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Highlights: [•] Grafting of thiol groups at the surface of carbon fibers. [•] Observation of the carbon fiber surface by scanning electron microscopy. [•] Characterization of the grafting mechanism by X-ray photoelectron spectroscopy. [•] Assessment of the adhesion strength by the pull-out test. [ABSTRACT FROM AUTHOR]

Acrylate functionalities were grafted at the surface of carbon fibers in order to improve the adhesion strength with an acrylate matrix cured by electron beam. An isocyanate bearing aliphatic urethane acrylate was used as a coupling agent. As revealed by X-ray photoelectron spectroscopy, the isocyanate groups reacted with carboxylic acids and hydroxyl groups located at the surface of the fiber, leading to a covalent bonding of the acrylate groups. The adhesion strength was measured by a micromechanical test derived from the pull-out test. A significant improvement of the interfacial shear strength was obtained (+91%) with an electron beam curing. For comparison, an isothermal cure by UV was also investigated and led to the same level of adhesion strength. The improvement was also proved by an increase in the 90° flexural strength of unidirectional composites (+38%). Grafting functionalities that were compatible with the radical mechanism of the polymerization of the matrix appeared to be a promising strategy for the improvement of the mechanical properties of carbon fiber–acrylate composites cured by electron beam. [ABSTRACT FROM AUTHOR]

Oxygen plasma was used to modify the surface properties of carbon fibers and their adhesion strength with an acrylate resin cured by electron beam. A characterization of the surface topography and the surface chemistry was carried out (topography at a micrometric and nanometric scale, specific surface area, temperature programmed desorption, and X-ray photoelectron spectroscopy). The topography remained unchanged. Regarding the surface chemistry, carboxylic acids, alcohols, lactones, and ethers were created and their location was at the outer surface of the fibers. A pull-out test was used to measure the adhesion strength with the acrylate resin cured by electron beam. For comparison, an isothermal UV curing was also investigated. The value of the interfacial shear strength was increased only in the case of UV curing. No improvement was observed with electron beam curing, which highlighted the generation of an interphase, the mechanical properties of which are dependent on the processing conditions. [ABSTRACT FROM PUBLISHER]

A time-dependent oxidation of carbon fibers in boiling nitric acid was used to investigate the influence of a modification of the fiber surface properties on the adhesion strength with an acrylate resin cured by electron beam (EB). For each time of treatment, a characterization of the surface topography and the surface chemistry was done (topography at a micrometric and nanometric scale, specific surface area, temperature programmed desorption, X-ray photoelectron spectroscopy analysis). The oxidation of the fiber surface in boiling nitric acid created a rough surface, which significantly increased the specific surface area, and also generated a high density of hydroxyl groups, carboxylic acids and lactones in comparison to untreated fibers. The adhesion strength with the acrylate resin cured by EB was measured by a pull-out test. For comparison, an isothermal ultraviolet curing of the matrix was also investigated. The value of the interfacial shear strength, determined by the Greszczuk's model, was increased by the oxidation of the carbon fiber surface for both curing processes, but lower values were systemically obtained with EB curing. Copyright © 2012 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]

Abstract: Zinc oxide thin films are deposited on polyethylene terephthalate (PET) by r.f. magnetron sputtering process from a ceramic target in oxygen–argon plasmas. Structural studies show that the thin films are highly oriented along the (002) direction of the würtzite phase when the oxygen partial pressure is lower than 0.2Pa. The crystallinity is accentuated when the oxygen partial pressure of the sputtering gas is increased from 0 to 0.02Pa. The composition of the films determined by Rutherford backscattering spectrometry (RBS) varies in a wide range and it is necessary to add a few amount of oxygen in the plasma composition to establish the stoichiometry. The oxygen partial pressure is found to influence also the microstructure and consequently the density of the coatings. Various cold plasmas are used to treat the polymer surface before the deposition of zinc oxide films. Wettability measurements show an increase in the polar component of the PET surface free energy whatever the nature of the plasma used for the treatment. This increase is more obvious with the carbon dioxide plasma. XPS examinations of the CO2 plasma treated PET surface in optimized conditions show a functionalisation of the polymer surface. The carbon dioxide plasma treatments of PET surface are found to enhance the peeling energy. The adhesion level depends also on the sputtering parameters, mainly the oxygen partial pressure and the r.f. power which influence the coating properties. The zinc oxide/PET interface is studied by XPS at the different stages of deposition and at various take-off angles. AFM observations show a regular growth of zinc oxide layers with smooth topographies on PET films. The different findings obtained from C1s, O1s, Zn2p3/2, Zn3p peaks and Auger Zn L3M4.5M4.5 peak are corroborated and discussed. New chemical bonds between the polymer and the further coming zinc oxide thin layer are evidenced. [Copyright &y& Elsevier]

Abstract: At first, X-ray photoelectron spectroscopy (XPS) analyses of reference and carbon dioxide plasma treated polyethylene terephthalate (PET) were carried out. Significant chemical modifications were outlined in the treated PET surface in comparison with the reference one. The formation of new oxygenated groups was evidenced. These modifications heighten the level of interactions between the polymer substrate and the deposited coating. In a second stage, zinc oxide thin films were elaborated by r.f. magnetron sputtering from a ceramic target and with a reactive gas (mixture of argon–1% oxygen) under optimised conditions on CO2 plasma treated PET. The interfacial chemistry between the plasma treated PET and the zinc oxide was also studied by XPS. The line shape changes in the high-resolution core level spectra of carbon C1s, oxygen O1s, and zinc (Zn2p3/2, Zn3p), with the progressive deposition of zinc oxide coatings being recorded. The obtained spectra were fitted to mixed Gaussian–Lorentzian components using XPS CASA software. An interaction scheme between the zinc oxide thin layer and its polymer substrate, in the first stage of deposition, was proposed and checked by corroborating the findings of the different XPS spectra and their decompositions. It suggests the formation of Znh name="sbnd" />C complexes at the interface, which are promoted by an electron transfer from zinc to oxygen in oxygenated species, mainly alcohol groups, generated by the CO2 plasma treatment of PET. [Copyright &y& Elsevier]