Crack-healing and mechanical behaviour of Al2O3/SiC composites at elevated temperature

Alumina/silicon carbide (Al₂O₃/SiC) composite ceramics with large self‐crack‐healing ability, high strength and high heat‐resistance limit temperature for strength were developed and subjected to three‐point bending. A semicircular surface crack 100 μm in diameter was made on each sample. Crack‐healing behaviour was systematically studied, as functions of crack‐healing temperature and healing time, and the fatigue strengths of the crack‐healed sample at room temperature and 1373 K were investigated. Four main conclusions were drawn from the present study. (1) Al₂O₃/SiC composite ceramics have the ability to heal after cracking from 1273to 1673 K in air. (2) The heat‐resistance limit temperature for strength of the crack‐healed sample is ?1573 K, and ?68% of the samples fractured from outside the crack‐healed zone in the testing‐temperature range 873–1573 K. (3) The crack‐healed sample exhibited very high fatigue limit at room temperature and also 1373 K. (4) The large self‐crack‐healing ability is a desirable technique for the high structural integrity of ceramic component.     

Strength recovery of machined Al2O3/SiC composite ceramics by crack healing

Alumina is used in various fields as a machine component. However, it has a low fracture toughness, which is a weakness. Thus, countless cracks may be initiated randomly by machining, and these cracks decrease the component's mechanical properties and reliability. To overcome this problem, a crack‐healing ability could be a very useful technology. In this study, Al₂O₃/SiC composite was sintered. This alumina exhibits excellent crack‐healing ability. Small specimens for a bending test were made from the Al₂O₃/SiC. A semicircular groove was machined using a diamond ball‐drill. The machining reduced the local fracture stress from approximately 820–300 MPa. The machined specimens were crack‐healed under various conditions. The fracture stress of these specimens after crack healing was evaluated systematically from room temperature (RT) to 1573 K. It was found that the local fracture stress of the machined specimen recovered almost completely after crack healing. Therefore, it was concluded that crack healing could be an effective method for improving the structural integrity of machined alumina and reducing machining costs.     

Fatigue strength of crack-healed Si3N4/SiC composite ceramics

Si₃ N₄ /SiC composite ceramics were sintered and subjected to three-point bending on specimens made according to the appropriate JIS standard. A semi-circular surface crack of 110 μm in diameter was made on each specimen. By using three kinds of specimen (smooth, cracked and crack healed), crack-healing behaviour, cyclic and static fatigue strengths were determined systematically at room temperature and 1000 °C. The main conclusions are as follows: (i) Si₃ N₄ /SiC composite ceramics have the ability to heal after cracking; (ii) crack-healed specimens showed similar cyclic and static fatigue strengths as smooth specimens, this being caused by crack healing; (iii) crack-healed zones had a sufficient fatigue strength and most fractures occurred outside the pre-cracked zone in those crack-healed specimens.     

Preliminary study of the crack healing and strength recovery of Al2O3-matrix composites

This study focused on the crack‐healing behaviour of three commercial Al₂O₃–ceramic‐matrix composites: TiC_P/Al₂O₃, ZrO₂/Al₂O₃ and SiC_W/Al₂O₃. Vickers indentation was used to introduce surface flaws with different loads of 49, 98 and 196 N. Then the cracked specimens were annealed in air for 1 h at 1000, 1200 and 1400 °C. The annealing treatment was also conducted at 1200 °C in vacuum for 1 h. Results showed that the annealing treatments increased the indentation strength, but the extent of the increase was different. When annealed in air, the main crack‐healing mechanism of TiC_P/Al₂O₃ and SiC_W/Al₂O₃ composites was chemical reaction. When annealed in vacuum, stress relaxation caused much less strength recovery. The main crack‐healing mechanism of ZrO₂/Al₂O₃ was the existence of low melting eutectic and the rearrangement of grains caused by ZrO_2(m)→ ZrO_2(t) transformation in the crack‐opening process zone. The effects of annealing temperature, atmosphere and indentation load on the degree of strength recovery were all related to the crack‐healing mechanisms.     

Crack-healing behaviour and resultant high-temperature fatigue strength of machined Si3N4/SiC composite ceramic

The crack‐healing behaviour of machining cracks in Si₃N₄/20 wt% SiC composite was investigated. The machining cracks were introduced by a heavy machining process, during the creation of a semicircular groove. The machined specimens were healed at various temperatures and times in air. The optimized crack‐healing condition of the machined specimens was found to be a temperature of 1673 K and a time of 10 h. The specimens healed by this condition exhibited almost the same strength as the smooth specimens healed. Moreover, the bending strengths and the fatigue limits of the machined specimens healed were systematically investigated at temperatures from room temperature to 1673 K. The machined specimens healed at the optimized condition exhibited an almost constant bending strength (～700 MPa) up to 1673 K. Also, the specimens exhibited considerably high cyclic and static fatigue limits at temperatures from 1073 to 1573 K. These results demonstrated that the crack‐healing could be an effective method for improving the structural integrity and reducing machining costs of the Si₃N₄/SiC composite ceramic.     

Threshold stress during crack-healing treatment of structural ceramics having the crack-healing ability

Alumina/15 vol.% SiC particles composite and mullite/15 vol.% SiC particles composite, that have excellent crack-healing ability are subjected to crack-healing under elevated static and cyclic stresses at 1373 K or 1473 K. The bending strengths of the specimens crack-healed under stress were investigated at the crack-healing temperature. From the results, the threshold stresses during crack-healing were determined. Crack-healing was found to occur although the pre-crack is grown by the applied stress. It is found that crack-healing can eliminate the pre-crack under stress below 64% fracture stress of the cracked specimen, if the ceramic components have an adequate crack-healing ability.     

Effect of cutting speed on the performance of Al2O3 based ceramic tools in turning nodular cast iron

This paper presents the results of an experimental investigation on the effect of cutting speed in turning nodular cast iron with alumina (Al₂O₃) based ceramic tools. Three different alumina based ceramic cutting tools were used, namely TiN coated Al₂O₃ + TiCN mixed ceramic, SiC whisker reinforced Al₂O₃ and uncoated Al₂O₃ + TiCN mixed ceramic tool. Turning experiments were carried out at four different cutting speeds, which were 300, 450, 600 and 750 m/min. Depth of cut and feed rate were kept constant at 1 mm and 0.1 mm/rev, respectively, throughout the experiments. Tool performance was evaluated with respect to tool wear, surface finish produced and cutting forces generated during turning. Uncoated Al₂O₃ + TiCN mixed ceramic was the worst performing tool with respect to tool wear and was the best with respect to surface finish. SiC whisker reinforced Al₂O₃ exhibited the worst performance with respect to cutting forces. If tool wear, surface finish and cutting force results are considered together, among the three tools studied, TiN coated Al₂O₃ + TiCN mixed ceramic tool is the most suitable one for turning nodular cast iron, especially at high cutting speeds (V_c > 600 m/min).     

Evaluating strength of thermally sprayed Al2O3 on aluminum

We evaluated the strength of thermally sprayed Al₂O₃ on aluminum. The thermally sprayed Al₂O₃ films were processed using low-pressure plasma spraying. The thickness of the thermally sprayed Al₂O₃ was 0.3 mm and 0.7 mm. We arranged a 4-point bending test and a heating test to evaluate the strength of the thermally sprayed Al₂O₃. We also investigated the effect of residual stress on the strength by measuring deformation of the thermally sprayed Al₂O₃ after removing the aluminum substrates. The bending strength was 120 MPa, regardless of thickness. We assumed that the bending strength would be equal to the tensile strength because the thermally sprayed Al₂O₃ films were very thin. A crack was generated at 433 K, regardless of thickness. The thermal stress was 160 MPa when the crack was generated. It was 40 MPa higher than we estimated. We found that the residual stress was compression stress that measured 40 MPa, which contributed to the prevention of the crack generation. We presume that the tensile strength was lower than the thermal stress because the residual stress was reduced by stress-relaxing of the aluminum near the interface in the bending test. The influence of heat-resisting strength is dominant over residual stress. Therefore, strength design should take into account residual stress.     

Sphere contact fatigue of a coarse-grained Al2O3 ceramic

The opposite sphere test is an appropriate tool to determine crack‐growth exponents for fatigue under repeated contact loading. Lifetime measurements for a coarse‐grained Al₂O₃ are reported. To explain the fatigue exponents that strongly deviated from those obtained in cyclic bending tests, a fracture mechanics analysis was carried out. It was aimed at determining the correct stress intensity factor solution for the tests, including limited dimensions of test specimens deviating from the case of a cone crack in a half space. Cone crack development was observed microscopically and the related stress intensity factors were computed for the observed crack shape. For modelling the fatigue behaviour, it is assumed that the fatigue effect is influenced by a reduction of the shielding term of crack growth resistance due to periodical friction between the grain‐interlock bridges in coarse‐grained alumina. This results in a loss of traction at the junctions, crack tip shielding is reduced, and the effective load at the crack tip is increased.     

Subzero tensile properties of 7010 aluminium alloy and Ti-6A1-4V and IMI550 titanium alloys in sheet form

Tensile properties are reported for Al-6Zn-2.5Mg-1.7Cu-0.12Zr (7010), Ti-6Al-4V and Ti-4Al-4Mo-2Sn-0.5Si (IMI550) alloy sheet, 1.7 mm thick tested at 293, 223, 173 and 77 K. The strength of these alloys increased and the reduction of area decreased with decreasing test temperature. The Young's Modulus (E), 0.1% proof stress (σ_0.1) and true tensile strength ($\text{σ}{}_{\mathrm{TS}}$) were related to temperature T in degrees absolute (in the range 293-173 K for E and 293-77 K for σ_0.1 and $\text{σ}$_TS) by     

Effect of Cr on the high temperature oxidation of L12-type Al3Ti intermetallics

Three kinds of L1₂-type Al₃Ti–Cr alloys, Al₆₇Ti₂₅Cr₈, Al₆₆Ti₂₄Cr₁₀ and Al₅₉Ti₂₆Cr₁₅, were prepared by induction melting followed by thermomechanical treatment. The oxidation behavior was investigated at 1273, 1373 and 1473 K in air. The oxidation resistance of the prepared alloys was excellent, however, there were some differences for each alloy. The isothermal oxidation resistance increased in the order of Al₅₉Ti₂₆Cr₁₅, Al₆₆Ti₂₄Cr₁₀ and Al₆₇Ti₂₅Cr₈, while the order became reversed in terms of the cyclic oxidation resistance. As more Al₂O₃ formed owing to the increased Al content in the alloy, the isothermal oxidation resistance increased, whereas the cyclic oxidation resistance decreased. The oxide scale was primarily composed of Al₂O₃, contaminated with Cr₂O₃ and TiO₂ that were present mainly at the lower part the oxide scale.     

Processing of Al2O3/SiC ceramic cake preforms and their liquid Al metal infiltration

In order to prepare ceramic preforms, chemical processes were used rather than using mixing of ceramic powders to obtain porous Al₂O₃/SiC ceramic foams. A slurry was prepared by mixing aluminium sulphate and ammonium sulphate in the water, and silicon carbide powder was added into the slurry so that a uniform mixture of Al₂O₃/SiC cake could be produced. The resulting product was (NH₄)₂SO₄·Al₂(SO₄)₃·24H₂O plus silicon carbide particles (SiC_p) after dissolving chemicals in the water. This product was heated up in a ceramic crucible in the furnace. With the effect of heat it foamed and Al₂O₃/SiC cake was obtained. Resulting Al₂O₃ grains were arranged in a 3D honeycomb structure and the SiC particles were surrounded by the alumina grains. Consequently, homogeneous powder mixing and porosity distribution were obtained within the cake. The morphology of the powder connections was networking with flake like particles. These alumina particles resulted in large amounts of porosity which was desired for ceramic preforms to allow liquid metal flow during infiltration. The resulting high porous ceramic cake (preform) was placed in a sealed die and liquid aluminium was infiltrated by Ar pressure. The infiltration was achieved successfully and microstructures of the composites were examined.     

Oxidation bonding of porous silicon carbide ceramics

A oxidation-bonding technique was successfully developed to fabricate porous SiC ceramics using the powder mixtures of SiC, Al₂O₃ and C. The oxidation-bonding behavior, mechanical strength, open porosity and pore-size distribution were investigated as a function of Al₂O₃ content as well as graphite particle size and volume fraction. The pore size and porosity were observed to be strongly dependent on graphite particle size and volume fraction. In contrast, the degree of SiC oxidation was not significantly affected by graphite particle size and volume fraction. In addition, it was found that the fracture strength of oxidation-bonded SiC ceramics at a given porosity decreases with the pore size but increases with the neck size. Due to the enhancement of neck growth by the additions of Al₂O₃, a high strength of 39.6 MPa was achieved at a porosity of 36.4%. Moreover, such a porous ceramic exhibited an excellent oxidation resistance and a high Weibull modulus.     

Wetting behaviour of SiC ceramics: Part I. E2O3/Al2O3 additive system

Wettability is the most important phenomenon in SiC liquid phase sintering. This paper discusses the ceramic–ceramic wetting of E₂O₃/Al₂O₃ additives on SiC, where E₂O₃ is a mixture of rare earth oxide. A sphere-shaped sample of additive was put on a SiC plate and the set placed in a graphite resistance furnace and heated to the additive sphere melting point at a rate of 10 °C/min. The behaviour of the additive on the SiC plate was observed by means of an imaging system using a CCD camera, while the contact angle was measured and analyzed using QWin Leica software. The tests were performed in argon or nitrogen atmospheres. The wettability curves displayed a fast decline and good spreading. The E₂O₃/Al₂O₃ system, which approached a eutectic composition when compared with the phase diagram of the Y₂O₃/Al₂O₃ system, displayed better spreading. Measurements of the contact angle could not be made when the test was conducted in a nitrogen atmosphere because of the bubbles that formed in the liquid during the test, damaging the interfacial zone between E₂O₃/Al₂O₃ and SiC. The results of these tests indicate that the best sintering atmosphere for this additive system is argon.     

Pressure-pulsed chemical vapour infiltration of SiC into two-dimensional-Tyranno/SiC particulate preforms from SiCl4–CH4–H2

SiC was infiltrated in two-dimensionally woven Tyranno/SiC particulate preforms from SiCl₄–CH₄–H₂ using pressure-pulsed chemical vapour infiltration (PCVI) in the temperature range 1348–1423 K. Above 1373 K, only β-SiC was deposited, whereas, at 1348 K, Si codeposition was found. At 1423 K, a macrosurface film was formed in the early stage of PCVI. At 1373 K, residual porosity decreased from 30% to 7.5% irrespective of the sample size. Three point flexural strength increased with decreasing residual porosity and increasing fibre volume fraction in the sample. Flexural strength of the sample having 48% fibre volume fraction reached about 325 MPa after 5 × 10⁴ pulses of CVI at 1373 K. Inter-laminar shear strength of the sample obtained at 1373 K reached 40 MPa at 7 × 10⁴ pulses. This revised version was published online in November 2006 with corrections to the Cover Date.     

The fracture toughness of Ni/Al2O3 laminates by digital image correlation II: Bridging-stresses and R-curve models

A composite of metal and brittle ceramic layers have increased fracture toughness as compared to ceramic monoliths. The property controlling the toughness enhancement is the, ‘bridging-stress’, exerted by the ductile phase astride the crack in the ceramic. This bridging-stress is a function of the crack-opening displacement (COD) which is a function of the size of the crack and the position along its profile. Depending on the accuracy of estimation of the bridging-stress, the modeled R-curve and experimental one match. In this study, a weight function based approach to generate the R-curve is reported and compared with the experimental results for Al₂O₃/Ni multilayer laminates.     

Phase Reactions and Diffusion Path of the SiC/Cr System

Solid-state bonding at pressureless-sintered SiC has been carried out using 25-m Cr foil at temperatures from 1373 to 1773 K for 1.8 ks in vacuum. The formation of reaction phases and microstructures at the interface between SiC and Cr was investigated by X-ray diffraction and microprobe analysis. At the bonding temperature of 1373 K the cubic Cr₂₃C₆phase formed next to Cr, and the hexagonal Cr₇C₃ phase formed next to SiC. At 1473 K the cubic phase Cr₃SiC_x appeared additionally on the SiC side. At 1573 K the complete diffusion path was established. Upon increasing the joining temperature beyond 1573 K all the chromium was consumed, and Cr₂₃C₆ and Cr₃SiC _x dissolved. A layered structure consisting of SiC/Cr₅Si₃ C _x /Cr₇C₃/Cr₅Si₃ C _x /SiC occurred.     

Microstructure and microchemistry of the Al/SiC interface

The characteristics of the Al/SiC interface play a critical role in controlling the properties of SiC-reinforced aluminium composites and aluminium-brazed SiC ceramic joints. Recently, a detailed investigation on the wettability of SiC single crystals by aluminium and several of its alloys was conducted. In order to understand further the nature of the Al/SiC interface, high resolution and conventional transmission electron microscope techniques have now been used to investigate its microchemistry and microstructure. The results revealed the coexistence of two polytype structures, rhombohedral and hexagonal, in the SiC single crystal structure. Aluminium carbide (Al₄C₃) and silicon were the reaction products found at the Al/SiC interface. From diffraction patterns, epitaxial orientation relationships between the SiC substrate and Al₄C₃, Si were determined.     

Studies on crack growth rate under high temperature creep,fatigue and creep-fatigue interaction—II: On the role of fracture mechanics parameter aeffσg

For high temperature creep, fatigue and creep-fatigue interaction, several authors have recently attempted to express crack growth rate in terms of stress intensity factor $\text{K}{}_{\mathrm{I}}\text{= α}\text{aσ}{}_{\mathrm{g}}$, where a is the equivalent crack length as the sum of the initial notch length a₀ and the actual crack length $\text{a}{}^1$, that is, $\text{a = a}{}_0\text{+ a}{}^1$. On the other hand, it has been shown by Yokobori and Konosu that under the large scale yielding condition, the local stress distribution near the notch tip is given by the fracture mechanics parameter of $\text{aσ}{}_{\mathrm{g}}\text{?(σ}{}_{\mathrm{g}}$), where a is the cycloidal notch length, σ_g is the gross section stress and $\text{?(σ}{}_{\mathrm{g}}$) is a function of σ_g. Furthermore, when the crack growth from the initial notch is concerned, it is more reasonable to use the effective crack length a_eff taking into account of the effect of the initial notch instead of the equivalent crack length a. Thus we believe mathematical formula for the crack growth rate under high temperature creep, fatigue and creep-fatigue interaction conditions may be expressed at least in principle as function of $\text{a}{}_{\mathrm{eff}}\text{σ}{}_{\mathrm{g}}\text{, σ}{}_{\mathrm{g}}$ and temperature.In the present paper, the geometrical change of notch shape from the instant of load application was continuously observed during the tests without interruption under high temperature creep, fatigue and creep-fatigue interaction conditions. Also, the effective crack length a_eff was calculated by the finite element method for the accurate estimation of local stress distribution near the tip of the crack initiated from the initial notch root. Furthermore, experimental data on crack growth rates previously obtained are analysed in terms of the parameter of $\text{a}{}_{\mathrm{eff}}\text{σ}{}_{\mathrm{g}}$ with gross section stresses and temperatures as parameters, respectively.     

Reinforcement and antioxidizing of porous carbon by pulse CVI of SiC

In order to reinforce and antioxidize porous carbon, chemical vapour infiltration (CVI) of SiC was investigated using a repetitive cycle of evacuation of vessel and instantaneous source-gas filling. From a source gas of 5% CH₃SiCl₃-H₂, a temperature range of 1273 to 1373 K was considered to be suitable to infiltrate SiC into a deep level, and surface deposition was enhanced at above 1373 K which led to pore blockage. With 3000 pulses, flexural strength was improved from 35 to about 90 MPa. Several specimens were exposed to air at 1573 K for 1070h during which the specimens were cooled to room temperature between four and seven times. SiC felt was also obtained by oxidation of a carbon skelton after pulse CVI.