Indirect estimation of fiber/polymer bond strength and interfacial friction from maximum load values recorded in the microbond and pull-out tests. Part I: local bond strength

The techniques aimed at adhesion strength measurement between reinforcing fibers and polymer matrices (the pull-out and microbond tests) involve the measurement of the force, F _max, required to pull out a fiber whose end is embedded in the matrix. Then, this maximum force value is used to calculate such interfacial parameters as the apparent bond strength, τ_app, and the local interfacial shear strength (IFSS), τ_d. However, it has been demonstrated that the F _max value is influenced by interfacial friction in already debonded regions, and, therefore, these parameters are not purely 'adhesional' but depend, in an intricate way, on interfacial adhesion and friction. In the last few years, several techniques for separate determination of adhesion and friction in micromechanical tests have been developed, but their experimental realization is rather complicated, because they require an accurate value of the external load at the moment of crack initiation. We have developed a new technique which uses the relationship between the maximum force and the embedded length ('scale factor') to separately measure fiber-matrix interfacial adhesion and friction. Using the equation for the current crack length as a function of the applied load, based on a stress criterion of interfacial debonding, we modeled the pull-out and microbond experiments and obtained the maximum force value versus the embedded length. By varying τ_d and interfacial friction, τ_f, to fit experimental plots, both interfacial parameters were estimated. The micromechanical tests were modeled for three types of specimen geometries (cylindrical specimens, spherical droplets, and matrix hemispheres in the pull-out test) with different levels of residual thermal stresses and interfacial friction. The effect of all these factors on the experimental results is discussed, and the importance of specimen geometry is demonstrated. One of the most interesting results is that the 'ultimate' IFSS (the limiting τ_app as the embedded length tends to zero) is not always equal to the 'local' bond strength.     

Indirect estimation of fiber/polymer bond strength and interfacial friction from maximum load values recorded in the microbond and pull-out tests. Part II: Critical energy release rate

A new approach to experimental data treatment in the pull-out and microbond tests has been developed. It uses the relationship between the maximum force recorded in these tests and the embedded length ('scale factor') to separately determine adhesional interfacial parameters (critical energy release rate, local bond strength) and interfacial friction in debonded regions. The new method does not require the measurement of the debond force, which corresponds to interfacial crack initiation, and is, therefore, much more convenient and simpler than 'direct' techniques involving continuous monitoring of crack growth. Using the equation for the current crack length as a function of the load applied to the fiber, based on a fracture mechanics analysis of interfacial debonding, we modeled the pull-out and microbond experiments and obtained the maximum force versus the embedded length. By varying the critical energy release rate and interfacial frictional stress to fit experimental plots, both interfacial parameters were determined for several fiber-polymer pairs. Effects of specimen geometry, residual thermal stresses, and interfacial friction on the measured values are discussed. The results are compared with those obtained with our similar stress-based approach. The energy criterion works when the embedded length is not very short, and in this range of embedded length it is better than the stress criterion. Both criteria can be complementarily used for interface characterization.     

Investigation of load transfer between the fiber and the matrix in pull-out tests with fibers having different diameters

Single-fiber pull-out tests were used for investigation of the interfacial bond strength or toughness and load transfer between polymeric matrices and glass fibers having different diameters. The interfacial bond strength was well characterized by an ultimate interfacial shear strength (τ_ult) whose values were nearly independent of the fiber diameter. The same experiments were also analyzed by fracture mechanics methods to determine the interfacial toughness (G_ic). The critical energy release rate (G_ic) was a good material property for constant fiber diameter, but G_ic for initiation of debonding typically became smaller as the fiber diameter became larger. It was also possible to measure an effective shear-lag parameter, β, characterizing the load transfer efficiency between the fiber and the matrix. β decreased considerably with the fiber radius; this decrease scaled roughly as expected from elasticity theory. The measured results for β were used to calculate the radius of matrix material surrounding the fiber that was significantly affected by the presence of the fiber. The ratio of this radius to the fiber radius (R_m/r _f) was a function of the fiber diameter.     

Comparison of the stress transfer in single- and multi-fiber composite pull-out tests

Analyses of the elastic stress transfer taking place across the fiber-matrix interface are presented for single- and multi-fiber composite pull-out tests. The multi-fiber composite is treated as a three-cylinder assemblage consisting of a central fiber, a matrix annulus, and a composite medium. The forms of the fiber axial stress and the interface shear stress distributions along the embedded fiber length are determined for single- and multi-fiber composite pull-out tests and their dependences on the fiber volume fraction, the dimensions of the specimen, the fiber-to-matrix modulus ratio, and the embedded fiber aspect ratio are displayed. The stress transfer for a perfectly bonded interface for the two pull-out tests is compared and the difference is clearly shown. In addition, for the single-fiber composite pull-out test, the present theory is compared with some existing theories.     

The effect of atmospheric pressure helium plasma treatment on the surface and mechanical properties of ultrahigh-modulus polyethylene fibers

Ultrahigh-modulus polyethylene fibers were treated with atmospheric pressure He plasma on a capacitively coupled device at a frequency of 7.5 kHz and a He partial vapor pressure of 3.43 × 10³ Pa. The fibers were treated for 0, 1, and 2 min. Microscopic analysis showed that the surfaces of the fibers treated with He plasma were etched and that the 2-min He plasma-treated group had rougher surfaces than the 1-min He plasma-treated group. XPS analysis showed a 200% increase in the oxygen content and a 200% increase in the concentration of C—O bonds (from 11.4% to 31%) and the appearance of C=O bonds (from 0% to 7.6%) on the surface of plasma-treated fibers for the 2-min He plasma-treated group. In the microbond test, the 2-min He plasma-treated group had a 100% increase of interfacial shear strength over that of the control group, while the 1-min He plasma-treated group did not show a significant difference from the control group. The 2-min He plasma-treated group also showed a 14% higher single-fiber tensile strength than the control group.     

The effect of silica (SiO2) nanoparticles and ammonia/ethylene plasma treatment on the interfacial and mechanical properties of carbon-fiber-reinforced epoxy composites

A nanoparticle dispersion is known to enhance the mechanical properties of a variety of polymers and resins. In this work, the effects of silica (SiO₂) nanoparticle loading (0–2 wt%) and ammonia/ethylene plasma-treated fibers on the interfacial and mechanical properties of carbon fiber–epoxy composites were characterized. Single fiber composite (SFC) tests were performed to determine the fiber/resin interfacial shear strength (IFSS). Tensile tests on pure epoxy resin specimens were also performed to quantify mechanical property changes with silica content. The results indicated that up to 2% SiO₂ nanoparticle loading had only a little effect on the mechanical properties. For untreated fibers, the IFSS was comparable for all epoxy resins. With ethylene/ammonia plasma treated fibers, specimens exhibited a substantial increase in IFSS by 2 to 3 times, independent of SiO₂ loading. The highest IFSS value obtained was 146 MPa for plasma-treated fibers. Interaction between the fiber sizing and plasma treatment may be a critical factor in this IFSS increase. The results suggest that the fiber/epoxy interface is not affected by the incorporation of up to 2% SiO₂ nanoparticles. Furthermore, the fiber surface modification through plasma treatment is an effective method to improve and control adhesion between fiber and resin.