PET非织造布等离子改性及抗菌性能研究

采用低温氧等离子体处理聚对苯二甲酸乙二酯(PET)非织造布接枝丙烯酸(AA)后,再接枝壳聚糖,探讨了氧等离子体参数对接枝AA后PET亲水性的影响,以及接枝壳聚糖后其PET非织造布抗菌性能的变化。结果表明:低温氧等离子体处理PET非织造布后,其纤维表面粗糙度增加,接枝AA后PET亲水性提高。低温氧等离子体处理PET非织造布接枝AA改性的最佳条件为:工作压强30 Pa,放电功率40 W,处理时间2 min。接枝壳聚糖后,PET非织造布具有抑菌性能,对大肠杆菌和金黄色葡萄球菌有明显的抑菌效果。     

Functional finishing by using atmospheric pressure plasma: Grafting of PET nonwoven fabric

Poly (ethylene terephtalate) (PET) nonwoven fabric was treated with He/O₂ plasma to produce peroxides and grafted with acrylic acid (AA) for introducing carboxyl groups onto PET surface. The graft yield increased with AA concentration from 1.5M to 2.5M, and then decreased with further increase in AA concentration. Graft yield increased with sodium pyrosulfite (SPS) concentration from 0.005M to 0.02M, and then decreased with further increase of SPS concentration. X‐ray photoelectron spectroscopy results indicated that both of plasma treatment and AA grafting increased oxygen content and decreased carbon content on the PET nonwoven fabric surface. The grafted PET nonwoven fabric showed increase in moisture regain and dye uptake. And drastic increase in wettability was observed after grafting. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3655–3659, 2007     

Functional finishing of nonwoven fabrics. I. Accessibility of surface modified PET spunbond by atmospheric pressure He/O2 plasma treatment

The surface of a polyethylene terephthalate (PET) spunbond nonwoven was modified by using atmospheric pressure He/O₂ plasma treatment. Accessibility of the modified PET nonwoven has been investigated in terms of crystallinity, surface chemical composition, hydrophilicity, and dye uptake. Differential scanning calorimetry (DSC) for crystallinity measurement and X‐ray photoelectron spectroscopy (XPS) for chemical composition measurement were used. Surface morphology was studied by using scanning electron microscopy (SEM) and atomic force microscopy (AFM). Percentage crystallinity increased due to the depletion of amorphous region by plasma etching. Redeposition of etched particles was observed. Oxygen‐based functional groups on the surface of PET increase from 27 to about 32% after 90 s exposure. Wettability increases by more than 10 times and moisture regain increases by three times, compared with the untreated sample. Dye uptake was not changed significantly. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 4306–4310, 2006     

Surface grafting polymerization of N‐vinyl‐2‐pyrrolidone onto a poly(ethylene terephthalate) nonwoven by plasma pretreatment and its antibacterial activities

The objective of this research was the surface grafting polymerization of biocompatible monomer N‐vinyl‐2‐pyrrolidone (NVP) onto a plasma‐treated nonwoven poly(ethylene terephthalate) (PET) substrate with ultraviolet (UV)‐induced methods. The effects of various parameters, such as the monomer concentration, reaction time, initiator (ammonium peroxodisulfate) concentration, and crosslinking agent (N,N′‐methylene bisacrylamide) concentration, on the grafting percentage were studied. The grafting efficiency of the modified nonwoven PET surfaces reached a maximum at 50 min of UV irradiation and with a 30 wt % aqueous NVP solution. After the plasma activation and/or grafting, the hydrophobic surface of the nonwoven was modified into a hydrophilic surface. NVP was successfully grafted onto nonwoven PET surfaces. The surface wettability showed that the water absorption of NVP‐grafted nonwoven PET (NVP‐g‐nonwoven PET) increased with increasing grafting time. NVP‐g‐nonwoven PET was verified by Fourier transform infrared spectra and scanning electron microscopy measurements. An antibacterial assessment using an anti‐Staphylococcus aureus test indicated that S. aureus was restrained from growing in NVP‐g‐nonwoven PET. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 803–809, 2006     

氩气等离子体处理对丙纶隔膜力学性能的影响

研究了应用氩气等离子体表面改性技术对丙纶非织造织物进行处理的技术,探讨了处理时放电功率、放电时间、反应压力等对丙纶非织造织物的力学性能的影响。结果表明,通过氩气等离子体表面活化处理,虽然会对无纺丙纶非织造物的力学性能造成影响,但是不会影响丙纶非织造物的使用。     

Graft polymerization of acrylic acid onto polyphenylene sulfide nonwoven initiated by low temperature plasma

Graft copolymerization of acrylic acid (AA) onto polyphenylene sulfide (PPS) nonwoven initiated by low temperature plasma was studied. The effects of various conditions on graft reaction and the grafting rate were investigated. SEM images showed that PPS nonwoven was grafted, and the graft copolymerization only occurred on the surface of PPS. It may be due to the chain transference going with the graft copolymerization. It was found that with the increasing of plasma power, treatment time, space between electrodes, monomer concentration, and temperature of graft polymerization, the grafting rate increased at first, went to the top, and then decreased. The PPS nonwoven surface graft reaction could be optimized by the following processing conditions: 120 s of plasma treatment time, 50 W of plasma power, 1.5 cm of space between electrodes, 30% (w/w) of monomer concentration, and 50°C of temperature of graft polymerization. Measurement of XPS showed that the peak of C1s of graft polyacrylic acid was existed, and the peak area increased with the increase of the grafting rate. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5884–5889, 2006     

Surface modification of polyester films by RF plasma

Plasma treatment of PET films was carried out under argon, followed by exposure to an oxygen atmosphere. The films underwent considerable changes in surface composition and morphology, as demonstrated by contact angle measurements, FTIR‐ATR, AFM, and XPS. It was found that the surface acquired oxygen containing polar functional groups such as —C=O, —OH, and —OOH, which increased in number as the plasma treatment time increased. During storage, the treated films underwent significant surface reorganization, and both the time and temperature contributed to the increase in the contact angle. As revealed by AFM measurements, these changes were accompanied by an increase in roughness in the form of ridges. The ridges were observed to grow in height with increasing treatment time, although their spacing showed little evolution. A correlation among the observations obtained from various techniques was established, giving a comprehensive picture of the structure and dynamics of plasma‐treated PET surfaces. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 1083–1091, 2000     

Surface modification of polyester and polyamide fabrics by low frequency plasma polymerization of acrylic acid

In this study, the surface characteristics of polyester and polyamide fabrics were changed by plasma polymerization technique utilizing acrylic acid as precursor. This monomer was used to produce hydrophilic materials with extended absorbency. The hydrophilicity, total wrinkle recovery angle (WRA°) and breaking strength of the fabrics were determined prior and after plasma polymerization treatment. The modification of surfaces was carried out at low pressure (<100 Pa) and low temperature (<50°C) plasma conditions. The effects of exposure time and discharge power parameters were optimized by comparing properties of the fabrics before and after plasma polymerization treatments. It was shown that two sides of polyester fabric samples were treated equally and homogeneously in plasma reactor. For polyester fabrics, the minimum wetting time, 0.5 s, was observed at two plasma processing parameters of 10 W–45 min and 10 W–20 min, where untreated fabric has a wetting time of 6 s. For polyester fabrics, the maximum value was obtained at 60 W–5 min with the wrinkle recovery angle of 306° where the untreated fabric has 290°. The optimum plasma conditions for polyamide fabrics were determined as 30 W–45 min where 2 s wetting time was observed. Wrinkle recovery angle of untreated polyamide fabric was 264°. In this study, after plasma polymerization of acrylic acid, wrinkle recovery angle values were increased by 13%. No significant change was observed in breaking strength of both fabrics after plasma treatment. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 2318–2322, 2007     

Facile fabrication of polyester filament fabric with highly and durable hydrophilic surface by microwave‐assisted glycolysis

Poly(ethylene terephthalate) (PET) fabric with highly and durable hydrophilic surface was fabricated using microwave‐assisted glycolysis. Sodium hydroxide (NaOH) as a catalyst was proven to be suitable for PET glycolysis under assistance of microwave. The modified PET fabric (0.5% NaOH, irradiation 120 s) showed high surface hydrophilicity with a contact angle of 17.4 ° and a wicking length of 19.36 mm. The exposure of the carboxyl‐ and hydroxyl‐end groups on the surface of PET and the introduction of etches were confirmed by Methylene Blue staining and field emission scanning electron microscopy (FESEM), receptively. Although the strength of PET fabric decreased after modification, it was still high enough for textile applications. The thermal properties of the modified PET fabrics were well maintained. The high hydrophilicity and its original properties of PET could be controlled by changing the irradiation time from 60 s to 120 s and adjusting the content of sodium hydroxide from 0.2% to 0.5%. These results suggest microwave‐assisted glycolysis with sodium hydroxide is an effective method for PET hydrophilic finishing. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44069.     

低温等离子体引发丙烯酸在PET纳米纤维膜上的接枝聚合

介绍了低温等离子体引发丙烯酸（AA）表面接枝聚合对聚苯二甲酸乙二醇酯（PET）纳米纤维薄膜的改性研究。实验探索了放电时间和放电功率对薄膜润湿性的影响,在真空度60 Pa、AA气体流量3 L/min条件下,放电功率75～150 W范围内,放电时间60 s和放电功率150 W、放电时间30~60 s范围内,处理后薄膜的水接触角均为0°,结果说明了此改性PET纳米纤维膜具有超亲水性。通过扫描电镜、红外和力学性能等测试讨论了接枝处理前后薄膜的形态及性能的变化。实验结果表明气相低温等离子体接枝处理后,薄膜的断裂伸长率和断裂强度有一定的增强。低温等离子体引发AA表面接枝PET纳米纤维薄膜的方法有望成为电纺PET纤维膜表面改性的有效手段,具有积极的应用价值。     

Analysis of the Effects of Atmospheric Helium Plasma Treatment on the Surface Structure of Jute Fibres and Resulting Composite Properties

This work investigates the mechanisms involved in the improvement of flexural properties of a jute/polyester composite when the reinforcement material has been atmospherically plasma treated using helium gas. All composites were laid-up by hand and cured using a Quickstep? cure cycle. Surface characterization techniques including scanning probe microscopy (SPM), and surface wettability combined with fabric tensile strength, composite flexural strength and composite Mode-I properties have been used to quantify the effects of plasma modification. Flexural strength and modulus increased with plasma treatment time, reaching a maximum at 25 passes before decreasing. SPM topographical analysis showed that roughness of the fibre decreased as the plasma treatment time increased until 25 passes after which the roughness was found to increase again. The coefficient of friction increased rapidly after only a short plasma treatment time (5 passes) whilst wettability continued to increase until 25 passes after which it remained constant. The fabric tensile strength followed the same trend as the flexural properties of the composites. Decreasing fibre surface roughness is postulated as a reason for decreasing Mode-I interlaminar fracture toughness properties of the composites.     

等离子体诱导PET纤维接枝丙烯酸的研究

利用低温等离子体技术对PET织物在氧气下经等离子处理后生成过氧化物,然后接枝丙烯酸进行研究。通过改变低温等离子体各种处理条件来研究其接枝后织物的吸水性、润湿性等性能变化。随着放电功率的增加、放电时间的延长,PET织物的吸液高度呈现先增大后减小的趋势;随着放电功率的增加,PET织物与去离子水接触角呈现先减小后增大的趋势;随着等离子体放电时间的增加,PET织物与去离子水的接触角迅速减小,然后趋于稳定。经过处理后试样的吸湿率、吸液高度和回潮率均随接枝率的增加而增加,染色性能提高。     

超疏水PET织物的制备及其抗菌性能

纺织物表面的超疏水特性将赋予其优异的自清洁性能。以PET无纺布为基材,探索了利用溶胶-凝胶法在预处理后的PET织物表面构筑具有微纳结构的超疏水涂层的方法;并利用扫描电镜（SEM）、接触角测量仪表征了改性PET织物表面的微观结构和润湿性。进一步地,分别以大肠杆菌和金黄色葡萄球菌为试验菌株,通过细菌转移法和抑菌圈法评价与分析了改性PET织物表面的抗菌性能。研究表明：利用改进的Stöber溶胶-凝胶过程能够在经碱减量法预处理的PET表面原位形成SiO₂纳米粒子;再用含疏水性长链的十二烷基硅烷对这一表面进行改性,并经过表面热处理,就能够成功地在PET织物表面构筑多层次的微/纳结构,从而制得表面具有超疏水特性的PET织物,其接触角可达到163°。这一超疏水PET织物能够抑制细菌在其表面的生长繁殖,表现出了明显的抗菌特性。     

Surface modification of polyester nonwoven fabrics by Al2O3 sol–gel coating

Nonwoven polyester (PET) fabrics have been extensively studied for various applications. However, the nonwoven PET fabrics have poor wettability. In this work, nonwoven PET fabrics were impregnated in a stable and transparent alumina sol that was prepared by the hydrolysis of aluminium isopropoxide using the sol–gel technique. The Al₂O₃ particles were coated on nonwoven PET fabrics after the rolling-drying process. The surface morphology of modified nonwoven PET fabrics was characterized by scanning electronic microscopy (SEM) and atomic force microscopy (AFM). The SEM and AFM observations revealed the formation of the Al₂O₃ particles on the fiber surface. The Al₂O₃ coating was also confirmed by Fourier transform infrared (FTIR). The mechanical properties of the coated nonwoven PET fabrics were investigated using a tensile strength test, and the results showed that the mechanical properties were improved after surface sol–gel coating. The effect of Al₂O₃ on the wetting behavior of the fabric was also significantly improved.     

Surface composition of carbon fibers subjected to oxidation in nitric acid followed by oxygen plasma

Type II, PAN-based carbon fibers (unsized and commercially treated) have been exposed to nitric acid and oxygen plasma individually and also to combined nitric acid/oxygen plasma treatments and the surface compositions have been determined using angle-resolved X-ray photoelectron spectroscopy (ARXPS) and ion scattering spectroscopy (ISS). Most of the oxygen on the as-received carbon fibers resides within the outermost 10-15 Å of the surface. Fiber exposure to nitric acid at 115°C for 20-90 min enhances the oxygen surface concentration to a point of saturation and the oxygen depth distribution is increased and becomes more uniform within the maximum XPS sampling depth (~60-100 Å). In addition, the fiber surface area is believed to be increased. After treating fibers to various degrees in nitric acid, subsequent exposure to oxygen plasma yields an additional increase in the surface oxygen content, particularly in the outermost fiber layers (10-15 Å). Under the conditions of the investigation, the maximum amount of surface oxidation occurs after sequential fiber exposure to nitric acid at 25°C for 30 s and oxygen plasma. As the extent of initial nitric acid treatment is increased, the synergism with subsequent plasma oxidation decreases, and the oxygen concentration becomes more uniform within the outer layers of the oxidized fibers. Overall, the data are consistent with a proposed oxidation mechanism in which oxygen plasma acts to enhance the surface density of oxygen on roughened and pitted nitric acid-oxidized fiber surfaces. As the duration of nitric acid exposure is increased, it is hypothesized that subsequent exposure to oxygen plasma smoothes the fiber surfaces but the surface density of oxygen remains essentially constant.     

Effect of supercritical carbon dioxide dyeing conditions on the chemical and morphological changes of poly(ethylene terephthalate) fibers

Commercially available regular denier poly(ethylene terephthalate) (PET) fabrics were used in this investigation. PET fabric samples were wound on a bobbin and then exposed to supercritical CO₂ under conditions representing a typical supercritical CO₂ dyeing cycle. Infrared spectroscopy, X‐ray diffraction, differential scanning calorimetry, and scanning electron microscopy were used to characterize the chemical and morphological changes of the PET fibers. The results showed that exposure to supercritical CO₂ did not cause chemical changes in the fibers; the crystal size and the T_mp of the PET fabric after treatment in supercritical CO₂ did not significantly change; the crystallinity decreased; and the treatment in supercritical CO₂ at higher temperature caused surface morphology changes (increased oligomer migration). However, there was no pitting, cracking, or crazing on the surface of the treated fibers. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 2008–2012, 2004     

Antimicrobial polyethylene terephthalate (PET) treated with an aromatic N‐halamine precursor,m‐aramid

A commercial m‐aramid as N‐halamine precursor has been coated onto polyethylene terephthalate (PET) fabric surface by pad‐dry‐curing process. The process is accomplished by padding the scoured PET fabric through the homogeneous m‐aramid solution, drying at 150°C for 3 min, and curing at 230°C for 3 min. The PET surface coated with m‐aramid was characterized using fourier transform infrared‐attenuated total reflection (FTIR‐ATR) spectroscopy, X‐ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). FTIR exhibits new bands in the 1645 and 1524 cm^?1 regions as characteristic of m‐aramid bands, which indicate the PET fabric coated with m‐aramid. XPS results show a distinguishable peak at binding energy 398.7 eV, which confirms the nitrogen atom of m‐aramid on the PET surface. In addition, SEM image shows a layer of coating onto the PET surfaces, which demonstrates the presence of m‐aramid coating on the surface of the PET. After exposure to dilute sodium hypochlorite solution, exhibition of antimicrobial activity on the coated PET is attributed to the conversion of N‐halamine moieties from the N‐halamine precursor. The chlorinated PET showed high antimicrobial activity against Gram‐negative and Gram‐positive bacteria. The chlorinated PET coated with 10% m‐aramid exhibited about 6 log reductions of S. aureus and E. coli O157:H7 at a contact time of 10 and 30 min, respectively. Furthermore, the antimicrobial activity was durable and rechargeable after 25 wash cycles. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

聚酯织物碱处理在粘接中的作用及机理

本文研究了聚酯织物和氟硅橡胶粘接过程中 ,碱处理对提高聚酯织物粘接性能的影响。并通过XPS ,SEM等表面分析 ,探讨了碱处理提高粘接性能的原因。研究表明 ,碱处理引起的纤维表面水解和对纤维的清洗作用是提高粘接的主要原因     

Plasma surface modification of poly(m-aramide) fabric for adhesion improvement to fluorosilicone rubber

Poly(m-phenylene isophthalamide) fabric is important as a reinforcement for highperformance rubber diaphragms, such as fluorosilicone diaphragms. Because of their low affinities for each other, it is difficult to develop a good adhesion bond between poly(m-aramide) fiber and fluorosilicone rubber. The present study demonstrates that the bond strength between a poly(maramide) fabric and fluorosilicone rubber can be improved through N₂ plasma treatment of the fabric in combination with a silane coupling agent. The effectiveness of the treatment is dependent on the gas species, the plasma input power, and the time of exposure. The chemical changes in the fabric surface were studied by X-ray photoelectron spectroscopy (XPS). It turned out that free radicals were formed on the surface after the N₂ plasma treatment, which enabled the bonding of the coupling agent to the fabric surface.     

In-situ synthesis of silica aerogel in polyethylene terephthalate fibre nonwovens and their composite properties on acoustical absorption behavior

In this research work we focus on engineering the silica aerogel/polyethylene terephthalate (PET) fibre nonwoven fabric composites with various silica content during in-situ synthesis of silica aerogels in the nonwovens and their composite properties on sound absorption. The silica content was varied by varying the molar ratio of methanol (MeOH)/tetraethyl orthosilicate (TEOS) from 110 to 28. The gelation of silica alcogel took place inside the fabric followed by silylation and atmospheric pressure drying. The aerogel/PET nonwoven composites were characterized by FTIR, TGA and contact angle to explain the aerogel content and its behavior. Moreover, the physical properties such as thickness, bulk density, specific airflow resistance, and mean flow pore size have been investigated. The two microphone transfer function method was used to test the sound absorption coefficient (SAC) of aerogel composites at 1/3rd octave frequencies of 50–6300 Hz. The aerogel/PET nonwoven composites have exhibited higher SAC than the untreated or control PET nonwoven for the entire frequency range. The suitable solvent molar ratio of 55 has been recommended for synthesis of silica aerogels by considering not only the silica content to have high sound absorption but also based on hydrophobic characteristics of aerogel/PET nonwoven composites.