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Textile Performance of Polyester, Nylon 6 and Acetate Fabrics Treated with Atmospheric Pressure Plasma Jet Transaction

Textile Performance of Polyester, Nylon 6 and Acetate Fabrics Treated with Atmospheric Pressure Plasma Jet Transaction

Transaction

Textile of Polyester, 6 and Acetate Fabrics Treated with Atmospheric Pressure Plasma Jet

Keiko Gotoh ＊1,#, Akiko Katsuura ＊1,AyaHonma＊1, and Yasuyuki Kobayashi ＊2

＊1 Faculty of Human Life and Environment, Nara Women’s University, Nara 630-8506, Japan ＊2 Electronic Materials Research Division, Osaka Municipal Technical Research Institute, Osaka 536-8553, Japan

Abstract: Three synthetic , polyester, nylon 6 and acetate fabrics, were treated by atmospheric pressure plasma (APP) jet with nitrogen gas. From the contact angle measurements using a single , the wettability and the base parameter of surface free energy of the three were found to increase drastically after the APP treatment. X-ray photoelectron spectroscopy and atomic force microscopy showed that the APP exposure increased the concentration and the roughness, respectively, for any fiber surface. It was confirmed from the stress-strain behavior and the visible reflection spectrum that the APP impact damage was negligibly small for any fabric. The increase in hydrophilic nature of the fiber surface resulted in promoting water wicking and soil release by laundering. Moreover, the color strength of the polyester and acetate fabrics dyed with disperse dyestuff was found to increase mainly by the topographical change in the fiber surface. Such improvement of performances by the APP treatment was remarkable for the polyester fabric. (Received 18 March, 2013 ; Accepted 26 July, 2013)

1. Introduction Recently, we have carried out the surface oxidation of synthetic fibers by two dry processes in the atmosphere. In general, synthetic textiles have many advantages Some synthetic textiles were treated by 172 nm ultraviolet of high modulus and strength, stiffness, stretch, wrinkle (UV) excimer light irradiation [21]. As a result, the water and abrasion resistances, relatively low cost, convenient absorbency for any fabric was enhanced because of the processability, tailorable performance and easy recycling increase in single fiber wettability. Such a tendency was [1, 2]. On the other hand, they have low wettability remarkable for polyester, which surface oxygen because of inherently hydrophobicity, which leads to less concentration and roughness much increased due to UV wearing comfort, low color strength, build-up of exposure compared with other synthetic fibers. The color electrostatic charge, the tendency to pilling and strength after and the detergency by laundering insufficient washability [2, 3]. Because of these were also improved after UV irradiation for the polyester disadvantages, surface modification to enhance fabric [22]. Moreover, we have applied atmospheric hydrophilicity has been carried out by conventional pressure plasma (APP) to polyester textile . The chemical modifications [4-7]. The chemical modification APP jet device used has attracted significant attention, can improve textile-specific performance by altering its because they generate plasma plumes in open space, have chemical structure due to a chemical reaction, such as no limitations on the sizes of the objects to be treated and esterification, grafting, and crosslinking. Therefore, large can achieve continuous in-line material processing at high amounts of modifying agents and solvents are required, speed [23-27]. To obtain basic information on resulting in undesired high-cost drying and pollutant- physicochemical properties of the treated surface, the treating steps [4, 7]. As alternative environmentally PET film with geometric simplicity was chosen [28, 29]. friendly technology, dry gas-phase oxidation of synthetic The increases in wettability and surface free energy were fiber surfaces after processing has been recently remarkable for the APP treatment in comparison with the attempted by ultraviolet light [8-13] and plasma [7, 14- UV treatment, which was not in contradiction with the 20] technologies. results characterized by X-ray photoelectron spectroscopy. Using polyester fabric, it was confirmed that the APP jet # corresponding author treatment increased oxygen concentration and roughness

（47） SEN’I GAKKAISHI（報文）Vol.69, No. 9 (2013) 169 of the fiber surface [30] and successfully enhanced the The water was purified (resistivity of 18 MΩcm) water wicking, the detergency and the color strength of using a Direct-Q UV apparatus (Millipore, USA). the fabric [31]. Moreover, it was found that the changes in 2.2 APP and UV exposure polyester fiber surface properties and fabric performances The APP exposure was performed using a plasma due to the APP exposure were dependent on the reactive pretreatment equipment (Plasmatreat GmbH, Germany) gas source used. [30, 31]. consisting of a plasma generator (FG1001), a high- In the present , polyester, nylon 6 and acetate voltage transformer (HTR1001) and a rotating nozzle jet filament fabrics were exposed to the APP with nitrogen (RD1004). The APP was generated by means of a high- gas, which was the most effective for the polyester voltage discharge inside the nozzle jet coupled to the surface modification. The optimum processing parameter stepped high-frequency pulse current power supply was determined from the balance between the fiber (plasma generator) [32]. The operating voltage, current wettability increase and the fabric damage. The fabric and frequency are 285±5V, 6.0±0.1A and 16±3 kHz, performances such as water wicking, detergency by respectively. The reactive gas used was nitrogen, which laundering and color strength after dyeing were evaluated was regulated the pressure and the flow rate to be from the viewpoint of multi-functionalized textiles. The 0.3 MPa and 20 l/min, respectively. The plasma nozzle jet changes in fiber surface characteristics and fabric of 40 mm in diameter was set vertically and a piece of performances were compared among the fabrics. fabric was horizontally placed from the nozzle at a separation distance of 3-7 mm. During the exposure, the 2. Experimental fabric was moved in the horizontal direction at 0.16 m/sec 2.1 Materials (exposure time : 0.25 s), which were chosen as the Three plain-woven fabrics composed of filament uniformly treatable velocity with references to the were used for the experiment. Polyester and nylon 6 experimental results in the previous [28]. Both fabrics (JIS Test Fabric) were purchased from Japanese sides of the polyester fabric were exposed to the APP. Standard Association, and acetate fabric from Shikisensha To compare with the APP treatment, the fabrics were Co., Ltd, Japan. The fabrics were purified in boiled water exposed to UV excimer light using a UV excimer lamp at twice prior to use. a wavelength of 172 nm in ambient air using a Xe2 Water, diiodomethane, glycol and n- excimer vacuum UV apparatus (UER20-172, Ushio, pentane were used for the contact angle measurement. Japan). The intensity of the UV excimer light at the upper

As model soils, we used black (SEAST SP, SiO2 glass window of the lamp house, on which the fabric Tokai Carbon Co. Ltd., Japan) and oleic acid. Sudan Ⅲ was placed, was determined to be 15.8 mW/cm2 using an (oily-soluble , CI 26100, Wako Pure Chemical UV monitor system (UIT-150 and VUV-S172, Ushio). Industries, Ltd., Japan)was chosen as a tracer of oleic acid. Both sides of the fabric were exposed to UV for 60 s [33]. Sodium dodecyl sulfate (SDS, Wako Pure Chemical 2.3 Evaluation of contact angle and surface free Industries, Ltd., Japan) and sodium chloride were used for energy preparation of the detergent solution. The advancing and receding contact angles of water Disperse for polyester, Sumikaron Yellow SE- on the fiber surface were determined by the wetting force 4G and Sumikaron Brilliant Violet SE-BL (Sumika measurement employing the Wilhelmy method [30, 34]. Chemtex Co., Ltd, Japan), acid dyes for nylon, Kiwacid G. A single fiber of 10 mm in length, which was taken from Yellow 4RL-N and Kiwacid Blue GL-N (Kiwa Chemtex the warp of the fabric, was suspended from the arm Co., Ltd, Japan), and disperse dyes for acetate, Kiwalon of the electrobalance (Model C-2000, Cahn Instruments Polyester Yellow DR and Kiwalon Polyester Blue DR-G Inc., USA). Just below the fiber, a glass vessel containing 150 (Kiwa Co., Ltd. Japan), were used. water was placed on the stage connected to a stepping As dispersing agents, Smipon SE (Sumika Chemtex Co., motor (MP-20L, MICOS, Germany). A continuous Ltd, Japan), Newbon TS-400 and Nicca Sansalt 1200K weight recording was made during an immersion- (Nicca Chemical Co., Ltd, Japan) were chosen. The pH of withdrawal cycle at an interfacial moving velocity of dye bath was adjusted with acetic acid and sodium acetate. 0.3 mm/min [35]. As after-treatment agents, Laccol ISF-2 (Meisei Chemical The weight recording for a treated single fiber Works, Ltd, Japan), Sunlife E-37 (Nicca Chemical Co., showed periodic variation along the fiber axis, indicating Ltd, Japan), and sodium hydrosulfate that the fiber surfaces were not treated uniformly because were used. of fiber crimps due to the structure of the fibrous

170 SEN’I GAKKAISHI（報文）Vol.69, No. 9 (2013) （48） assembly [30]. Therefore, the minimum advancing and 2.6 Evaluation of water wicking receding contact angles were obtained from the advancing The wicking rate, the movement of water in the and receding wetting forces, respectively, using the capillaries of a fabric, was evaluated by two methods on Wilhelmy equation. referring to JIS L1907 [40]. The contact angles of diiodomethane and ethylene A water drop was placed on the fabric (50 × 50 mm2) glycol were also measured for the estimation of the and photographs were taken at given times until 60 sec. surface free energy of the fiber. The Lifshitz-van der The spreading area on the fabric was determined by Waals and the Lewis acid-base and components were binary processing using 2D image analysis software calculated from the advancing contact angles of water, (WinRoof Ver. 6.3.1, Mitani Corporation, Japan). The diiodomethane and and their referential photograph of the fabric was converted from an original surface free energy components [36] using the van Oss- gray-scale digital image with 256 possible intensity Chaudhury-Good equation [37]. values to a binary image using a suitable threshold level, Contact angle measurements were carried out in a from which the spreading area was obtained. room maintained at 20℃ and 65%RH. The fabric strip with 25 mm width and 200 mm 2.4 Surface analyses length was hung vertically and its lower end was dipped X-ray photoelectron spectroscopy (XPS) was into water. The height of water penetrated into the fabric performed using an Axis-Ultra DLD spectrometer (Kratos, due to capillary rise was measured as a function of time

UK) fitted with a monochromatic Al Kα radiation at until 10 min. 1486.7 eV (120W) X-ray source. Survey spectra and Measurements were carried out in a room high-resolution spectra of the core levels of C1s, O1s and maintained at 20℃ and 65%RH. N1s were acquired with a pass energy of 80 and 20 eV, 2.7 Evaluation of detergency respectively, and a slot aperture of 0.3 × 0.7 mm2. Spectra As a soil bath, 0.1 dm3 ethanol containing 0.03 g were collected at a photoelectron take-off angle of 90 carbon black or 5 g oleic acid/0.02 g Sudan Ⅲ mixture degrees. All XPS binding energies were referenced to the was ultrasonically prepared [41]. Then, a piece of fabric C1s peak of adventitious carbon at a binding energy of (50 × 50 mm2) was immersed in each soil bath for 3 min 284.8 eV. with applying ultrasound. After soiling, the fabric was The atomic force microscopy (AFM) observations dried and aged in a refrigerator for 7 days prior to the were carried out using a Nanoscope IIIa (Digital washing. Instruments, USA) in a tapping mode. The surface The Kubelka-Munk function values, K/S, of the roughness parameters, root mean square roughness, Rms, soiled and unsoiled fabrics were determined by the average roughness, Ra, and maximum roughness depth, surface reflectance measurement as mentioned in 2.5.

Rmax, were determined from the images obtained in a 1×1 Each side of the fabric was read in two different spots and μm2 area. the average surface reflectance of those four readings was 2.5 Evaluation of fabric damage noted as the final value, from which the K/S was The APP impact damage to the fabrics was checked calculated. The wavelengths used were 460 nm and 500 by the stress-strain behavior and the surface reflectance. nm for the fabrics soiled with carbon black and oleic acid, Tensile strength and breaking extension of the warp and respectively. weft yarns taken from the fabric were determined using The washing test was carried out immediately after an autograph (AG-1, Shimadzu, Japan) in accordance measuring the surface reflectance of the fabrics. Soiled with JIS L1095 [38]. The gauge length was 250 mm and and unsoiled fabrics were stacked with the soiled fabric the extension speed was 300 mm/min. on top and placed horizontally in a beaker containing an The visible reflection spectrum of the fabric surface aqueous detergent solution of 8 mmol/dm3 SDS (~critical was obtained using a spectrophotometer (NF333, micelle concentration) and 1 mmol/dm3 NaCl with bath NIPPON DENSHOKU, Japan), stacking the same kinds ratio of 30. of fabric in fours. According to the CIE L* a* b* *system As a source of mechanical action for soil removal,

[39], the total color difference, ΔE*ab, between the frequency modulated ultrasound (38 kHz, 120 W) was untreated and treated fabrics was obtained. applied using an ultrasonic cleaner system (64106 Measurements were carried out in a room oscillator and 64801VS washing bath, KAIJO, Japan). maintained at 20℃ and 65%RH. [42]. The wash time and temperature were 5 min and 25℃, respectively. After washing, the soiled and the

（49） SEN’I GAKKAISHI（報文）Vol.69, No. 9 (2013) 171 unsoiled fabrics were rinsed for 60 s with 0.1 dm3 water 10 min. and dried. The K/S values of the soiled and unsoiled After rinsing thoroughly and drying of the dyed fabrics were measured again. fabric, the surface reflectance of the dyed fabric in the The soil removal was calculated from the K/S of the visible wavelength region was measured as mentioned in soiled and unsoiled fabrics before washing and the K/S of 2.5, from which the K/S at maximum absorption the soiled fabric after washing [41] : wavelength and the total color difference, ΔE* ab, between the untreated and treated fabrics after dyeing were (1) obtained.

Where the subscripts s and w refer to the soiled fabrics 3. Results and Discussion before and after washing, respectively, and the subscripts o refer to the unsoiled fabrics before washing. 3.1 APP exposure condition As a measure of the soil redeposition, the change in Fig. 1 shows advancing and receding contact angles K/S of an unsoiled fabric due to washing was used [41]. of water on the fibers immediately after the APP Because the soil redeposition is dependent on the amount treatment as a function of the distance from the nozzle jet of soil removed from the fabric in the wash bath, the soil to the fabric, D. For all fibers, both contact angles were redeposition was calculated by the following equation dependent on D, and the minimum contact angle, the [43] : maximum wettability, was obtained at D = 5 mm. In the previous paper [44], similar results were obtained for the (2) poly (ethylene terephthalate) film that was cut off to a fine strip. The PET film was often deformed for D<5 mm Where ow refer to the unsoiled fabrics after washing because of partial melting at high temperature. The and the term [(K/S) S - (K/S) W] is corresponding to the temperature of plasma jet was determined to be 100℃ at soil amount removed from the soiled fabric. D = 5 mm, and hence the fiber surface was considerably 2.8 Evaluation of color strength heated during plasma treatment. Therefore, the results in The polyester fabric (50 × 50 mm2) was immersed in Fig. 1 was caused by the balance between plasma-surface a0.1dm3 aqueous solution containing 20% owf disperse reaction and heat damage such as partial melting with dye and 1 g/dm3 Smipon SE. The dye solution was heated respect to the APP exposure distance. in a commercial pressure cooker to boiling after 30 min. The angles were also dependent on the treatment The solution was still boiled for 60 min and allowed to cycle, N, at D = 5 mm. The angle considerably decreased cool for 30 min. After dyeing, the fabric was rinsed and from N = 2 to N = 4, but little change was observed from was immersed in a 0.1dm3 aqueous solution containing N = 4 to N = 8. Therefore, the APP treatment in this study 1g/dm3 Laccol ISF-2, 0.5 g/dm3 sodium hydroxide and was performed under the optimum exposure condition, 1g/dm3 sodium hydrosulfate at 80℃ for 15 min. D=5mmandN=4. The nylon 6 fabric (50 × 50 mm2) was immersed in a 0.025 dm3 aqueous solution containing 15% owf acid dye, 1g/dm3 Newbon TS-400, 0.9 ml/dm3 glacial acetic acid and 0.5 g/dm3 sodium acetate. The dye solution was heated and was boiled for 40 min (after 20 min-boiling, 1 ml/dm3 glacial acetic acid was added). After the dyeing, the fabric was rinsed and was immersed in 0.025 dm3 solution containing 5% owf Sunlife E-37 at 85℃ for 30 min. The acetate fabric (50 × 50 mm2) was immersed in a 0.05 dm3 aqueous solution containing 15% owf disperse Fig. 1 The effect of the distance from the nozzle to the fabric, D, on the advancing (closed symbols) dye, 0.5 g/dm3 Nicca Sansalt 1200K and 0.2 ml/dm3 and receding (open symbols) contact angles of glacial acetic acid. The dye solution was heated and was water on the polyester, nylon 6 and acetate kept at 90℃ for 30 min. After the dyeing, the fabric was fibers immediately after the APP treatment rinsed and immersed for 10 min in a 0.05 dm3 aqueous (treatment cycles, N= 2 (triangles), 4 (circles) solution containing 1 g/dm3 Laccol ISF-2 at 70℃ for and 8 (squares).

172 SEN’I GAKKAISHI（報文）Vol.69, No. 9 (2013) （50） 3.2 Single fiber wettability increased, especially for the polyester fiber, which was corresponding to the wettability increase of the fiber surface in Fig. 2.

Table 1 Total surface free energy, γT, and its component (Lifshitz-van der Waals component, γLW, Lewis acid parameter, γ+, and Lewis base parameter, γ−) for untreated and APP-treated polyester, nylon 6 and acetate fibers.

Fig. 2 Advancing and receding contact angles of water on the polyester, nylon 6 and acetate fibers untreated and treated with APP (without and with aging) and UV (with aging). The advancing and receding contact angles of water on the fiber before and immediately after the APP treatment (without aging) are given in Fig. 2. It was clear that both angles drastically decreased due to the APP treatment, especially for the polyester fiber. It was observed that the water contact angles on the APP-treated fibers slightly increased during the storage in air until 1 week. This is called hydrophobic recovery, due to the surface rearrangement of hydrophilic via reorientation and migration [45-49]. The contact angles on the UV-treated fibers after 1 week aging are also presented in Fig. 2, together with the APP-treated fibers. At least within the limits of the experimental conditions in the present study, the APP treatment can enhance fiber wettability in comparison with the UV treatment for any fiber. The differences in the receding angles among the Fig. 3 Surface atomic concentrations obtained from fiber species, between with and without aging and XPS spectra for untreated and APP-treated between APP and UV treatments were small compared polyester, nylon 6 and acetate fibers. with the advancing angles. According to the theoretical calculation of the advancing and receding contact angles Surface elemental composition obtained from XPS on the model heterogeneous surfaces with low- and high- spectra for the untreated and APP-treated fibers is shown energy regions [50], the advancing contact angle is in Fig. 3. After the APP-treatment, nitrogen concentration strongly dependent on the proportion of the high-energy slightly increased and oxygen concentration considerably region and the receding angle is insensitive to high- increased for any fiber. The XPS results indicate that energy region for predominately high-energy surfaces oxygen atoms rather than nitrogen atoms were such as the APP- and UV-treated PET surfaces. The incorporated into the fiber surface by the APP treatment experimental data in Fig. 2 are consistent with the above with nitrogen as reactive gas. This suggests that the calculation. activation mechanism for the APP jet is not only plasma- In the present study, the APP-treated sample was surface reaction but also post-plasma processes, diffusion aged for a week prior to the measurements. of oxygen or water vapor into the plasma jet and 3.3 Physicochemical properties of fiber surface subsequent incorporation into the surface [51]. Table 1 gives the total surface free energy and its The introduction of the functional groups with hydrogen Lifshitz-van der Waals and Lewis acid-base components. bonding ability to the fiber surface by the APP treatment After the APP treatment, the acid (electron-acceptor) will increase the base, electron-donor, parameter of the parameter and the base (electron-donor) parameter surface free energy as shown in Table 1 and Fig. 3.

（51） SEN’I GAKKAISHI（報文）Vol.69, No. 9 (2013) 173 Fig. 4 demonstrates the AFM images and the The results of tensile test are presented in Fig. 5. The roughness parameters for the untreated and APP-treated changes in tensile strength and breaking extension of the fibers. The topographical change in the fiber surface due warp and weft yarns due to the APP treatment have little to the APP exposure was observed, which may be caused statistical meaning, because their experimental errors by the ablative interaction of APP with polymer surfaces. were ±5-10%. These results show that the APP impact Especially for the polyester fiber, the surface roughness damage to the fabric is negligibly small. parameters increased by a factor of about 5 after the APP 3.5 Fabric performances treatment. The spreading area and the wicking height of water penetrated into the untreated and APP-treated fabrics are shown in Fig. 6 as a function of time. For each fabric, the water wicking rate increased after the APP treatment. Comparing the results in Fig. 6 with those in Fig. 2, it was found that the increase in wettability of the fiber surface due to the APP exposure promoted water wicking into the fibrous assembly.

Fig. 6 Changes in spreading area and wicking height of water penetrated into the untreated (open symbols) and APP-treated (closed symbols) polyester (circles), nylon 6 (triangles) and acetate (squares) fabrics.

Fig. 7 shows the effect of the APP treatment on soil removal and redeposition. For carbon black, the removal Fig. 4 AFM images and the surface roughness from the polyester and nylon 6 fabrics was promoted and parameters for untreated and APP-treated the redeposition onto these fabrics was prevented by the polyester, nylon 6 and acetate fibers. APP treatment. However, such detergency improvement 3.4 Fabric damage was not observed for the acetate fabric. In the of

The total color difference, ΔE*ab, between the oleic acid, the soil removal from any fabric was promoted untreated and APP-treated fabrics was 0.3-0.5, by the APP treatment. In general, the increase in the corresponding to “Trace” for all fabrics. surface free energy of the substrate can promote the soil release and prevent the soil redeposition via. the decrease in the work of adhesion [52]. Therefore, the hydrophilization of the fiber surface by APP treatment can improve the detergency of synthetic textiles in aqueous solutions [43], overcoming the disadvantage for removing soil by the surface roughness increase in Fig. 4. The K/S values at the maximum absorption wavelength of the untreated and APP-treated fabrics after dyeing are presented in Fig. 8. For polyester and acetate fabrics, the considerable increase in K/S due to the APP Fig. 5 Tensile strength and breaking extension for treatment was observed and the total color difference, untreated and APP-treated polyester, nylon 6 ΔE*ab, between the untreated and APP-treated fabrics and acetate yarns. after dyeing was calculated to be 4-11, corresponding to

174 SEN’I GAKKAISHI（報文）Vol.69, No. 9 (2013) （52） with nitrogen gas. The wettability, the surface free energy, the atomic oxygen concentration and the roughness of each single fiber surface considerably increased after the APP treatment, especially for polyester. The enhancement in hydrophilicity of the fiber surfaces due to incorporation of oxygen atoms resulted in the increments of the water wicking and the detergency of the fabrics. Moreover, the increase in roughness due to ablative interaction of APP with the polyester and acetate fiber surfaces resulted in the deep coloring of their fabrics after dyeing. The Fig. 7 Soil removal and redeposition of carbon black experimental findings obtained in this study will give and oleic acid by laundering for untreated and fundamental information of the plasma processing for APP-treated polyester, nylon 6 and acetate fabrics. synthetic textile materials.

Acknowledgements

We wish to express our gratitude to Sumika Chemtex Co., Ltd., Kiwa Chemtex Co., Ltd, Nicca Chemical Co., Ltd and Meisei Chemical Works, Ltd. for providing chemicals for dyeing. Gratitude is expressed to the Ministry of Education, Sports, Culture, Science and Technology, Japan for a Grant-in-Aid for Scientific Research to carry out this work.

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