Monotonic properties of unidirectional glass fiber (U)/random glass fiber (R)/epoxy hybrid composites

The main objective of the present paper is to study the tensile and bending behaviors of unidirectional glass fiber (U)/random glass fiber (R)/epoxy hybrid composites with total fiber volume fraction (V_fT) = 37%. Six kinds of laminated composites of average thickness 5.5 mm were manufactured using hand lay-up technique; i.e. [R]₅, [U/R/U/R/U], [U/0.5R/U]_S, [0.5R/U/U]_S, [U/U/0.5R]_S, and [U]₅. In bending test, notched and unnotched specimens were tested. For this purpose different circular notch sizes (D = 3, 6, 9 mm) were drilled at the specimen center. Tensile strength, tensile modulus, Poisson’s ratio, bending strength and bending modulus were determined experimentally. The effect of stacking sequences, random fiber relative volume fraction (V_fR/V_fT), and notch diameter on the mechanical properties of the mentioned composite types were studied. Failure modes of all specimens were investigated.     

An investigation into the damage development and residual strengths of open-hole specimens in fatigue

An extensive experimental program was carried out to investigate and understand the sequence of damage development throughout the life of open-hole composite laminates loaded in tension–tension fatigue. Quasi-isotropic carbon/epoxy laminates, with stacking sequence [45₂/90₂/−45₂/0₂]_S, [45/90/−45/0]_2S and [45/90/−45/0]_4S were examined. These were selected on the basis that under quasi-static loading the [45₂/90₂/−45₂/0₂]_S configuration exhibited a delamination dominated mode of failure whilst the [45/90/−45/0]_2S and [45/90/−45/0]_4S configurations showed a fibre dominated failure mode, previously described as “pull-out” and “brittle” respectively. Specimens were fatigue loaded to 1 × 10⁶ cycles or catastrophic failure, which ever occurred first. A number of tests were interrupted at various points as the stiffness dropped with increasing cycles, which were inspected using X-ray computed tomography (CT) scanning. A static residual strength program was carried out for run-out specimens of each configuration.     

Toughness,flexural, damping and interfacial properties of hybridized GFRE composites with MWCNTs

As the improved damping in fiber-reinforced composites can affect the other mechanical properties, therefore, the aim of this work is to investigate the effect of multiwall carbon nanotube (MWCNT) on the interfacial bond strength, flexural strength and stiffness, toughness and damping properties of hybridized glass-fiber reinforced epoxy (GFRE) composites. Nanophased epoxy resin was used to hybridize unidirectional and quasi-isotropic GFRE composites with [0/±45/90]_s and [90/±45/0]_s stacking sequences. Results from the interfacial characterizations of the hybridized composites showed improvement up to 30% compared to the control laminates. Hybridization of GFRE laminates with MWCNTs leads to decreasing the flexural and storage moduli, increasing flexural strength, toughness, natural frequencies and damping ratio. A high correlation coefficient of 0.9985 was obtained between static flexural and dynamic storage moduli. The highest flexural strength, flexural and storage moduli and natural frequency of quasi-isotropic laminate were observed for [0/±45/90]_s stacking sequence and vice versa for damping ratio.     

Fatigue life evaluation for carbon/epoxy laminate composites under constant and variable block loading

This paper presents the results of current research on the fatigue life prediction of carbon/epoxy laminate composites involving twelve balanced woven bidirectional layers of carbon fibres and epoxy resin manufactured by a vacuum moulding method. The plates were produced with 3 mm thickness and 0.66 fibre weight fraction. The dog bone shape specimens were cut from these plates with the load line aligned with one of the fibre directions. The fatigue tests were performed using load control with a frequency of 10 Hz and at room temperature. The fatigue behaviour was studied for different stress ratios and for variable amplitude block loadings. The damage process was monitored in terms of the stiffness loss. The fatigue life of specimens submitted to block loading tests was modelled using Palmgren–Miner’s law and taking in to account the stress ratio effect. The estimated and experimental fatigue lives were compared and good agreement was observed.     

3D damage characterisation and the role of voids in the fatigue of wind turbine blade materials

The fatigue mechanisms of Glass Fibre Reinforced Polymer (GFRP) used in wind turbine blades were examined using computed tomography (CT). Prior to mechanical testing, as-manufactured [+45/−45/0]_3,s glass/epoxy specimens were CT scanned to provide 3-dimensional images of their internal microstructure, including voids. Voids were segmented and extracted, and individual characteristics and volumetric distributions were quantified. The coupons were then fatigue tested in uniaxial loading at R = −1% to 40% of the nominal tensile failure stress. Some tests were conducted to failure for correlation with the initial void analysis and to establish failure modes. Other tests were stopped at various life fractions and examined using CT to identify key damage mechanisms. These scans revealed transverse matrix cracking in the surface layer, occurring predominantly at free edges. These free-edge cracks then appeared to facilitate edge delamination at the 45/−45° interface. Propagation from sub-critical, surface ply damage to critical, inner ply damage was identified with either a −45/0° delamination, or a 0° fibre tow failure allowing a crack to propagate into the specimen bulk. Final failure occurred in compression and was characterised by total delamination between all the 45/−45° plies. A quantitative void analysis, taken from the pre-test CT scans, was also performed and compared against the specimens’ fatigue lives. This analysis, to the authors’ knowledge the first of its kind, measured and plotted approximately 10,000 voids within the gauge length of each specimen. The global void measurement parameters and distributions showed no correlation with fatigue life. A local ply-level investigation revealed a significant correlation between the largest void and fatigue life in the region of the laminate associated with the crack propagation from sub-critical to critical damage.     

Transverse crack growth behavior considering free-edge effect in quasi-isotropic CFRP laminates under high-cycle fatigue loading

The high-cycle fatigue characteristics focused on the behavior of the transverse crack growth up to 10⁸ cycles were investigated using quasi-isotropic carbon fiber reinforced plastic (CFRP) laminates whose stacking sequence was [−45/0/45/90]_s. To assess the fatigue behavior in the high-cycle region, fatigue tests were conducted at a frequency of 100 Hz in addition to 5 Hz. In this study, to evaluate quantitative characteristics of the transverse crack growth in the high-cycle region, the energy release rate considering the free-edge effect was calculated. Transverse crack growth behavior was evaluated based on a modified Paris law approach. The results revealed that transverse crack growth was delayed under the test conditions of the applied stress level of σ_max/σ_b = 0.2.     

An experimental investigation into quasi-static and fatigue damage development in bolted-hole specimens

An extensive experimental program has been carried out to investigate and understand the sequence of damage development throughout the life of bolted-hole composite laminates under quasi-static loading and tension–tension fatigue. Quasi-isotropic carbon/epoxy laminates, with stacking sequence [45₂/90₂/-45₂/0₂]_S defined as ply scaled and [45/90/-45/0]_2S defined as sub-laminate scaled, were used. Specimens were cycled at 5 Hz with various amplitudes to 1 × 10⁶ cycles unless failure occurred prior to this limit. For all cases an R ratio of 0.1 was used. Bolt washer pressures of 23 MPa and 70 MPa were investigated. For the ply-level case, the quasi-static test showed both delamination and fibre-dominated pull-out failures for a washer pressure of 23 MPa, and pull-out failure only for 70 MPa. Delamination dominates in fatigue tests. For the sub-laminate case the tests failed by pull-out in both quasi-static and fatigue tests for all washer pressures. It is shown in this paper how the role of delamination is critical in the case of fatigue loading and how this interacts with bolt clamp-up forces. A number of tests were analysed for damage using X-ray CT scanning and comparisons of damage are made with tests from previous open-hole studies.     

Non-linear characterization of PP/Twaron laminates based on a model of plasticity with damage

The non-linear stress–strain response of thermoplastic laminates was investigated for a polypropylene matrix composite reinforced with continuous Twaron fibers. Tensile tests were performed on unidirectional composites with a fiber orientation of [0]₅, [24]₅, [33]₅, [45]₅ and [90]₅ and also on a [±45]_2S laminate. The inelastic strains of these materials were described with a modification made to a model of plasticity with damage, originally proposed by Ladeveze (1992). This approach considers the longitudinal plasticity and stiffening behavior of a thermoplastic composite, and models the damaged elastoplastic stress–strain response of the material. The theoretical stress–strain curves and experimental results from the model composites [0]₅, [90]₅ and [±45]_2S were compared, demonstrating that the model can be used as a designing tool for laminated thermoplastic composites.     

Cyclic fatigue crack propagation of nanoparticle modified epoxy

An experimental study on the fatigue performance of nanoparticle modified epoxy was conducted. Seven material systems were examined which were: neat epoxy (E), 6 and 12 weight percent (wt.%) silica nanoparticle modified epoxy (S6, S12), 6 and 12 wt.% rubber nanoparticle modified epoxy (R6, R12), 3 wt.% each of silica and rubber nanoparticle modified epoxy (S3R3) and 6 wt.% each of silica and rubber nanoparticle modified epoxy (S6R6). Effects of those nanoparticles on the fatigue threshold (ΔG_th and ΔK_th) and fatigue crack propagation rates (da/dN) were studied. It was found that, compared to neat epoxy (E), nanosilica (S6, S12) increased ΔG_th (and ΔK_th) but nanorubber (R6 and R12) did not. However, a synergistic effect was observed on the fatigue threshold when both silica and rubber nanoparticles were added into epoxy. All these nanoparticles, individually or conjointly, decreased da/dN with silica the most effective. Morphology of the fracture surface was examined to understand the role of nanoparticles on toughening mechanisms under cyclic loading, which depended on the applied ΔG levels.     

Preparation and investigation of the quaternary alloy CuTaInSe3

Polycrystalline samples of the quaternary alloy CuTaInSe₃ were prepared by the usual melt and anneal technique. The analysis of the diffraction pattern indicates a single phase which indexes as a tetragonal chalcopyrite-like structure with lattice parameters a = 5.7837 ± 0.0002 Å; c = 11.6208 ± 0.0007 Å and V = 389 ± 1 Å³. Differential thermal analysis shows that the melting transition of CuTaInSe₃ is incongruent with large liquid + solids regions.     

High resolution tomographic imaging and modelling of notch tip damage in a laminated composite

Synchrotron radiation computed tomography (SRCT) has been used to observe in situ damage growth and enable micromechanical damage characterization in [90/0]_S carbon fibre–epoxy composite samples loaded in uniaxial tension to stresses ranging from 30% to 90% of the nominal failure stress. A 3-D finite element model has been constructed to predict crack opening displacements and shear displacements in the 0° plies resulting from thermal residual stress imposed during autoclave cure and from the application of mechanical load. Of particular interest is the demonstration of SRCT as a technique to enable direct, in situ, 3-D, non-destructive damage quantification to assist model development and provide model validation. In addition it has been identified that SRCT has the potential for full field analysis of strain re-distributions during damage growth.     

New compounds Cu2MnTi3S8 and Cu2NiTi3S8 with thiospinel structure

Cu₂MnTi₃S₈ and Cu₂NiTi₃S₈ compounds were prepared by high-temperature synthesis. The crystal structure of these quaternary phases was investigated by X-ray powder diffraction. The compounds are described in the thiospinel structure (space group ) with the lattice constants a = 1.00353(1) nm (Cu₂MnTi₃S₈) and a = 0.99716(1) nm (Cu₂NiTi₃S₈). The atomic parameters were calculated in anisotropic approximation (R_I = 0.0456 and R_I = 0.0520 for Cu₂MnTi₃S₈ and Cu₂NiTi₃S₈, respectively).     

Failure behavior of quasi-isotropic laminates with three-pin loaded holes

This paper presents the effect of hole positions on the failure behavior of glass–epoxy laminated composite plates fabricated from stacking sequence [0/90/±45]_S subjected to a traction force by three-pins. Three different hole distance parameters, namely the ratio of free edge distance to the outer holes/pin diameter (E/D = 1, 2, 3, 4, 5), the ratio of longitudinal distance between the holes/pin diameter (F/D = 2, 4, 6) and the ratio of transverse distance between the parallel holes/pin diameter (G/D = 3, 4, 5) were used to investigate the effects of hole positions on failure load and failure mode. Shear out failure mode which is not the desired mode for a structure occurs around the first and second pin holes very close to the free edge of the specimen (E/D = 1). The other specimens were damaged in bearing mode which is the most desired mode.     

Highly porous polycaprolactone-45S5 Bioglass® scaffolds for bone tissue engineering

Highly porous biocompatible composites made of polycaprolactone (PCL) and 45S5 Bioglass® (BG) were prepared by a solid–liquid phase separation method (SLPS). The composites were obtained with BG weight contents varying in the range 0–50%, using either dimethylcarbonate (DMC) or dioxane (DIOX) as solvent, and ethanol as extracting medium. The porosity of the scaffolds was estimated to be about 88–92%. Mechanical properties showed a dependence on the amount of BG in the composites, but also on the kind of solvent used for preparation, composites prepared with DIOX showing enhanced stress at deformation with respect to composites prepared with DMC (stress at 60% of deformation being as high as 214 ± 17 kPa for DIOX-prepared composites and 98 ± 24 kPa for DMC-prepared ones, with 50 wt/wt_PCL% of glass), as well as higher elastic modulus (whose value was 251 ± 32 kPa for DIOX-prepared scaffolds and 156 ± 36 kPa for DMC-prepared ones, always with 50 wt/wt_PCL% of glass). The ability of the composites to induce precipitation of hydroxyapatite was positively evaluated by means of immersion in simulated body fluid and the best results were achieved with high glass amounts (50 wt/wt_PCL%). In vitro tests of cytotoxicity and osteoblast proliferation showed that, even if the scaffolds are to be considered non-cytotoxic, cells suffer from the scarce wettability of the composites.     

Microhardness studies on calcium hydrogen phosphate (brushite) crystals

Vicker's and Knoop microhardness studies were carried out on grown calcium hydrogen phosphate dihydrate (CaHPO₄·2H₂O) crystals over a load range of 10-50 g. The Vickers (H_V) and Knoop (H_K) microhardness numbers for the above loads were found to be in the range of 94-170 kg/mm² and 28-35 kg/mm² respectively. It was also found that these numbers increased with increase in load. The Mayer's index (n) was found to be greater than 1.6 showing soft-material characteristics. The fracture toughness values (K_c), determined from measurements of crack length, were estimated to be 6 ± 0.5 × 10³ kg m^−3/2 and 4.5 ± 0.5 × 10³ kg m^−3/2 at 25 g and 50 g respectively. The brittleness indices (B_i) were found as 2.3 ± 0.1 × 10⁴ m^−1/2 for 25 g and 3.7 ± 0.1 × 10⁴ m^−1/2 for 50 g. Using Wooster's empirical relation, the elastic stiffness coefficient (c₁₁) has been calculated from Vicker's hardness values as 4.8 ± 0.5 × 10¹⁵ Pa for 10 g, 9.7 ± 0.5 × 10¹⁵ Pa for 25 g and 13.3 ± 0.5 × 10¹⁵ Pa for 50 g. The Young's modulus was calculated as 1.5 ± 0.1 × 10¹⁰ N m⁻² from Knoop microhardness values.     

Tensile properties and fatigue characteristics of hybrid composites with non-woven carbon tissue

The mechanical characteristics of hybrid composites with non-woven carbon tissue (NWCT) are investigated under static tensile and tension–tension fatigue loadings. The hybrid composites are made by stacking NWCT and CFRP prepregs. Thirteen kinds of composites are studied; i.e. NWCT composites, CFRP longitudinal [0]₈, transverse [90]₁₂, off-axis [45]₁₂ and angle-ply [±45]_3S, hybrid longitudinal ([0/0]₄, [/0/0/]₄), transverse ([90/90]₆, [/90/90/]₆), off-axis ([45/45]₆, [/45/45/]₆), and angle-ply ([+45/−45]_3S, [/+45/−45/]_3S). The symbol ‘/’ means that the NWCT is located between the CFRP layers. To estimate the stiffness of hybrid composites, the rule of mixtures is used. The effects of NWCT on the tension–tension fatigue life, the residual strength and stiffness of hybrid specimens are evaluated. The fatigue damage and failure mechanisms of the hybrid composites are analyzed with an optical microscope.     

Crashworthiness characteristics investigation of silk/epoxy composite square tubes

This research concentrates on the evaluation of crashworthiness characteristics of natural silk/epoxy composite square tubes energy-absorbers. Composite laminate specimens were subjected to static axial compression load and experimental evaluation of the energy absorption capability of silk/epoxy composite. Specimens were in the form of square cross-sections with the dimension of 80 mm × 80 mm and a radius curvature of 5 mm. The variables in the experiment were the length of the tubes built 50 mm, 80 mm and 120 mm. Meanwhile, the thickness of the walls, consisting of laminates of silk/epoxy of 12, 24 and 30 plies, correspond to equivalent wall thickness of 1.7 mm, 3.4 mm and 4.2 mm, respectively. The parameters measured were the total absorbed energy (E_total), and the crash force efficiency (CFE). E_total is the measure of the amount of energy that the structure can withstand without failure and thus is a measure of its strength, while CFE gives a quantitative indication of the mode of failure of the composites. The mode of failure was observed using photography.     

Large-scale synthesis of ultralong Sb2S3 sub-microwires via a hydrothermal process

This paper describes an ethylene glycol (EG)-assisted approach to the large-scale ultralong Sb₂S₃ sub-microwires, formed by a simple hydrothermal reaction between SbCl₃ and Na₂S in the presence of distilled water. Transmission electron microscopy and scanning electron microscopy studies indicate that these Sb₂S₃ sub-microwires possess a diameter around 200 nm and length up to 100 μm. High-resolution transmission electron microscopy and selected area electron diffraction studies reveal that each Sb₂S₃ sub-microwire is a single-crystal along the [0 0 1] direction. The possible formation mechanism of the sub-microwires was discussed. The effects of volume ratio of EG/water, reaction temperature and the concentration of CO(NH₂)₂ on the morphology of Sb₂S₃ sub-microwires were also investigated.     

Electrical conductivity of yttrium-doped SrTiO3: influence of transition metal additives

The electrical conductivity of yttrium-doped SrTiO₃ with transition metals added as acceptor dopants (V, Mn, Fe, Co, Ni, Cu, Zn, Mo, Mg, Zr, Al, or Ga) was measured by the dc four-probe method at 600-900°C in reducing atmospheres. The replacement of 5 mol% titanium by acceptors leads to a decrease of conductivity of Sr_1−1.5xY_xTiO_3−δ. The degree of the decrease depends strongly on the type of dopant. Of the 5 mol% acceptor-doped compositions, the system Sr_0.85Y_0.10Ti_0.95Co_0.05O_3−δ had the highest conductivity of 45 S/cm at 800°C and oxygen partial pressure of 10⁻¹⁹ atm. The oxidation kinetics of yttrium-doped SrTiO₃ was significantly retarded by the addition of cobalt or manganese dopants. The ionic conductivity of SrTiO₃ doped with 5 mol% acceptors at Ti-sites was estimated from the total conductivity to lie in the vicinity of 10⁻⁴ S/cm, depending on oxygen partial pressure and temperature.     

Prediction of initiation of transverse cracks in cross-ply CFRP laminates under fatigue loading by fatigue properties of unidirectional CFRP in 90° direction

A fatigue life to the initiation of transverse cracks in cross-ply carbon fiber-reinforced plastic (CFRP) laminates has been predicted using properties of the fatigue strength of unidirectional CFRP in the 90° direction. In the experiments, unidirectional [90]₁₂ laminates were used to obtain a plot of maximum stress versus number of cycles to breaking, and two types of cross-ply laminates of [0/90₄]_S and [0/90₆]_S were used to evaluate the initiation and multiplication of transverse cracks under fatigue loading. Transverse cracks were studied by optical microscopy and soft X-ray photography. Analytical and experimental results showed good agreement, and the fatigue life for transverse crack initiation in cross-ply laminates was predicted successfully from the fatigue strength properties of the unidirectional CFRP in the 90° direction. The prediction results showed a conservative fatigue life than the experimental results.