Application of continuously-monitored single fiber fragmentation tests to carbon nanotube/carbon microfiber hybrid composites

To assess the effect of carbon nanotube (CNT) grafting on interfacial stress transfer in fiber composites, CNTs were grown upon individual carbon T-300 fibers by chemical vapor deposition. Continuously-monitored single fiber composite (SFC) fragmentation tests were performed on both pristine and CNT-decorated fibers embedded in epoxy. The critical fragment length, fiber tensile strength at critical length, and interfacial shear strength were evaluated. Despite the fiber strength degradation resulting from the harsh CNT growth conditions, the CNT-modified fibers lead to a twofold increase in interfacial shear strength which correlates with the nearly threefold increase in apparent fiber diameter resulting from CNT grafting. These observations corroborate recently published studies with other CNT-grafted fibers. An analysis of the relative contributions to the interfacial strength of the fiber diameter and strength due to surface treatment is presented. It is concluded that the common view whereby an experimentally observed shorter average fragment length leads to a stronger interfacial adhesion is not necessarily correct, if the treatment has changed the fiber tensile strength or its diameter.     

Mechanical behavior of self-assembled carbon nanotube reinforced nylon 6,6 fibers

The versatile electrospinning technique was used to successfully align and disperse multiwalled carbon nanotubes (MWCNT) in nylon 6,6 matrix to obtain composite fibers. The morphology of the composite fibers and the dispersion of the CNTs within the fibers were analyzed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. TEM analysis revealed that the CNTs were well-dispersed, separated and aligned along the fiber axis. The thermal and mechanical properties of the composite fibers were characterized as a function of weight fraction of the CNTs. Incorporation of the CNTs in the fibers resulted in an increase in glass-transition temperature (T_g) by ∼7 °C, indicating that the addition of CNTs has restricted the mobility of the polymer chains and provided confinement to neighboring molecular chains. Tensile and nanoindentation experiments were performed to investigate the mechanical deformation behavior of the composite fibers. The results suggested that incorporation of high strength and high aspect ratio CNTs into the fiber matrix enhanced significantly the stiffness and strength of nylon 6,6 fibers. An understanding of the structure–property relationships can provide fruitful insights to develop electrospun fibers with superior properties for miniaturized and load-bearing applications.     

Creep of Nextel™720/alumina–mullite ceramic composite at 1200 °C in air,argon, and steam

The tensile creep behavior of an oxide–oxide continuous fiber ceramic composite was investigated at 1200 °C in laboratory air, in steam and in argon. The composite consists of a porous alumina–mullite matrix reinforced with laminated, woven mullite/alumina (Nextel™720) fibers, has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. The tensile stress–strain behavior was investigated and the tensile properties measured at 1200 °C. The elastic modulus was 74.5 GPa and the ultimate tensile strength was 153 MPa. Tensile creep behavior was examined for creep stresses in the 70–140 MPa range. Primary and secondary creep regimes were observed in all tests. Creep run-out (set to 100 h) was achieved in laboratory air for creep stress levels ?91 MPa. The presence of either steam or argon accelerated creep rates and reduced creep lifetimes. Composite microstructure, as well as damage and failure mechanisms were investigated.     

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.     

High mechanical performance SiC/SiC composites by NITE process with tailoring of appropriate fabrication temperature to fiber volume fraction

Unidirectional SiC/SiC composites are prepared by nano-powder infiltration and transient eutectic-phase (NITE) process, using pyrolytic carbon (PyC)-coated Tyranno-SA SiC fibers as reinforcement and SiC nano-powder with sintering additives for matrix formation. The effects of two kinds of fiber volume fraction incorporating fabrication temperature were characterized on densification, microstructure and mechanical properties. Densification of the composites with low fiber volume fraction (appropriately 30 vol%) was developed even at lower fabrication temperature of 1800 °C, and then saturated at 3rd stage of matrix densification corresponding to classic liquid phase sintering. Hence, densification of the composites with high volume fraction (above 50 vol%) became restricted because the many fibers retarded the infiltration of SiC nano-powder at lower fabrication temperature of 1800 °C. When fabrication temperature increased by 1900 °C, densification of the composites was effectively enhanced in the intra-fiber-bundles and simultaneously the interaction between PyC interface and matrix was strengthened. SEM observation on the fracture surface revealed that fiber pull-out length was accordingly changed with fabrication temperature as well as fiber volume fraction, which dominated tensile fracture behaviors. Through NITE process, SiC/SiC composites with two fracture types were successfully developed by tailoring of appropriate fabrication temperature to fiber volume fraction as follows: (1) high ductility type and (2) high strength type.     

Orientation in high-density polyethylene/inorganic whisker composite fibers as studied via polarized Fourier transform infrared spectroscopy

In this article, a quantitative measurement of orientation functions for both the polymer matrix and the filler has been carried out, for the first time, in high-density polyethylene (HDPE)/inorganic whisker (SMCW) composite fibers, with aid of polarized Fourier transform infrared (FTIR) spectroscopy. A highly oriented structure was observed in the as-spun fibers, and the orientation functions of both polyethylene and the whisker decreased with the increase of whisker content. During tensile deformation of the fibers, the orientation functions were continuously enhanced as increasing of the strain for the matrix and the filler. However, a fast increase of orientation was found for pure polyethylene fiber and composite fibers with less whisker content, and a slow increase for composite fibers with higher whisker content. Very interestingly, a formation of hybrid shish-kebab structure with whisker acting as shish and polyethylene lamellae as kebab was observed in the as-spun fiber with low loading of whisker (less than 10 wt.%), resulting in a strong interfacial interaction between polyethylene and whisker. As a result, the highest tensile strength was observed in this sample even it had a lower orientation compared with that of pure HDPE. For the composite fiber with 10 and 20 wt.% whisker, no obvious formation of hybrid shish-kebab was observed, resulting in a poor interfacial interaction and subsequently, lower tensile strength. That result indicates that the tensile strength of the fibers depends not only on the orientations of the polyethylene and the whisker, more importantly, on the interfacial interaction between matrix and the filler. The change of orientations of the composite fibers by adding whisker and the formation of hybrid shish-kebab structure were discussed based on rheological measurement.     

Effect of frequency and environment on fatigue behavior of a CVI SiC/SiC ceramic matrix composite at 1200 °C

The fatigue behavior of a SiC/SiC CMC (ceramic matrix composite) was investigated at 1200 °C in laboratory air and in steam environment. The composite consists of a SiC matrix reinforced with laminated woven Hi-Nicalon™ fibers. Fiber preforms had boron nitride fiber coating applied and were then densified with CVI SiC. Tensile stress-strain behavior and tensile properties were evaluated at 1200 °C. Tension-tension fatigue tests were conducted at frequencies of 0.1, 1.0, and 10 Hz for fatigue stresses ranging from 80 to 120 MPa in air and from 60 to 110 MPa in steam. Fatigue run-out was defined as 10⁵ cycles at the frequency of 0.1 Hz and as 2 × 10⁵ cycles at the frequencies of 1.0 and 10 Hz. Presence of steam significantly degraded the fatigue performance. In both test environments the fatigue limit and fatigue lifetime decreased with increasing frequency. Specimens that achieved run-out were subjected to tensile tests to failure to characterize the retained tensile properties. The material retained 100% of its tensile strength, yet modulus loss up to 22% was observed. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Enchanced high-temperature performances of SiC/SiC composites by high densification and crystalline structure

We report the enchanced in situ performances of tensile strength and thermal conductivity at elevated temperatures of the PCS-free SiC/SiC composite with a high fiber volume fraction above 50% fabricated by NITE process for nuclear applications. The composite was fabricated by the optimized combination of the fiber coating, the matrix slurry and the pressure-sintering conditions, based on our previous composites’ study history. The composite showed the excellent tensile strength up to 1500 °C, that it retained approximately 88% of the room-temperature strength. Also, the thermal conductivity of the composites represented over 20 W/m K up to 1500 °C, which was enough high to take the advantage of the assumed design value for nuclear applications. Microstructural observation indicated that the excellent high-temperature performances regarding tensile strength and thermal conductivity up to 1500 °C were the contribution to the high densification and crystalline structure in matrix.     

Deformation and failure of PP composites reinforced with lignocellulosic fibers: Effect of inherent strength of the particles

PP/wood composites were prepared from two lignocellulosic fibers with different particle size and aspect ratio in order to determine the effect of these factors on the deformation and failure mechanism as well as on the properties of the composites. Wood content was changed from 0 to 80 wt%. Maleinated polypropylene (MAPP) was added to improve interfacial adhesion. The MAPP/wood ratio was kept constant at 0.1. Mechanical properties were determined by tensile testing. Micromechanical deformation processes were followed by acoustic emission (AE) and volume strain (VOLS) measurements, and by the study of fracture surfaces. The results proved that micromechanical deformations change drastically both with decreasing particle size and changing interfacial adhesion. Less debonding, fiber pull out and fiber fracture occur in composites containing small particles. Hardly any change was observed in the mechanical properties of the composites with decreasing particle size, in spite of the drastic modification of the deformation mechanism. The apparently slight influence of particle size on composite strength results from the smaller aspect ratio of the small particles, which indicates that orientation and orientation distribution must have a strong effect on reinforcement. Further improvement in composite strength is possible only through the optimization of particle size, aspect ratio and the inherent strength of wood.     

Mechanical properties of basalt fibers and their adhesion to polypropylene matrices

This work is aimed to study the mechanical properties of basalt fibers, and their adhesion to polypropylene (PP) matrices. Single filament tensile tests were used to calculate the strength of different types of fibers, characterized by different providers and surface treatment. Single fiber fragmentation tests (SFFT) were used to calculate the critical length of the fibers, in a homopolymer PP matrix and in a maleic anhydride modified PP matrix. It was shown that the tensile strength of the fibers is not significantly influenced by the origin or the surface treatment. Only fibers without any sizing show very reduced mechanical properties. On the other hand, the tensile strength was shown to be severely dependent on the filament length. Weibull theory was used in order to calculate the fitting parameters σ₀ and β, which were necessary in order to extrapolate the tensile strength to the critical length determined by SFFT. This allowed calculating the adhesion properties of the basalt fibers. It was shown that fiber–matrix adhesion is dependent on both the presence of sizing on the fiber surface, as well as on the modification of the matrix.     

Fabrication and characterization of recyclable carbon nanotube/polyvinyl butyral composite fiber

A surface-draw method to fabricate recyclable carbon nanotube/polyvinyl butyral (CNT/PVB) composite fibers is reported. This method is effective for both single-walled carbon nanotube (SWCNT) and multi-walled carbon nanotube. The CNT mass content of CNT/PVB composite fibers can vary from 0 to 80 wt.%, which is higher than most CNT/polymer composites reported to date. The diameter of the composite fibers can be controlled in the range of 10-100 μm, with essentially unlimited draw length. The composite fibers with 7.4 wt.% SWCNTs showed optimal tensile properties. Compared with pure PVB fibers, the tensile strength, failure strain, and elastic modulus of the composite fiber have improved about 127%, 27%, and 73%, respectively. In addition, SWCNT/PVB composites with 66.7 wt.% SWCNTs have the highest conductivity of 42.9 S m⁻¹. More importantly, the major benefit is the “greenness” of the method, which involves environment friendly ethanol-water solvent with no functionalization of the nanotube required, and only simple apparatus are needed. The CNT/PVB composite fibers obtained can be dissolved in ethanol solution and reformed with the surface draw method without any additional treatment; and the material properties after recycle is comparable to those fabricated in the first round.     

Effect of alkali treatment on interfacial bonding in abaca fiber-reinforced composites

Abaca fibers demonstrate enormous potential as reinforcing agents in composite materials. In this study, abaca fibers were immersed in 5, 10 or 15 wt.% NaOH solutions for 2 h, and the effects of the alkali treatments on the mechanical characteristics and interfacial adhesion of the fibers in a model abaca fiber/epoxy composite system systematically evaluated. After 5 wt.% NaOH treatment, abaca fibers showed increased crystallinity, tensile strength and Young’s modulus compared to untreated fibers, and also improved interfacial shear strength with an epoxy. Stronger alkali treatments negatively impacted fiber stiffness and suitability for composite applications. Results suggest that mild alkali treatments (e.g. 5 wt.% NaOH for 2 h) are highly beneficial for the manufacture of abaca fiber-reinforced polymer composites.     

Reinforcing potential of micro- and nano-sized fibers in the starch-based biocomposites

Starch-based biocomposites reinforced with jute (micro-sized fiber) and bacterial cellulose (BC) (nano-sized fiber) were prepared by film casting. Reinforcement in the composites is essentially influenced by fiber nature, and amount of loading. The optimum amount of fiber loading for jute and bacterial cellulose in each composite system are 60 wt% and 50 wt% (of starch weight), respectively. Mechanical properties are largely improved due to the strong hydrogen interaction between the starch matrix and cellulose fiber together with good fiber dispersion and impregnation in these composites revealed by SEM. The composites reinforced with 40 wt% or higher bacterial cellulose contents have markedly superior mechanical properties than those reinforced with jute. Young’s modulus and tensile strength of the optimum 50 wt% bacterial cellulose reinforced composite averaged 2.6 GPa and 58 MPa, respectively. These values are 106-fold and 20-fold more than the pure starch/glycerol film. DMTA revealed that the presence of bacterial cellulose (with optimum loading) significantly enhanced the storage modulus and glass transition temperature of the composite, with a 35 °C increment. Thermal degradation of the bacterial cellulose component occurred at higher temperatures implying improved thermal stability. The composites reinforced with bacterial cellulose also had much better water resistance than those associated with jute. In addition, even at high fiber loading, the composites reinforced by bacterial cellulose clearly retain an exceptional level of optical transparency owing to the effect of the nano-sized fibers and also good interfacial bonding between the matrix and bacterial cellulose.     

Effect of ZnO nanowire morphology on the interfacial strength of nanowire coated carbon fibers

The ability to tailor interfacial shear strength for a particular fiber and resin system is critical to the development of composite materials that perform optimally in specific applications. One approach to tailor the interface is to introduce a secondary phase between the fiber and matrix, which can act to functionally grade the material properties and enhance load transfer across the interface. This approach has been applied in the past using nanowires, nanotubes, and whiskers and was demonstrated to significantly enhance interface performance. Unfortunately, these processes lack control over the interphase morphology to allow design of the interface for optimal properties. Recently, ZnO nanowires grown on the surface of carbon fibers have demonstrated more than a 110% increase in interfacial strength [1]. Unlike other treatments, this interfacial reinforcement allows precise morphology control. Here, we develop the parameters for the growth of nanowires with varying lengths and diameters and study the influence of the nanowire’s morphology on the interfacial shear strength. ZnO nanowire arrays are grown on carbon fibers, with nanowire diameters ranging from 50 to 200 nm and lengths up to 4 μm. The interfacial shear strength with varying nanowire dimensions is shown to increase by up to 228%, ranging from 45.72 to 154.64 MPa. Unlike existing whiskerization approaches, it is shown that the tensile strength of the ZnO nanowire coated fibers remains constant throughout all growth procedures. The development of an interphase offering control over the interface strength and toughness will provide a means to produce multifunctional composites with optimized performance for multiple applications.     

Studies on the characterization of piassava fibers and their epoxy composites

This paper presents morphology, physical and strength properties of piassava fiber, a very rigid fiber having a potential to be used as composite reinforcement. Composites of continuous and aligned piassava fibers with and without alkali treatment dispersed in epoxy matrix were subjected to three point bend, tensile, and Izod impact tests. Composites with fibers above 20 vol.% showed an effective reinforcement behavior both in flexural and tensile tests, while the impact energy linearly increased for the amount of piassava fibers used in this study. Fractographic study revealed a relatively weaker fiber/matrix adhesion acting as preferential site for crack nucleation. Evidence was also found for crack arrest by the fiber above 20 vol.%. This, together with spiny surface protrusion in the piassava fibers, was found to be responsible for the reinforcement of the epoxy composites.     

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.     

Allyloxy-modified starch with low degree of substitution for fiber reinforced thermoset starch composites

In the present work dough moulding compound premixes of allyl glycidyl ether modified (AGE)-potato starch, (DS) = 0.2, has been prepared and tested for its fiber reinforced composite properties. The AGE-starch was hydrolyzed with α-amylase under neutral condition for 6 h at 45 °C for improved process ability. The grafting and hydrolytic scission was confirmed by nuclear magnetic resonance (NMR) and size exclusion chromatography (SEC), respectively. Homogeneous composite premixes of AGE-starch, wood fibers, various amount of glycerol and ethylene glycol dimethacrylate were successfully mixed with a Brabender-kneader at 55 °C and cured by compression molding at 150 °C using 2 wt% of dibenzoyl peroxide. Adding 5 wt% of glycerol did not reduce the ultimate strength of the composites; 10% glycerol reduced the strength from 60 MPa to 40 MPa, and 16% glycerol to 14 MPa. The results with 5 wt% glycerol are comparable with earlier achieved results. The water absorption rate increased with increased glycerol content and the mechanical strength of the composites was lost completely when the moisture uptake reached 15 wt%.     

High-performance composites based on all-aromatic liquid crystal thermosets

In this study, a new high-performance liquid crystal ester-based thermoset for composite applications was investigated. All-aromatic liquid crystalline thermosets (LCTs) are a promising class of polymers that offer a unique combination of properties such as solvent resistivity, high modulus, high strength, low coefficient of thermal expansion and high after cure glass-transition temperatures (T_g ? 150 °C). Fully cured LCTs offer superior thermo-mechanical properties over high-performance thermoplastic polymers such as PPS, PEEK and PEI. For this study we used a 9000 g mol⁻¹ ester-based LCT based on cheap and readily available monomers, i.e. 4-hydroxybenzoic acid (H), isophthalic acid (I) and hydroquinone (Q), abbreviated by us as HIQ-9. Composite panels prepared from T300 carbon fiber (5-harness satin weave) showed in-plane shear strength of 154 MPa and an in-plane shear modulus of 3.7 GPa. The tensile strength and modulus were measured to be 696 MPa and 57 GPa, respectively. A post-mortem inspection showed that the interfacial strength was excellent and no delamination was observed in the test specimen. Preliminary results show that LCT-based composites exhibit a better combination of (thermo) mechanical properties over PPS and PEI-based composites.     

Covalent functionalization of graphene with organosilane and its use as a reinforcement in epoxy composites

Functionalized graphene nanosheets (f-GNSs) produced by chemically grafting organosilane were synthesized by a simple covalent functionalization with 3-aminopropyl triethoxysilane. The f-GNSs showed a larger thickness, but smaller width and than the un-treated graphene. The covalent functionalization of graphene with silane was favorable for their homogeneous dispersion in the polymer matrix even at a high nanofiller loading (1 wt.%). The initial thermal degradation temperature of epoxy composite was increased from 314 °C to 334 °C, at a f-GNS content of 1 wt.%. Meanwhile, the addition of 1 wt.% f-GNSs increased the tensile strength and elongation to failure of epoxy resins by 45% and 133%, respectively. This is believed to be attributed to the strong interfacial interactions between f-GNSs and the epoxy resins by covalent functionalization. The experimentally determined Young’s modulus corresponded well with theoretical simulation under the hypothesis that the graphene sheets randomly dispersed in the polymer matrix.     

Optimum dispersion conditions and interfacial modification of carbon fiber and CNT–phenolic composites by atmospheric pressure plasma treatment

Electric resistance measurements were used to determine the optimal dispersion conditions for carbon nanotubes (CNTs) in phenolic resins. Plasma treatment is frequently used to modify carbon fiber surfaces to improve adhesion of the fibers to matrices. Such treatment might also influence carbon fiber tensile strength. In order to determine the effect of atmospheric pressure plasma treatment on carbon fiber tensile strength and interfacial bonding strength, change in tensile strength of the fiber was studied at different gage lengths before and after the plasma treatment. The wettability of carbon fibers was improved significantly after only 10 s of plasma treatment. Such plasma treatment resulted in a decrease in the advancing contact angle from 65° to 28°. Surface energies of carbon fiber and CNT–phenolic composites were measured using the Wilhelmy plate technique, indicating that the work of adhesion between plasma treated carbon fibers and CNT–phenolic composites was higher than it before plasma modification. The interfacial shear strength (IFSS) and apparent modulus were also increased by plasma treatment of the carbon fibers.