Surface analysis of plasma grafted carbon fiber

The surface characteristics of carbon fibers were studied by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and wetting measurements. The surface of carbon fiber was modified by means of plasma graft silsesquioxane. The oxygen/carbon and silicon/carbon ratio increased rapidly after treatments. Fitting the C 1s, O 1s, and Si 2p spectra demonstrated that new photopeaks were emerged, which were indicated C-Si, Si-O groups, respectively. The degree of surface roughness and the wettability of carbon fiber surface were both increased by plasma graft silsesquioxane. The results may shed some light on the design of the appropriate surface structure, which could react with resin, and the manufacture of the carbon fiber reinforced composites.     

Photo-irradiation effects on the surface morphology of poly(p-phenylene vinylene) films

In this work, we have studied the surface morphology of photo-irradiated poly(p-phenylene vinylene) (PPV) thin films by using atomic force microscopy (AFM). We have analyzed the first-order statistical parameters, the height distribution and the distance between selected peaks. The second-order statistical analysis was introduced calculating the auto-covariance function to determine the correlation length between heights. We have observed that the photo-irradiation process produces a surface topology more homogeneous and isotropic such as a normal surface. In addition, the polymer surface irradiation can be used as a new methodology to obtain materials optically modified.     

Surface modification of porous poly(tetrafluoroethylene) film via cold plasma treatment

In this study, cold plasma technology was applied for the surface modification of porous polytetrafluoroethylene (PTFE) film to improve the hydrophilicity. The surface properties of PTFE, modified by air, helium (He) or acrylic acid (AAc), were investigated with scanning electron microscopy (SEM), scanning probe microscope (SPM), in situ X-ray photoelectron spectroscopy (XPS) and water contact angle measurements. The changes of the surface property before and after plasma treatment were discussed. According to SEM and SPM measurements, the surface roughness increased at different levels after plasma treatment. Compared to air and AAc plasma treatment, the He plasma treatment introduced large amounts of oxygen into the surface, as known from XPS results. Contact angle measurements revealed that the hydrophilicity of the PTFE film surface was greatly improved due to the surface roughness and changes of chemical elements on the PTFE surface.     

Surface state of TiO2 treated with low ion energy plasma

The effect of low pressure radio frequency (rf) plasma treatment on TiO₂ surface states has been studied using X-ray photoelectron spectroscopy. Three different oxidation states of oxygen in untreated TiO₂ powder were observed, which suggests the existence of adsorbed water and carbon on the surface. The ratio of oxygen to titanium (O/Ti) was decreased for the low ion dose plasma treated samples due to desorption of water from the surface. In the case of Ti 2p about 20% of surface states were converted to Ti³⁺ 2p_3/2 state after plasma treatment with a very good stability, whereas untreated TiO₂ remained mostly as Ti⁴⁺ state. A rapid decrease in the ratio of carbon to titanium (C/Ti) at TiO₂ surface was also observed after plasma treatment and more than 90% of carbon atoms were removed from the surface. Therefore, the plasma treatment of TiO₂ has advantages to surface carbon cleaning, increasing O⁻ and Ti³⁺ surface states, hence improving the activity of TiO₂ for different environmental, energy and biological applications.     

Improvement and mechanism of interfacial adhesion in PBO fiber/bismaleimide composite by oxygen plasma treatment

The improved interfacial adhesion of PBO fiber-reinforced bismaleimide composite by oxygen plasma processing was investigated in this paper. After treatment, the maximum value of interlaminar shear strength was 57.5 MPa, with an increase of 28.9%. The oxygen concentration of the fiber surface increased, as did the surface roughness, resulting in improvement of the surface wettability. The cleavage and rearrangement of surface bonds created new functional groups OCO, NCO and NO, thereby activating the fiber surface. And long-time treatment increased the reaction degree of surface groups while destroyed the newly-created physical structures. The enhancement of adhesion relied primarily on the strengthening of chemical bonding and mechanical interlocking between the fiber and the matrix. The composite rupture planes indicated that the fracture failure shifted from the interface to the matrix or the fiber.     

Thermal conductivity of stretched and annealed poly (p-phenylene sulfide) films

The temperature variation of the thermal conductivities of as-prepared, mechanically stretched, as-prepared and then annealed PPS samples are presented. Unusually high thermal conductivity values are observed as compared to other polymeric materials. In agreement with the X-ray diffraction observations, the thermal conductivity of the oriented film is higher than that of the as-prepared or annealed films. The differences observed after stretching are comparable to those previously reported for polyethylene and polyacetylene films for the same draw ratios. These unusually high thermal conductivity values justify the use of PPS in devices where efficient heat dissipation, associated with electrical insulation, is required.     

Surface physical-morphological and chemical changes leading to performance enhancement of atmospheric pressure plasma treated polyester fabrics for inkjet printing

Without any preprocessing, polyester fabric has lower ability to hold on water due to the smooth morphology and chemistry property of polyester fibers. Therefore, patterns directly printed with pigment inks have poor color yields and easily bleed. In this paper, atmospheric pressure plasma was used to pretreat polyester fabric in order to provide an active surface for the inkjet printing. The results showed that surface-modified polyester fabrics could obtain the effects of features with enhanced color yields and excellent pattern sharpness. SEM images indicated that the rough surface of plasma treated fibers could provide more capacities for the fabric to capture inks and also facilitate the penetration of colorant particles into the polyester fabric. XPS analysis revealed that air + 50%Ar plasma introduced more oxygen-containing groups onto the fabric surface than air plasma. Although AFM images indicated that etching effects generated by air plasma treatments were more evident, the air/Ar plasma treated sample has higher K/S value and better color performance. These studies have also shown that the chemical modification of plasma appears to be relatively more significant for improving the effect of inkjet printing.     

Interchain interactions effects on emission efficiency of poly(p-phenylene vinylene) films

In attempts to obtain poly(p-phenylene vinylene) (PPV) molecules without intermacromolecular aggregation two strategies were employed: the addition of a strong electrolyte, lithium chloride, to the solution of the precursor, or/and the preparation of solid solutions from co-dissolved precursor and poly(vinyl alcohol) (PVA). The effects on the thermal conversion process of PPV were studied. Complete isolation of the PPV chains was not attained, but a significant degree of chain separation was achieved, as demonstrated by spectroscopic data. The main observations were that strong intermacromolecular forces operate during the PPV elimination step, resulting in simultaneous aggregation with the formation of the final chains. The relative emission efficiency increases up to 115% for PPV and PPV:PVA films when 0.7% and 1.4% of LiCl, respectively, are added and lower conversion temperature (100 °C) procedure is employed. In the case of total annealing procedure (230 °C) the emission efficiency increases 65% for PPV:PVA film with 0.7% of LiCl. For PPV:LiCl films, this parameter decreases substantially (∼11%) when the salt concentration increases above 10%.     

Asymmetric surface modification of poly(ethylene terephthalate) film by CF4 plasma immersion

Poly(ethylene terephthalate) (PET) films were treated with CF₄ plasma immersion. The samples were processed at different RF powers and treatment time. The surface modification of PET films was evaluated by water contact angle (CA), X-ray photoelectron spectroscopy (XPS) and atomic force microscope (AFM). Decrease in contact angle of both sides of PET films was observed under mild treatment conditions. However, as raising treatment power and/or time, the change in contact angle between the two sides of PET films was different. The relatively hydrophobic and hydrophilic surfaces were being in situ formed on the two sides of PET films, respectively. And the extreme values of water contact angle reached 108.63 and 7.56°, respectively. XPS analyses revealed that there was a substantial incorporation of fluorine and/or oxygen atoms in both side surfaces. The relative chemical composition of the C (ls) spectra's showed the incorporation of non-polar fluorine-based functionalities (i.e. CFCF_n, CF₂ or CF₃ groups) and polar oxygen-based functionalities (i.e. COOH or OH groups) in the surfaces. Correlation between the plasma parameters and the surface modification of PET films is also discussed.     

Wettability and sizing property improvement of raw cotton yarns treated with He/O2 atmospheric pressure plasma jet

Raw cotton fiber is water repellent due to the existence of the water repellent cuticle layer. This study is designed to systematically investigate how He/O₂ atmospheric pressure plasma jet (APPJ) treatments influence the wettability and the sizing property of cotton yarns. Water absorption time and adhesion of the sizing agent to the cotton roving are used to evaluate the improvement of wettability and sizing property of the yarn respectively. The water absorption time decreases with the increase of the treatment time and the oxygen flow rate, and the decrease of the jet to substrate distance (JTSD). An optimal water absorption time of 0.8 s is obtained with a treatment time of 20 s, JTSD of 1 mm and O₂ flow rate of 0.2 L/min. Scanning electron microscopy (SEM) shows that the etching effect increases with the decrease of the JTSD and X-ray photoelectron spectroscopy (XPS) presents increased oxygen contents after the plasma treatments. An increase of O-CO bonds while a decrease of C-OH/C-O-C bonds are observed when the JTSD is set at 2 mm. However, a remarkable increase of both C-OH/C-O-C and O-CO bonds are achieved when the JTSD is 1 mm. The roving impregnation test results show a nearly doubled adhesion of sizing and a slightly improved breaking elongation, indicating that the plasma treatment does effectively enhance the bonding strength between the fiber and the sizing.     

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.     

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.     

Oxygen plasma functionalization of poly(p-phenilene sulphide)

Surface effects during plasma activation of poly(p-phenilene sulphide)—PPS have been studied. Samples that were exposed to weakly ionized highly dissociated oxygen plasma created an inductively coupled radiofrequency discharge with the power of 100 W. The electron density and temperature were measured with a double Langmuir probe and were 4 × 10¹⁵ m⁻³ and 3 eV, respectively, while the neutral atom density was measured with a fiber optics catalytic probe and was 4 × 10²¹ m⁻³. The surface tension was determined by measuring the contact angle of deionized water, while the appearance of surface functional groups was detected by XPS. The surface tension of untreated PPS was 7 × 10⁻³ N/m or/and increased to 7 × 10⁻² N/m in few seconds of plasma treatment. It remained fairly constant for longer plasma treatments. The XPS survey spectrum showed little oxygen on untreated samples, but its concentration increased to about 20 at.% in few seconds. Detailed high resolution XPS C 1s peak showed that the carbon was left fairly stable during plasma treatment. The main functional groups formed were rather sulphate in sulphite groups, as determined from high resolution S 2p peak. Namely, a strong transition from sulphide to sulphate state of sulfur was observed. The spontaneous deactivation of the polymer surface was measured as well. The deactivation was fairly logarithmic with the characteristic decay time of several hours.     

Studies on wettability of medical poly(vinyl chloride) by remote argon plasma

The paper studies surface modification of medical poly(vinyl chloride) (PVC) by remote argon plasma and characterized surface structure, performance of treated PVC by the water contact angle measurement, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Results show that the remote argon plasma makes the surface of the PVC film higher hydrophilic than the direct argon plasma and does not give remarkable degradation on the PVC film surface. The hydrophilicity depends on sample position as well as the RF power and the plasma exposure time. The remote argon plasma contributes more effectively to the dechlorination (Cl/C = 0.01) from the PVC film than the direct argon plasmas (Cl/C = 0.03) and more effectively to the formation oxygen functionalities on the PVC film surface. These experimental results show the possibility that remote argon plasma treatment can enhance interaction reactions with argon radicals relative to those with electron and argon ions.     

ESEM study of size removal from ceramic fibers by plasma treatment

Plasma treatment has been increasingly used for surface cleaning, activation and polymerisation in many industries. In this study, the oxygen plasma treatment was used to remove the organic size from the ceramic fiber surface. The size removal from the fiber surface was characterized using an environmental scanning electron microscope. The combination of electron microanalysis and energy-dispersive X-ray allowed the observation of the fibre surface and the determination of the change in elements on the fiber surface. The use of low energy plasmas has been shown to be effective in the removal of the organic size from the ceramic fiber surfaces. It has also been revealed that the ESEM is a useful tool for surface characterization.     

Improvement of aramid fiber III reinforced bismaleimide composite interfacial adhesion by oxygen plasma treatment

Domestic Aramid Fiber III (DAF III) was modified by oxygen plasma treatment. The effects of oxygen plasma treatment power on fiber surface and DAF III reinforced bismaleimides (BMI) composite interfacial properties were investigated, respectively. The fiber surface characteristics were analyzed by X-ray photoelectron spectroscopy, Scanning Electron Microscopy, Atomic Force Microscopy and Dynamic Contact Angles Analysis, respectively. The results showed that oxygen plasma treatment introduced new oxygen containing groups such as C=O and –COO on to the fiber surfaces, changed the fiber surface morphologies and enhanced surface roughness by oxidative reactions and plasma etching. Finally, the fiber surface wettability was effectively improved. The total free energy increased from 49.8 to 71.7 mJ/m2 at maximum with 300 W oxygen plasma treatment. The composite interlaminar shear strength (ILSS) was evaluated by short beam shear measurement. The ILSS value increased from 49.3 to 59.8 MPa (by 21.3%) within 300 W plasma treatment.     

Effects of air dielectric barrier discharge plasma treatment time on surface properties of PBO fiber

In this paper, the effects of air dielectric barrier discharge (DBD) plasma treatment time on surface properties of poly(p-phenylene benzobisoxazole) (PBO) fiber were investigated. The surface characteristics of PBO fiber before and after the plasma treatments were analyzed by dynamic contact angle (DCA) analysis, scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). DCA measurements indicated that the surface wettability of PBO fiber was improved significantly by increasing the fiber surface free energy via air DBD plasma treatments. The results were confirmed by the improvement of adhesion of a kind of thermoplastic resin to PBO fiber which was observed by SEM, showing that more resin was adhering evenly to the fiber surface. AFM measurement revealed that the surface topography of PBO fiber became more complicated and the surface roughness was greatly enhanced after the plasma treatments, and XPS analysis showed that some new polar groups (e.g. OCO) were introduced on plasma treated PBO fiber surface. The results of this study also showed that the surface properties of PBO fiber changed with the elongation of plasma treatment time.     

Mechanism of adhesion between protein-based hydrogels and plasma treated polypropylene backing

We studied the mechanism of adhesion between N₂ plasma treated polypropylene (PP/N₂) backing and a hybrid hydrogel (HG) produced by chemical crosslinking between poly(ethylene glycol) and soy albumin. The work of adhesion, measured by peel testing, was found to be 25 times higher for PP/N₂ compared to untreated PP (≈5.0 J/m² versus ≈0.2 J/m²). In order to understand the adhesion mechanism, we performed a detailed analysis of the surface chemical composition of PP and PP/N₂ using X-ray photoelectron spectroscopy (XPS), chemical derivatization and attenuated total reflectance infra-red (ATR-IR) measurements. The results confirm incorporation of different nitrogen- (amine, amide,…) and oxygen- (hydroxyl, carboxyl,…) containing chemical groups on the PP/N₂ surface. The derivatized functions were primary amine, hydroxyl, carboxyl and carbonyl groups. Chemical derivatization reactions validated the XPS results (except for carbonyl groups), and they clearly underlined the essential role of primary amine groups in the adhesion process. In fact, after derivatization of the amine functions, the work of adhesion was found to be 0.41 ± 0.12 J/m². Participation of amine groups in the formation of covalent bonds at the interface between PP/N₂ and HG was directly confirmed by ATR-IR measurements.     

GaAs（100）表面氧化的XPS 研究

用X射线光电子能谱仪 (XPS)研究了砷化镓 (GaAs)晶片在空气中的热氧化和在紫外光 臭氧激发下的氧化反应 .分析了氧化层中的微观化学构成、表面化学计量比以及表面氧化层的厚度等 .研究表明 ,两种氧化方法的氧化过程不同 ,在砷化镓表面形成的氧化膜的厚度以及组成也不同 ,热氧化下氧化层主要由Ga2 O3、As2 O3、As2 O5 以及少量元素As组成 ,而且表面明显富镓 ;紫外光激发下生成的氧化物主要为Ga2 O3 和As2 O3 ,镓砷比与本体一致 .讨论了可能的反应机理 ,紫外光不仅将氧分子激发为激发态氧原子 ,增加了氧的反应活性 ;同时也激发了GaAs材料的价电子 ,使其更容易被氧化     

XPS analysis of down stream plasma treated wool: Influence of the nature of the gas on the surface modification of wool

A microwave plasma treatment in a down stream configuration was used to modify the natural hydrophobocity of untreated wool fibers. This property is a consequence of the presence of a Fatty acid monolayer (F-layer) on the outermost part of the fiber surface. The wool fibers treated with plasma were analyzed by means of X-ray photoelectron spectroscopy (XPS) without previous exposure to the air. Experiments have been carried out with air, water vapor, oxygen and nitrogen as plasma gas. The “in situ” analysis of the treated samples has permitted to differentiate between the plasma effects and those other linked to the exposure of the fibers to the air after their treatment. The results have evidenced the effects induced by the different active species generated by plasma from the different components of the air. In general, the intensity of CC peaks decreases and that of the CO, CO and OCO increases when using a gas containing oxygen species. Simultaneously, the intensity of the SS groups decreases and that of the sulphonate (SO₃⁻) increases. Other changes are also detected in the intensity of the N 1s level. The extent and characteristics of the oxidation and functionalisation of the hydrocarbon chains of the F-layer depend on the nature of gas. Thus, whereas treatments with plasmas of air and water vapor strongly affect the hydrocarbon chains of the F-layer, oxygen is less effective in the oxidation process. It has been also noted that the active species formed in the nitrogen plasma do not induce any significant change in the surface composition of the wool fibers.