Evaluation of effects of crack deflection and grain bridging on toughening of nanocrystalline SiO2 stishovite

Nanocrystalline SiO₂ stishovite has a fracture toughness higher than 10 MPa m^1/2 due to the toughening mechanism by fracture-induced amorphization. In order to identify other toughening mechanisms which may operate simultaneously, we evaluated effect of crack deflection on fracture toughness. The median deflection angle of nanocrystalline stishovite was lower than polycrystalline ceramics such as silicon nitride and Y-TZP. While the crack deflection can contribute to fracture toughness to some extent, it cannot be the major origin of high fracture toughness of nanocrystalline stishovite. We discussed also the role of grain bridging from the relation between the fracture toughness and grain size.     

Effects of SiC content on the densification,microstructure, and mechanical properties of HfB2–SiC composites

To investigate the effects of SiC on microstructure, hardness, and fracture toughness, 0, 10, 20, and 30 vol% SiC were added to HfB₂ and sintered by SPS. Upon adding SiC to 30 vol%, relative density increased about 4%; but HfB₂ grain growth had a minimum at 20 vol% SiC. This may be due to grain boundary silicate glass, responsible for surface oxide wash out, enriched in SiO₂ with higher fraction of SiC. By SiO₂ enrichment, the glass viscosity increased and higher HfO₂ remained unsolved which subsequently lead to higher grain growth. Hardness has increased from about 13 to 15 GPa by SiC introduction with no sensible variation with SiC increase. Residual stress measurements by Rietveld method indicated high levels of tensile residual stresses in the HfB₂ Matrix. Despite the peak residual stress value at 20 vol% SiC, fracture toughness of this sample was the highest (6.43 MPa m^0.5) which implied that fracture toughness is mainly a grain size function. Tracking crack trajectory showed a mainly trans-granular fracture, but grain boundaries imposed a partial deflection on the crack pathway. SiC had a higher percentage in fracture surface images than the cross-section which implied a weak crack deflection.     

Microstructure and fracture toughness of SiAlCN ceramics toughened by SiCw or GNPs

Mechanical alloying and spark plasma sintering (SPS) were used to prepare dense SiAlCN ceramic and SiAlCN ceramic toughened by SiC whiskers (SiC_w) or graphene nanoplatelets (GNPs). The influences of different reinforcements on the microstructure and fracture toughness were investigated. The SiAlCN ceramic exhibited a fracture toughness of 4.4 MPa m^1/2 and the fracture characteristics of grain bridging, alternative intergranular and transgranular fracture. The fracture toughness of SiC_w/SiAlCN ceramic increased to 5.8 MPa m^1/2 and toughening mechanisms were crack deflection, SiC_w bridging and pull-out. The fracture toughness of GNP/SiAlCN ceramic increased significantly, which was up to 6.6 MPa m^1/2. GNPs played an important role in grain refinement, which resulted in the smallest grain size. Multiple toughening mechanisms, including crack deflection, crack branch, GNP bridging and pull-out could be found. The better toughening effect could be attributed to the larger specific surface area of GNPs and the appropriate interface bonding between GNPs and matrix.     

Effect of cooling rate and crack propagation direction on the mode 1 interlaminar fracture toughness of biaxial noncrimp warp‐knitted fabric composites made of glass/PP commingled yarn

The mode 1 interlaminar fracture toughness of biaxial (±45°) noncrimp warp‐knitted fabric composites made of glass/PP commingled yarn was investigated. The crack propagation along the warp and weft directions, respectively, was considered for the composites cooled at two different rates during laminate molding. The interlaminar fracture toughness was characterized by determining the critical strain energy release rate (G_IC) of initiation and propagation measured from the double cantilever beam tests. In the case of a slow cooling rate (1°C/min), most specimens possess pure interlaminar crack propagation and direction‐independence characteristics. Nevertheless, the high‐cooled (10°C/min) specimens fractured in both directions suffer extensive intraply damage (crack branching, debonding, and bridging of 45°‐oriented interfacial yarns) and knit thread breakage, leading to G_IC of propagation two times higher than that of the slow‐cooled specimens, and the clear difference in the G_IC values of initiation between the two directions may be due to the contribution of the knit thread breakage to the fracture energy. POLYM. COMPOS., 2008 © 2007 Society of Plastics Engineers     

Determination of initiation value of mode I interlaminar fracture toughness of unidirectional polymer composites

The use of interlaminar fracture tests to measure the delamination resistance of unidirectional composite laminates is now widespread. However, because of the frequent occurrence of fiber bridging and multiple cracking during the tests, it leads to artificially high values of delamination resistance, which will not represent the behavior of the laminates. Initiation fracture from the crack starter, on the other hand, does not involve bridging, and should be more representative of the delamination resistance of the composite laminates. Since there is some uncertainty involved in determining the initiation value of delamination resistance in mode I tests in the literature, a power law of the form G_IC= A · Δ a^b (where G_IC is mode I interlaminar fracture toughness and Δ a is delamination growth) is presented in this paper to determine initiation value of mode I interlaminar fracture toughness. It is found that initiation values of the mode I interlaminar fracture toughness. G_ICini, can be defined as the G_IC value at which 1 mm of delamination from the crack starter has occurred. Examples of initiation values determined by this method are given for both carbon fiber reinforced thermoplastic and thermosetting polymers.     

Strengthening and toughening of TiN-based and TiB2-based ceramic tool materials with HfC additive

Effects of HfC addition on the microstructures and mechanical properties of TiN-based and TiB₂-based ceramic tool materials have been investigated. Their pore number decreased gradually and relative densities increased progressively when the HfC content increased from 15 wt% to 25 wt%. The achieved high relative densities to some extent derived from the high sintering pressure and the metal phases. HfC grains of about 1 µm evenly dispersed in these materials. Both TiN and TiB₂ grains become smaller with increasing HfC content from 15 wt% to 25 wt%, which indicated that HfC additive can inhibit TiN grain and TiB₂ grain growth, leading to the formation of a fine microstructure advantageous to improve flexural strength. Especially, TiB₂-HfC ceramics exhibited the typical core-rim structure that can enhance flexural strength and fracture toughness. The toughening mechanisms of TiB₂-HfC ceramics mainly included the pullout of HfC grain, crack deflection, crack bridging, transgranular fracture and the core-rim structure, while the toughening mechanisms of TiN-HfC ceramics mainly included pullout of HfC grain, fine grain, crack deflection and crack bridging. Besides, HfC hardness had an important influence on the hardness of these materials. Higher HfC content increased Vickers hardness of TiN-HfC composite, but lowered Vickers hardness of TiB₂-HfC composite, being HfC hardness higher than for TiN while HfC hardness is lower than for TiB₂. The decrease of fracture toughness of TiN-HfC ceramic tool materials with the increase of HfC content was attributed to the formation of a weaker interface strength.     

Fabrication and mechanical properties of Al2O3-SiCw-TiCnp ceramic tool material

Whiskers and nanoparticles are usually used as reinforcing additives of ceramic composite materials due to the synergistically toughening and strengthening mechanisms. In this paper, the effects of TiC nanoparticle content, particle size and preparation process on the mechanical properties of hot pressed Al₂O₃-SiC_w ceramic tool materials were investigated. The results showed that the Vickers hardness and fracture toughness of the materials increased with the increasing of TiC content. The optimized flexural strength was obtained with TiC content of 4 vol% and particle size of 40 nm. The particle size has been found to have a great influence on flexural strength and small influence on hardness and fracture toughness. It was concluded that the flexural strength increased remarkably with the decreasing of the TiC particle size, which was resulted from the improved density and refined grain size of the composite material due to the dispersion of the smaller TiC particle size. SEM micrographs of fracture surface showed the whiskers to be mainly distributed along the direction perpendicular to the hot-pressing direction. The fracture toughness was improved by whisker crack bridging, crack deflection and whisker pullout; the TiC nanoparticles in Al₂O₃ grains caused transgranular fracture and crack deflection, which improved the flexural strength and fracture toughness with whiskers synergistically. Uniaxial hot-pressing of SiC whisker reinforced Al₂O₃ ceramic composites resulted in the anisotropy of whiskers’ distribution, which led to crack propagation differences between lateral crack and radical crack.     

Local Fracture Toughness of Si3N4 Ceramics Measured using Single‐Edge Notched Microcantilever Beam Specimens

Local fracture toughness gives us useful and important information to understand and improve mechanical properties of bulk ceramics. In this study, the local fracture toughness of silicon nitride (Si₃N₄) ceramics was directly measured using single‐edge notched microcantilever beam specimens prepared by the focused ion beam technique. The measured fracture toughness of grain boundary of the Si₃N₄ ceramics is higher than the fracture toughness of SiAlON glass, which exists in the grain boundaries of Si₃N₄ ceramics. It is also shown that the fracture toughness of grain boundary depends on the rare earth oxide added as a sintering aid, which is expected in terms of the difference in the grain‐boundary structure. The fracture toughness of a single β‐Si₃N₄ grains is higher than the grain‐boundary fracture toughness. It was also higher than the value estimated from ab initio calculations and surface energy, which means that any dissipative energy should be included in the fracture toughness of a grain in spite of the brittle fracture in Si₃N₄. The fracture toughness of polycrystals of Si₃N₄ ceramics measured using single‐edge notched microcantilever beam specimens is intermediate between those of grains and grain boundaries, and it agrees with the estimated initial value of the Rcurve, K_I0, in Si₃N₄ ceramics.     

Zirconium nitride nano-particulate reinforced Alon composites: Fabrication, mechanical properties and toughening mechanisms

Aluminium oxynitride (Alon) exhibits excellent stability, high rigidity and good thermal shock resistance, but it has relatively low strength and poor fracture toughness. The aim of this investigation was to develop a new type of zirconium nitride (ZrN) nano-particulate reinforced Alon composites via a change of ZrO₂ nano-particles during sintering. A reduction of porosity and grain size was observed in the composite. With increasing amount of ZrN nano-particles up to 2.7%, the relative density, hardness, Young's modulus, flexural strength, and fracture toughness all increased. When the ZrN nano-particles exceeded 2.7%, while the flexural strength and fracture toughness decreased slightly, the density, hardness and Young's modulus continued to increase. Different toughening mechanisms including crack bridging, crack branching and crack deflection were observed, thus effectively increasing the crack propagation resistance and leading to a considerable improvement in the flexural strength and fracture toughness of the composites.     

Fracture toughness of filled polypropylene copolymer systems

The impact strength to stiffness balance of a toughened polypropylene copolymer was modified through the addition of mineral fillers. The stiffness was improved over the base resin value for all formulations. However, the impact strength exhibited complex behavior. The fracture toughness G_c calculated using the linear elastic fracture mechanics theory was indicative of the materials resistance to crack propagation. The G_c values were modified significantly with the addition of fillers and for some formulations was greater than the base resin value. The LEFM analysis indicates that this is due to an increase in the damage zone size r_p where the energy absorbing mechanisms are concentrated. However, the specific energy absorbed per unit volume decreased with the addition of fillers. The total energy to fracture measured using unnotched samples was indicative of crack initiation and crack propagation energies. This upper bound value decreased for all formulations indicating a reduction in the crack initiation resistance, in the presence of stress concentrating heterogeneities in the filled systems.     

Quantitative analysis of toughening effect of crack deflection on Si3N4/Si2N2O composites through improved indentation method

In this study, Si₃N₄/Si₂N₂O composite ceramics prepared by hot pressing were used as an example, and the material fracture morphology and fracture mechanism were analyzed. Based on the formula of fracture toughness measured by an indentation method, a quantitative computation method was proposed to determine the toughened effect of ceramic materials resulting from the crack deflection by the second phase. The grain size and sintering density are increased with the increase of sintering temperature. The toughening effects resulting from the crack deflection is increased, and the main mode of fracture is transformed into the transgranular fracture. The Si₂N₂O grains can play a role in the toughening process because these grains can hinder the cracks extending along the radial direction. However, when the cracks extend in the axial direction, the toughening effect of Si₂N₂O grains is not obvious because of the internal stacking faults in the axial direction. The improved indentation method can quantitatively analyze the toughening effect of the second phase of composite ceramics, and the validity of this method are verified by comparing the fracture toughness of Si₃N4/Si₂N₂O and fine grained β- Si₃N₄ ceramics.     

Toughness of syndiotactic polystyrene/epoxy polymer blends: microstructure and toughening mechanisms

Thermoplastic/epoxy blends were formed using an amine-cured epoxy polymer and a semi-crystalline thermoplastic: syndiotactic polystyrene (sPS). Complete phase-separation of the initially soluble sPS from the epoxy occurred via ‘reaction-induced phase-separation’ (RIPS) or via ‘crystallisation-induced phase-separation’ (CIPS), depending upon the thermal processing history employed. Dynamic mechanical thermal analysis showed that no sPS was retained dissolved in the epoxy polymer. For RIPS, at concentrations of sPS of up to 8 wt%, the sPS is present solely as spherical particles. However, macro phase-separation, giving a co-continuous microstructure, accompanied by local phase-inversion, dominates the RIPS blends containing more than 8 wt% sPS. In the CIPS blends, the sPS is present as spherulitic particles, and this microstructure does not change over the range of sPS concentrations employed, i.e. from 1 to 12 wt% sPS. The pure epoxy polymer was very brittle with a value of fracture energy, G_Ic, of about 175 J/m². However, the addition of the sPS significantly increases the value of G_Ic, though the toughness of the RIPS and CIPS blends differs markedly. For the RIPS blends, there is a steady increase in the toughness with increasing content of sPS and an apparent maximum value of G_Ic of about 810 J/m² is obtained for 8-10 wt% sPS. On the other hand, the measured toughness of the CIPS blends increases relatively slowly with the concentration of sPS, and a maximum plateau value of only about 350 J/m² was measured in the range of 8-12 wt% sPS. The relationships between the microstructure of the RIPS and CIPS sPS/epoxy blends and the measured fracture energies are discussed. Further, from scanning electron microscopy studies of the fracture surfaces and optical microscopy of the damage zone around the crack tip, the nature of the micromechanisms responsible for the increases in toughness of the blends are identified. For the RIPS blends, (i) debonding of the sPS particles, followed by (ii) plastic void growth of the epoxy matrix are the major toughening micromechanisms. The increase in toughness due to such micromechanisms is successfully predicted theoretically using an analytical model. In the case of the CIPS blends, the increase in the value of G_Ic results from (i) crack deflection and (ii) microcracking and crack bifurcation.     

Numerical and experimental evaluation of the Mode III interlaminar fracture toughness of composite materials

The Crack Rail Shear (CRS) specimen is a proposed test method to characterize the interlaminar Mode III critical strain energy release rate (G_IIIc) of continuous fiber-reinforced composite materials. The specimen utilizes the two rail shear test fixture and contains embedded Kapton film between designated plies to provide a starter crack for subsequent fracture testing. Analytical expressions for specimen compliance and G_III are based upon Strength of Materials (SM) principles. The model identifies important material and geometric parameters and provides a simple data reduction scheme. A quasi-three-dimensional, linear elastic finite element stress analysis verifies the purity of the Mode III fracture state and identifies admissible crack lengths to be used in the experimental study. A fully three-dimensional linear elastic finite element analysis of the CRS is employed to investigate the influence of edge effects on the fracture state for the finite length sample. Results based upon a uniform crack extension indicate a small region of mixed mode behavior at traction free edges which decay to a pure Model III fracture state in the interior of the sample. Furthermore, the G_III distribution along the crack front decreases at the free edges from a maximum plateau region in the interior. The three-dimensional analysis allows edge effects to be minimized by selecting appropriate specimen lengths. Compliance and strain energy release rates are in good agreement with the SM model. An experimental program was performed to measure G_IIIc of two graphite epoxy systems. G_IIIc results for AS4/3501-6 were found to be 1.6 times the Mode II fracture toughness, while IM7/8551-7 exhibited equivalent Mode II and Mode III fracture toughnesses. Mode III fracture surfaces revealed microstructural deformations characteristic of Mode II fracture.     

Design of crack deflection induced high toughness laminated Si3N4 ceramics based on hollow oriented one-dimensional microstructure

A laminated silicon nitride (Si₃N₄) ceramic material with a hollow, oriented, one-dimensional microstructure was successfully prepared based on the tape casting and sacrificial template method. The results show that hollow, oriented, one-dimensional microstructures can effectively induce crack deflection. Different arrangements of the structural design layer and dense layer will have different effects on the material. In particular, bulks with a single-layer orthogonal arrangement of the structural design layer possess high toughness and obvious crack deflection during the fracture process. A kind of multiscale crack deflection mode was realized. Compared with the fracture toughness of the monolithic Si₃N₄ ceramic bulk (5.55 MPa m^1/2), the fracture toughness can reach 8.73 MPa m^1/2, and the flexural strength can still reach 391.47 MPa with only a slight decrease.     

Additive effect of micro-damage zones from nano-scale crack tip and nano-grains for fracture toughness measurements of 3Y-TZP zirconia ceramics

A nano-scale crack tip around 500 nm wide introduced by femtosecond laser still affects the accuracy of fracture toughness K_IC measurements of 3Y-TZP zirconia ceramics with average grain size G from 200 to 500 nm. A simple formula was proposed to estimate the additive effect of crack-tip damage zones from an infinitely sharp crack to a nano-scale blunt notch. The error in fracture toughness measurements is less than 8 % if the nano-scale crack-tip width < 0.5·G. The intrinsic K_IC can be deduced from the simple formula if the nano-scale crack tip > 0.5·G. This study shows the same K_IC was deduced from two different sets of 3Y-TZP measurements with nano- and micro-scale notches of 500 nm and 18 µm wide. Furthermore, the simple formula specifies the relation between the fracture toughness K_IC and intrinsic strength f_t via grain size G, which means K_IC can also be estimated from f_t and G without testing pre-cracked specimens. K_IC values of 3Y-TZP from specimens with and without pre-cracks were compared.     

SiC and ZrN nano-particulate reinforced AlON composites: Preparation,mechanical properties and toughening mechanisms

Due to excellent chemical stability, high rigidity, superior corrosion and wear resistance, aluminum oxynitride (AlON) has been considered as one of most promising candidate ceramic materials in high-performance structural, advanced abrasives and refractory fields. However, it usually exhibited relatively low flexural strength and poor fracture toughness. The study is aimed to develop silicon carbide (SiC) and zirconium nitride (ZrN) nano-particulate reinforced AlON composites with improved mechanical properties and fracture resistance via a hot-press sintering process. It was found that the addition of ZrO₂ nanoparticles would be transformed into ZrN during sintering. Due to the pinning effect of SiC and ZrN nano-particles positioned at grain boundaries of micro-sized AlON particles, the presence of SiC and ZrN nano-particles resulted in the reduction of both porosity and grain size, and a change of fracture mode from intergranular cracking in AlON to intragranular cracking in composites. With presence of 8 wt% SiC and 5.2 wt% ZrN nano-particles, the relative density, microhardness, Young’s modulus, flexural strength and fracture toughness increased. Different toughening mechanisms including crack bridging, crack branching and crack deflection were observed, thus effectively increasing the crack propagation resistance and leading to a considerable improvement in flexural strength and fracture toughness.     

Design,fabrication and mechanical properties of multidimensional graded ceramic tool materials

A type of multidimensional graded ceramic tool materials (MGTMs) was designed and fabricated by vacuum hot-pressing sintering technology. The microstructure and compositional distribution of tool simultaneously changed in two different directions. The tool-chip and tool-workpiece contact regions were designed to have high hardness, and metal phases Mo and Ni were added to produce a gradual increase in toughness from the outer layer to core layer. The effect of orientation angle, thickness ratio and sintering parameters on the mechanical properties and microstructure were investigated. The experimental results showed that the composites, sintered at 1700 °C for 15 min, with the orientation angle of 30° and a thickness ratio of 0.4, had the optimal comprehensive mechanical properties. In addition, the crack propagation paths were observed to analyze the toughening mechanisms for the multidimensional graded ceramic tool materials. It was found that there is a crack resistance behavior when the crack extended from the outer layer to transition layer. The effect of the angle between the crack and graded interface on crack propagation paths was also investigated and the results indicated that the small angle was favorable for the crack deflection when the cracks passed through the graded interface. The residual thermal stress contributed to the occurrence of the crack bridging and transgranular fracture inside the Al₂O₃ grains, while the intergranular fracture and crack deflection were observed around the TiC grains.     

The toughening mechanism and mechanical properties of graphene-reinforced zirconia ceramics by microwave sintering

ABSTRACT

The graphene/ZrO₂ composites were fabricated by impregnating graphene dispersion into the ZrO₂ ceramic matrix and sintered by microwave, and the microstructure and mechanical properties were investigated. The results showed that the graphene was well dispersed in the ceramic matrix and refined the grain size. The fracture toughness reached 8.62?MPa?m^1/2, confirmed by single-edge notched beam, which was 42% higher than that of the pure ZrO₂. Also, the toughening mechanisms were investigated by micro-hardness testing and showed that a combination of crack deflection, micro-crack and crack bridging increased the fracture toughness.     

Toughening epoxies with halloysite nanotubes

An experimental attempt was made to characterize the fracture behaviour of epoxies modified by halloysite nanotubes and to investigate toughening mechanisms with nanoparticles other than carbon nanotubes (CNTs) and montmorillonite particles (MMTs). Halloysite-epoxy nanocomposites were prepared by mixing epoxy resin with halloysite particles (5 wt% and 10 wt%, respectively). It was found that halloysite nanoparticles, mainly nanotubes, are effective additives in increasing the fracture toughness of epoxy resins without sacrificing other properties such as strength, modulus and glass transition temperature. Indeed, there were also noticeable enhancements in strength and modulus for halloysite-epoxy nanocomposites because of the reinforcing effect of the halloysite nanotubes due to their large aspect ratios. Fracture toughness of the halloysite particle modified epoxies was markedly increased with the greatest improvement up to 50% in K_IC and 127% in G_IC. Increases in fracture toughness are mainly due to mechanisms such as crack bridging, crack deflection and plastic deformation of the epoxy around the halloysite particle clusters. Halloysite particle clusters can interact with cracks at the crack front, resisting the advance of the crack and resulting in an increase in fracture toughness.     

The Effect of Relative Density on the Mechanical Properties of Hot‐Pressed Cubic Li7La3Zr2O12

The effect of relative density on the hardness and fracture toughness of Al‐substituted cubic garnet Li_6.19Al_0.27La₃Zr₂O₁₂ (LLZO) was investigated. Polycrystalline LLZO was made using solid‐state synthesis and hot‐pressing. The relative density was controlled by varying the densification time at fixed temperature (1050°C) and pressure (62 MPa). After hot‐pressing, the average grain size varied from approximately 2.7–3.7 μm for the 85% and 98% relative density samples, respectively. Examination of fracture surfaces revealed a transition from inter‐ to intragranular fracture as the relative density increased. The Vickers hardness increased with relative density up to 96%, above which the hardness was constant. At 98% relative density, the Vickers hardness was equal to the hardness measured by nanoindentation 9.1 GPa, which is estimated as the single‐crystal hardness value. An inverse correlation between relative density and fracture toughness was observed. The fracture toughness increased linearly from 0.97 to 2.37 MPa√m for the 98% and 85% relative density samples, respectively. It is suggested that crack deflection along grain boundaries can explain the increase in fracture toughness with decreasing relative density. It was also observed that the total ionic conductivity increased from 0.0094 to 0.34 mS/cm for the 85%–98% relative density samples, respectively. The results of this study suggest that the microstructure of LLZO must be optimized to maximize mechanical integrity and ionic conductivity.