Improvement of fracture properties of hydroxyapatite particle filled poly(l-lactide)/poly(ε-caprolactone) biocomposites using lysine tri-isocyanate

Effects of LTI addition on the mode I fracture energy of HA/PLLA/PCL were examined and the micro-structural modification due to LTI addition was investigated. Both the mode I energy release rate, G _in, and averaged fracture energy, E _f, are improved dramatically due to LTI addition. The reason is considered to be the improvements of the interfacial structure connecting HA particles with PLLA/PCL matrix and the miscibility between PLLA and PCL. These changes of blend morphology and interfacial structure reduce the stress concentration and lead to the ductile deformation and resulted in the increase of those fracture properties.     

Characteristic crack-tip distances in fracture criteria: Is crack propagation discontinuous?

The present paper describes a possible mechanism for discontinuous crack advance in which surface separation occurs initially not at the crack-tip itself but within the crack-tip plastic zone of size r_p, at the mid-point of the crack-tip characteristic distance d (identified here with the finite growth step Δa), i.e., at the region of maximum opening tensile stress, spreading towards (and also away from) the crack-tip. The crack extension occurs when the crack-tip is reached and full opening over the distance d is completed.Finite element analyses show that this mechanism causes the formation of a rippled crack face surface in elastic-plastic materials in which irreversible plastic deformations take place during each growth step, in sharp contrast with the smooth surface created in ideal elastic materials in which all deformations are fully reversible. Some pictorial evidence of void formation ahead of the crack tip and of ripples during propagation, found in the literature, is presented.Although the present analysis is from a continuum standpoint it is acknowledged that micro structural features and mechanisms can condition the fracture events taking place in the process zone.The implication to the brittle-ductile transition of the dependence of the energy release rate, G^ΔΞ, on the ratio q (=Δa/r_p) is also discussed.     

Fracture criterion for kinking cracks in a tri-material adhesively bonded joint under mixed mode loading

The fracture behavior of a composite/adhesive/steel bonded joint was investigated by using double cantilever beam specimens. A starter crack is embedded at the steel/adhesive interface by inserting Teflon tape. The composite adherend is a random carbon fiber reinforced vinyl ester resin composite while the other adherend is cold rolled steel. The adhesive is a one-part epoxy that is heat cured. The Fernlund-Spelt mixed mode loading fixture was employed to generate five different mode mixities. Due to the dissimilar adherends, crack turning into the adhesive (or crack kinking) associated with joint failure, was observed. The bulk fracture toughness of the adhesive was measured separately by using standard compact tension specimens. The strain energy release rates for kinking cracks at the critical loads were calculated by a commercial finite element analysis software ABAQUS in conjunction with the virtual crack closure technique. Two fracture criteria related to strain energy release rates were examined. These are (1) maximum energy release rate criterion (G_max) and, (2) mode I facture criterion (G_II = 0). They are shown to be equivalent in this study. That is, crack kinking takes place at the angle close to maximum G or G_I (also minimum G_II, with a value that is approximately zero). The average value of G_IC obtained from bulk adhesive tests using compact tension specimens is shown to be an accurate indicator of the mode I fracture toughness of the kinking cracks within the adhesive layer. It is concluded that the crack in tri-material adhesively bonded joint tends to initiate into the adhesive along a path that promotes failure in pure mode I, locally.     

Preparation of electrospun nanofibers of star-shaped polycaprolactone and its blends with polyaniline

The electrospun nanofibers of synthetic star-shaped poly(?-caprolactone) (PCL) and its blends with polyaniline (PANI) were prepared. We utilized the advantages of star-shaped PCL and benefits of electrospinning method for obtainment of the uniform nanofibers with improved properties for tissue engineering. Biodegradable star-shaped PCL with four arms was synthesized by Sn(Oct)₂-catalyzed ring-opening polymerization (ROP) of ?-caprolactone (CL) from a pentaerythritol core. The chemical structure of star-shaped PCL was investigated by FTIR, and average molecular weight of polymer was determined by ¹HNMR (about 38000 g mol^?1). Thermal behavior of star-shaped PCL was also studied by Thermogravimetric Analysis (TGA). Moreover, the cyclic voltammetry (CV) measurement confirmed the preparation of electroactive nanofibers. The scanning electron microscopy (SEM) was also used to investigate the morphology of electrospun nanofibers produced from star-shaped PCL and its blends with PANI with different feed ratios. The presence of PANI resulted in fibers with diameters less than 100 nm and significant decrease of bead formation.     

Crack toughness behavior of binary poly(styrene-butadiene) block copolymer blends

Fracture behavior of binary blends comprising styrene-butadiene block copolymers having star and triblock architectures was studied by instrumented Charpy impact test. The toughness of the ductile blends was characterized by the dynamic crack resistance concept (R curves). While the lamellar thermoplastic star block copolymer shows elastic behavior (small scale yielding and unstable crack growth), adding 20 wt% of a triblock copolymer (thermoplastic elastomer, TPE) leads to a strong increase in crack toughness. The stable crack propagation behavior of these blends was described by the crack resistance curve (R) concept of elastic-plastic fracture mechanics. This concept allows the determination of fracture mechanics parameters as resistance against stable crack initiation and propagation. Two brittle to tough transitions (BTT) are observed in the binary block copolymer blend: BTT1 at 20% TPE and BTT2 at about 60% TPE. The strong increase of toughness at 60 wt% TPE indicates a tough/high-impact transition as a measure for the protection against stable crack initiation.The kinetics of stable crack propagation is discussed with respect to deformation mechanisms and crack-tip blunting behavior. The analysis of fracture surface by SEM revealed three different types of deformation mechanisms depending on the weight fraction of TPE: coalescence of microvoids (similar to semicrystalline polymers), shear flow (typical of many amorphous polymers like polycarbonate) and tearing (similar to elastomers). Our investigations on nanostructured binary block copolymer blends show new possibilities to tailor the toughness of polymer materials associated with complex morphology-toughness correlations. This may lead to new materials concepts for toughened nanostructured polymers, which still maintain excellent transparency.     

Isotactic polypropylene/EPDM blends: Effect of testing temperature and rubber content on fracture

Charpy impact tests in the temperature range ?100 to +20° C have been carried out on two isotactic polypropylenes (PP) having different molecular weight and their blends containing as rubbery phase an ethylene-propylene-diene terpolymer (EPDM). For fractures of brittle nature the impact data were analysed in terms of the linear elastic fracture mechanics andK _c andG _c were determined. This behaviour was observed for the homopolymers over the temperature range investigated, and for the blends only up to ?20° C. At higher temperatures such materials showed fracture of a semiductile type with visible evidence of craze whitening around the crack tip, followed by brittle type fracture. In this case the results were analysed in terms of a ductile contribution (energy required to form the crazed area) and of a brittle one (relative to the crack propagation area) from whichG _c could be derived according to a procedure proposed in the literature. Tentative interpretations of the results also on a molecular and structural basis have been given. A critical discussion of the elaboration of the semiductile fracture data proposed in the literature has also been provided.     

Fracture analysis of a surface through-thickness crack in PZT thin film under a continuous laser irradiation

In this paper, the surface crack problem in PZT thin films under a continuous laser irradiation has been investigated by the superposition principle. Using commercial (FEM) software ANSYS 9.0, the piezoelectric fields near the crack tip were solved for surface crack in the finite PZT thin film. The SIFs for crack-tip fields were obtained by using the limited stress extrapolation technique (LSET) and then the energy release rates were calculated by the relation to the intensity factors. When the irradiation time and crack location were changed, the energy release rates G, G_I, and G_e for total, mechanical terms (mode I) and electric contribution were investigated. The results show that the mechanical opening mode I is the main mode for the surface crack under a continuous laser irradiation. However, electric mode IV has inhibiting effect on crack growth. At the beginning of laser irradiation, the surface tiny crack which is close to the centre of film will propagate more easily. During the laser irradiation, the crack which is far from the centre of film will propagate more easily.     

Relation between work of fracture and fracture toughness of short-fibre reinforced polymers

On the basis of micromechanical failure mechanisms acting in short-fibre reinforced polymers we derive the crack resistance curve (R-rmcurve) as a function of crack extension. With the conditions characterizing the point of crack instability, the critical crack extension and fracture toughness, G_c, are calculated. By comparing G_c to the work of fracture we are able to conclude that, depending on the relevant failure characteristics, two parameters are necessary to describe the failure behaviour—the fracture toughness for crack instability or strength and the work of fracture as the energy necessary to drive the crack through the sample.     

Fracture and fatigue of natural fiber-reinforced cementitious composites

This paper presents the results of an experimental study of resistance-curve behavior and fatigue crack growth in cementitious matrices reinforced with eco-friendly natural fibers obtained from agricultural by-products. The composites include: blast furnace slag cement reinforced with pulped fibers of sisal, banana and bleached eucalyptus pulp, and ordinary Portland cement composites reinforced with bleached eucalyptus pulp. Fracture resistance (R-curve) and fatigue crack growth behavior were studied using single-edge notched bend specimens. The observed stable crack growth behavior was then related to crack/microstructure interactions that were elucidated via scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Fracture mechanics models were used to quantify the observed crack-tip shielding due to crack-bridging. The implications of the results are also discussed for the design of natural fiber-reinforced composite materials for affordable housing.     

Damage zone around crack tip and fracture toughness of rubber-modified epoxy resin under mixed-mode conditions

Damage zones that form around crack tips before the onset of fracture provide significant data for evaluating the fracture behavior of polymeric materials. The size of the damage zone correlates closely with the fracture toughness of the resin. In this study, we investigate the relationship between the fracture toughness and damage zone size around crack tips of a rubber-modified epoxy resin under mixed-mode conditions. The fracture toughness, G_C, based on the energy release rate, is measured using an end-notched circle type (ENC) specimen. The deformation of rubber particles in the damage zones is also observed using an optical microscope. The results show that the fracture toughness, G_C, of the rubber-modified epoxy resin is closely related to the area of the damage zone. In the specimen with a loading angle of 30°, the rubber particles were deformed ellipsoidally due to the difference between the first and second principal stresses.     

Investigation of the effect of addition of calcium stearate on the properties of low-density polyethylene/poly(ε-caprolactone) blends

Low-density polyethylene (LDPE) was blended with poly(ε-caprolactone) (PCL), prepared in proportions of 75/25, 50/50, and 25/75 (LDPE/PCL, wt/wt%). The effect of the addition of calcium stearate (CaSt) of these polymers was assessed by melting flow index, differential scanning calorimetry, tensile test, scanning electron microscopy (SEM), biodegradation in simulated soil with calcium determination, and enzymatic degradation. The addition of CaSt reduced the MFI of the PCL and of the 75/25 blend. The incorporation of 25 % of PCL slightly increased the T _m of LDPE. The tensile strength had no significant changes with the addition of CaSt and the polymers showed that they are incompatible according to this property. SEM showed poor interfacial interaction between PCL and LDPE, as well as that they are immiscible, and showed no significant changes on the morphology of the materials with the addition of CaSt. The results show that polymer samples after biodegradation in simulated soil present more calcium content than initial samples polymer. The soil analysis shows that the soil that contains the polymers submitted to thermal aging show smaller calcium content than the samples that were not aged. Lipase enzyme reinforced its specificity over PCL, and the addition of CaSt reduced the degradation of PCL and the 75/25 PCL/LDPE blend, however, it increased the rate of degradation of 50/50 and 25/75 blends.     

Interlaminar and intralaminar fracture modes in 0/90 cross-ply glass/epoxy laminate

Delamination of a cross-ply 0/90 glass fibre-reinforced composite laminate with an epoxy-phenol matrix was studied using a double cantilever beam test. Fracture toughness was determined by measurement of bend angle of the cantilever beams. Results obtained with this method were in agreement with those from conventional compliance and area methods. Two different fracture modes were observed: interlaminar and intralaminar. In the interlaminar fracture mode, crack jumps in the space between two neighbouring 0° and 90° plies were observed. With the interlaminar fracture mode, during crack initiation G_Ic decreased with crack length. Intralaminar fracture mode consisted of the gradual growth of a crack through a 0° ply. Fibres bridging the opposite sides of the crack were observed in this case, and fracture toughness G_Ic did not change with crack length. G_Ic (420 J m⁻²) at intralaminar fracture mode was approximately twice that at interlaminar fracture mode (220 J m⁻²). The difference in fracture toughness was explained by the dissipation of energy by fibres bridging the opposite sides of the crack at intralaminar fracture mode.     

An integrated approach based on acoustic emission and mechanical information to evaluate the delamination fracture toughness at mode I in composite laminate

This paper addresses a new method based on the combination of mechanical behavior and acoustic emission (AE) information of composite materials during mode I delamination. The method is based on a special purpose function, called sentry function, which is defined as the logarithm of the ratio between mechanical energy and acoustic energy (f = Ln(E_s/E_a)). The sentry function is used to study the delamination process and to evaluate the delamination fracture toughness in mode I. The relationship between cumulative fracture toughness energy release rate (G_I) and the integral of the sentry function during crack propagation showed a transition point with two sensitive regions below and above it. This behavior can be followed to obtain the critical strain energy release rate value (G_Ic). Results obtained by means of the sentry function are compared with results obtained by a methodology proposed by other authors.     

Orientation and loading condition dependence of fracture toughness in cortical bone

The fracture toughness at crack initiation were determined for bovine cortical bone under tension (mode I), shear (mode II), and tear (mode III). A total of 140 compact tension specimens, compact shear specimens and triple pantleg (TP) specimens were used to measure fracture toughness under tension, shear, and tear, respectively. Multiple-sample compliance method was utilized to measure the critical strain energy release rate (G_c) at the a/W=0.55 (crack length, a, to specimen width, W, ratio). The critical stress intensity factor (K_c) was also calculates from the critical loading (P_c) of the specimens at the a/W=0.55. The effect of the anisotropy of bone on its resistance to crack initiation under shear and tear loading was investigated as well. Fracture toughness of bone with precrack orientations parallel (designed as longitudinal fracture) and vertical (designed as transverse fracture) to the longitudinal axis of bone were compared. In longitudinal fracture, the critical strain energy release rate (G_c) of cortical bone under tension, shear, and tear was 644±102, 2430±836, and 1723±486 N/m, respectively. In transverse fracture, the critical strain energy release rate (G_c) of cortical bone under tension, shear, and tear was 1374±183, 4710±1284, and 4016±948 N/m, respectively. An unpaired t-test analysis demonstrated that the crack initiation fracture toughness of bone under shear and tear loading were significantly greater than that under tensile loading in both longitudinal and transverse fracture (P<0.0001 for all). Our results also suggest that cortical bone has been “designed” to prevent crack initiation in transverse fracture under tension, shear, and tear.     

Mixed mode fracture of a brittle orthotropic material—example of strongly textured zinc sheets

The response to mixed mode fracture of strongly textured sheets of impure zinc has been investigated using centrally cracked panels tested at 77 K. The specimens were designed such that the crack which was oriented at various angles to the tensile axis was always parallel to the basal plane direction. In this orthotropic material the strain energy release rate at fracture (G_c) is calculated using the analytical results published in the literature. The angular variation of G is calculated using the Nuismer's approximation. It is shown that the energy approach has some limitations as far as the prediction of mixed mode fracture in anisotropic materials is concerned. A local approach in terms of a combination of the resolved normal stress σ_n and the resolved shear stress (τ) applied to the basal slip plane is proposed to account for the fracture behavior of this material in mixed mode loading.     

Fracture toughness investigation of the dynamically vulcanized EPDM/PP/ionomer ternary blends using the J-integral via the locus method

The fracture mechanics investigation of the dynamically vulcanized EPDM and PP/ionomer ternary blends was performed in terms of the J-integral by measuring fracture energy via the locus method. The ternary blends consisting of EPDM, PP and ionomer were prepared in a laboratory internal mixer by blending and vulcanizing simultaneously. Vulcanization was performed with dicumyl peroxide (DCP) and the composition of EPDM and PP was fixed at 50/50 by weight. Two kinds of poly(ethylene-co-methacrylic acid) (EMA) ionomers were used. The J-integral values at crack initiation, J _c, of the dynamically vulcanized EPDM and PP/EMA ionomer ternary blends were affected by the cation types (Na⁺ or Zn²⁺) and contents (5–20 wt%) of the added EMA ionomers. The ternary blend containing 20 wt% zinc-neutralized EMA ionomer and 1.0 p.h.r. DCP showed the highest J _c values of the blends. The results have been discussed with regard to the fracture topology observed by scanning electron microscopy (SEM).     

The toughness of epoxy-poly(butylene terephthalate) blends

Blends containing 5% poly(butylene terephthalate) (PBT) in an anhydride-cured epoxy with three different PBT morphologies were studied. The three morphologies were a dispersion of spherulites, a structureless gel and a gel with spherulites. The average fracture toughnesses, K _Ic, and fracture energies, G _Ic, for those morphologies were 0.83, 2.3 and 1.8 MPa m^1/2 and 240, 2000 and 1150 J m^–2, respectively. These values should be compared with the values of 0.72 MPa m^1/2 and 180 J m^–2, respectively, for the cured epoxy without PBT. The elastic moduli and yield strengths in compression for all three blend morphologies remained essentially unchanged from those of the cured epoxy without PBT, namely, 2.9 GPa for the modulus and 115 MPa for the yield strength. The fracture surfaces of the cured spherulitic dispersion blends indicate the absorption of fracture energy by crack bifurcation induced by the spherulites. The fracture surfaces of the cured structureless gel blends indicate that fracture energy was absorbed by matrix and PBT plastic deformation and by spontaneous crack bifurcation. But phase transformation of the PBT and anelastic strain of the matrix below the fracture surfaces may account for most of the large fracture energy of the cured structureless gel blends.     

The effect of siloxane-type molecules on the interlaminar toughness of CFRP

The effect of the addition of two different release agents (high and low molecular weight), and one adhesion promoter have on the interlaminar chemistry and morphology of a carbon fibre reinforced polymer (CFRP) system has been studied by the use of time-of-flight secondary ion mass spectrometry (ToF-SIMS) and scanning electron microscopy (SEM). This was compared with the critical strain-energy release rate (G_IC) values measured by a double cantilever beam test. Unexpectedly, it was found that a low molecular weight polydimethylsiloxane (PDMS) had the effect of increasing the G_IC value of the composite by a factor of two. Both the addition of an adhesion promoter, 3-aminopropyltriethoxysilane, and the removal of residual PDMS from the manufacturing process were found to have very little effect on the measured G_IC values, whilst the use of a viscous PDMS induces this parameter to fall by a factor of two. SEM micrographs revealed an unusual fracture morphology in the composite that displayed improved resistance to delamination, where the presence of voids or bubbles was observed on approximately 50% of the fracture surface. ToF-SIMS revealed that PDMS (residual from the manufacturing process) was present on all Mode I fracture surfaces, and mechanical data indicated that it did not prove to be detrimental to the toughness of the composite.     

Influence of electroless nickel-plating on fracture toughness of pitch-based carbon fibre reinforced composites

Nickel-Pitch-based carbon fibres (Ni-PFs) were prepared by electroless nickel-plating to enhance fracture toughness of Ni-PFs reinforced epoxy matrix composites (Ni-PFs/epoxy). The surface properties of Ni-PFs were determined by scanning electron microscopy (SEM), X-ray photoelectron spectrometry (XPS), and X-ray diffraction (XRD). The fracture toughness of the Ni-PFs/epoxy was assessed by critical stress intensity factor (K_IC) and critical strain energy release rate (G_IC). The fracture toughness of Ni-PFs/epoxy was enhanced compared to those of PFs/epoxy. These results were attributed to the increase of the degree of adhesion at interfaces between Ni-PFs and matrix resins in the composites.     

Three-dimensional fracture analysis of thin-film debonding

A simplified mixed-mode fracture analysis combining nonlinear thin-plate stress solutions with crack-tip elasticity results has been developed to account for local variations of G _I, G _II and G _III in thin-film debond problems associated with large film deformations. Membrane and bending stresses from the plate analysis are matched with the crack-tip singularity solution over a small boundary region at the crack tip where the effect of geometric nonlinearity is small. Local variations in each of the individual components of the energy release rate are directly related to the jump in these stresses across the crack border.Specific results are presented for 1-D and elliptical planeform cracks. Deformations were induced either by a pressure acting normal to the film surface or biaxial compression or tension stresses applied to the substrate in which the loading axes and debond axes coincide. The latter type of loading involves buckling of the delaminated film. The model predictions compare well with more rigorous solutions provided the film thickness is small compared to the debond dimensions. In all cases analyzed, G _III was negligible. The ratio G _I/G _II typically decreases with increasing load or film deformation, the rate was moderate for pressure loading while generally sharp for compression loading. Film-substrate overlap may occur for certain debond geometry and loading conditions. Prevention of this by the substrate may critically increase the energy available for crack propagation.