No significant effect of plasma treatment on the load at break of the samples was observed in the cross direction. As reported in the literature, in carded and needle-punched nonwoven fabrics, fibers are more aligned in the machine direction than in the cross direction. Therefore, a decrease in the strength of the fiber would be more evident in the machine direction than in the cross direction. The effect of APT on the extension at break of the samples is presented in Figure 5. As is evident from the figure, neither of the treatments had a significant effect on the extension at break of the samples because the plasma treatments were not severe enough to cause changes in the microscopic structural units of the fiber.34 The influence of APT on the abrasion resistance of cotton nonwovens is quantified in terms of percentage loss in weight over a given number of rubs, as summarized in Figure 6. Statistical analysis of abrasion data suggests that only Plasma II treatment results in an increase in the abrasion resistance of cotton nonwovens at 95% confidence interval. This result corroborates with the findings of Sivashani et al. in 2014.35 Abrasion resistance of textile substrates is a surface phenomenon that could be affected by both physical and chemical modifications imparted by a given treatment. In this study, the physical and chemical modifications to cotton nonwoven substrates were depicted by SEM and further substantiated by
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AUTHOR INFORMATION
Corresponding Author
*E-mail:
[email protected]. Author Contributions ‡
Contributed equally to the work.
Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS S.R. gratefully acknowledges The CH Foundation, Lubbock, TX, for funding this study. The authors also thank Dr. Eric Hequet of FBRI, Texas Tech University, for his help with cotton characteristics evaluation.
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REFERENCES
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Figure 6. Abrasion resistance of cotton nonwovens. 12592
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dx.doi.org/10.1021/ie502384g | Ind. Eng. Chem. Res. 2014, 53, 12587−12593
