Preparation of polybutylene terephthalate/silica nanocomposites by melt compounding: Evaluation of surface properties

Influence of nanosilica on surface properties of poly(butylene terephthalate) 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). FTIR results indicated that surface groups of silica have some interfacial interactions and bonding with carboxyl or hydroxyl end groups of PBT chains. AFM and SEM figures of the resultant nanocomposites illustrated increased surface roughness compared to pure PBT. Optical properties of nanocomposite films were finally determined by the aid of reflectance spectrophotometer.     

Surface properties of polypropylene/organoclay nanocomposites

Influence of nanoclay amount on surface properties of the nanocomposites was investigated using Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), contact angle measurement, scanning electron microscopy (SEM) and transmission spectroscopy (TS). Polypropylene based nanocomposites containing various loads of nanoclay were prepared by melt compounding. X-ray diffraction (XRD) characterized the dispersion of nanoclay in polymer matrix. AFM and SEM studies have shown increase in surface roughness by raising the amount of nanoclay. Contact angle measurements of the resultant nanocomposites have also shown improvement in wettability related to disperse part of surface tension. POM images illustrated an increase in the number of spherulite simultaneously with a decrease in their size; this result was also supported by differential scanning calorimetry (DSC).     

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.     

用分散聚合反应制备SiO2/PS包覆粒子（英）

采用分散聚合反应制备了纳米SiO2/PS包覆粒子,并对其结构进行了表征。首先在超声波场中用表面活性剂对纳米SiO2粒子进行亲油化处理,然后在氮气保护下利用超声波的分散、粉碎、活化、引发等多重作用,在实现纳米SiO2粒子在反应介质中纳米分散的同时,引发苯乙烯单体在纳米SiO2粒子表面发生分散聚合反应,制备出纳米SiO2/PS包覆粒子。最后,采用SEM,TEM,FTIR,XPS等测试手段对纳米SiO2/PS包覆粒子进行了表征,测试结果表明,PS实现了对纳米SiO2的包覆,形成了核壳包覆结构。     

用分散聚合反应制备SiO2/PS包覆粒子（英）

采用分散聚合反应制备了纳米SiO2/PS包覆粒子,并对其结构进行了表征。首先在超声波场中用表面活性剂对纳米SiO2粒子进行亲油化处理,然后在氮气保护下利用超声波的分散、粉碎、活化、引发等多重作用,在实现纳米SiO2粒子在反应介质中纳米分散的同时,引发苯乙烯单体在纳米SiO2粒子表面发生分散聚合反应,制备出纳米SiO2/PS包覆粒子。最后,采用SEM,TEM,FTIR,XPS等测试手段对纳米SiO2/PS包覆粒子进行了表征,测试结果表明,PS实现了对纳米SiO2的包覆,形成了核壳包覆结构。     

Effect of clay surface modification on the structure and electro-optical properties of liquid crystal/clay nanocomposites

FTIR spectroscopy, atomic force microscopy (AFM) and electro-optical measurements were used to study nanocomposites consisting of nematic liquid crystal (LC) ZLI-2293 and organophilic montmorillonite (MMT) nanoparticles. The initial MMT was modified by two different surfactants: octadecylbenzyldimethylammonium chloride (OBDM) and dioctadecylldimethylammonium chloride (DODM). According to spectroscopic results, Van der Waals interactions between the components of the LC/clay composites are stronger in OBDM-MMT case. AFM images of two types of the LC/clay nanocomposites showed different morphology consisting of large-scale structures. Correlation between the spectroscopic results and electro-optical behaviour of the LC/clay nanocomposites was observed. It was inferred that the memory effect is more pronounced for composites with OBDM-MMT due to colloid network formation, whereas the electro-optical contrast is higher for DODM-MMT, where the clay particles are not organized in any ordered structure.     

Preparation and Properties of Polystyrene/Bacterial Cellulose Nanocomposites by In Situ Polymerization

Polystyrene/bacterial cellulose (PS/BC) nanocomposites were prepared via in situ polymerization. Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), themogravimetry (TG), and mechanical testing were employed to characterize the PS/BC nanocomposites. The polystyrene filled in the network of the BC and a lamellar structure was formed. The FTIR results show that no chemical reaction between PS and BC occurred during the polymerization. These composites showed good mechanical properties.     

Surface modification of polypropylene using argon plasma: Statistical optimization of the process variables

Low pressure plasma treatment using radiofrequency (rf) discharge of argon gas was employed to improve the hydrophilicity of polypropylene. The effects of argon plasma on the wettability, surface chemistry and surface morphology of polypropylene were studied using static contact angle measurements, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and atomic force microscopy (AFM). Increase in surface energy of polypropylene was observed as a result of argon plasma treatment. SEM and AFM images revealed the increased surface roughness. A set of identified process variables (rf power, pressure, argon flow rate and time) were used in this study and were optimized using central composite design (CCD) of response surface methodology (RSM). A statistical model was developed to represent the surface energy in terms of the process variables mentioned above. Accuracy of the model was verified and found to be high.     

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.     

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.     

Minimizing permeability of PET substrates using Oxygen plasma treatment

Surface plasma treatment in a reactive ion etching system is used to observe a considerable decrease in permeability of polyethylene terephthalate to gases. The effects of oxygen plasma on the surface properties and morphology of PET polymers are investigated by scanning electron microscopy (SEM), x-ray photo-electron spectroscopy (XPS) and atomic force microscopy (AFM). In addition, the optical transmission properties of the treated samples have been investigated corroborating the findings of SEM and AFM analyses. Moreover, the penetration of air through the treated substrates was investigated using a vacuum test. The treated PET substrates can be used to realize flexible plasma display panels.     

Comparing the Effect of Micro- and Nano-Scale Silica on the Rheological,Dynamic Mechanical Properties and Flame Resistance of Nylon 6,6

Nylon 6,6 micro- and nano-silica composites were prepared by melt processing using a twin-screw extruder. Three nanocomposites containing 4, 8, and 12 wt.% of nanosilica were prepared. In order to compare the effect of size, a microcomposite containing 4 wt.% of micron-size silica was also prepared. The effects of particle type (micro- and nano-size) on the dynamic thermomechanical and rheological properties, morphology, and flame resistance of the composites were examined. The dynamic thermomechanical properties (DMTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), dynamic rheometry, thermogravimetry analysis (TGA), and limiting oxygen index (LOI) data are reported. The particles were observed to be dispersed uniformly, but with a different level of coalescence, by means of SEM and TEM. The DMTA results showed that the damping factor peak positions of the nanocomposites at low content of nanofiller shifted more to higher temperature compared to those of nanocomposites containing high concentrations of nanofiller. Dynamic rheometry, using a parallel plate rheometer, showed that the rheological moduli of the nanocomposites increased with increase in nanofiller concentration; however, this increase was greater in the high-frequency region. These results showed that increasing the concentration of nanofiller, and the consequent coalescence effect within the nanocomposites, led to rheological moduli values similar to those of the microcomposite. The TGA and LOI results of the microcomposite and nanocomposite containing 4wt.% of nanosilica showed that nanosilica had a more significant effect to enhance the heat and flame resistance of nylon 6,6 compared to that of micron-sized silica.     

Improving the hydrophilicity of poly(vinylidene fluoride) porous membranes by electron beam initiated surface grafting of AA/SSS binary monomers

Poly(vinylidene fluoride) (PVDF) membranes were pre-irradiated by electron beam in vacuum, and then the hydrophilic sulfonate groups were introduced by the single step grafting method with binary monomer solution of acrylic acid (AA) and sodium 4-styrenesulfonate (SSS). The effect of binary monomer ratio and pH of reaction solution on the degree of grafting was investigated. The surface chemical change was characterized by Fourier transform infrared attenuated total reflection spectroscopy (FT-IR-ATR) and X-ray photoelectron spectroscopy (XPS). Morphological changes on the membrane surface were characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The surface hydrophilicity of the modified membrane was characterized through water contact angle measurement. It was found that the water contact angle of the membrane surface decreased significantly when compared with the original one, indicating the improvement of the surface hydrophilicity.     

Cashew tree wood flour activated with cashew nut shell liquid for the production of functionalized composites

This work is aimed at the one-step chemical modification of the surface of cashew wood flour particles using the technical grade cashew nut shell liquid (CNSL). The goal is to develop an alternative way to introduce chemically active sites on the surface of the particles, which allows the addition of new functionalities to such particles. The influence of time and temperature and catalyst on the substitution of lignocellulosic hydroxyls with cardanol/cardol urethane derivatives was evaluated by thermogravimetric analysis, scanning electron microscopy, Fourier-transform infrared spectroscopy (FTIR), and contact angle measurements. The mechanical behavior of the modified particles in polypropylene composites was also evaluated by mechanical testing and dynamic mechanical thermal analysis. The FTIR, thermogravimetry, and contact angle results indicated changes on the particle surface, and the mechanical and thermomechanical behavior of the mercerized and modified particles in the composites was found to be similar. These results point that the CNSL approach is a viable way to chemically modify cashew wood flour particle surfaces, while maintaining their properties.     

Surface chemistry of atmospheric plasma modified polycarbonate substrates

Surface of polycarbonate substrates were activated by atmospheric plasma torch using different gas pressure, distance from the substrates, velocity of the torch and number of treatments. The modifications were analyzed by contact angle measurements, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and UV-vis spectrophotometry. Plasma treatment caused the surface characteristics to become more hydrophilic as measured by the water contact angle, which decreased from 88° to 18°. The decrease in contact angle was mainly due to oxidation of the surface groups, leading to formation of polar groups with hydrophilic property. XPS results showed an increase in the intensity of -(C-O)- groups and also introduction of new functional groups i.e. -(O-CO)- after the treatment process. AFM topographic images demonstrated an increase in the rms roughness of the surface from 2.0 nm to 4.0 nm caused by the treatment. Increase in rms roughness of the surface caused relevant decrease in transmission up to ∼2-5%.     

Study on hydrophilicity of polymer surfaces improved by plasma treatment

Surface properties of polycarbonate (PC), polypropylene (PP), polyethylene terephthalate (PET) samples treated by microwave-induced argon plasma have been studied with contact angle measurement, X-ray photoelectron spectroscopy (XPS) and scanned electron microscopy (SEM). It is found that plasma treatment modified the surfaces both in composition and roughness. Modification of composition makes polymer surfaces tend to be highly hydrophilic, which mainly depended on the increase of ratio of oxygen-containing group as same as other papers reported. And this experiment further revealed that CO bond is the key factor to the improvement of the hydrophilicity of polymer surfaces. Our SEM observation on PET shown that the roughness of the surface has also been improved in micron scale and it has influence on the surface hydrophilicity.     

One-stage fabrication of sub-micron hydrophilic microchannels on PDMS

A sub-micron hydrophilic microchannel was fabricated on poly(dimethylsiloxane) (PDMS) in one step using vacuum ultraviolet light (VUV) lithography in vacuum. The topographies and properties of the irradiated PDMS surface were characterized and analyzed by atomic force microscopy (AFM), and the chemical composition changes on VUV-treated PDMS analyzed by X-ray photoelectron spectroscopy (XPS). The hydrophilic stability of irradiated PDMS surface was studied by static water contact angle. As demonstrated, the hydrophilicity on surface of PDMS microchannel can be kept for a longer term even three months after the treatment.     

Microstructure and interfacial interaction of polyimide/silica hybrid nanocomposites prepared with 3-aminopropyltriethoxysilane

A series of polyimide (PI)-silica hybrid nanocomposites are prepared from 3,3′,4,4′biphenyltetracarboxylic dianhydride (BPDA)-4,4′-oxydianiline (ODA) polyamic acid (PAA) and tetraethoxysilane (TEOS) or tetramethoxysilane (TMOS) by the sol-gel process. 3-Aminopropyltriethoxysilane (3-APS) is used to enhance the interfacial interaction between polyimide and silica. The morphology, interfacial interaction, and properties of the hybrids are investigated using scanning electron microscope (SEM), UV-vis spectroscopy, atomic force microscope (AFM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). SEM and AFM images indicate that silica particles of ca. 45-55 nm size are uniformly distributed in polyimide matrices and that the interfacial interaction between PI and TEOS is better than that between PI and TMOS. The optical transparencies of the PI/TEOS hybrids are better than that of the PI/TMOS hybrids. FTIR spectra confirm the Si O Si bond as well as the conversion of PAA to polyimide and PI/silica hybrid films. The thermal stability is increased after incorporation of the silicas in the polyimide matrix.     

Excimer UV lamp irradiation induced grafting on synthetic polymers

Surface modifications on polyethyleneterephthalate (PET) films following excimer UV lamp irradiation induced grafting were studied. Characteristics of the modifications depending on the conditions during the irradiation were analysed using contact-angle measurements, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), differential scanning calorimetry (DSC) and Fourier-transform infrared spectroscopy (FTIR). Depending on the conditions during the irradiation different surface modifications were obtained, which can generally be classified regarding the hydrophilic or hydrophobic characteristics of the resulting surface. It is shown that not every substance that meets the general demands will be grafted on synthetic polymers using excimer UV radiation. Examples of agents that can simply be grafted onto polymer surfaces and those that undergo further crosslinking, building up thin films are listed. Agents used for grafting on polymers are 1,5-hexadiene, perfluoro-4-methyl-pent-2-ene, polyethyleneglycol 200, monosilane and polyethylene. The transferability of the effects achieved to substrates such as polyparaphenylene terephthalamide or polymetaphenylene isophthalamide is shown. Received: 23 June 2000 / Accepted: 28 June 2000 / Published online: 5 October 2000     

Fabrication of a superhydrophobic surface on a wood substrate

A layer of lamellar superhydrophobic coating was fabricated on a wood surface through a wet chemical process. The superhydrophobic property of the wood surface was measured by contact angle (CA) measurements. The microstructure and chemical composition of the superhydrophobic coating were analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). An analytical characterization revealed that the microscale roughness of the lamellar particles was uniformly distributed on the wood surface and that a zinc stearate monolayer (with the hydrophobic groups oriented outward) formed on the ZnO surface as the result of the reaction between stearic acid and ZnO. This process transformed the wood surface from hydrophilic to superhydrophobic: the water contact angle of the surface was 151°, and the sliding angle was less than 5°.