Fluorocarbon nano-coating of polyester fabrics by atmospheric air plasma with aerosol

A fluorocarbon coating was deposited on polyester (PET) woven fabric using pulse discharge plasma treatment by injecting a fluoropolymer directly into the plasma dielectric barrier discharge. The objective of the treatment was to improve the hydrophobic properties as well as the repellent behaviour of the polyester fabric. Plasma treatment conditions were optimised to obtain optimal hydrophobic properties which were evaluated using water contact angle measurement as well as spray-test method at the polyester fabric surface. The study showed that adhesion of the fluoropolymer to the woven PET was greatly enhanced by the air plasma treatment. X-ray photoemission spectroscopy (XPS) analyses revealed chemical surface modifications occurring after the plasma treatments.     

Surface modification of a biomedical polyethylene terephthalate (PET) by air plasma

In this work, low-pressure air plasma has been used to improve polyethylene terephthalate (PET) surface properties for technical applications. Surface free energy values have been estimated using contact angle value for different exposure times and different test liquids. Surface composition and morphology of the films were analyzed by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Surface topography changes related with the etching mechanism have been followed by weight loss study. The results show a considerable improvement in surface wettability and the surface free energy values even for short exposure times in the different discharge areas (discharge area, afterglow area and remote area), as observed by a remarkable decrease in contact angle values. Change of chemical composition made the polymer surfaces to be highly hydrophilic, which mainly depends on the increase in oxygen-containing groups. In addition to, the surface activation and AFM analyses show obvious changes in surface topography as a consequence of the plasma-etching mechanism.     

Formation of a high hydrophilic/hydrophobic contrast surface on PET substrates by ECR generated sulfur hexafluoride plasma

High hydrophilic/hydrophobic contrast surfaces on polyethylene terephthalate (PET) substrates were formed by shadow mask technique in electron cyclotron resonance generated sulfur hexafluoride plasma atmosphere. The X-ray photoelectron spectroscopy (XPS) analyses indicate that the unmasked PET surfaces contained a high proportion of the CF₂-CF₂ groups, and therefore were hydrophobic with large water contact angle. However, the surface wettability was found to increase drastically on the masked PET surfaces. This could be resulted from a mass of COF (acid fluoride) compounds observed by XPS on the masked film surfaces. The COF compounds could react with atmospheric moisture to form -COOH groups, which in turn increased the surface wettability. In addition, the surface wetting property of the masked areas was found to change significantly with the plasma treatment time, the mask-to-substrate distance and the storage time after the treatment. The best contract in water contact angle obtained from the treated PET samples was larger than 100° after 168 h of storage.     

Study on the surface properties of wood/polyethylene composites treated under plasma

Wood/polyethylene (PE) composites are widely used in many fields for its excellent properties, but they are hard to adhere for the surface lacking of polarity. So low-pressure glow discharge of air plasma was used to improve the adhesion properties of wood/PE composites. The composites were treated by plasma under different discharge power. And the changes on the surface properties of the treated and untreated composites were studied by contact angle, Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS) analysis. The measurement showed that the contact angle decreased after plasma treatment, and the contact angle decreased gradually with the increasing of discharge power. The FTIR analysis results showed that the polar groups such as hydroxyl, carbonyl and carboxyl were formed on the surface of the composites treated under plasma. SEM and AFM results showed that the roughness of plasma treated samples increased. XPS analysis results indicated that the content of carbon element decreased while the content of oxygen element in the composition of wood/PE composites surface element increased and it reached a balance in a higher power, meanwhile a lot of carboxyl groups were formed. The newly formed polar groups are benefit for the adhesion of composites. The shear bonding strength test showed that the adhesion properties of wood/PE composites improved effectively after plasma treatment.     

Oil absorption capacity of bare and PDMS-coated PET non-woven fabric; dependency of fiber strand thickness and oil viscosity

Water and oil absorption behaviors of the bare and PDMS (polydimethylsiloxane)-coated PET (polyethylene terephthalate) fabrics with two different fiber strand thicknesses were investigated. PET fabrics were superhydrophobically modified by PDMS-coating via a thermal vapor deposition process. The modification greatly enhanced the selectivity of PET fabric to oil absorption from oil/water mixture, making the PDMS-coated fabric a promising candidate as an absorbent of oil spills. We have also studied oil sorption behaviors of PDMS-coated PET fabric as a function of fiber strand thicknesses and oil viscosities. In general, fabric with a thinner fiber strand thickness showed a higher maximum oil absorption capacity, whereas uptake of the oil in thicker-fiber-absorbent was faster. Based on our results, we suggest that different absorbent structures with various fiber strand thicknesses can be chosen to maximize the efficiency of oil removal, depending on oil viscosity and available oil absorption time.     

Superhydrophobic cotton fabric fabricated by electrostatic assembly of silica nanoparticles and its remarkable buoyancy

Highly hydrophilic cotton fabrics were rendered superhydrophobic via electrostatic layer-by-layer assembly of polyelectrolyte/silica nanoparticle multilayers on cotton fibers, followed with a fluoroalkylsilane treatment. The surface morphology of the silica nanoparticle-coated fibers, which results in the variety of the hydrophobicity, can be tailored by controlling the multilayer number. Although with the static contact angle larger than 150°, in the case of 1 or 3 multilayers, the fabrics showed sticky property with a high contact angle hysteresis (>45°). For the cotton fabrics assembled with 5 multilayers or more, slippery superhydrophobicity with a contact angle hysteresis lower than 10° was achieved. The buoyancy of the superhydrophobic fabric was examined by using a miniature boat made with the fabric. The superhydrophobic fabric boat exhibited a remarkable loading capacity; for a boat with a volume of 8.0 cm³, the maximum loading was 11.6 or 12.2 g when the boat weight is included. Moreover, the superhydrophobic cotton fabric showed a reasonable durability to withstand at least 30 machine washing cycles.     

Surface characterization of polyethylene terephthalate/silica nanocomposites

Poly(ethylene terephthalate) (PET) based nanocomposites containing hydrophilic (i.e. Aerosil 200 or Aerosil TT 600) or hydrophobic (i.e. Aerosil R 972) nano-silica were prepared by melt compounding. Influence of nano-silica type on surface properties of the resultant nanocomposites was investigated by the use of Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), contact angle measurement (CAM), scanning electron microscopy (SEM) and reflectance spectroscopy (RS). The possible interaction between nano-silica particles and PET functional groups at bulk and surface were elucidated by transmission FTIR and FTIR-ATR spectroscopy, respectively. AFM studies of the resultant nanocomposites showed increased surface roughness compared to pure PET. Contact angle measurements of the resultant PET composites demonstrated that the wettability of such composites depends on surface treatment of the particular nano-silica particles used. SEM images illustrated that hydrophilic nano-silica particles tended to migrate to the surface of the PET matrix.     

Graft copolymerization of acrylic acid onto polyamide fibers

The grafting of acrylic acid (AA) monomer (CH₂CHCOOH) on polyamide 6.6 monofilaments (PA 6.6) using benzoyl peroxide (BPO) as initiator was carried out in order to enhance the hydrophilic nature of fibers. The grafting rate depends on the AA concentration, the BPO concentration, the time and the temperature of reaction.The best conditions for optimum rate of grafting were obtained with a AA concentration of 0.5 M, a BPO concentration of 0.03 M, a reaction temperature of T = 85 °C and a reaction time of 120 mn.The fiber surface has been investigated by many experimental techniques of characterization such as Fourier transform infrared spectroscopy (FTIR), calorimetric analysis (DSC), scanning electron microscopy (SEM), and contact angle measurements.The effect of grafting of acrylic acid onto PA 6.6 fibers on their moisture and mechanical resistances was analyzed from water sorption and elongation at break measurements.The analysis of the experimental data shows clearly the efficiency of the grafting reaction used, leading to a significant increase of the hydrophilic character of the PA 6.6 surface.     

重复频率纳秒脉冲介质阻挡放电对聚对苯二甲酸乙二酯表面改性

介绍了0.1 MPa下的纳秒脉冲介质阻挡放电(DBD)对聚对苯二甲酸乙二酯(PET)材料表面进行的亲水性改善。分别采用均匀和丝状放电模式对PET表面改性处理,并采用水接触角测量、原子力显微镜观察、X射线光电子能谱分析对改性材料进行表面分析。实验发现介质阻挡放电处理后PET表面水接触角明显减小,接触角从78°下降到25°,但随处理时间的增加有饱和效应;PET表面粗糙程度增加,亲水性含氧基团被引入,从而改善了材料表面亲水性;纳秒脉冲下的均匀DBD比丝状DBD处理效果更为显著。     

Fabrication of a superhydrophobic ZnO nanorod array film on cotton fabrics via a wet chemical route and hydrophobic modification

A superhydrophobic ZnO nanorod array film on cotton substrate was fabricated via a wet chemical route and subsequent modification with a layer of n-dodecyltrimethoxysilane (DTMS). The as-obtained cotton sample was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), scanning probe microscope (SPM) and X-ray photoelectron spectroscopy (XPS), respectively. The wettability of the cotton fabric sample was also studied by contact angle measurements. The modified cotton fabrics exhibited superhydrophobicity with a contact angle of 161° for 8 μL water droplet and a roll-off angle of 9° for 40 μL water droplet. It was shown that the proper surface roughness and the lower surface energy both played important roles in creating the superhydrophobic surface, in which the Cassie state dominated.     

Surface modification of polypropylene non-woven fabric using atmospheric nitrogen dielectric barrier discharge plasma

In this paper, a dielectric barrier discharge operating in nitrogen at atmospheric pressure has been used to improve the surface hydrophilic property of polypropylene (PP) non-woven fabric. The changes in the hydrophilic property of the modified PP samples are investigated by the contact angle measurements and the variation of water contact angle is obtained as a function of the energy density; micrographs of the PP before and after plasma treatment are observed by scanning electron microscopy (SEM) and the chemical composition of the PP surface before and after plasma treatment is also analyzed by Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The results show that the surface hydrophilic property of the PP samples is greatly improved with plasma treatment for a few seconds, as evidenced by the fact that the contact angle of the treated PP samples significantly decreases after plasma treatment. The analysis of SEM shows that the surface roughness of the treated PP samples increases due to bonding and etching in plasma processing. The analyses of FTIR and the C1s peak in the high-resolution XPS indicate that oxygen-containing and nitrogen-containing polar functional groups are introduced into PP surface in plasma processing. It can be concluded that the surface hydrophilic property of the modified PP samples has been obviously improved due to the introduction of oxygen-containing and nitrogen-containing polar groups and the increase of the surface roughness on the PP surface.     

纳秒脉冲放电对聚对苯二甲酸乙二酯憎水改性

基于自主研制的ns脉冲电源（上升沿约70 ns, 脉宽约100 ns）激励介质阻挡放电产生大气压低温等离子体, 在CF4气氛下对聚对苯二甲酸乙二酯（PET）表面进行了憎水改性处理, 测量了改性前后的薄膜表面的水接触角, 给出了CF4气流量、放电电压、处理时间和CF4比例等参数对改性效果的影响规律。结果表明, 大气压ns脉冲DBD表面处理能够实现PET材料的憎水性, 改性后的PET表面水接触角由66提高到最大100。     

纳秒脉冲放电对聚对苯二甲酸乙二酯憎水改性

基于自主研制的ns脉冲电源(上升沿约70ns,脉宽约100ns)激励介质阻挡放电产生大气压低温等离子体,在CF4气氛下对聚对苯二甲酸乙二酯(PET)表面进行了憎水改性处理,测量了改性前后的薄膜表面的水接触角,给出了CF4气流量、放电电压、处理时间和CF4比例等参数对改性效果的影响规律。结果表明,大气压ns脉冲DBD表面处理能够实现PET材料的憎水性,改性后的PET表面水接触角由66°提高到最大100°。     

Uniformity analysis of dielectric barrier discharge (DBD) processed polyethylene terephthalate (PET) surface

A dielectric barrier discharge (DBD) plasma, operating in air at atmospheric pressure, has been used to induce changes in the surface properties of polyethylene terephthalate (PET) films. The effects that the key DBD operating parameters: discharge power, processing speed, processing duration, and electrode configurations, have on producing wettability changes in the PET surface region have been investigated. The approach taken involves the application of an Taguchi experimental design and robust analysis methodology. The various data sets obtained from these analyses have been used to studies the effect of the operating parameters on the surface uniformity and efficiency of the said treatment.In general, the results obtained indicate that DBD plasma processing is an effective method for the controlled surface modification of PET. Relatively short exposures to the atmospheric pressure discharge produces significant wettability changes at the polymer film surface, as indicted by pronounced reductions in the water contact angle measured. It was observed that the wettability of the resultant surface shows no significant differences in respect to orientation parallel (L-direction) or perpendicular (T-direction) to the electrode long axis. However, there was significant differences between the data obtained from these two orientations. Analysis of the role of each of the operating parameters concerned shows that they have a selective effectiveness with respect to resultant surface modification in terms of uniformity of modification and wettability. The number of treatment cycles and the electrode configuration used were found to have the most significant effects on the homogeneity of the resultant PET surface changes in L- and T-orientation, respectively. On the other hand, the applied power showed no significant role in this regard. The number of treatment cycles was found to be the dominant factor (at significance level of 0.05) in respect of water contact angle changes at the processed PET surface in both orientations. The driven metal electrodes (stainless steel or aluminium) were apparently superior to the driven dielectric electrode (ceramic or quartz) configurations. The grounded electrode in each case was a silicon rubber-covered aluminium plate (see later). The nature and scale of the surface changes that originate from the various processing conditions employed have been considered so as to determine the optimum treatment conditions in respect of processing outcomes, properties and any orientation dependence. Thus, it was revealed that higher processing speeds and longer processing durations are key for uniformity along the electrode axial orientation, while lower processing speeds and short exposure durations are key considerations, in the corresponding perpendicular orientation. In general, longer processing durations (low processing speeds and a high number of treatment cycles) and higher plasma powers induced greater changes in the surface wettability of the PET, as demonstrated by the observed water contact angles. This behaviour is taken to indicate that different combinations of DBD operating parameters and electrodes produce discharge conditions that can result in different plasma chemical processes in respect of uniformity, treatment efficiency and orientation dependence.     

Superhydrophobic cotton fabric coating based on a complex layer of silica nanoparticles and perfluorooctylated quaternary ammonium silane coupling agent

A superhydrophobic complex coating for cotton fabrics based on silica nanoparticles and perfluorooctylated quaternary ammonium silane coupling agent (PFSC) was reported in this article. The complex thin film was prepared through a sol-gel process using cotton fabrics as a substrate. Silica nanoparticles in the coating made the textile surface much rougher, and perfluorooctylated quaternary ammonium silane coupling agent on the top layer of the surface lowered the surface free energy. Textiles coated with this coating showed excellent water repellent property, and water contact angle (CA) increased from 133° on cotton fabrics treated with pure PFSC without silica sol pretreatment up to 145°. The oil repellency was also improved and the contact angle of CH₂I₂ droplet on the fabric surface reached to 131°. In contrast, the contact angle of CH₂I₂ on the fabric surface treated with pure PFSC was only 125°.     

Hydrophobization of cotton fabric by Gliding Arc plasma discharge

The surface modification in order to obtain hydrophobic cotton fabrics was carried out using air/HMDSO Gliding Arc plasma discharge. The dependence of the surface wettability on used process parameters, such as air flow, sample distance and treatment time were investigated. The wettability of cotton fabrics was evaluated by the drop test method by measuring the time of droplet absorption and water contact angle (WCA). The changes in the surface morphology were examined by optical microscopy and scanning electron microscopy (SEM). The treated hydrophobic fabrics were subjected to the analysis of chemical composition of the applied coatings using the ATR-FTIR spectroscopy. Hydrophobic cotton fabrics were obtained, especially with a high resistance to static wetting. In addition, the treated cotton fabrics were tested using a spray test measurement and were subjected to multiple washing.     

ADBD plasma surface treatment of PES fabric sheets

Plasma treatment of textile fabrics is investigated as an alternative to the environmentally hazardous wet chemical fabric treatment and pretreatment processes. Plasma treatment usually results in modification of the uppermost atomic layers of a material surface and leaves the bulk characteristics unaffected. It may result in desirable surface modifications, e.g. surface etching, surface activation, cross-linking, chain scission and oxidation. Presented paper contains results of the applicability study of the atmospheric pressure dielectric discharge (ADBD), i.e. dielectric barrier discharge sustaining in air at atmospheric pressure and ambient temperature for synchronous treatment of several sheets of fabric. For tests sheets of polyester fabric were used. Effectivity of the modification process was determined with hydrophilicity measurements evaluated by means of the drop test. Hydrophilicity of individual sheets of fabric has distinctly increased after plasma treatment. Plasma induced surface changes of textiles were also proven by identification of new functional groups at the modified polyester fabric surface. Existence of new functional groups was detected by ESCA scans. For verification of surface changes we also applied high-resolution microphotography. It has shown distinct variation of the textile surface after plasma treatment. Important aspect for practical application of the plasma treatment is the modification effect time-stability, i.e. time stability of acquired surface changes of the fabric. The recovery of hydrophobicity was fastest in first days after treatment, later gradually diminished until reached almost original untreated state.     

重复频率纳秒脉冲介质阻挡放电对聚对苯二甲酸乙二酯表面改性

介绍了0.1 MPa下的纳秒脉冲介质阻挡放电(DBD)对聚对苯二甲酸乙二酯(PET)材料表面进行的亲水性改善。分别采用均匀和丝状放电模式对PET表面改性处理,并采用水接触角测量、原子力显微镜观察、X射线光电子能谱分析对改性材料进行表面分析。实验发现介质阻挡放电处理后PET表面水接触角明显减小,接触角从78°下降到25°,但随处理时间的增加有饱和效应;PET表面粗糙程度增加,亲水性含氧基团被引入,从而改善了材料表面亲水性;纳秒脉冲下的均匀DBD比丝状DBD处理效果更为显著。     

The effect of discharge power density on polyethylene terephthalate film surface modification by dielectric barrier discharge in atmospheric air

Polyethylene terephthalate (PET) films are modified using non-equilibrium plasma generated by DBD in atmospheric air, and the effects of discharge power density on the surface modification are studied. It is found that increasing discharge power density can induce more effective treatment of PET films, because this leads to a faster decrease in water contact angle and a faster increase in surface energy due to more creation of polar groups and more obvious etching occurring on the PET surface. So the treatment time needed to achieve the same level of surface treatment can be reduced by increasing the discharge power density.     

Surface modification of a polyamide 6 film by He/CF4 plasma using atmospheric pressure plasma jet

Polyamide 6 (PA 6) films are treated with helium(He)/CF₄ plasma at atmospheric pressure. The samples are treated at different treatment times. The surface modification of the PA 6 films is evaluated by water contact angle, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The etching rate is used to study the etching effect of He/CF₄ plasma on the PA 6 films. The T-peel strengths of the control and plasma treated films are measured to show the surface adhesion properties of the films. As the treatment time increases, the etching rate decreases steadily, the contact angle decreases initially and then increases, while the T-peel strength increases first and then decreases. AFM analyses show that the surface roughness increases after the plasma treatment. XPS analyses reveal substantial incorporation of fluorine and/or oxygen atoms to the polymer chains on the film surfaces.