A case study of mechanical properties of perovskite-structured Ba0.5Sr0.5Co0.8Fe0.2O3−δ oxygen transport membrane

This study has investigated mechanical properties of perovskite-structured Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3-δ (BSCF) oxygen transport membrane. The Young’s modulus and fracture toughness are determined by both macroscopic-scale and microscopic-scale methods. Both three-point and ring-on-ring bending tests as macroscopic-scale methods produce broadly similar results with a Young’s modulus, which is lower than that measured from micro-indentation method under a 10 N load. Young’s modulus and fracture toughness of BSCF show strongly dependent of the porosity. However, the fracture toughness of BSCF is independent of grain size. The fracture toughness determined by macroscopic-scale method is similar with that measured by microscopic-scale method. The crack shape of BSCF under a 10 N load is determined to be a median-radial mode. The intrinsic Young’s modulus and fracture toughness are determined to be 105.6 GPa and 1.49 MPa m^0.5, respectively, according the Minimum Solid Area (MSA) model. Annealing decreases the fracture toughness of BSCF between RT and 800 °C.     

A Fracture Toughness Test Using the Ball‐on‐Three‐Balls Test

A method for fracture toughness measurement of ceramics using small disks and plates is presented. Similar to the surface‐crack‐in‐flexure (SCF) method a semielliptical surface crack is introduced centrally into one plane side of the specimen which is fractured in a ball‐on‐three‐balls test. Finite element simulations are used to evaluate the stress intensity factor (SIF) for this loading geometry for a range of crack sizes and crack geometries. Empirical formulae for the geometric function are provided for evaluation of the test. The effect of position uncertainties is investigated using FEM and experiments. Other sources which may contribute to the measurement error are identified and quantified, resulting in recommendations for the practical realization of the test. A determination of the fracture toughness within ±10% measurement uncertainty is possible with specimens larger than 8 mm in diameter and thicker than 0.5 mm. With larger specimens an uncertainty comparable to other fracture toughness tests can be achieved. For precise measurements it is important to position the crack within ±120 μm of the stress maximum, to know Poisson's ratio exactly and to test cracks that have the maximum SIF at their deepest point. A method how this can be achieved is presented.     

Crack-healing behavior and resultant strength properties of silicon carbide ceramic

Silicon carbide (SiC) has good high temperature strength and resistance to radioactivity. However, it has poor fracture toughness. To overcome this weakness, a crack-healing ability is very desirable. This study focuses on the crack-healing behavior of commercial SiC ceramic. The crack-healing behaviors of SiC ceramic were investigated systematically, as a function of crack-healing temperature, time, crack size and temperature dependence of the resultant bending strength. Three-point bending specimens were made and a semi-elliptical crack was introduced on the specimen by a Vickers indenter. Pre-cracked specimens were healed at various conditions. All fracture tests were performed on a three-point loading system with a 16 mm bending span. The main conclusions obtained were: (1) optimized crack-healing condition is; temperature: 1773 K, 1 h in air. (2) The maximum crack size that can be healed completely under the optimized condition was semi-elliptical surface crack of 450 μm in diameter. (3) Limiting temperature for bending strength of crack-healed zone for bending strength was about 873 K.     

Spark plasma sintering of TiC-based composites toughened by submicron SiC particles

TiC-based composites toughened by submicron SiC particles with improved fracture toughness were fabricated and fracture mechanism has been investigated. It has been found that the improvement in fracture toughness of TiC–SiC composites is due to both crack paths propagating through uniformly distributed SiC particles and the fracture mode transition from intergranular type to transgranular type caused by the change of residual stresses originating from the addition of SiC particles. The optimum of fracture toughness (5.2 MPa m^1/2) was achieved at 14.6 vol% SiC, whereas the toughness decreased with increasing amount of SiC beyond 30 vol%.     

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.     

The effects of fine WC contents and temperature on the microstructure and mechanical properties of inhomogeneous WC-(fine WC-Co) cemented carbides

Inhomogeneous WC-(fine WC-Co) cemented carbides with improved hardness and toughness were successfully prepared through the addition of fine WC using planetary ball milling combined with sinter isostatic hot pressing (SHIP) technology. The inhomogeneous microstructure of the alloys consisted of coarsened WC grains and WC-Co consisting of fine WC dispersoids and Co binder phase. The increase of temperature and the addition of fine WC enhanced the sintering process. The morphologies of the coarsened WC and of the fine WC consisted of triangular and near-hexangular prisms, respectively. Due to crack path deflection and crack bridging, the prism-like coarsened WC crystals efficiently hindered cracks propagation. Intergranular fracture became predominant when adding fine WC. However, the excessively coarsened WC and some pores in alloys with 20 wt% fine WC could decrease the mechanical properties. The inhomogeneous WC-(fine WC-Co) cemented carbides with 10 wt% fine WC, sintered at 1430 °C for 40 min, could provide a combination of superior hardness and toughness.     

Fracture characteristics of SiC/graphene platelet composites

Silicon carbide/graphene platelet (SiC/GPLs) composites were prepared using different weight percent of GPLs filler by hot pressing (HP) technology at 2100 °C in argon. The influence of the GPLs addition on bending strength, fracture toughness and related fracture characteristics was investigated. Both the bending strength and fracture toughness increased with increasing GPLs additives. The main fracture origins – strength degrading defects were pores at the low content of platelets and combination of pores and GPLs or clusters of GPLs particles in systems with a higher content of platelets. The fracture toughness increased due to the activated toughening mechanisms mainly in the form of crack bridging and crack branching, while the crack deflection was limited. The highest fracture toughness of 4.4 MPa m^1/2 was achieved at 6 wt.% of GPLs addition, which was ∼30% higher than the K_IC value of the reference material.     

Mechanical behaviour of a low-clay translucent whiteware

A novel low-clay translucent whiteware body, using mostly non-plastic prefired materials and only a small amount of clay, was fabricated by slip casting and the effect of slip's solid content and sintering temperature on the mechanical behaviour was investigated. The degree of densification in the sintered specimens was determined by measuring the bulk density. The mechanical behaviour was determined by measuring the flexural strength and fracture toughness. Young's modulus and hardness were also measured. X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies were carried out to analyse the microstructure.The flexural strength and fracture toughness increase with both increasing the slip's solid content and the sintering temperature up to a certain level, but further increase in solid content and sintering temperature had an adverse effect on the properties. The maximum flexural strength (∼135 MPa) and fracture toughness (∼1.85 MPa m^1/2) values were attained with specimens produced from a slip having 45 vol.% solid content at a sintering temperature of 1350 °C. It was found that the amount and distribution of closed pores, their size and possible link with each other control the flexural strength and fracture toughness of the low-clay translucent whiteware.     

Toughness measurement on ball specimens. Part I: Theoretical analysis

A new toughness test for ball-shaped specimens is presented. In analogy to the “Surface Crack in Flexure”-method the fracture toughness is determined by making a semi-elliptical surface crack with a Knoop indenter into the surface of the specimen. In our case the specimen is a notched ball with an indent opposite to the notch. The recently developed “Notched Ball Test” produces a well defined and almost uniaxial stress field.The stress intensity factor of the crack in the notched ball is determined with FE methods in a parametric study in the practical range of the notch geometries, crack shapes and other parameters. The results correlate well with established calculations based on the Newman-Raju model.The new test is regarded as a component test for bearing balls and offers new possibilities for material selection and characterisation. An experimental evaluation on several ceramic materials will be presented in a consecutive paper.     

Fracture behavior of Ce-TZP/alumina/aluminate composites with different amounts of transformation toughening. Influence of the testing methods

The fracture behavior of four Ce-TZP zirconia composites containing 8 vol% alumina and 8 vol% strontium hexa-aluminate was investigated. The composites exhibited different degrees of transformation toughening obtained by varying the amount of the CeO₂ stabilizer and the sintering temperature. The strength was measured by 4-point bending (4PB) and piston-on-three balls (POB) methods Toughness and crack growth resistance (R-curve) were determined from Single Edge V-Notched Beam (SEVNB) and double torsion (DT) samples, and slow crack growth (SCG) curves were determined by DT method.Increasing the transformability of the composites enhanced their crack growth resistance and consequently, increased their resistance to SCG, which was completely inhibited for the most transformable composites. Simultaneously, flaw tolerance was also improved although a decrease in strength was observed. Under all configurations, the composites exhibited a plastic behavior and it was shown that their properties are correlated to the crack shielding due to autocatalytic phase transformation that not only depend on the material transformability, but is also strongly influenced by the testing method.     

Influence of diamond particles content on the critical load for crack initiation and fracture toughness of SiOC glass–diamond composites

The crack initiation load and fracture toughness were characterized as a function of diamond particle content, up to 25 vol%, in silicon oxycarbide glass matrix by means of Vickers indentation and single edge notch beam (SENB) technique, respectively. The larger fracture toughness value of 3.21 ± 0.3 MPa m^1/2 was reached for 20 vol% diamond content composites and the value was 4 times higher than that of the unreinforced glass. The addition of diamond particles greatly influenced the crack initiation load, which increased from 2.9 to 49.0 N. The enhancement in the fracture toughness and crack initiation load can be explained by both the intrinsic mechanical properties of diamond (especially the elastic properties; E ～ 1100 GPa) and the diamond/SiOC glass interfacial bonding. A clear correlation was found between the fracture energy, the reinforced interparticle spacing and the residual stress arising upon cooling due to thermal expansion mismatch between the matrix and the diamond particles.     

Biaxial strength and slow crack growth in porous alumina with silica sintering aid

Biaxial strength, fracture toughness and subcritical crack growth are reported for coarse grained porous alumina ceramics. The materials were prepared with a varying amount of a silica sintering aid, which resulted in the formation of a glassy secondary phase at the grain boundaries. Crystalline mullite was additionally found in the material with the highest silica content. The biaxial strength, measured by Ball-on-Ring and Ball-on-3-Balls, was highest for the material without mullite at the grain boundaries, and the biaxial strength decreased with increasing porosity. The fracture toughness of the materials was in the range of 1.7–1.9 MPa m^0.5. Measurements of subcritical crack growth by a modified lifetime method in air and aqueous environments demonstrated a higher crack growth rate in water and acid relative to in air. The effect of porosity and grain boundary phase were discussed in relation to subcritical crack growth and fracture mode in the coarse grained alumina ceramics.     

Influence of in-situ synthesized Zr-Al-C on microstructure and toughening of ZrB2-SiC composite ceramics fabricated by spark plasma sintering

Zr-Al-C was in-situ synthesized as a toughening component in ZrB₂-SiC ceramics by spark plasma sintering (SPS) ball-milled ZrB₂-based composite powders with SiC and graphite powders. The phase composition of Zr-Al-C toughened ZrB₂-SiC (ZSA) composite ceramics fabricated through the two-step process (ball milling and SPS) did not change dramatically with varying content of Zr-Al-C which shows a major phase of Zr₃Al₄C₆. With increasing Zr-Al-C content, the fracture toughness of the ZSA ceramics initially increased and then decreased when the content reached 40 vol%. The ZSA ceramic with 30 vol% Zr-Al-C exhibited a maximum fracture toughness value of 5.96 ± 0.31 MPa m^1/2, about 22% higher than that of the ZSA ceramic with 10 vol% Zr-Al-C. When the Zr-Al-C content goes beyond 30 vol%, the higher open porosity and component agglomeration led to the relatively lower fracture toughness. Crack deflection and bridging resulted from the weak interface bonding between Zr-Al-C and matrix phases and the weak internal layers of Zr-Al-C crystals, leading to longer crack paths and, hence, the toughened ZSA composite ceramics. Compared to the one-step in-situ synthesis process of Zr-Al-C and the direct incorporation process of synthesized Zr-Al-C grains, the two-step in-situ synthesis process not only led to the more uniform distribution of different components but also resulted in a much larger size of Zr-Al-C grains with a large aspect ratio causing longer crack propagation path as the result of crack deflection and bridging. The larger Zr-Al-C grains combined with the more homogeneous microstructure achieve the most substantial toughening of the ZSA composite ceramics. This work points out a promising approach to control and optimize the microstructure and improve the fracture toughness of ZrB₂-SiC composite ceramics by selecting the incorporation process of compound reinforcement components.     

Crack closure stresses in fiber reinforced brittle matrix composites

The fracture toughness of an alumina ceramic and a continuous SiC fiber reinforced alumina composite processed by pressureless sintering was studied in situ in a Scanning Electron Microscope (SEM). The applied stress intensity factor was obtained as a function of both applied load and crack extension. Closure stresses across crack surfaces imposed by grain-bridging and fiber-bridging, and hence fracture resistance from bridging were studied by both stress intensity factor and J-integral considerations. Theoretical calculations agree with experimental results. An average fracture resistance of ≈40 J m⁻² per fiber and a corresponding toughness of ≈1·6 MPam^1/2 per fiber was obtained for fiber elastic bridging before fiber failure. Fiber-matrix interfacial properties were examined and a technique for evaluating interfacial frictional shear stress was developed.     

SiC–AlN Particulate Composite

A SiC–AlN composite was fabricated by mechanical mixing of SiC and AlN powders, hot pressed under 40 MPa at 1950°C in Ar atmosphere. The object of this attempt was to achieve full density and a little solid solution formation. Fine microstructure and crack deflection behaviour are to improve the mechanical properties of the SiC–AlN composite. The bending strength and fracture toughness were achieved 800 MPa and 7·6 MPa m^1/2 at room temperature, respectively. The fracture toughness of the SiC–AlN composite shows minimal change between room temperature and 1400°C. Post-HIP improves the surface densification of the SiC–AlN composite resulting in an increase of the strength and the ability to resist oxidization. The bending strength of SiC–AlN composite increases from 800 to 1170 MPa after HIP treatment for 1 h under 187 MPa at 1700°C in N₂ atmosphere.     

Hard and tough carbon nanotube-reinforced zirconia-toughened alumina composites prepared by spark plasma sintering

It is demonstrated that 0.1 wt% of multi-walled carbon nanotubes (MWCNTs) or single-walled carbon nanotubes (SWCNTs) added to zirconia toughened alumina (ZTA) composites is enough to obtain high hardness and fracture toughness at indentation loads of 1, 5, and 10 kg. ZTA composites with 0.01 and 0.1 wt% of MWCNTs or SWCNTs were densified by spark plasma sintering (SPS) at 1520 °C resulting in a higher hardness and comparable fracture toughness to the ZTA matrix material. The observed toughening mechanisms include crack deflection, pullout of CNTs as well as bridged cracks leading to improved fracture toughness without evidence of transformation toughening of the ZrO₂ phase. Scanning electron microscopy showed that MWCNTs rupture by a sword-in-sheath mechanism in the tensile direction contributing to an additional increase in fracture toughness.     

Evaluation of biphasic calcium phosphate/nanosized 3YSZ composites as toughened materials for bone substitution

In this research, biphasic calcium phosphate (BCP), comprising 70 wt% of beta tricalcium phosphate and 30 wt% of hydroxyapatite, was mixed with different amounts of 3 mol% yttria-stabilized zirconia (3YSZ) and sintered at 1200 °C to produce toughened bone substitutes. The fracture toughness (K_Ic) of the obtained bodies was determined using the indentation-strength fracture method. Scanning electron microscopy and energy dispersive X-ray spectroscopy analysis were utilized to study the microstructure of the samples. The phase composition of the samples was also determined using X-ray diffraction technique. In order to investigate the cell supporting ability of the samples, G-292 cells were cultured on them and cell morphology was evaluated after 48 h. Based on the results, the maximum fracture toughness and compressive strength values (i.e., 2.11 MPa m^0.5 and 150 MPa, respectively) were obtained for the sample containing 3 vol% of 3YSZ. The obtained fracture toughness value was approximately two times higher than that of the original BCP (1.07 MPa m^0.5) and also was comparable with that of the cortical human bone. The following mechanisms for the improved K_Ic of the β-tricalcium phosphate were determined: Grain bridging of 3YSZ particles during crack growth resistance, formation of microcracks on the tip of the larger cracks, absorbing crack extension energy due to the volume expansion during 3YSZ tetragonal-monoclinic transformation and crack deflection by the presence of 3YSZ particles. Also, 3YSZ additive encourages transformation of HA phase into β-TCP during sintering BCP. Finally, based on the cell studies, the samples exhibited an adequate cell attachment and a good cell spreading condition.     

A new test to determine the tensile strength of brittle balls—The notched ball test

A new strength test for ceramic spheres (balls) is presented. A long narrow notch is cut in the equatorial plane of the ball and the ball is then loaded in compression perpendicular to the notch. This causes tensile stresses in the outer surface region of the ball opposite to the notch, which are analysed carefully with finite element (FE) methods. The tensile stress amplitude depends on the bending moment in the notch ligament – given by the applied force – and on details of the notch geometry. The stress state in the highly stressed surface is almost uniaxial showing only a slight influence of Poisson's ratio. Numerical solutions for balls with quite different notch geometries are given.Strength tests have been performed on commercial silicon nitride balls of 5 mm diameter. Two sets of specimens having notches of different length have been tested. Although the typical fracture loads in both sets of data are quite different, the tensile strengths are closely similar. This indicates the validity of the data evaluations. Experimental details are discussed and an analysis of the experimental uncertainties on the test results is made. For balls with 5 mm the uncertainties are estimated to be less than ±3% (of the measured value). For balls having a diameter of 10 mm or more the uncertainties are less than ±1%.     

Microstructure and mechanical properties of Ti3SiC2/3Y-TZP composites by spark plasma sintering

Ti₃SiC₂/3Y-TZP (3 mol% Yttria-stabilized tetragonal zirconia polycrystal) composites were fabricated by spark plasma sintering (SPS). The effect of Ti₃SiC₂ content on room-temperature mechanical properties and microstructures of the composites were investigated. The Vickers hardness and bending strength of the composites decreased with the increasing of Ti₃SiC₂ content whereas the fracture toughness increased. The maximum fracture toughness of 9.88 MPa m^1/2 was achieved for the composite with 50 vol.% Ti₃SiC₂. The improvement of the fracture toughness is owing to the crack deflection, crack bridging, the transformation toughening effects.     

Effect of suspension stability on bonding strength and electrochemical behavior of electrophoretically deposited HA–YSZ nanostructured composite coatings

In the present study, HA–YSZ nanostructured composites were deposited on Ti–6Al–4 V substrates by electrophoretic deposition of suspensions containing 0, 10, 20 and 40 wt% YSZ. The stability of each suspension was determined by applying response surface methodology, DLVO theory and zeta potential measurement for different YSZ contents and dispersant concentrations. The maximum zeta potential and electromobility of suspended particles was obtained for the suspension with 20 wt% YSZ. The electrophoretic deposition of HA–YSZ nanostructured composites was carried out at a constant voltage of 20 V for 120 s. The deposition kinetics was studied based on a mass-charge correlating approach under ranges of voltage (20–60 V), time (30–300 s) and wt% YSZ (0–40). The as–deposited and sintered HA–YSZ coatings were characterized by SEM, XRD, DSC–TG and FT–IR analyses. The micro-scratch behavior of coated samples indicated the highest critical contact pressures of crack initiation, P_c1 = 4.50 GPa, crack delamination, P_c2 = 5.14 GPa and fracture toughness, K_IC = 0.622 MPa m^1/2 for HA-20 wt% YSZ sample. The results of potentiodynamic polarization measurements showed that the implementation of 20 wt% YSZ could efficiently decrease the corrosion current density and corrosion rate of coated samples, while corrosion potential and linear polarization resistance were increased.