Microstructure and fracture-mechanical properties of carbon derived Si3N4 + SiC nanomaterials

The microstructure and basic mechanical properties, as hardness, fracture toughness, fracture strength and subcritical crack growth at room temperature were investigated and creep behavior at high temperatures was established. The presence of SiC particles refined the microstructure of Si₃N₄ grains in the Si₃N₄ + SiC nanocomposite. Higher hardness values resulted from introducing SiC nanoparticles into the material. A lower fracture toughness of the nanocomposite is associated with its finer microstructure; crack bridging mechanisms are not so effective as in the case of monolithic Si₃N₄. The strength value of the monolithic Si₃N₄ is higher than the characteristic strength of nanocomposites. Fractographic analysis of the fracture surface revealed that a failure started principally from an internal flaw in the form of cluster of free carbon, and on large SiC grains which degraded strength of the nanocomposite. The creep resistance of nanocomposite is significantly higher when compared to the creep resistance of the monolithic material. Nanocomposite exhibited no creep deformation, creep cracks have not been detected even at a test at 1400 °C and a long loading time, therefore the creep is probably controlled mainly by diffusion. The intergranular SiC nanoparticles hinder the Si₃N₄ grain growth, interlock the neighboring Si₃N₄ grains and change the volume fraction, geometry and chemical composition of the grain boundary phase.     

The effects of pre-oxidation on the sintering and mechanical property of powder injection moulded SiC material

Usually, injection moulded SiC green parts are debound in inert atmosphere or vacuum, which induces the residual carbon and increases forming cycle and production cost. In this paper, injection moulded SiC with Al₂O₃ and Y₂O₃ as sintering assistant was thermal debound in air and Ar, respectively. The paper investigates the effects of pre-oxidation during debinding stage on the sintering and mechanical property of SiC material. During sintering, the oxide SiO₂ is in favour of the shrinkage of debound samples at lower temperature. After sintering, the linear shrinkage of sintered samples with pre-oxidation is bigger than the sample without pre-oxidation. Test results by TEM and XRD indicate that SiO₂ disappear from the inside of the sintered samples. The loss of SiO₂ decreases the content of Al₂O₃, which affects the formation of YAG (Y₃Al₅O₁₂). Sintered Sic samples contain α-SiC phase and intergranular phase. There is no hetero-phase between the boundaries of α-SiC phase and intergranular phase. The bending and compression strength values of sintered samples with pre-oxidation reach to 537 MPa and 2.89 GPa, respectively. These values approach the strength of sintered samples without pre-oxidation (594 MPa and 3.0 GPa).     

SiC nanoparticle-reinforced Al2O3–Nb composite as a potential femoral head material in total hip arthroplasty

A ceramic–metal composite consisting of SiC nanoparticle-reinforced Al₂O₃ and Nb (referred to as SiC/Al₂O₃–Nb), was prepared and evaluated in vitro for potential application as a femoral head material in total hip arthroplasty. Dense bi-layer laminates of SiC nanoparticle-reinforced Al₂O₃ and Nb were fabricated by hot pressing of powders (1425 °C; 35 MPa), and evaluated using scanning electron microscopy, microchemical analysis, and mechanical testing. The flexural strength of the SiC/Al₂O₃–Nb laminate (960 ± 20 MPa) was higher than the value (720 ± 40 MPa) for an Al₂O₃–Nb laminate, and far higher than the value (620 ± 50 MPa) for SiC nanoparticle-reinforced Al₂O₃ (SiC/Al₂O₃). The Vickers hardness of SiC/Al₂O₃ was 17 ± 2 GPa, compared to 12 ± 1 GPa for Al₂O₃. A high interfacial shear strength of the SiC/Al₂O₃–Nb laminate (310 ± 100 MPa), coupled with SEM observation of the interfacial region, showed strong bonding between the SiC/Al₂O₃ and Nb layers. Composite femoral heads consisting of a SiC/Al₂O₃ surface layer and a Nb core could potentially lead to a reduction in the tendency for brittle failure as well as to lower wear, when compared to Al₂O₃ femoral heads.     

Mechanical properties of rolled A356 based composites reinforced by Cu-coated bimodal ceramic particles

Three kinds of A356 based composites reinforced with 3 wt.% Al₂O₃ (average particle size: 170 μm), 3 wt.% SiC (average particle size: 15 μm), and 3 wt.% of mixed Al₂O₃–SiC powders (a novel composite with equal weights of reinforcement) were fabricated in this study via a two-step approach. This first process step was semi-solid stir casting, which was followed by rolling as the second process step. Electroless deposition of a copper coating onto the reinforcement was used to improve the wettability of the ceramic particles by the molten A356 alloy. From microstructural characterization, it was found that coarse alumina particles were most effective as obstacles for grain growth during solidification. The rolling process broke the otherwise present fine silicon platelets, which were mostly present around the Al₂O₃ particles. The rolling process was also found to cause fracture of silicon particles, improve the distribution of fine SiC particles, and eliminate porosity remaining after the first casting process step. Examination of the mechanical properties of the obtained composites revealed that samples which contained a bimodal ceramic reinforecment of fine SiC and coarse Al₂O₃ particles had the highest strength and hardness.     

BN/Si3N4 nanocomposite with high strength and good machinability

BN/Si₃N₄ nanocomposite was prepared using BN/Si₃N₄ powder obtained by nitriding Si₃N₄/NH₄HB₄O₇ mixture in ammonia gas as the starting powder. Microstructural investigations by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) showed that BN particles were homogeneously distributed within the matrix grains as well as at the matrix grain boundaries, and the growth of Si₃N₄ matrix grain was significantly retarded by BN particles. The BN/Si₃N₄ nanocomposite showed a higher strength than the conventional BN/Si₃N₄ microcomposite due to the formation of fine and homogeneous microstructure in it. BN/Si₃N₄ nanocomposite with a BN content of 20 vol% and above showed excellent machinability, because of the formation of weak BN/Si₃N₄ interfaces and the cleavage behavior of BN particles.     

Spark plasma sintering of silicon nitride using nanocomposite particles

The spark plasma sintering (SPS) of silicon nitride (Si₃N₄) was investigated using nanocomposite particles composed of submicron-size α-Si₃N₄ and nano-size sintering aids of 5 wt% Y₂O₃ and 2 wt% MgO prepared through a mechanical treatment. As a result of the SPS, Si₃N₄ ceramics with a higher density were obtained using the nanocomposite particles compared with a powder mixture prepared using conventional wet ball-milling. The shrinkage curve of the powder compact prepared using the mechanical treatment was also different from that prepared using the ball-milling, because the formation of the secondary phase identified by the X-ray diffraction (XRD) method and liquid phase was influenced by the presence of the sintering aids in the powder compact. Scanning electron microscopy (SEM) observations showed that elongated grain structure in the Si₃N₄ ceramics with the nanocomposite particles was more developed than that using the powder mixture and ball-milling because of the enhancement of the densification and α-β phase transformation. The fracture toughness was improved by the development of the microstructure using the nanocomposite particles as the raw material. Consequently, it was shown that the powder design of the Si₃N₄ and sintering aids is important to fabricate denser Si₃N₄ ceramics with better mechanical properties using SPS.     

Preparation and mechanical properties of self-reinforced in situ Si3N4 composite with La2O3 and Y2O3 additives

Self-reinforced in situ Si₃N₄ composite material was prepared with high amount of La₂O₃ and Y₂O₃ additives by two-step hot pressing, and the optimum amount of additives was determined. The volume fraction of boundary glass phase was calculated based on the equilibrium of equivalent number in chemical reaction. For material with 15 mol% additives, flexural strength and fracture toughness at room temperature were 960 MPa and 12.3 MPa m^1/2, respectively. At temperature of 1350°C, flexural strength was maintained to 720 MPa and fracture toughness was significantly increased to 23.9 MPa m^1/2 because of the high refractory of oxynitride glass containing compositions of La and Y. Self-reinforced mechanism was mainly responsible for crack deflection along the elongated β-Si₃N₄ grains.     

Preparation of polycrystalline YAG/alumina composite fibers and YAG fiber by sol–gel method

Polycrystalline yttrium–aluminum garnet, Y₃Al₅O₁₂ (YAG) fiber and α-alumina and YAG matrix composite fiber were prepared by the sol–gel method. α-Alumina and YAG matrix composite fiber with fine and homogeneous microstructure could be successfully fabricated by interpenetrating YAG in alumina matrix and adding α-alumina of seed particles to fibers. Effect of α-alumina seed particles and YAG on crystallization and microstructure of composite fiber were discussed. The size of alumina matrix of the composite fibers heated at 1600°C for 4 h was below 2 μm. The tensile of strength alumina fiber heat-treated at 1500°C was 0.2 GPa, while that of the composite fiber was 1.1 GPa.     

Evaluation of microstructure and mechanical properties of Al/Al2O3/SiC hybrid composite fabricated by accumulative roll bonding process

In this investigation, a new kind of metal matrix composites with a matrix of pure aluminum and hybrid reinforcement of Al₂O₃ and SiC particles was fabricated for the first time by anodizing followed by eight cycles accumulative roll bonding (ARB). The resulting microstructures and the corresponding mechanical properties of composites within different stages of ARB process were studied. It was found that with increasing the ARB cycles, alumina layers were fractured, resulting in homogenous distribution of Al₂O₃ particles in the aluminum matrix. Also, the distribution of SiC particles was improved and the porosity between particles and the matrix was decreased. It was observed that the tensile strength of composites improved by increasing the ARB passes, i.e. the tensile strength of the Al/1.6 vol.% Al₂O₃/1 vol.% SiC composite was measured to be about 3.1 times higher than as-received material. In addition, tensile strength of composites decreased by increasing volume fraction of SiC particles to more than 1 vol.%. Scanning electron microscopy (SEM) observation of fractured surfaces showed that the failure mechanism of broken hybrid composite was shear ductile rupture.     

Effect of 10Ce-TZP/Al2O3 nanocomposite particle amount and sintering temperature on the microstructure and mechanical properties of Al/(10Ce-TZP/Al2O3) nanocomposites

A zirconia/alumina nanocomposite stabilized with cerium oxide (Ce-TZP/Al₂O₃ nanocomposite) can be a good substitute as reinforcement in metal matrix composites. In the present study, the effect of the amount of 10Ce-TZP/Al₂O₃ particles on the microstructure and properties of Al/(10Ce-TZP/Al₂O₃) nanocomposites was investigated. For this purpose, aluminum powders with average size of 30 μm were ball-milled with 10Ce-TZP/Al₂O₃ nanocomposite powders (synthesized by aqueous combustion) in varying amounts of 1, 3, 5, 7, and 10 wt.%. Cylindrical-shape samples were prepared by pressing the powders at 600 MPa for 60 min while heating at 400–450 °C. The specimens were then characterized by scanning and transmission electron microscopy (SEM and TEM) in addition to different physical and mechanical testing methods in order to establish the optimal processing conditions. The highest compression strength was obtained in the composite with 7 wt.% (10Ce-TZP/Al₂O₃) sintered at 450 °C.     

A study on the mechanochemical behavior of TiO2–Al–Si system to produce Ti5Si3–Al2O3 nanocomposite

In the present study Ti₅Si₃–Al₂O₃ nanocomposite was synthesized by a displacement reaction between Al and TiO₂ in ball milling of TiO₂, Al and Si powders. The effect of milling time and heat treatment temperatures were also investigated. The structural changes of powder particles during mechanical alloying were investigated by X-ray diffraction (XRD). Morphology and microstructure of powders were characterized by scanning electron microscopy (SEM). It was found that after 10 h of MA, the reaction between Al and TiO₂ initiated in a gradual mode and after about 45 h of milling, the reaction was successfully completed. The final product consisted of Ti₅Si₃ intermetallic compound with a crystallite size of 13 nm and amorphous Al₂O₃. Heat treatment of this structure at 1050 °C led to the crystallization of Al₂O₃ and ordering of Ti₅Si₃. The crystallite size of Ti₅Si₃ and Al₂O₃ after annealing at 1050 °C for 1 h remained in nanometer scale. So the final product appeared to be stable upon annealing.     

Effect of Al2O3 layer on improving high-temperature oxidation resistance of siliconized TiAl-based alloy

TiAl-based specimens were siliconized with two different kinds of cementation respectively, one is 23 vol.% Si + 77 vol.% Al₂O₃, and the other is 23 vol.% Si + 77 vol.% ZrO₂. SEM observation showed that a Ti₅Si₃-based layer, in which some Al₂O₃ particles dispersed, formed on the surface after siliconization. Further observation showed that an extra outer Al₂O₃ layer existed on the surface of specimens siliconized with 23 vol.% Si + 77 vol.% Al₂O₃, while no such Al₂O₃ layer was found in specimens siliconized with 23 vol.% Si + 77 vol.% ZrO₂. The cyclic oxidation test performed at 900 °C shows that the oxidation resistance was significantly improved by siliconizing. By comparison, the specimens that siliconized with 23 vol.% Si + 77 vol.% Al₂O₃ exhibits a better oxidation resistance than that with 23 vol.% Si + 77 vol.% ZrO₂. It was deduced that the extra outer Al₂O₃ layer is beneficial to the oxidation resistance of siliconized TiAl-based alloy.     

Improvement of yield strength of LM24 alloy

In this study, Al₂O₃ particles were employed to improve the microstructure of LM24 and therefore, to increase the yield strength and tensile strength of this kind of alloy. In situ Al₂O₃ particles were obtained by direct reaction between oxygen and Al melt at 750–800 °C. Microstructure examination shows that the size of in situ formed Al₂O₃ particles was about 1–2 μm, and interestingly, with addition of in situ Al₂O₃ particles, the coarse primary Si phase was disappeared completely. More important, the yield strength and the tensile strength of Al₂O₃/LM24 are increased by 52 MPa, 16 MPa than that of LM24 alloy with 0.1% Sb addition. The value of 181 MPa and 315 MPa is for yield strength and tensile strength of Al₂O₃/LM24 respectively. Besides, the yield strength and tensile strength are 180 MPa and 314 MPa respectively for Al₂O₃/LM24 alloy after remelting and casting. This verifies that the improvement of mechanical properties of such kind of material possesses stability and reliability.     

Fabrication and properties of mechanically alloyed and Ni activated sintered W matrix composites reinforced with Y2O3 and TiB2 particles

Microstructural and physical properties of W–1 wt.% Ni matrix composites reinforced with Y₂O₃ and TiB₂ particles produced via mechanical alloying and sintering at 1400 °C for 1 h under Ar, H₂ gas flowing conditions were investigated. XRD patterns of the sintered samples revealed the presence of W, Ni and TiB₂ phases, whereas W₂B and NiTi phases were detected in the samples containing 4 wt.% and 5 wt.% TiB₂. Relative density value of W–1 wt.% Ni sample was measured as 97%, which decreased to 95.4% with the addition of 0.5 wt.% Y₂O₃. Relative density values varied between 95.4% and 97.3% for the sintered samples containing varying TiB₂ between 1 wt.% and 5 wt.%. Average W grain size in the sintered samples decreased with the addition of Y₂O₃ and TiB₂ particles, from 5.38 μm in the W–1 wt.% Ni sample to 0.8 μm in the W–1 wt.% Ni sample containing 0.5 wt.% Y₂O₃ and 5 wt.% TiB₂ particles. Vickers microhardness values varied between 4.53 GPa and 8.54 GPa. The sample with the composition of W–1 wt.% Ni/0.5 wt.% Y₂O₃ and 5 wt.% TiB₂ had a relative density value of about 95.7% and hardness value of 8.54 GPa after sintering at 1400 °C for 1 h.     

Influence of yttrium dopant on the synthesis of ultrafine AlN powders by CRN route from a sol–gel low temperature combustion precursor

Y-doped ultrafine AlN powders were synthesized by a carbothermal reduction nitridation (CRN) route from precursors of Al₂O₃, C and Y₂O₃ prepared by a sol–gel low temperature combustion technology. The Y dopant reacted with alumina and thus forming yttrium aluminate of AlYO₃, Al₃Y₅O₁₂ and Al₂Y₄O₉, which formed a liquid at about 1400 °C and promoted the transformation of Al₂O₃ to AlN and the growth of AlN particles. Compared with the conventional solid CRN process, Y dopant reduced the synthesis temperature by 150 °C, and Al₂O₃ transformed to AlN completely at 1450 °C. The content of Y dopant had little effect on the synthesis temperature of AlN whereas it influenced the phase of Y compounds in the products. As the Y/Al molar ratio was in the range of 0.007648–0.022944, the particle sizes of Y-doped AlN powders synthesized at 1450 °C were 150–300 nm.     

Preparation of SiC ceramics by aqueous gelcasting and pressureless sintering

Gelcasting is an attractive forming process to fabricate ceramic parts with complex shape. In the present work, aqueous gelcasting of SiC was studied. SiC slurry (50 vol.%) for gelcasting was prepared with sintering assistants, Al₂O₃ and Y₂O₃. The slurry was solidified in situ to green body with relative density of 55.9 ± 0.9% and flexural strength of 13.9 ± 0.7 MPa. SEM shows that ceramic powders in green body compact closely by the connection of polymer networks, and that the pores decrease greatly with the size less than 1 μm. SiC samples were also obtained by the process of gelcasting and pressureless sintering at 2000 °C for 1 h in Ar atmosphere. The relative density and flexural strength of SiC sintered body are 97.3 ± 0.4% and 637 ± 156 MPa, and the hardness and toughness are 20.68 ± 0.80 GPa and 3.85 ± 0.23 MPa m^1/2, respectively.     

Fracture behaviour of α-Al2O3 ceramics reinforced with a mixture of single-wall and multi-wall carbon nanotubes

The extraordinary mechanical properties of single-wall carbon nanotubes (SWCNTs) and multi-wall carbon nanotubes (MWCNTs) have generated interest in incorporating them as toughening agents in ceramics. This work describes the fracture behaviour of an alumina (Al₂O₃) ceramic reinforced with a mixture of 0.05 wt% MWCNTs + 0.05 wt% SWCNTs. The CNT/Al₂O₃ nanocomposite was pressureless sintered in air using graphite powder as bed powder at 1520 °C for 1 h. The hardnesses and fracture toughnesses were lower than for pure Al₂O₃ and Al₂O₃ + 0.1 wt% SWCNTs and Al₂O₃ + 0.1 wt% MWCNTs. A predominantly transgranular fracture mode with a decrease in crack deflection and no pull-out was observed in the SWCNT + MWCNT–Al₂O₃ nanocomposite. MWCNTs had to the best reinforcing effect in Al₂O₃ nanocomposite.     

The role of oxidation and counterface in the high temperature tribological properties of TiAl intermetallics

Clarification of how oxidation and counterface materials influence the high temperature tribological properties of TiAl alloy is the main object of this research. As evident from the comparison tests in air and argon, surface oxidation is detrimental to the tribological properties of the alloy at low temperature, but favorable above 600 °C.Counterface (Si₃N₄, SiC and Al₂O₃) is an important factor that largely affects the tribological properties of TiAl alloys, and this effect is strongly dependent on the system environment. In general, TiAl alloy shows superior tribological properties when Al₂O₃ is mating surface, excluding at 800 °C in argon.     

Effect of alumina particles loading on the mechanical properties of light-cured dental resin composites

The purpose of this study is to evaluate the effect of alumina (Al₂O₃) loading on the mechanical properties of dental resin composites (DRCs). The DRCs were prepared based on Al₂O₃ particles and bisphenol A-glycidyl methacrylate (Bis-GMA) was used as the base monomer. The silane-treated Al₂O₃ particles were mixed with the resin matrix in proportions of 40, 50, and 60 wt%, respectively. Resin matrix without filler was used as the control sample. The Vickers hardness (HV) and flexural modulus (FM) of the DRCs mixed with Al₂O₃ particles were found to be superior compared to the control sample; the values increased from 14.4 to 23.5 kg/mm² and 1.5 to 5.7 GPa, respectively. However, the flexural strength (FS) values of DRCs were slightly decreased as the filler loading increased i.e. from 84.5 to 74.2 MPa. The results also revealed statistically significant increases in the HV and FM. On the other hand, FS values showed significant decrease when filler loading was increased (P < 0.05).     

Microstructural evolutions of nickel-aluminide nanocomposites during powder synthesis and thermal spray processes

The synthesis and microstructural evolutions of the NiAl-15 wt% (Al₂O₃–13% TiO₂) nanocomposite powders were studied. These nanocomposite powders are used as feedstock materials for thermal spray applications. These powders were prepared using high and low-energy mechanical milling of the Ni, Al powders and Al₂O₃–13% TiO₂ nanoparticle mixtures. High and low-energy ball-milled nanocomposite powders were also sprayed by means of high-velocity oxy fuel (HVOF) and air plasma spraying (APS) techniques respectively. The results showed that the formation of the NiAl intermetallic phase was noticed after 8 h of high-energy ball milling with nanometric grain sizes but in a low-energy ball mill, the powder particles contained only α-Ni solid solution with no trace of the intermetallic phase after 25 h of milling. The crystallite sizes in HVOF coating were in the nanometric range and the coating and feedstock powders showed the same phases. However, under the APS conditions, the coating was composed of the NiAl intermetallic phase in the α-Ni solid solution matrix. In both of the nanocomposite coatings, reinforcing nanoparticles (Al₂O₃–13% TiO₂) were located at the grain boundaries of the coatings and pinned the boundaries, therefore, the grain growth was prohibited during the thermal spraying processes.