Dense pure binderless WC bulk material prepared by spark plasma sintering

The phases, microstructures and mechanical properties of binderless WC bulk materials prepared by the spark plasma sintering technique were investigated systematically. The addition of carbon was added to eliminate the impurity phase W₂C. The relative density, Vickers hardness and grain size increase obviously with increasing sintering temperature, but increase weakly with increasing pressure or sintering time. The high relative density of 99·1%, HV30 of 27·5 GPa and fracture toughness K_IC of 4·5 MPa m^1/2 of pure binderless WC bulk with a grain size of 400 nm was obtained by sintering the WC powders with a particle size of 200 nm and the addition of 0·63 wt-%C at 1800°C for 6 min under 70 MPa.     

Observations on the effect of calcium segregation on the fracture behaviour of polycrystalline alumina

The influence of calcium segregation to the grain boundaries of polycrystalline alumina on room temperature fracture behaviour has been investigated. In a commercial high-density single-phase alumina containing less than 5 ppm calcium by weight, thermal treatments were employed to achieve equilibrium segregation from 0.6 to 1.6 at % calcium without detectable changes in grain size (18m) or porosity distribution. Room temperature SENB test results revealed an inverse dependence of K _IC on calcium segregation levels in the range examined. Fractures were primarily intergranular in all specimens. Qualitatively, the relationship between K _IC and calcium segregation would be predicted from a consideration of the effect of such an ion on the interatomic spacing at the boundary. However, quantitative agreement with the model is poor, the measured effect being much greater than predicted. A relatively high K _IC value was achieved in a fine grained (2m) hot-pressed alumina containing very low levels of segregated impurities. This material exhibited substantial amounts of cleavage fracture. The higher fracture toughness of this alumina is discussed in terms of both increased intergranular and transgranular fracture stresses promoted by the relatively clean grain boundaries and small grain size, respectively.     

A new method to estimate the plane strain fracture toughness of materials

Although the testing method for fracture toughness K_IC has been implemented for decades, the strict specimen size requirements make it difficult to get the accurate K_IC for the high‐toughness materials. In this study, different specimen sizes of high‐strength steels were adopted in fracture toughness testing. Through the observations on the fracture surfaces of the K_IC specimen, it is shown that the fracture energy can be divided into 2 distinct parts: (1) the energy for flat fracture and (2) the energy for shear fracture. According to the energy criterion, the K_IC values can be acquired by small‐size specimens through derivation. The results reveal that the estimated toughness value is consistent with the experimental data. The new method would be widely applied to predict the fracture toughness of metallic materials with small‐size specimens.     

Y(E)-doped tetragonal zirconia polycrystalline solid electrolyte

Polycrystalline dense zirconia containing 100% metastable tetragonal phase was obtained by alloying zirconia with 2 to 3 mol % Y₂O₃ (Er₂O₃). A critical temperature, approximately 1400°C, for full densification (100% theoretical density) was found, and above that a sudden density decrease in all sintered bodies took place. The fracture toughness (K _IC) was found to be strongly dependent on the grain size, and a critical grain size (0.29μm in Y-TZP and 0.38μm in Er-TZP) existed beyond which a steepK _IC decrease was produced. Phase composition and microstructural development seem to influence such mechanical behaviour.     

A fractographic criterion for subcritical crack-growth boundaries in hot-pressed alumina

The percent intergranular fracture (PIF) was measured along radii extending from fracture origins in hot-pressed alumina specimens, fractured at various loading rates and temperatures, and plotted versus estimates of stress intensity factors (K _I) at the various crack lengths. Minima in PIF occur at values ofK _I that are close to the critical stress intensity factors (K _IC) for cleavage on various crystal lattice planes in sapphire. The subcritical crack-growth boundary (K _I=K _IC of the polycrystalline material) occurs near the primary minimum in PIF suggesting that this minimum can be used as a criterion for locating this boundary. In addition, it was noted that the polycrystallineK _IC (4.2 MPa m^1/2) is very close to theK _IC for fracture on {¯1 ¯1 2 6} planes which is 4.3 MPa m^1/2. These observations suggest that critical crack growth begins when increased fracture energy can no longer be absorbed by cleavage on these planes. There is a secondary minimum atK _I>K _IC that appears to be associated with theK _IC necessary for fracture on combinations of planes selected by the fracture as alternatives to the high fracture-toughness basal plane.     

Crack-size dependence of fracture toughness in transformation-toughened ceramics

Fracture toughness (K _IC) has been determined for Y₂O₃-partially stabilized zirconia, Y₂O₃-partially stabilized hafnia, CaO-partially stabilized zirconia and Al₂O₃+ZrO₂ composites. It is shown thatK _IC determined using the identation technique may not yield a unique number but may depend upon the crack size (C) (on the indent load). The slope ofK _IC againstC ^1/2 yields the magnitude of the surface stress created by the tetragonal monoclinic transition on the surface induced by grinding.K _IC determined using the double cantilever beam (DCB) technique, on the other hand, is shown to be independent of crack length.     

Effect of V content on the microstructure and mechanical properties of Mo2FeB2 based cermets

Four series of cermets with V content between 0 and 7.5 wt.% in 2.5 wt.% increments were studied by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The transverse rupture strength (TRS), hardness (HRA) and fracture toughness (K_IC) were also measured. It was found that the grain size was affected by the V content. The cermets with 2.5 wt.% V addition exhibited the smallest grain size. An increasing V content decreased the wettability of the binder on the Mo₂FeB₂ hard phase, and accordingly resulted in the increase of porosity and aggregation of ceramic grains. EDS results showed that V addition occurred primarily in the hard phase, with a little amount in the Fe alloy binder. In addition, the content of Mo element in the binder decreased with increasing V content. The cermets with 2.5 wt.% V addition showed the highest TRS, hardness and fracture toughness of 2350 MPa, HRA 90.6 and 15.1 MPa m^1/2, respectively.     

A study on the ASTM E1921 standard in determining the fracture toughness of ferritic steels

One of the most important aims of the fracture mechanics is to determine the fracture toughness of a material. Various methods were developed for this purpose and have been still used nowadays. In the J‐integral method that is one of them, providing of a dominant linear elastic condition on the specimen is not required. However, in ferritic steels, the fracture toughness values (K_JC) obtained by the J‐integral method show some inconsistencies. Therefore, the ASTM E1921 standard was developed on ferritic steels, which are instabilities in the values of elastic or elastoplastic fracture toughness. In this study, a new method was used to determine the fracture toughness (K_IC) of ferritic steels, and it was compared with the standard. Three steels with different mechanical properties and average grain size were investigated in this study.     

Fracture toughness of CaO-P2O5-B2O3 glasses and glass-ceramics determined by indentation

The fracture toughness, (K _IC) of CaO-P₂O₅-B₂O₃ glasses and glass-ceramics was investigated using both Vickers indentation and the notched beam technique (NBT). Five representative equations were applied and it was found that for the variation of K _IC with B₂O₃ content, the Lawn and Fuller equation showed the best correspondence with the NBT. The values of fracture toughness obtained from the Lawn and Fuller equation showed the same trend with B₂O₃ content as that determined by NBT, although the values from indentation were on average 33% lower. The determination of absolute fracture toughness by indentation requires a correction factor which can be obtained by calibration using NBT. A significant increase in K _IC occurred after a 37CaO-37P₂O₅-20B₂O₃-6Al₂O₃ (mol%) glass was converted to a glass-ceramic. The much higher K _IC for the glass-ceramic measured by NBT (1.32 MN m^–3/2) compared with that from indentation (0.89 MN m^–3/2) is attributed to internal stresses due to thermal expansion differences between the crystalline and residual glass phases leading to additional microcrack toughening.     

Effect of SiC whisker addition on the microstructures and mechanical properties of Ti(C,N)-based cermets

Ti(C, N)-based cermets with addition of SiC whisker (SiC_w) were prepared by vacuum sintering. The microstructures of the prepared cermets were investigated by using X-ray diffractometry (XRD) and scanning electron microscopy (SEM). Mechanical properties such as transverse rupture strength (TRS), fracture toughness (K_IC) and hardness (HRA) were also measured. It was found that the grain size of the cermets was affected by the SiC whisker addition. The cermets with 1.0 wt.% SiC whisker addition exhibited the smallest grain size. The porosities of the cermets increased with increasing SiC whisker additions. The addition of the SiC whisker had no influence on the phase constituents of the cermets. Compared with the cermets with no whisker addition, the highest TRS and fracture toughness for cermets with 1.0 wt.% SiC whisker addition increased by about 24% and 29%, respectively. The strengthening mechanisms were attributed to finer grain size, homogeneous microstructure and moderate thickness of rim phase. The toughening mechanisms were characterized by crack deflection, whisker bridging and whisker pulling-out.     

Correlation of fracture toughness with microstructural features for ultrafine‐grained 6082 Al alloy

In the present work, cryorolling (CR) and room temperature rolling (RTR) followed by annealing (AN) at 200°C were carried out to investigate the effects of grain size, precipitates (Mg‐Si‐phases), and AlFeMnSi‐phases on the fracture toughness of 6082 Al alloy. Using the values of the conditional fracture toughness, (K_Q), in the critical fracture toughness (K_IC) validation criteria, it was found that the sample size is inappropriate, which implies that the conditional fracture toughness obtained cannot be considered as the critical fracture toughness. Therefore, to establish the relative improvement in fracture toughness, the equivalent energy fracture toughness (K_ee) and J‐integral were calculated and used. The results show that the values of K_ee (89.91 MPa √m) and J (89.86 kJ/m²) obtained for the sample processed via CR followed by AN (CR + AN) are the highest when compared with the other samples processed through CR, RTR, and RTR followed by AN, RTR + AN. Microstructural features such as high fraction of low Taylor factor, high fraction of kernel average misorientation, Si‐rich particles, small size AlFeMnSi‐phases, and mixed mode of failure (transgranular shear and micro‐void coalescence) also support the high fracture toughness in the CR + AN sample. It was also observed that the effect of residual stresses on the fracture toughness of CR and RTR samples is minimal. Therefore, the correlation between microstructure and residual stresses is not considered in the present work due to very small values of the residual stresses for CR and RTR samples and the absence of residual stress from the heat‐treated samples.     

Evaluation of the KIC and JIC fracture parameters in a sand cast AZ91 magnesium alloy

The critical fracture parameters K_IC and J_IC were determined on compact tension (CT) specimens designed according to ASTM standards. The minimum specimen thickness B required for a valid K_IC test is suggested to be directly proportional to the σ_ys/E ratio, which is very high for magnesium alloys. As consequence, the value of B is more than 128 mm. Valid K_IC values were obtained using specimens with B=110 mm. Research on the effect of specimen thickness on the K_Q value was performed. The specimen thickness proposed by ASTM E 399 is overestimated. The experimental results show that not so large specimens are needed for a valid K_IC test. K_IC experimental value was 22 MPa m^1/2, that is two times the value reported in the literature for this alloy. The determination of both K_IC and J_IC has offered also the possibility of evaluating the real efficacy of formulas relating the two parameters: starting from the J_IC experimental data, formulas give some underestimation of the K_IC values. SEM fractographic examinations revealed the influence of grain size on the fracture resistance of AZ91.     

Improvement of tensile properties and toughness of an epoxy resin by nanozirconium-dioxide reinforcement

Zirconium dioxide (ZrO₂) nanoparticles were systematically added as reinforcement to a diglycidyl ether of bisphenol A (DGEBA)-based epoxy resin. A series of composites with varying amounts of nanoparticles was prepared and their morphology and mechanical properties were studied. The obtained nanocomposites were characterized by tensile tests, dynamic mechanical thermal analysis, and fracture toughness (K_IC) investigations; by standardized methods, to define the influence of the nanoparticle content on their mechanical and thermal properties. The morphological analysis of the composites shows that nanoparticles form small clusters, which are uniformly distributed into the matrix bulk. The tensile modulus (E) and the K_IC of the epoxy matrix increase at rising zirconia content. Improvements of more than 37% on modulus and 100% on K_IC were reached by the nanocomposite containing 10 vol.-% ZrO₂ with respect to the neat epoxy (E_o = 3.1 GPa, K_ICo = 0.74 MPam^0.5). The presence of nanoparticles produces also an increment on glass transition temperature (T _g). The epoxy resin added with 8 vol.-% ZrO₂ records a T _g approximately 8% higher than the unmodified matrix (T _go = 100.3 °C).     

On the Applicability of the Schwalbe's Model to the Fracture Toughness Calculation in 7075 Aluminum Alloys

Four 7075-T651 aluminum alloys have been tested in tension in order to assess the applicability of the Schwalbe's model to the fracture toughness calculation. Standard K _IC tests were performed on compact tension samples at room temperature, and the results compared with those from the Schwalbe's model which takes into account several mechanical properties derived from a conventional tensile test applied on round unnotched tensile samples, and the average dimple size of the corresponding fracture surfaces. The values of K _IC calculated through the Schwalbe's model, correlate qualitatively well with those from the standard technique.Fracture toughness deterioration is accompanied by a loss of the true fracture strain, strain hardening capacity and average dimple size. On the other hand, the higher the Zn/Mg ratio, the volume fraction of precipitates and the yield strength, the lower the fracture toughness. All these effects are originated in the presence of matrix precipitates. Therefore, the reduction in K _IC can be explained in terms of the matrix response to the applied stress field as a function of the differences in volume fraction of the strengthening precipitates.The round tension samples corresponding to the four materials, failed in a predominantly ductile transgranular fashion, which facilitates the application of the Schwalbe's model based in the characteristic dimples, developed in this mode of fracture, as a microstructural element size.     

Evaluation by indentation of fracture toughness of ceramic materials

A transition fracture mode from Palmqvist to median has been observed in a number of ceramic materials. A new expression to determine the fracture toughness (K _IC) by indentation is presented. The K _IC values calculated by this formula are independent of the crack profile (median or Palmqvist) and of the applied load. This formula has been obtained by modifying the universal curve of Evans and Charles to incorporate Palmqvist and median cracks over a wide range of loads in the case of brittle materials with different mechanical properties (elastic properties: E, v, K _IC).     

The effect of repeated annealing temperature on the structural,optical, and electrical properties of TiO<Subscript>2</Subscript> thin films prepared by dip-coating sol–gel method

In this study, we have studied the effect of repeated annealing temperatures on TiO₂ thin films prepared by dip-coating sol–gel method onto the glasses and silicon substrates. The TiO₂ thin films coated samples were repeatedly annealed in the air at temperatures 100, 200, and 300 °C for 5 min period. The dipping processes were repeated 5 to 10 times in order to increase the thickness of the films and then the TiO₂ thin films were annealed at a fixed temperature of 500 °C for 1 h period. The effect of repeated annealing temperature on the TiO₂ thin films prepared on glass substrate were investigated by means of UV–VIS spectroscopy, X-ray diffraction (XRD), and atomic force microscopy (AFM). It was observed that the thickness, average crystallite size, and average grain size of TiO₂ samples decreased with increasing pre-heating temperature. On the other hand, thickness, average crystallite size, and average grain size of TiO₂ films were increased with increasing number of the layer. Al/TiO₂/p-Si metal–insulator–semiconductor (MIS) structures were obtained from the films prepared on p-type single silicon wafer substrate. Capacitance–voltage (C–V) and conductance–voltage (G/ω–V) measurements of the prepared MIS structures were conducted at room temperature. Series resistance (R _s) and oxide capacitance (C _ox) of each structures were determined by means of the C–V curves.     

Effects of solidification structure on tear resistance of Al–7% Si–0.4% Mg cast alloys

The tear resistance behaviour of Al–7% Si–0.4% Mg cast alloys was examined using Kahn‐type tear test specimens. Tests were performed for two permanent mould casts with an ordinary dendrite structure and a semi‐liquid die cast with a globular cell and fine grain structure. The microstructure of the two permanent mould casts was controlled by the cooling rates and the addition of Ti elements. Tear resistance was evaluated by the ‘pop‐in’ stress, the energies required for crack initiation, UE_i and the crack propagation, UE_p. Special attention was paid to an effective microstructural parameter for tear resistance improvement. Pop‐in, indicating sudden crack extension and arrest, was observed in all specimens. Homogeneous deformation occurs near the notch tip of the semi‐liquid die cast, characterized by a refined grain structure. Refinement of the grain size is more effective than that of the dendrite cell size or eutectic Si particle size to increase the energy for crack initiation. Unit propagation energy, UE_p, can be converted into a critical stress intensity factor, K_c, which in the semi‐liquid die cast was improved due to an increased amount of slant or shear fracture surface.     

Grain-size dependence of Snoek peaks in niobium

The effect of grain size on the oxygen and nitrogen Snoek peaks in niobium has been studied. It has been observed that the conversion factor K given by C = K _max, where C is the concentration of oxygen or nitrogen and _max the height of the corresponding Snoek peak, is concentration independent up to about 0.06 and 0.04 wt % oxygen and nitrogen respectively.The variation of K with grain size (d) obeys the relationship K = K ₀ + k_Kd^–1/2, where K ₀ represents the value of K for an aggregate of crystals without boundaries and k _K the grain size dependence of K.     

A MODEL FOR THE COMBINED EFFECTS OF STRESS RATIO AND GRAIN SIZE ON THE LEFM FATIGUE THRESHOLD CONDITION

A long-crack, fatigue-threshold model which explains and predicts the commonly observed effects of stress ratio, R, and grain size, d, on δK₀, is proposed. The inclusion of a grain-size-effect is an extension of a recently proposed model that examined the effect of the R ratio. The extended model is based on the hypothesis that near-threshold, crack growth involves two micro-mechanical processes of fracture; K_max-controlled submicroscopic cleavage, which predominates when the defect concentration is small, and δK-controlled reversed shear which predominates when the defect concentration is large, both processes occurring in a critically stressed volume, V_c, ahead of the crack tip. Defect concentration in V_c is reduced by a low value of R and a coarse grain size and is increased by a high value of R and a fine grain size. Good agreement is shown to exist between predicted and experimental curves of δK₀ versus R and δK₀ versus grain size for several steels and aluminium alloys. In particular, δK₀ is shown to have an upper and a lower bound value for a material. The model may be used as an alternative procedure for obtaining quick, approximate but conservative estimates of δK₀ for practical design applications.     

A simplified method for determining K IC in glass with liquid solutions impregnation

In order to determine K _IC in a simplified form, rectangular pieces of glass were scratched with a glazier's diamond, considering this scratch as the crack tip. The sides of the crack were made by sticking two rectangular pieces of proper thickness with epoxy resin as was made in a previous work. The K _IC was determined in glass in which the cracks are impregnated with liquid solutions of kerosene, sodium hydroxide and sodium silicate. For the samples impregnated with kerosene the mean value of K _IC remains constant, whereas for the other two solutions a decrease in the mean value of K _IC is observed, a 10% in samples impregnated with sodium hydroxide and 16% in samples impregnated with sodium silicate, when comparing them with their respective groups of samples of glass without impregnating. The corresponding Weibull diagrams were made and Weibull functions of three parameters were obtained. The respective parameters of the probability distribution functions of K _IC were estimated by means of the graphic method of nomograms.