Failure detection and monitoring in polymer matrix composites subjected to static and dynamic loads using carbon nanotube networks

In this work, multiwall carbon nanotubes (MWCNTs) have been used as a network of sensors to predict the failure region and to monitor the degradation of mechanical properties in laminated composites subjected to tensile and cyclic fatigue loadings. This is achieved by measuring the electrical resistance change in the semi-conductive MWCNT-fiber glass–epoxy polymer matrix composites. By partitioning the tensile and fatigue samples with electrically conductive probes, it is shown that with both increasing tensile load and number of cycles different resistance changes are detected in different regions and failure happens in the part in which higher resistance change was detected. In cyclic loading, when compared to strain gauge readings, resistance change measurements show more sensitivity in identifying the crack location, which gives this technique a good potential for monitoring damage during fatigue.     

Electromagnetic interference shielding of composites consisting of a polyester matrix and carbon nanotube-coated fiber reinforcement

We investigated the electromagnetic interference shielding effectiveness (EMI SE) of composites consisting of an unsaturated polyester matrix containing woven glass or carbon fibers that had been coated with multiwalled carbon nanotubes (MWCNTs). Composite panels consisting of fiber fabrics with various combinations of fabric type and stacking sequence were fabricated. Their EMI SE was measured in the frequency range of 30 MHz–1.5 GHz. The underlying physics governing the EMI shielding mechanisms of the materials, namely, absorption, reflection, and multiple reflections, was investigated and used in analytical models to predict the EMI SE. Simulation and experimental results showed that the contributions of reflection and absorption to EMI shielding is enhanced by sufficient impedance mismatching, while multiple reflections have a negative effect. For a given amount of MWCNTs in the glass-fiber–reinforced composite, coating the outermost, instead of intermediate, glass fiber plies with MWCNTs was found to maximize the conductivity and SE.     

Fabrication of multi-walled carbon nanotube–carbon fiber hybrid material via electrophoretic deposition followed by pyrolysis process

An integrated multi-walled carbon nanotube (MWCNT)–carbon fiber (CF) hybrid material has been fabricated by electrophoretic deposition of acid-functionalized MWCNTs on CF surface followed by soaking in a 10% solution of petroleum pitch in toluene, followed by pyrolysis in a nitrogen atmosphere. It has been revealed that MWCNTs entirely covered the CF surface. Mechanical properties of composites reinforced by MWCNT–CF hybrids were considerably enhanced (up to 120% in tensile strength and 100% in elastic modulus) compared to composites reinforce by as-received CFs. According to fractography observations, robust interlocking occurred between epoxy matrix and MWCNT–CF hybrids.     

Crystalline morphology and properties of multi-walled carbon nanotube filled isotactic polypropylene nanocomposites: Influence of filler size and loading

Isotactic polypropylene (PP) nanocomposites with multi-walled carbon nanotubes (MWCNTs) of various diameters (10–50 nm) were fabricated by extrusion and compression-molding techniques and characterized by X-ray diffraction measurements, differential scanning calorimetry, scanning electron microscopy, mechanical test and differential thermal analyses. The pure PP exhibits both the a- and b-axes oriented α-crystal, whereas the MWCNTs induce the b-axis orientation of the α-crystal along with the formation of minor γ-phase crystal in nanocomposites. Crystallinity, long period of lamellae, tensile strength, tensile modulus (TM) and microhardness (H) of PP considerably change by different loading and sizes of MWCNTs. The estimated values H/TM = 0.09–0.10 for all samples approach the predicted value of 0.10 for polymers. The increase in crystallinity has been demonstrated by both XRD and DSC studies. Mathematical models have been invoked to explain the changes in mechanical properties. An increase in thermal stability of polymer matrix occurs with increasing MWCNTs size and loading.     

Strain sensing in polymer/carbon nanotube composites by electrical resistance measurement

In this work multiwall carbon nanotubes (MWCNTs) dispersed in a polymer matrix have been used for strain sensing of the resulting nanocomposite under tensile loading. This was achieved by measuring the relative electrical resistance change (ΔR/R₀) in conductive polyvinylidenefluoride (PVDF)/MWCNTs nanocomposites prepared by melt-mixing with varying filler content from 0.5 wt.% to 8 wt.%. Two main parameters were systematically studied. The PVDF/MWCNTs mixing procedure that results in a successful MWCNTs dispersion, and the effect of MWCNTs content on material’s sensing behaviour. The samples were subjected to tensile loading and the longitudinal strain was monitored together with the longitudinal electrical resistance. The results showed that MWCNTs dispersed in insulating PVDF matrix have the potential to be used as a sensitive network to monitor the strain levels in polymer/carbon nanotube nanocomposites as the deformation level of each sample was being reflected by the resistance changes.     

Interlaminar and intralaminar reinforcement of composite laminates with aligned carbon nanotubes

Three-dimensional reinforcement of woven advanced polymer–matrix composites using aligned carbon nanotubes (CNTs) is explored experimentally and theoretically. Radially-aligned CNTs grown in situ on the surface of fibers in a woven cloth provide significant three-dimensional reinforcement, as measured by Mode I interlaminar fracture testing and tension-bearing experiments. Aligned CNTs bridge the ply interfaces giving enhancement in both initiation and steady-state toughness, improving the already tough system by 76% in steady state (more than 1.5 kJ/m² increase). CNT pull-out on the crack faces is the observed toughening mechanism, and an analytical model is correlated to the experimental fracture data. In the plane of the laminate, aligned CNTs enhance the tension-bearing response with increases of: 19% in bearing stiffness, 9% in critical strength, and 5% in ultimate strength accompanied by a clear change in failure mode from shear-out failure (matrix dominated) without CNTs to tensile fracture (fiber dominated) with CNTs.     

Hierarchical composites of carbon nanotubes on carbon fiber: Influence of growth condition on fiber tensile properties

Growing carbon nanotubes (CNT) on the surface of high performance carbon fibers (CF) provides a means to tailor the thermal, electrical and mechanical properties of the fiber–resin interface of a composite. However, many CNT growth processes require pretreatment of the fiber, deposition of an intermediate layer, or harsh growth conditions which can degrade tensile properties and limit the conduction between the fiber and the nanotubes. In this study, high density multi-wall carbon nanotubes were grown directly on two different polyacrylonitrile (PAN)-based carbon fibers (T650 and IM-7) using thermal Chemical Vapor Deposition (CVD). The influence of CVD growth conditions on the single-fiber tensile properties and CNT morphology was investigated. The mechanical properties of the resultant hybrid fibers were shown to depend on the carbon fiber used, the presence of a sizing (coating), the CNT growth temperature, growth time, and atmospheric conditions within the CVD chamber. The CNT density and alignment morphology was varied with growth temperature and precursor flow rate. Overall, it was concluded that a hybrid fiber with a well-adhered array of dense MWCNTs could be grown on the unsized T650 fiber with no significant degradation in tensile properties.     

Impact behavior and fractographic study of carbon nanotubes grafted carbon fiber-reinforced epoxy matrix multi-scale hybrid composites

Carbon nanotubes are the most promising reinforcement for high performance composites. Multiwall carbon nanotubes were directly grown onto the carbon fiber surface by catalytic thermal chemical vapor deposition technique. Multi-scale hybrid composites were fabricated using the carbon nanotubes grown fibers with epoxy matrix. Morphology of the grown carbon nanotubes was investigated using field emission scanning electron microscopy and transmission electron microscopy. The fabricated composites were subjected to impact tests which showed 48.7% and 42.2% higher energy absorption in Charpy and Izod impact tests respectively. Fractographic analysis of the impact tested specimens revealed the presence of carbon nanotubes both at the fiber surface and within the matrix which explained the reason for improved energy absorption capability of these composites. Carbon nanotubes presence at various cracks formed during loading provided a direct evidence of micro crack bridging. Thus the enhanced fracture strength of these composites is attributed to stronger fiber–matrix interfacial bonding and simultaneous matrix strengthening due to the grown carbon nanotubes.     

Preparation,characterization and properties of polycaprolactone diol-functionalized multi-walled carbon nanotube/thermoplastic polyurethane composite

Multi-walled carbon nanotubes (MWCNTs) were chemically functionalized to prepare thermoplastic polyurethane (PU) composites with enhanced properties. In order to achieve a high compatibility of functionalized MWCNTs with the PU matrix, polycaprolactone diol (PCL), as one of PU’s monomers, was selectively grafted on the surface of MWCNTs (MWCNT–PCL), while carboxylic acid groups functionalized MWCNTs (MWCNT–COOH) and raw MWCNTs served as control. Both MWCNT–COOH and MWCNT–PCL improved the dispersion of MWCNTs in the PU matrix and interfacial bonding between them at 1 wt% loading fraction. The MWCNT–PCL/PU composite showed the greatest extent of improvement, where the tensile strength and modulus were 51.2% and 33.5% higher than those of pure PU respectively, without sacrificing the elongation at break. The considerable improvement in both mechanical properties and thermal stability of MWCNT–PCL/PU composite should result from the homogeneous dispersion of MWCNT–PCL in the PU matrix and strong interfacial bonding between them.     

Grain size effect on the strengthening behavior of aluminum-based composites containing multi-walled carbon nanotubes

Strengthening efficiency of multi-walled carbon nanotubes (MWCNTs) is investigated for aluminum-based composites with grain sizes ranging from ∼250 to ∼65 nm. The strength of composites is significantly enhanced proportional to an increase of the MWCNT volume. However, the increment differs depending on deformation mode of the matrix. The strengthening efficiency of MWCNTs in ultrafine-grained composites is comparable with that predicted by the discontinuous fiber model, whereas the efficiency becomes half of the theoretical prediction as grain size is reduced below ∼70 nm. For nano-grained aluminum, activities of forest dislocations diminish and dislocations emitted from grain boundaries are dynamically annihilated during the recovery process, providing a weak plastic strain field around MWCNTs. The observation may provide a basic understanding of the strengthening behavior of nano-grained metal matrix composites.     

In situ assessment of carbon nanotube flow and filtration monitoring through glass fabric using electrical resistance measurement

Filtration of nanofillers into porous fabric media is still an issue during the preparation of advanced fiber-reinforced composites. The assessment of resin/multiwall carbon nanotube (MWCNT) flow, MWCNT filtration, and the cure monitoring of glass fiber/carbon nanotube-polyester composites by means of the measurement of the electrical resistance was introduced. The vacuum-assisted resin transfer molding technique was used. The electrical resistances measured over the span of a composite were qualitatively correlated with MWCNT flow and the degree of MWCNT filtration. It was found that while the complexity of the fabrics could likely introduce preferential deposition of MWCNTs, their filtration is mainly affected by their dispersion state in the resin suspension. Relationships among critical parameters such as the lengths and diameters of MWCNTs, the inter- and intra-tow dimensions of glass fabrics, the dispersion level of MWCNTs, and the viscosity of nanocomposite samples are discussed and correlated to the filtration, cure, and flow phenomena. We showed that our method can also serve as an early warning to obviate defects in the resulting composite.     

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.     

Can carbon nanotubes grown on fibers fundamentally change stress distribution in a composite?

In carbon fiber reinforced polymer composites the onset of damage occurs at the fiber/matrix interface, where stress concentrations are the highest due to the property mismatch of the two materials. This article reports results of a modelling study indicating that carbon nanotubes (CNTs) grown on fibers are effective in suppressing stress concentrations at the fiber/matrix interface. In the case of high density CNT forests, they can even fundamentally change a profile of the interfacial stress. The study is performed using a novel two-scale finite element model of a nano-engineered composite based on the embedded regions technique.     

Compressibility of carbon woven fabrics with carbon nanotubes/nanofibres grown on the fibres

Growth of carbon nanotubes (CNT) or carbon nano-fibres (CNF) on carbon fibrous substrates is a way to increase the fracture toughness of fibre reinforced composites (FRC), with encouraging results reported in the recent years. If these nano-engineered FRC (nFRC) are destined to leave laboratories and enter industrial-scale production, a question of adapting the existing composite manufacturing methods will arise. The paper studies compressibility of woven carbon fibre performs (two types of fabrics) with CNT/CNF grown on the fibres using the CVD method. The results include pressure vs thickness and pressure vs fibre volume fraction diagrams for one and four layers of the fabric. Morphology of the nFRC is studied with SEM. It is shown that the pressure needed to achieve the target fibre volume fraction of the preform increases drastically (for example, from 0.05 MPa to more than 0.5 MPa for a fibre volume fraction of 52%) when CNT/CNF are grown on it. No change in nesting of the fabric plies is noticed. The poor compressibility can lower the achievable fibre volume fraction in composite for economical vacuum assisted light-RTM techniques and increase the pressure requirements in autoclave processing.     

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.     

Effects of grafted chain length on mechanical and electrical properties of nanocomposites containing polylactide-grafted carbon nanotubes

We herein report the effects of interfacial reinforcement on mechanical and electrical properties of nanocomposites based on polylactide (PLA) and multi-walled carbon nanotube (MWCNT). For this purpose, a series of MWCNTs grafted with PLA chains of various lengths (MWCNT-g-PLAs) were prepared by ring-opening polymerization of l-lactide with carboxylic acid-functionalized MWCNT (MWCNT-COOH). MWCNT-g-PLAs were then mixed with commercial PLA to obtain PLA/MWCNT-g-PLA nanocomposites with 1.0 wt.% MWCNT content. It was revealed that morphological, mechanical, and electrical properties of PLA/MWCNT-g-PLA nanocomposites were strongly dependent on the PLA chain length of MWCNT-g-PLAs. FE-SEM images exhibited that the nanocomposites containing MWCNT-g-PLA with longer PLA chain length exhibited better dispersion of MWCNTs in the PLA matrix. Initial moduli and tensile strengths of PLA/MWCNT-g-PLA composites increased with the increment of chain length of PLA grafted on MWCNTs, which attributes to the improved interfacial adhesion between the grafted PLA chains of MWCNT-g-PLA and the PLA matrix. As a result, the experimental initial modulus (2775 ± 193 MPa) of the nanocomposite including MWCNT-g-PLA with PLA chains of average molecular weight of 530 g/mol was quite close to the theoretical value (2911 MPa) predicted for the nanocomposite with perfect interfacial adhesion. Unexpectedly, electrical resistivities of PLA/MWCNT-g-PLA nanocomposites were found to increase from ∼10⁴ to ∼10¹² Ω/sq with increasing the PLA chain length of MWCNT-g-PLA, which is due to the fact that the PLA chains grafted on MWCNTs prevent the formation of the electrical conduction path of MWCNTs in the PLA matrix.     

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.     

Fracture behavior of carbon nanotube/carbon microfiber hybrid polymer composites

Growing carbon nanotubes (CNTs) on the surface of fibers has the potential to modify fiber–matrix interfacial adhesion, enhance composite delamination resistance, and possibly improve toughness. In the present study, aligned CNTs were grown upon carbon fabric via chemical vapor deposition. Continuously monitored single-fiber composite fragmentation tests were performed on pristine and CNT-grafted fibers embedded in epoxy, and single-laminate compact-tension specimens were tested for fracture behavior. A significant increase (up to 20 %) was observed in the interfacial adhesion, at the cost of a decrease in the fiber tensile strength. As a result, the maximum load of the composite was decreased, but its residual load-bearing capacity more than doubled. The likely sources of these effects are discussed, as well as their implications.     

Impact damage of carbon fiber polymer–matrix composites, studied by electrical resistance measurement

Drop impact damage of continuous carbon fiber epoxy–matrix composite laminates, was studied by electrical resistance measurement, which was shown to be more sensitive than the ultrasonic method. The oblique resistance at an angle between the longitudinal and through-thickness directions was more effective than the surface longitudinal resistance in indicating damage, particularly interior damage. The oblique resistance values from longitudinal segments of a specimen were not additive, but the surface resistance values were. In the case of a unidirectional composite, electrical contacts at 45° from the longitudinal direction in the plane of the laminate were more effective than those at 90°. Even minor damage associated with negligible indentation was sensed. The spatial distribution of damage was also studied.     

Microstructure changes of polyurethane by inclusion of chemically modified carbon nanotubes at low filler contents

The surface of multi-walled carbon nanotubes (MWCNTs) was modified to introduce acidic groups in either covalent or van der Waals interaction bonding environments to establish cross-linking sites with a host polymer. Nanocomposites based on a polyurethane matrix (PU) containing chemically functionalised multi-walled carbon nanotubes (MWCNTs) have been shown to alter its mechanical performance depending on the nature of the surface functional groups on MWCNTs, which correlates to the type of bonding interaction of the surface group and also the dispersibility of MWCNTs and their influence on the domain structure of polyurethane. The stress at break for nanocomposites containing 0.25 wt% of acid-oxidised MWCNTs (MWCNT-ox), bearing covalently attached carboxylic, lactone and phenolic groups, was twice that of the native PU and Young’s Modulus for the nanocomposites increased by four times. Whereas when hemin, which contains carboxylic functionality, was immobilised to the surface of pure MWCNTs, the improvement in Young’s Modulus was only around twice that of pure PU. Differences in the disaggregation of MWCNTs into PU were observed between the samples as well as variation of the native domain structure of PU. The results also infer that the purification of MWCNTs from acid-oxidative lattice fragments (fulvic acids) is vital prior to conducting surface chemistry and polymerisation in order to ensure maximum mechanical performance enhancement in their reinforcement of the host polymer.