Self-sensing and dispersive evaluation of single carbon fiber/carbon nanotube (CNT)-epoxy composites using electro-micromechanical technique and nondestructive acoustic emission

Self-sensing and interfacial evaluation were investigated with different dispersion solvents for single carbon fiber/carbon nanotube (CNT)-epoxy composites by electro-micromechanical technique and acoustic emission (AE) under loading/subsequent unloading. The optimized dispersion procedure was set up to obtain improved mechanical and electrical properties. Apparent modulus and electrical contact resistivity for CNT-epoxy composites were correlated with different dispersion solvents for CNT. CNT-epoxy composites using good dispersion solvents exhibited a higher apparent modulus because of better stress transferring effects due to the relatively uniform dispersion of CNT in epoxy and enhanced interfacial adhesion between CNT and the epoxy matrix. However, good solvents exhibited a higher apparent modulus but lower thermodynamic work of adhesion, W_a for single carbon microfiber/CNT-epoxy composite. It is attributed to the fact that hydrophobic behavior with high advanced contact angle was observed for CNT-epoxy in the good solvent, which might not be compatible well with the carbon microfiber. Damage sensing was also detected simultaneously using AE combined with electrical resistance measurement. Electrical resistivity increased stepwise with progressing fiber fracture due to the decrease in electrical contact by the CNT.     

Non-destructive damage sensing and cure monitoring of carbon fiber/epoxyacrylate composites with UV and thermal curing using electro-micromechanical techniques

Interfacial properties and cure monitoring of single-carbon fiber/thermosetting composites by thermal and different ultraviolet (UV) curing processes were investigated using electro-micromechanical test and electrical resistance measurement. During curing process the residual stress was monitored in terms of the electrical resistance and then they were compared to various curing conditions. In thermal cure the tensile strength and modulus of epoxyacrylate matrix were higher than those of UV cure, whereas the failure strain was lower. Interfacial shear strength (IFSS) increased gradually with elapsing UV exposing time and then saturated. For thermal cure the IFSS was significantly higher than that of UV cure, and cure shrinkage was observed due to matrix shrinkage and residual stress due to the difference in thermal expansion coefficient (TEC). The difference in electrical resistance, ΔR during thermal curing was larger than that of UV cure. In thermal cure apparent modulus indicating embedding matrix modulus and interfacial adhesion was highest and reaching time up to same stress was shortest. Thermal cure showed the strong durability against the IFSS deterioration after boiling test compared to UV cure.     

Nondestructive sensing evaluation of surface modified single-carbon fiber reinforced epoxy composites by electrical resistivity measurement

Nondestructive sensing of a single-carbon fiber reinforced epoxy composites was evaluated by the measurement of electrical resistivity under reversible cyclic loading. For the strain–stress sensing, the strain up to the maximum load of a bare carbon fiber itself is larger than that of carbon fiber composite. As curing temperature increased, apparent modulus up to the maximum load increased and the elapsed time became shorter. Higher residual stress might contribute to the improved interfacial adhesion. The strain up to the maximum load at low temperature was larger than that at higher temperature. The strain of electrodeposition (ED) treated carbon fiber was smaller than that of the untreated carbon fiber composite until the maximum load reached. This could be due to higher apparent modulus of composite based on the improved interfacial shear strength (IFSS). Since the electrical resistivity was responded well quantitatively with various parameters, such as matrix modulus, the fiber surface modification, the electrical resistivity measurement can be a feasible method of nondestructive sensing evaluation for conductive fiber reinforced composites inherently.     

Interfacial and hydrophobic evaluation of glass fiber/CNT–epoxy nanocomposites using electro-micromechanical technique and wettability test

Interfacial evaluation of glass fiber reinforced carbon nanotube (CNT)–epoxy nanocomposites and the hydrophobicity of CNT–epoxy nanocomposites were investigated by micromechanical and wettability tests. The contact resistance of the CNT–epoxy nanocomposites was measured using a gradient specimen, containing electrical contacts with gradually-increasing spacing. The contact resistance of CNT–epoxy nanocomposites could be better valuated by mainly the two-point method. Due to the presence of hydrophobic domains on the heterogeneous surface, the static contact angle of CNT–epoxy nanocomposites was about 120°, which was somewhat lower than that for super-hydrophobicity (>150°). For surface treated glass fiber, tensile strength decreased dramatically, whereas tensile modulus exhibited little change despite the presence of flaws on the etched fiber surface. The interfacial shear strength (IFSS) between the etched glass fiber and the CNT–epoxy nanocomposites increased due to enhanced surface energy and roughness. As thermodynamic work of energy, W_a increased, both the mechanical IFSS and the apparent modulus increased.     

CF/EP composite laminates with carbon black and copper chloride for improved electrical conductivity and interlaminar fracture toughness

An experimental study was conducted to improve the electrical conductivity of continuous carbon fibre/epoxy (CF/EP) composite laminate, with simultaneous improvement in mechanical performance, by incorporating nano-scale carbon black (CB) particles and copper chloride (CC) electrolyte into the epoxy matrix. CF/EP laminates of 65 vol.% of carbon fibres were manufactured using a vacuum-assisted resin infusion (VARI) technique. The effects of CB and the synergy of CB/CC on electrical resistivity, tensile strength and elastic modulus and fracture toughness (K_IC) of the epoxy matrix were experimentally characterised, as well as the transverse tensile modulus and strength, Mode I and Mode II interlaminar fracture toughness of the CF/EP laminates. The results showed that the addition of up to 3.0 wt.% CB in the epoxy matrix, with the assistance of CC, noticeably improved the electrical conductivity of the epoxy and the CF/EP laminates, with mechanical performance also enhanced to a certain extent.     

Inherent sensing and interfacial evaluation of carbon nanofiber and nanotube/epoxy composites using electrical resistance measurement and micromechanical technique

Inherent sensing of load, micro-damage and stress transferring effects were evaluated for carbon nanotube (CNT) and carbon nanofiber (CNF)/epoxy composites (with various added contents) by an electro-micromechanical technique, using the four-point probe method. Carbon black (CB)/epoxy composites, with conventional nanosize material added, were used for the comparison with CNT and CNF composites. Subsequent fracture of the carbon fiber in the dual matrix composites (DMC) was detected by acoustic emission (AE) and by the change in electrical resistance, ΔR due to electrical contacts of neighboring CNMs. Stress/strain sensing of the nanocomposites was detected by an electro-pullout test under uniform cyclic loading/subsequent unloading. CNT/epoxy composites showed the best sensitivity to fiber fracture, matrix deformation and stress/strain sensing, whereas CB/epoxy composite exhibited poorer sensitivity. From the apparent modulus (as a result of matrix modulus and interfacial adhesion), the stress transferring effects reinforced by CNT was highest among three CNMs. The thermodynamic work of adhesion, W_a as found by dynamic contact angle measurements of the CNT/epoxy composite as a function of added CNT content was correlated and found to be consistent with the apparent mechanical modulus. Uniform dispersion and interfacial adhesion appear to be key factors for improving both sensing and mechanical performance of nanocomposite. Thermally treated-CNF composites exhibited a slightly higher apparent modulus, whereas higher testing temperatures appeared to lower the apparent modulus.     

Effects of thermal histories on interfacial properties of carbon fiber/polyamide 6 composites: Thickness,modulus, adhesion and shear strength

Interface thickness and modulus of carbon fiber (CF) reinforced polyamide 6 (PA 6) composites with different thermal histories are characterized as 331–394 nm and 0.24–0.30 times to fiber modulus, respectively. Transverse fiber bundle (TFB) test is firstly employed for evaluating semi-crystalline PA 6 interfacial adhesion. TFB Failure mechanisms are schematically given. Besides enhanced molecular entangling on fiber surface, increased matrix toughness is also found to have a great effect on improved TFB results. Droplet micro-debonding results show that decreasing cooling rate and increasing annealing temperature both decrease interfacial shear strength (IFSS) though residual PA 6 on carbon fiber surface increases. In the end, the above data are normalized together with some previous measured parameters. It shows that quenching of the CF/PA 6 composites and subsequent annealing are shown to give similar results as slow cooling. Relationships between each other are also discussed.     

Structural health monitoring of glass fiber reinforced composites using embedded carbon nanotube (CNT) fibers

In the present work, carbon nanotube (CNT) fibers had been embedded to glass fiber reinforced polymers (GFRP) for the structural health monitoring of the composite material. The addition of the conductive CNT fiber to the non-conductive GFRP material aims to enhance its multi-function ability; the test specimen’s response to mechanical load and the insitu CNT fiber’s electrical resistance measurements were correlated for sensing and damage monitoring purposes. It is the first time this fiber is used in composite materials for sensing purposes; CNT fiber is easy to be embedded and does not downgrade the material’s mechanical properties. Various incremental loading–unloading steps had been applied to the manufactured specimens in tension as well as in three-point bending tests. The CNT fiber worked as a sensor in both, tensile and compression loadings. A direct correlation between the mechanical loading and the electrical resistance change had been established for the investigated specimens. For high stress (or strain) level loadings, residual resistance measurements of the CNT fiber were observed after unloading. Accumulating damage to the composite material had been calculated and was correlated to the electrical resistance readings. The established correlation between these parameters changed according to the material’s loading history.     

Interfacial strength and fracture energy of individual carbon nanofibers in epoxy matrix as a function of surface conditions

The interfacial shear strength (IFSS) and fracture energy of individual carbon nanofibers embedded in epoxy were obtained for different surface conditions and treatments by novel, MEMS-based, nanoscale fiber pull-out experiments. As-grown vapor grown carbon nanofibers (VGCNFs) with turbostratic surface and 5 nm peak-to-valley surface roughness exhibited high IFSS and interfacial fracture energy, averaging 106 ± 29 MPa and 1.9 ± 0.9 J/m², respectively. Subsequent high temperature heat treatment and graphitization resulted in drastically reduced IFSS of 66 ± 10 MPa and interfacial fracture energy of 0.65 ± 0.14 J/m². The smaller IFSS values and the reduced standard deviation were due to significant reduction of the fiber surface roughness to 1–2 nm, as well as a decrease in surface defect density during conversion of turbostratic and amorphous carbon to highly ordered graphitic carbon. For both grades of VGCNFs failure was adhesive with clear nanofiber surfaces after debonding. Oxidative functionalization of high temperature heat-treated VGCNFs resulted in much higher IFSS of 189 ± 15 MPa and interfacial fracture energy of 3.3 ± 1.0 J/m². The debond surfaces of functionalized nanofibers had signs of matrix residue and/or shearing of the outer graphitic layer of the VGCNFs, namely the failure mode was a combination of cohesive matrix and/or cohesive fiber failure which contributed to the high IFSS. For all three grades of VGCNFs the IFSS was independent of fiber length and diameter. The findings of this experimental study emphasized the critical role of nanofiber surface morphology and chemistry in determining the shear strength and fracture energy of nanofiber interfaces, and shed light to prior composite-level strength and fracture toughness measurements.     

Interfacial evaluation of carbon fiber/epoxy composites using electrical resistance measurements at room and a cryogenic temperature

Interfacial properties between fiber and matrix were evaluated using an electrical resistance (ER) fragmentation method. The single carbon fiber (CF) tensile test was performed in conjunction with electrical resistance measurements. The relationship between tensile properties of single carbon fiber specimens and the electrical resistance ratio (ERR) was investigated. The data showed a linear relationship between these properties. Fragmentation specimens were tested under tensile loading, and it was observed that, due to stress transfer from the matrix to the reinforcing fiber, the single carbon fiber broke first. The stress distribution along the carbon fiber was monitored via electrical resistance changes. ER fragmentation measurements were performed to predict CF fractured strength embedded in epoxy by an empirical formula of CF tensile results. These interfacial properties of CF epoxy composites were measured at room and a cryogenic temperature. Work of adhesion between the carbon fiber and the matrix was measured to verify the results of the ER fragmentation method, and the two procedures yielded consistent results and conclusions.     

Fabrication and mechanical properties of well-dispersed multiwalled carbon nanotubes/epoxy composites

Multiwalled carbon nanotubes (MWCNTs)/epoxy nanocomposites were fabricated by using ultrasonication and the cast molding method. In this process, MWCNTs modified by mixed acids were well dispersed and highly loaded in an epoxy matrix. The effects of MWCNTs addition and surface modification on the mechanical performances and fracture morphologies of composites were investigated. It was found that the tensile strength improved with the increase of MWCNTs addition, and when the content of MWCNTs loading reached 8 wt.%, the tensile strength reached the highest value of 69.7 MPa. In addition, the fracture strain also enhanced distinctly, implying that MWCNTs loading not only elevated the tensile strength of the epoxy matrix, but also increased the fracture toughness. Nevertheless, the elastic modulus reduced with the increase of MWCNTs loading. The reasons for the mechanical property changes are discussed.     

Development of aligned-hemp yarn-reinforced green composites with soy protein resin: Effect of pH on mechanical and interfacial properties

Unidirectional hemp yarn-reinforced green composites were fabricated with soy protein concentrate (SPC) resin processed at various pH values. To preserve the yarn alignment during the fabrication of green composites, hemp yarn was wound onto a metal frame with slight tension and precured SPC resin was applied to the yarns. Effects of pH values on the tensile properties of the SPC resin and hemp yarn/SPC resin interfacial shear strength (IFSS) were investigated. Increasing pH of the SPC resin from 7 to 12 decreased its fracture stress and Young’s modulus from 13.1 MPa and 357.5 MPa to 8.1 MPa and 156.2 MPa, respectively. At the same time fracture strain and moisture content increased from 31.5% and 15.65% to 53·4% and 19.30%, respectively, indicating resin plasticization. However, hemp yarn/SPC resin IFSS increased from 17.7 MPa at pH 7 up to 28.0 MPa at pH 10, after which it decreased. The fracture toughness of the composites increased up to pH of 10 but further increase in pH reduced the toughness. SEM photomicrographs showed fracture surfaces of hemp yarn-reinforced green composites that indicated better resin/fiber interaction at pH of 10 than 7 or 12.     

Modeling hysteresis behavior of cross-ply C/SiC ceramic matrix composites

In this paper, the loading/unloading tensile behavior of cross-ply C/SiC ceramic matrix composites at room temperature has been investigated. The loading/unloading stress–strain curve exhibits obvious hysteresis behavior. An approach to model the hysteresis loops of cross-ply ceranic matrix composites including the effect of matrix cracking has been developed. Based on the damage mechanisms of fiber sliding relative to matrix during unloading and subsequent reloading, the unloading interface reverse slip length and reloading interface new slip length of different matrix cracking modes are obtained by the fracture mechanics approach. The hysteresis loops of cross-ply C/SiC ceramic matrix composites corresponding to different peak stresses have been predicted.     

Interfacial properties and microfailure degradation mechanisms of bioabsorbable fibers/poly-l-lactide composites using micromechanical test and nondestructive acoustic emission

Interfacial properties and microfailure degradation mechanisms of the bioabsorbable composites for implant materials were investigated using micromechanical technique and nondestructive acoustic emission (AE). The tensile strength of absorbable fibers with hydrolysis was analyzed statistically using either uni- or bimodal Weibull distribution. As hydrolysis time increased, the tensile strength, the modulus and the elongation of poly(ester-amide) (PEA) and bioactive glass fibers decreased, whereas those of chitosan fiber almost did not change. Interfacial shear strength (IFSS) between bioactive glass fiber and poly-l-lactide (PLLA) was much higher than PEA or chitosan fiber/PLLA systems using dual matrix composite (DMC) specimen. The decreasing rate of IFSS was the fastest in bioactive glass fiber/PLLA composites whereas that of chitosan fiber/PLLA composites was the slowest. Work of adhesion, W_a between bioactive glass fiber and PLLA was the highest, and the wettability results were consistent with the IFSS. AE energies of PEA fiber decreased gradually, and their distributions became narrower than those in the initial state with hydrolysis time. In case of bioactive glass fiber, AE energies in tensile failure were much higher than those in compression. In addition, AE parameters at the initial state were much higher than those after degradation under both tensile and compressive tests. Interfacial properties and microfailure degradation mechanisms can be important factors to control bioabsorbable composite performance.     

Synchronous effects of multiscale reinforced and toughened CFRP composites by MWNTs-EP/PSF hybrid nanofibers with preferred orientation

MWNTs-EP/PSF (polysulfone) hybrid nanofibers with preferred orientation were directly electrospun onto carbon fiber/epoxy prepregs and interlaminar synchronously reinforced and toughened CFRP composites were successfully fabricated. With MWNTs-EP loading increasing, the oriented nanofibers were obtained accompanying with enhanced alignment of inner MWNTs-EP. Flexural properties and interlaminar shear strength of composites were improved with increasing MWNTs-EP loadings, whereas fracture toughness attained maximum at 10 wt% MWNTs-EP loading and then decreased. Based on these results, multiscale schematic modeling and mechanism schematic of hybrid nanofibers reinforced and toughened composites were suggested. Due to the preferred orientation of nanofibers, MWNTs-EP was inclined to align vertically to carbon fiber direction along the in-plane of interface layer. The proposed network structures, containing four correlative phases of MWNTs-EP/PSF sphere/carbon fiber/epoxy matrix, contributed to simultaneous improvement of strength and toughness of composites, which was realized by crack pinning, crack deflection, crack bridging and effective load transfer.     

Characterization of epoxy functionalized graphite nanoparticles and the physical properties of epoxy matrix nanocomposites

This work presents a novel approach to the functionalization of graphite nanoparticles. The technique provides a mechanism for covalent bonding between the filler and matrix, with minimal disruption to the sp² hybridization of the pristine graphene sheet. Functionalization proceeded by covalently bonding an epoxy monomer to the surface of expanded graphite, via a coupling agent, such that the epoxy concentration was measured as approximately 4 wt.%. The impact of dispersing this material into an epoxy resin was evaluated with respect to the mechanical properties and electrical conductivity of the graphite–epoxy nanocomposite. At a loading as low as 0.5 wt.%, the electrical conductivity was increased by five orders of magnitude relative to the base resin. The material yield strength was increased by 30% and Young’s modulus by 50%. These results were realized without compromise to the resin toughness.     

Mechanical properties of epoxy composites filled with silane-functionalized graphene oxide

In this work, the effects of as-produced GO and silane functionalized GO (silane-f-GO) loading and silane functionalization on the mechanical properties of epoxy composites are investigated and compared. Such silane functionalization containing epoxy ended-groups is found to effectively improve the compatibility between the silane-f-GO and the epoxy matrix. Increased storage modulus, glass transition temperature, thermal stability, tensile and flexural properties and fracture toughness of epoxy composites filled with the silane-f-GO sheets are observed compared with those of the neat epoxy and GO/epoxy composites. These findings confirm the improved dispersion and interfacial interaction in the composites arising from covalent bonds between the silane-f-GO and the epoxy matrix. Moreover, several possible fracture mechanisms, i.e. crack pinning/deflection, crack bridging, and matrix plastic deformation initiated by the debonding/delamination of GO sheets, were identified and evaluated.     

Mode I interlaminar fracture behavior and mechanical properties of CFRPs with nanoclay-filled epoxy matrix

The mechanical properties and fracture behavior of nanocomposites and carbon fiber composites (CFRPs) containing organoclay in the epoxy matrix have been investigated. Morphological studies using TEM and XRD revealed that the clay particles within the epoxy resin were intercalated or orderly exfoliated. The organoclay brought about a significant improvement in flexural modulus, especially in the first few wt% of loading, and the improvement of flexural modulus was at the expense of a reduction in flexural strength. The quasi-static fracture toughness increased, whereas the impact fracture toughness dropped sharply with increasing the clay content.Flexural properties of CFRPs containing organoclay modified epoxy matrix generally followed the trend similar to the epoxy nanocomposite although the variation was much smaller for the CFRPs. Both the initiation and propagation values of mode I interlaminar fracture toughness of CFRP composites increased with increasing clay concentration. In particular, the propagation fracture toughness almost doubled with 7 wt% clay loading. A strong correlation was established between the fracture toughness of organoclay-modified epoxy matrix and the CFRP composite interlaminar fracture toughness.     

Reinforcement effects of MWCNT and VGCF in bulk composites and interlayer of CFRP laminates

The reinforcement effects of two nanofillers, i.e., multi-walled carbon nanotube (MWCNT) and vapor grown carbon fiber (VGCF), which are used at the interface of conventional CFRP laminates, and in epoxy bulk composites, have been investigated. When using the two nanofillers at the interface between two conventional CFRP sublaminates, the Mode-I interlaminar tensile strength and fracture toughness of CFRP laminates are improved significantly. The performance of VGCF is better than that of MWCNT in this case. For epoxy bulk composites, the two nanofillers play a similar role of good reinforcement in Young’s modulus and tensile strength. However, the Mode-I fracture toughness of epoxy/MWCNT is much better than that of epoxy/VGCF.     

Interfacial shear strength of a glass fiber/epoxy bonding in composites modified with carbon nanotubes

In recent years, carbon nanotubes (CNTs) grown on fibers have attracted a lot of interest as an additional reinforcing component in conventional fiber-reinforced composites to improve the properties of the fiber/matrix interface. Due to harsh growth conditions, the CNT-grafted fibers often exhibit degraded tensile properties. In the current study we explore an alternative approach to deliver CNTs to the fiber surface by dispersing CNTs in the fiber sizing formulation. This route takes advantage of the developed techniques for CNT dispersion in resins and introduces no damage to the fibers. We focus on unidirectional glass fiber/epoxy macro-composites where CNTs are introduced in three ways: (1) in the fiber sizing, (2) in the matrix and (3) in the fiber sizing and matrix simultaneously. Interfacial shear strength (IFSS) is investigated using single-fiber push-out microindentation. The results of the test reveal an increase of IFSS in all three cases. The maximum gain (over 90%) is achieved in the composite where CNTs are introduced solely in the fiber sizing.