Surface treatment of CFRP composites using femtosecond laser radiation

In the present work, we investigate the surface treatment of carbon fiber-reinforced polymer (CFRP) composites by laser ablation with femtosecond laser radiation. For this purpose, unidirectional carbon fiber-reinforced epoxy matrix composites were treated with femtosecond laser pulses of 1024 nm wavelength and 550 fs duration. Laser tracks were inscribed on the material surface using pulse energies and scanning speeds in the range 0.1–0.5 mJ and 0.1–5 mm/s, respectively. The morphology of the laser treated surfaces was investigated by field emission scanning electron microscopy. We show that, by using the appropriate processing parameters, a selective removal of the epoxy resin can be achieved, leaving the carbon fibers exposed. In addition, sub-micron laser induced periodic surface structures (LIPSS) are created on the carbon fibers surface, which may be potentially beneficial for the improvement of the fiber to matrix adhesion in adhesive bonds between CFRP parts.     

Effect of Alkali Treatment on Structure and Mechanical Properties of Acrylonitrile–Butadiene–Styrene/Bamboo Fiber Composites

The preparation and properties of wood–plastic composites (WPCs) based on acrylonitrile–butadiene–styrene (ABS) and bamboo fibers (BFs) are described. The BFs were first modified by alkali treatment in order to improve their adhesion to an ABS matrix. The BF modifications were monitored by Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). Styrene–maleic anhydride (SMA) copolymer, as a compatibilizer, was added to both the untreated and alkali-treated composites. The changes in the structure and the properties resulting from these treatments were observed by the SEM and mechanical tests. The experimental results indicated that both the alkali treatment of the BF and the inclusion of the SMA copolymer improved the interactions between the BF and ABS matrix, and promoted better mechanical properties of the composites.     

Effect of fiber surface treatments on the fiber–matrix interaction in banana fiber reinforced polyester composites

Cellulosic fibers have been used as cost-cutting fillers in plastic industry. Among the various factors, the final performance of the composite materials depends to a large extent on the adhesion between the polymer matrix and the reinforcement and therefore on the quality of the interface. To achieve optimum performance of the end product, sufficient interaction between the matrix resin and the cellulosic material is desired. This is often achieved by surface modification of the resin or the filler. Banana fiber, the cellulosic fibers obtained from the pseudo-stem of banana plant (Musa sepientum) is a bast fiber with relatively good mechanical properties. The fiber surface was modified chemically to bring about improved interfacial interaction between the fiber and the polyester matrix. Various silanes and alkali were used to modify the fiber surface. Modified surfaces were characterized by SEM and FTIR. The polarity parameters of the chemically modified fibers were investigated using the solvatochromic technique. The results were further confirmed by electrokinetic measurements. Chemical modification was found to have a profound effect on the fiber–matrix interactions. The improved fiber–matrix interaction is evident from the enhanced tensile and flexural properties. The lower impact properties of the treated composites compared to the untreated composites further point to the improved fiber–matrix adhesion. In order to know more about the fiber–matrix adhesion, fractured surfaces of the failed composites where further investigated by SEM. Of the various chemical treatments, simple alkali treatment with NaOH of 1% concentration was found to be the most effective. The fiber–matrix interactions were found to be dependent on the polarity of the modified fiber surface.     

Studies of dielectric relaxation in natural fiber–polymer composites

Polymer composites of a polyester resin matrix filled with short palm tree lignocellulosic fibers were studies by means of dielectric spectroscopy in the frequency range 0, 1–100 kHz and temperature interval from 40 °C to 200 °C. Three relaxations processes were identified, namely the orientation polarization imputed to the presence of polar water molecules in Palm fiber, the relaxation process associated with conductivity occurring as a result of the carriers charges diffusion noted for high temperature above glass transition and low frequencies, and the interfacial relaxation that is attributable to the accumulation of charges at the Palm fibers/polyester interfaces.     

Enhanced surface free energy of polyimide fibers by alkali treatment and its interfacial adhesion behavior to epoxy resins

In this article, polyimide (PI) fibers were modified by alkali treatment, and PI fiber-reinforced epoxy composites were fabricated. The effects of different alkali treatment times on the surface properties of the PI fibers and the adhesion behaviors of PI fiber/epoxy composites were studied. The surface morphologies, chemical compositions, mechanical properties, and surface free energy of the PI fibers were characterized by atomic force microscopy, X-ray photoelectron spectroscopy, single-fiber tensile strength analysis, and dynamic contact angle analysis, respectively. The results show that alkali treatment plays an important role in the improvement of the surface free energy and the wettability of PI fibers. We also found that, after the 3 min, 30 °C, 20 wt% NaOH solution treatment, the fibers possessed good mechanical properties and surface activities, and the interlaminar shear strength of the composites increased to 64.52 MPa, indicating good interfacial adhesion properties.     

Dielectric and impedance studies of DBSA doped polyaniline/PVC composites

Polyaniline (PANI) was doped with dodecylbenzene sulfonic acid (DBSA) and then mixed with PVC by solution blending method to prepare DBSA doped PANI (PAND)/PVC composites. FTIR spectroscopy indicates the strong dipole–dipole interaction between the individual components of the composites. The ac electrical properties of the synthesized composites were investigated by complex impedance spectroscopy in the frequency range of 0.5–10⁶ Hz at room temperature. Both dielectric loss factor and permittivity increase with the decrease of frequency exhibiting strong interfacial polarization at low frequency. Addition of PAND in PVC reduces the charge trapping centers by increasing the number of conducting channels participating in the relaxation process; hence an increase in conductivity is observed.     

Fabrication and Flexural Properties of Bagasse Fiber Reinforced Biodegradable Composites

Biodegradable composites made from bagasse fiber and biodegradable resin were fabricated and the flexural properties of the composites investigated in terms of the effects of fiber length, fiber volume fraction, and different alkali treatments of the bagasse fibers. The flexural properties of the composites increased with the increase in fiber length but decreased below the critical fiber length. The flexural properties increased with the increase in fiber volume fraction. The scanning electron microscope (SEM) micrographs showed that compression of the cellulose structure of bagasse fiber after preparation could have caused enhancement in the flexural properties. Furthermore, when comparing the effects of different alkali treatments of the bagasse fibers, maximum improvement in the flexural properties was observed for the 1% NaOH solution treated fiber composites. After alkali treatment, fibrillation occurred and the surface of the treated fibers became finer; this could contribute to improvement in the fiber‐matrix adhesion and result in enhancing the flexural properties.     

Short sisal fiber reinforced polypropylene composites: the role of interface modification on ultimate properties

Sisal fibers have been used for the reinforcement of polypropylene matrix. The compatibilization between the hydrophilic cellulose fiber and hydrophobic PP has been achieved through treatment of cellulose fibers with sodium hydroxide, isocyanates, maleic anhydride modified polypropylene (MAPP), benzyl chloride and by using permanganate. Various fiber treatments enhanced the tensile properties of the composites considerably, but to varying degrees. The SEM photomicrographs of fracture surfaces of the treated composites clearly indicated the extent of fiber–matrix interface adhesion, fiber pullout and fiber surface topography. Surface fibrillation is found to occur during alkali treatment which improves interfacial adhesion between the fiber and PP matrix. The grafting of the fibers by MAPP enhances the tensile strength of the resulting composite. It has been found that the urethane derivative of polypropylene glycol and cardanol treatments reduced the hydrophilic nature of sisal fiber and thereby enhanced the tensile properties of the sisal–PP composites, as evident from the SEM photomicrographs of the fracture surface. The IR spectrum of the urethane derivative of polypropylene glycol gave evidence for the existence of a urethane linkage. Benzoylation of the fiber improves the adhesion of the fiber to the PP matrix. The benzoylated fiber was analyzed by IR spectroscopy. Experimental results indicated a better compatibility between benzoylated fiber and PP. The observed enhancement in tensile properties of permanganate-treated composites at a low concentration is due to the permanganate-induced grafting of PP on to sisal fibers. Among the various treatments, MAPP treatment gave superior mechanical properties. Finally, experimental results of the mechanical properties of the composite have been compared with theoretical predictions.     

Study of impact properties and morphology of unidirectional bamboo strips–polyester composites: effect of mercerization

Composites were fabricated with alkali (10%, 15% and 20%) treated bamboo fibers incorporated to the extent of 50% (by volume) and polyester resin. Impact test was made on bamboo strips and composites samples. It was observed that the fracture energy undergoes an increase from untreated to alkali treated bamboo strips. Alkali treated bamboo fiber composites show higher fracture energy value than the untreated bamboo fiber composites. The phenomenal change was quite evident from scanning electron micrographs of the fractured surface. Considering the effects of all factors, the work of fracture shows maximum value in the case of 20% alkali treated bamboo strip composites. It was also observed that the rate of increase of work of fracture value is much higher in the case of composite samples than the bamboo sample. It was explained on the basis of synergism obtained by improved interfacial adhesion between fiber and matrix, and removal of hemicellulose from the bamboo itself, which was evident from the intermolecular H-bonding formation studied by FT-IR.     

Microcellular and Solid Polylactide–Flax Fiber Composites

Polylactide–flax fiber composites with 1, 10 and 20 wt% fiber were melt-compounded and subsequently molded via the conventional and microcellular injection-molding processes. Silane was used as a coupling agent. The effects of fiber and silane content on cell morphology, static and dynamic mechanical properties, and crystallization properties have been studied. The average cell size decreased while the cell density increased with the fiber content. The degree of crystallinity increased with the fiber content. Silane treatment of fibers affected neither the cell morphology nor the degree of crystallinity. The toughness and strain-at-break of solid samples decreased with the fiber content while silane treatment increased both properties; however, neither fiber content nor silane treatment had much influence on the toughness and strain-at-break of microcellular samples. The specific modulus of both solid and microcellular samples increased with the fiber content. The specific strength of the solid and microcellular PLA–flax composites were only slightly lower than that of their solid and microcellular pure PLA counterparts. Overall, the toughness, strain-at-break, and specific strength of microcellular samples were found to be lower than that of their solid counterparts. The storage modulus of the PLA–flax composites with 10 and 20% fiber contents was higher than that of pure PLA.     

Dielectric properties of short sisal/coir hybrid fibre reinforced natural rubber composites

The dielectric properties, such as dielectric constant, volume resistivity and dielectric loss factor, of sisal/coir hybrid fibre reinforced natural rubber composites have been studied as a function of fibre loading, fibre ratio, frequency, chemical modification of fibres and the presence of a bonding agent. The dielectric constant values have been found to be higher for fibre filled systems than pure natural rubber. This has been attributed to the polarization exerted by the incorporation of fibres into the matrix. Dielectric constant values were observed to be decreased with increase in frequency due to the decreased interfacial and orientation polarization at higher frequencies. Whereas dielectric constant increases with fibre loading because of the increment in number of polar groups after the addition of hydrophilic lignocellulosic fibres. The volume resistivity of the composites was found to be decreased with fibre loading and a percolation threshold has been obtained at 15.6% volume of fibres. Fibre treatment, such as alkali, acetylation, benzoylation, peroxide and permanganate, were carried out to improve the adhesion between fibres and matrix. The dielectric constant values were lower for systems consisting of fibres subjected to chemical treatments due to the increased hydrophobicity of fibres. The addition of a two-component dry bonding agent consisting of hexamethylene tetramine and resorcinol, used for the improvement of interfacial adhesion between the matrix and fibres, reduced the dielectric constant of the composites. When the weight percentage of sisal fibre was increased in the total fibre content of the hybrid composites, the dielectric constant was found to increase. The added fibres and different chemical treatments for them increased the dielectric dissipation factor. A dielectric relaxation has been observed at a frequency of 5 MHz.     

Effects of atomization conditions on morphology and SOFC anode performance of spray pyrolyzed NiO–Sm0.2Ce0.8O1.9 composite particles

NiO–Sm_0.2Ce_0.8O_1.9 (NiO–SDC) composite particles were synthesized by spray pyrolysis (SP). SP resulted in composite particles of NiO enveloped with SDC and these capsule-type composite particles would reduce aggregation of Ni during the reduction from NiO to Ni metals. SOFC anode microstructures and morphologies of NiO–SDC composite precursor particles much affects on SOFC power densities or anode polarization. Therefore, we focused on atomizing conditions of SP process. Relationship between ultrasonic atomization conditions and morphologies of NiO–SDC composites were investigated by controlling temperatures of atomization vessels. The atomizing temperature changed concentration of mists in the vessel, and mean particle size and particle size distribution were increased with an increase in temperature of the atomization vessels. Some extremely large particles were observed by synthesizing at higher atomization temperatures. Large particles contained voids in the particles. The voids in the composite particles would play a role of pore-formers. SOFC measurement showed the synthesis at the atomizing temperature of 30 °C resulted in the high-performance anode. The atomizing process of SP much affected morphology of anode precursor particles, and the atomizing conditions were important to improve anode performance.     

Properties of Eu-doped zinc oxide thin films grown on glass substrates by radio-frequency magnetron sputtering

Eu-doped ZnO (EZO) thin films were prepared on glass substrates at various growth temperatures by radio-frequency magnetron sputtering. The properties of deposited thin films showed a significant dependence on the growth temperature. The preferential growth orientation of all the thin films was occurred along the ZnO (002) plane. The maximum crystallite size and the minimum average transmittance in the wavelength range of 450–1100 nm were observed for the EZO thin film deposited at 25 °C. A red shift of the optical band gap was observed in the growth temperature range of 25–300 °C. The highest figure of merit, an index for evaluating the performance of transparent conducting thin films, was obtained at 200 °C of growth temperature. These results indicated that the high-quality EZO film was obtained at a growth temperature of 200 °C.     

Evidence of sustained ferroelectricity in glycine sodium nitrate single crystal

The nonlinear optical single crystals of glycine sodium nitrate were grown by the slow evaporation method. XRD confirmed monoclinic structure. Thermal stability and melting point (225 °C) were investigated. The dielectric behaviour of the crystals in the frequency range 20 Hz–2 MHz at different temperatures is reported in which a ferroelectric to paraelectric phase transition at T_c = 56 °C is observed. The activation energies of GSN were found to be 3.615 eV, 0.593 eV and 0.0733 eV in three temperature regions of conductivity plot due to a hopping conduction mechanism. The crystal has shown high piezoelectric charge coefficient (d₃₃) of 16 pC/N which is nearly double of observed value for γ-glycine single crystal. The spontaneous polarization P_s at room temperature was found to be 1.489 μC/cm² at applied maximum field of 26 kV/cm (1.194 μC/cm² at 12 kV/cm) and the pyroelectric coefficient was determined to be 400 μC/m²/°C. High value of squareness parameter (1.93) makes the GSN crystal suitable for switching applications. Detailed investigations of Ferro-/Piezoelectricity were observed for the first time in glycine sodium nitrate crystals which was found to preserve the ferroelectricity even after applying an electric field much higher than the saturation electric field (12–26 kV/cm). Application of GSN crystals as sensor, high power switch gears and storage memories has been established.     

Effect of curing temperature,fibre loading and bonding agent on the equilibrium swelling of isora-natural rubber composites

Isora fibre-reinforced natural rubber (NR) composites were cured at 80, 100, 120 and 150°C using a low temperature curing accelerator system. Composites were also prepared using a conventional accelerator system and cured at 150°C. The swelling behavior of these composites at varying fibre loadings was studied in toluene and hexane. Results show that the uptake of solvent and volume fraction of rubber due to swelling was lower for the low temperature cured vulcanizates which is an indication of the better fibre/rubber adhesion. The uptake of aromatic solvent was higher than that of aliphatic solvent, for all the composites. As the fibre content increased, the solvent uptake decreased, due to the superior solvent resistance of the fibre and good fibre–rubber interactions. The bonding agent improved the swelling resistance of the composites due to the strong interfacial adhesion. Due to the improved adhesion between the fibre and rubber, the ratio of the change in volume fraction of rubber due to swelling to the volume fraction of rubber in the dry sample (V_τ ) was found to decrease in the presence of bonding agent. At a fixed fibre loading, the alkali treated fibre composite showed a lower percentage swelling than untreated one for both systems showing superior rubber–fibre interactions.     

Ultrasound-assisted synthesis of ZnO photocatalysts for gas phase pollutant remediation: Role of the synthetic parameters and of promotion with WO3

The synthesis of ZnO photocatalysts by ultrasound-assisted technique was here investigated. Several experimental parameters including the zinc precursor (acetate, chloride, nitrate), sonication conditions (amplitude, pulse) and post-synthetic thermal treatment (up to 500 °C) were studied. Crystalline ZnO samples were obtained without thermal treatments due to the adopted reactant ratios and synthesis temperature. Sonication plays a major role on the morphological oxide features in terms of particle size and surface area, the latter showing a 20-fold increase with respect to conventional synthesis. Interestingly, 1 and 3 s sonication pulses led to morphological properties similar to continuous sonication. A thermal treatment at moderate temperatures (400–450 °C) promoted the loss of surface hydroxylation and the formation of lattice defects, while higher temperatures were detrimental for the sample morphology. The prepared ZnO was decorated with WO₃ particles comparing an ultrasound-assisted technique using 1 s pulses with a conventional approach, giving rise to composites with promoted visible light absorption. Samples were tested towards the photocatalytic degradation of nitrogen oxides (500–1000 ppb) in humidified air under both UV and visible light. By carefully controlling the synthetic procedure, better performance were observed with respect to the commercial benchmark. Samples from ultrasound-assisted syntheses, also in the case of pulsed sonication, showed consistently better results than conventional references, in particular for ZnO-WO₃ composites. The composite by ultrasound-assisted synthesis showed > 95% degradation in 180 min and doubled NO_x degradation under visible light with respect to the conventional composite.     

Densification mechanism of polyacrylonitrile-based carbon fiber during heat treatment

Polyacrylonitrile (PAN)-based carbon fibers were heat treated at various temperatures for varying durations to simulate the graphitization process in the manufacture of C/C composites. Densification of the resulting fibers was confirmed by density measurement. The composition and structure of the fibers were investigated by means of elemental analysis, X-ray diffraction and Raman spectroscopy. For specified isothermal heat treatment time, the structural parameters depended strongly on heat treatment temperature. The nitrogen content decreased with increased heat treatment temperature and extended time at constant temperature. Nitrogen loss was complete at temperatures above 1900 °C. The graphite crystallite size increased rapidly with increasing heat treatment temperature, and slowly with extended isothermal heat treatment time. At 2100 °C a more ordered graphitic structure appeared. Denitrogenation induced “puffing”, which made the fibers expand. Decrease in density in the heat treatment temperature range 1500-1900 °C originated from the abrupt evolution of nitrogen, and above 1900 °C the graphitization transition induced steadily increasing density. Densification of the carbon fibers was determined both by the rate of denitrogenation and the rearrangement of carbon atoms.     

Temperature-induced changes in morphology and structure of TiO2-Al2O3 fibers

Electrospinning of a sol-gel and polymer mixture is used to produce titania-alumina (TiO₂-Al₂O₃) fibers with diameters ranging from 200 to 800 nm. These composite metal-oxide fibers were calcined at various temperatures and their morphology is studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The decrease in the average diameter of the fibers with increasing temperature is observed. Powder X-ray diffraction (XRD) reveals that up to 800 °C the composite fibers have anatase titania structure whereas at 900 °C the fibers exhibit mixture of anatase and rutile phases. It is found that specific surface area decreases as a function of temperature in the 700-900 °C range. The change in phase (anatase-to-rutile) and the increase in crystallite size occur simultaneously. The presence of smaller amount of amorphous alumina in the primarily titania-based structure seems to play the role in stabilizing the anatase phase.     

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.     

Modified flax fibers reinforced soy-based composites: mechanical properties and water absorption behavior

Flax fibers are often used in reinforced composites which have exhibited numerous advantages such as high mechanical properties, low density and biodegradablility. On the other hand, the hydrophilic nature of flax fiber is a major problem. In this study, we prepare the soybean oil based composites reinforced with protein coated and lipid acylated flax fibers and compare their water uptake properties. Results showed that water resistance properties of the composites are improved where treated flax fibers are used. The composite with lipid acylation of the flax fiber exhibited to enhance tensile strength and water resistance properties. Influences of fiber length, fiber loading and pressure on mechanical properties are also reported.