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.     

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.     

Effects of plasma surface modification on the mechanical properties of carbon fiber and carbon fiber/epoxy composite

_The effect of surface treatment on mechanical properties of carbon fibers has been investigated by application of plasma polymerization of selected monomers in the vapor phase. The role of the fiber-matrix interface on carbon fiber-reinforced epoxy resin composites has also been studied. Composites have been prepared separately by the use of plasma-modified and unmodified carbon fibers in the epoxy resin matrix. The mechanical properties of carbon fibers (Hercules and Grafil) as well as of fiber/epoxy composites were examined by using single filament and three-point bending tests, respectively. It was observed that plasma polymerization treatment at selected plasma conditions led to significant improvement of interlaminar shear and flexural strength values of composites.     

Quantitative evaluation of interfacial adhesion between fiber and resin in carbon fiber/epoxy composite cured by semiconductor microwave device

Interfacial adhesion between carbon fiber (CF) and epoxy resin in carbon fiber-reinforced epoxy composite, which was prepared by different heating process such as semiconductor microwave (MW) device and conventional electric oven, has been evaluated quantitatively. The interfacial shear strength (IFSS) between CF and epoxy resin, which was an indicator of adhesion on the interface, was measured by a single fiber fragmentation test. The single fiber fragmentation test showed that the IFSSs of the prepared specimens were different by heating methods. In the case of MW process, the curing reaction of epoxy resin on the CF interface would be progressed preferentially due to the selective heating of CF, resulting that the IFSSs of specimens prepared by MW irradiation were increased by enhancing the output power of MW. However, the IFSSs of the specimens were decreased by excessively high output power because the matrix resin on the CF interface was thermally degraded. As results, by optimizing the MW conditions of output power and irradiation time, the IFSS of the sample cured by MW was increased by 21% as compared to oven-heated one. It was found that the interfacial adhesion between CF and epoxy resin would be improved by the MW-assisted curing reaction on the surface of CF.     

The effect of surface modification on the properties of sisal fiber and improvement of interfacial adhesion in sisal/starch composites induced by starch nanocrystals

A facile approach was utilized to introduce starch nanocrystals (SNCs) onto sisal fiber (SF) to improve the interfacial adhesion between SF and starch. For this, fibers were treated with alkali and then subjected to cold plasma treatment to increase the accessibility with SNCs, which was confirmed through X-ray photoelectron spectroscopy (XPS). It was found that due to the influence of cold plasma treatment, new functional groups were introduced onto SF. The surface characteristics of SF were examined by Fourier transform infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM). The observed results suggested that SNCs were successfully distributed onto SF. Tensile strength and interfacial shear strength of fibers treated under different conditions were calculated and compared through a two-parameter Weibull model. The highest interfacial shear strength of 3.05 MPa was obtained by Alkali-300 W-SNCs, which indicated an increase of 80.6% than untreated SF. It has also been proved that the starch nanocrystals produced hydrogen bonding and physical interlocking between sisal fiber and starch. Notably, the outcome of this investigation indicates that SNCs may be applied for the fabrication of high performance, environmentally friendly sisal/starch composites for a range of technological applications.     

Improvement of interfacial adhesion in vertical GaN-based LEDs by introducing O2 plasma cleaning and intermediate layers

Interfacial adhesion between an indium tin oxide (ITO)/Ni/Ag/Ni/Au p-electrode, and Au and Ni/Au seeds in vertical GaN-based light emitting diodes (LEDs) was enhanced by O₂ plasma cleaning treatment of the Au surface in the p-electrode. However, AES and REELS analyses of the Au surface in the p-electrode detected surface damage to the p-electrode and photoresist (PR) passivation structure from O₂ plasma cleaning. W/Ni and Al/Ni adhesion layers were introduced in the Au seed to increase interfacial adhesion between Au seed and untreated PR passivation. Forward leakage current as low as 0.91 nA at 2 V was observed for the vertical LED with the Al/Ni/Au seed, for which adhesion strength to O₂ plasma-cleaned Au and untreated PR was 141.2 MPa and 62.8 MPa, respectively.     

表面等离子体波光纤传感器应用于复合材料固化监测的研究

对适用于机敏结构的表面等离子体波光纤传感器进行了初步的研究。将这种光纤传感器埋入复合材料结构就构成了所谓机敏结构。这种机敏结构既可进行复合材料的固化监测,又可进行应变检测。有利于传感器数量的减少和布置的简化,减少了传感元件的埋入对结构本身性能的影响。可以充分发挥光纤传感器对结构进行全过程监测的优点,具有广泛的应用前景。     

The gamma irradiation of PBO fiber on the mechanical and tribological properties of PTFE composites

The mechanical and tribological behavior of gamma irradiated poly(p-phenylene benzobisoxazole) (PBO) fiber filled polytetrafluoroethylene (PTFE) composites was investigated. The gamma irradiated PBO fiber composite had the highest inter-laminar shear strength value of all the combinations because its higher bond strength may have hindered a large fiber/matrix debonding. X-ray photoelectron spectroscopy results indicate that the contents of polar groups on the surface of gamma irradiated PBO fiber increase compared to PBO fiber. The wear tests were conducted on a ring-on-block apparatus using composite block against polished metal counterparts under dry sliding conditions. It can also be found that gamma irradiation treatment was helpful to the improvement of the anti-wear ability of the PTFE composite which was related to the abrasive wear mechanism.     

Improvement in micro-structural and mechanical properties of zinc film by surface treatment with low temperature argon plasma

Nanocrystalline zinc films were deposited on gold coated borosilicate glass substrates by thermal evaporation method using zinc powders as the source material and then treated with argon plasma at various temperatures. From X-ray diffraction study, the as-deposited films are found to be metallic Zn and polycrystalline in nature. The crystalline nature improves with the increase of temperature up to 200 °C and decreases with the further increase of temperature to 300 °C. The binding energy observed for Zn 2p_3/2, and the binding energy separation between Zn 2p_3/2 and Zn 2p_1/2 in the X-ray photoelectron spectrum indicate that the films are metallic zinc films. Transmission electron microscopic study shows hexagonal shaped grains having size ∼58 nm upon treatment with Ar plasma. It is clearly shown the grain growth and distinct grain boundary with the increase in temperature. The average Young's modulus (E) and hardness (H) are measured to be 84 GPa and 4.0 GPa for as-deposited film, whereas 98 GPa and 5.8 GPa for plasma treated film at 200 °C. The enhancement in mechanical properties is attributed to improvement in crystalline nature of the film and better interlinking between grains and boundaries.     

Enhancement of the molecular nitrogen dissociation and ionization levels by argon mixture in flue nitrogen plasma

In this work, the nitrogen molecular dissociation and ionization levels in Ar/N₂ flue plasma are evaluated as functions of plasma parameters such as Ar mixture quantity and N₂ flux in order to obtain the best condition for various applications such as thin film deposition and material surface modification. This plasma is operated at 10 kV and the nitrogen dissociation rate is determined by analyzing the optical emission of the nitrogen band. For different operating conditions, the dissociation rate [N] of N₂ molecules was enhanced, as the mixture quantity of Ar increased from 0.06 m³/h to 0.9 m³/h and the max of enhancement factor is 4.3. This factor becomes bigger when the N₂ flux becomes bigger. Moreover, the molecular nitrogen ionization density is calculated from the current intensity of the plasma. The ionization density was also enhanced, as the mixture quantity of Ar increased from 0.1 m³/h to 1.5 m³/h, under three different voltages. The max of enhancement factor of 1.96 is much smaller than the factor of the dissociation rate. These results are discussed in terms of the kinetics of the electrons, nitrogen ions, atoms and molecules.     

Surface treatment of aramid fiber by air dielectric barrier discharge plasma at atmospheric pressure

Aramid fiber samples are treated by air dielectric barrier discharge (DBD) plasma at atmospheric pressure; the plasma treatment time is investigated as the major parameter. The effects of this treatment on the fiber surface physical and chemical properties are studied by using surface characterization techniques. Scanning electron microscopy (SEM) is performed to determine the surface morphology changes, X-ray photoelectron spectroscopy (XPS) is analyzed to reveal the surface chemical composition variations and dynamic contact angle analysis (DCAA) is used to examine the changes of the fiber surface wettability. In addition, the wetting behavior of a kind of thermoplastic resin, poly(phthalazinone ether sulfone ketone) (PPESK), on aramid fiber surface is also observed by SEM photos. The study shows that there seems to be an optimum treatment condition for surface modification of aramid fiber by the air DBD plasma. In this paper, after the 12 s, 27.6 W/cm³ plasma treatment the aramid fiber surface roughness is significantly improved, some new oxygen-containing groups such as C-O, CO and OC-O are generated on the fiber surface and the fiber surface wettability is greatly enhanced, which results in the better wetting behavior of PPESK resin on the plasma-treated aramid fiber.     

Influence of ethylene glycol pretreatment on effectiveness of atmospheric pressure plasma treatment of polyethylene fibers

For atmospheric pressure plasma treatments, the results of plasma treatments may be influenced by liquids adsorbed into the substrate. This paper studies the influence of ethylene glycol (EG) pretreatment on the effectiveness of atmospheric plasma jet (APPJ) treatment of ultrahigh molecular weight polyethylene (UHMWPE) fibers with 0.31% and 0.42% weight gain after soaked in EG/water solution with concentration of 0.15 and 0.3 mol/l for 24 h, respectively. Scanning electron microscopy (SEM) shows that the surface of fibers pretreated with EG/water solution does not have observable difference from that of the control group. The X-ray photoelectron spectroscopy (XPS) results show that the oxygen concentration on the surface of EG-pretreated fibers is increased less than the plasma directly treated fibers. The interfacial shear strength (IFSS) of plasma directly treated fibers to epoxy is increased almost 3 times compared with the control group while that of EG-pretreated fibers to epoxy does not change except for the fibers pretreated with lower EG concentration and longer plasma treatment time. EG pretreatment reduces the water contact angle of UHMWPE fibers. In conclusion, EG pretreatment can hamper the effect of plasma treatment of UHMWPE fibers and therefore longer plasma treatment duration is required for fibers pretreated with EG.     

The research on the interfacial compatibility of polypropylene composite filled with surface treated carbon fiber

Dielectric barrier discharges (DBD) in ambient air are used on carbon fiber to improve the fiber surface activity. Carbon fibers with length of 75 μm are placed into the plasma configuration. The interaction between modified carbon fibers and polypropylene (PP) was studied by three-point bending (TPB) test. The chemical changes induced by the treatments on carbon fiber surface are examined using X-ray photoelectron spectroscopy (XPS). XPS results reveal that the carbon fiber modified with the DBD at atmospheric pressure show a significant increase in oxygen and nitrogen concentration. These results demonstrate that the surface of the carbon fiber is more active and hydrophilic after plasma treatments using a DBD operating in ambient air.     

Relation between interfacial shear strength and compressive strength of carbon fiber/epoxy resin composite strands

The mechanism with which the fiber-matrix interfacial strength exerts its influence on the compressive strength of fiber reinforced composites has been studied by measuring the axial compressive strength of carbon fiber/epoxy resin unidirectional composite strands having different levels of interfacial shear strength. The composite strands are used for experiments in order to investigate the compressive strength which is not affected by the delamination taking place at a weak interlayer of the laminated composites. The interfacial strength is varied by applying various degrees of liquid-phase surface treatment to the fibers. The efficiency of the compressive strength of the fibers utilized in the strength of the composite strands is estimated by measuring the compressive strength of the single carbon filaments with a micro-compression test. The compressive strength of the composite strands does not increase monotonically with increasing interfacial shear strength but showes lower values at higher interfacial shear strengths. With increasing interfacial shear strength, the suppression of the interfacial failure in the misaligned fiber region increases the compressive strength, while at higher interfacial shear strengths, the enhancement of the crack sensitivity decreases the compressive strength.     

Effects of residual stress and interfacial frictional shear stress on interfacial debonding at notch-tip in two-dimensional unidirectional composite

A calculation method based on the shear lag approach was presented to get an approximate estimate of influences of residual stresses and frictional shear stress at the debonded interface on the interfacial debonding behavior at the notch-tip along fiber direction in two-dimensional unidirectional double-edge-notched composites. With this method, the energy release rate for initiation and growth of debonding as a function of composite stress were calculated for some examples. The calculation results showed in outline how much the tensile and compressive residual stresses in the matrix and fiber along fiber direction, respectively, act to hasten the initiation and growth of the debonding when the final cut element in the notch is matrix, while they act to retard them when the final cut element is fiber, and how much the frictional shear stress at the debonded interface reduces the growth rate of the debonding.     

Improving the interfacial strength of PMMA resin composites by chemically grafting graphene oxide on UHMWPE fiber

Controlling interfacial microstructure and interactions between (ultra high molecular weight polyethylene) UHMWPE fiber and matrix is of crucial importance for the fabrication of advanced polymer composites. In this paper, (UHMWPE fiber-g-graphene oxide [GO]) was prepared. GO nanoparticles distributed onto the ?ber surface uniformly, which could increase surface polarity and roughness. Increases of interlaminar shear strength (ILSS) and interfacial shear strength (IFSS) of UHMWPE fiber-g-GO composites were achieved. These enhancements can be attributed to the existent of GO interface with providing chemical bonding and strong mechanical interlocking between the ?ber and matrix. Moreover, impact resistance of UHMWPE fiber-g-GO composites was enhanced.     

氦等离子体处理对纳米二氧化硅溶胶涂覆T300碳纤维拉伸性能的影响

氦等离子体处理纳米二氧化硅溶胶涂覆T300碳纤维能构造出特定空间结构形态的纳米涂覆层.扫描电子显微镜照片显示,经氦等离子体处理后纳米二氧化硅溶胶涂覆T300碳纤维的纳米涂覆层在纤维表面分布均匀,起到填补纤维表面微观缺陷的功能.X射线光电子能谱及傅里叶变换红外光谱显示,纤维表面被引入了活性官能团,纳米二氧化硅涂覆层与碳纤维间有表面激活反应.形成纳米界面结构的T300碳纤维表面与纳米二氧化硅涂覆层间的相互作用符合艾琳方程,利用热激活体积可以对其相互作用进行定量分析.拉伸试验表明,屈服塑性变形导致纳米界面结构热激活,纳米微粒阻碍碳纤维表面大分子链形貌变化的热激活体积是纳米界面结构性能的重要表征. 关键词： 激活体积 溶胶涂覆 氦等离子体 纳米界面结构     

Preparation of vertically aligned carbon nanotube arrays grown onto carbon fiber fabric and evaluating its wettability on effect of composite

Vertically aligned carbon nanotube (CNT) arrays have been grown onto the carbon fiber fabric using a catalytic chemical vapor deposition (CCVD) method. The as-synthesized CNT arrays are about 20 μm in height, and the nanotube has a mean inner and outer diameter of 2.6 nm, 5.5 nm, respectively. The CNT-grafted carbon fabric shows a hydrophobic property with a contact angle over 145°, and the single CNT-grafted carbon fiber shows a sharp increase of dynamic contact angle in de-ionized water from original 71.70° to about 103°, but a little increase does in diiodomethane or E-51 epoxy resin. However, the total surface energy of carbon nanotube-grafted carbon fiber is almost as same as that of as-received carbon fiber. After CNTs growth, single fiber tensile tests indicated a slight tensile strength degradation within 10% for all different lengths of fibers, while the fiber modulus has not been significantly damaged. Compared with the as-received carbon fibers, a nearly 110% increase of interfacial shear strength (IFSS) from 65 to 135 MPa has been identified by single fiber pull-out tests for the micro-droplet composite, which is reinforced by as-received carbon fiber or CNT-grafted carbon fiber.