Preparation of Si3N4-SiC composites by microwave route

Si₃N₄-SiC composites have been microwave sintered using β-Si₃N₄ and β-SiC as starting materials. Si₃N₄ rich compositions (95 and 90 vol.% Si₃N₄) have been sintered above 96% of theoretical density without using any sintering additives in 40 min. A monotonic decrease in relative density is observed with increase in SiC proportion in the composite. Decrease in relative density has manifested in the reduction of fracture toughness and microhardness values of the composite with increase in SiC content although the good sintering of matrix Si₃N₄ limits the decrease of fracture toughness. Highest value of fracture toughness of 6.1 MPa m^1/2 is observed in 10 vol.% SiC composite. Crack propagation appears to be transgranular in the Si₃N₄ matrix and the toughening of the composites is through crack deflection around hard SiC particles in addition to its debonding from the matrix.     

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.     

Analyses of the role of grain boundaries in mesoscale dynamic fracture resistance of SiC-Si3N4 intergranular nanocomposites

Silicon carbide (SiC)-silicon nitride (Si₃N₄) nanocomposites with SiC dispersions as well as Si₃N₄ matrix of mesoscale dimensions (∼1 μm) are considered to have exceptional strength attributed to interactions of SiC dispersions with Si₃N₄ grain boundaries (GBs). However, an account of GBs on the strength of these nanocomposites is not available. In order to analyze this issue, cohesive finite element method (CFEM) based mesoscale dynamic fracture analyses of SiC-Si₃N₄ nanocomposites with an explicit account of length scales associated with Si₃N₄ GBs, SiC particles, and Si₃N₄ grains are performed. Analyses indicate that primary mechanism of fracture in the nanocomposite microstructures is intergranular Si₃N₄ matrix cracking. GBs are responsible for crack deflection and accordingly damage is limited to a smaller geometric region in microstructures with GBs. On an average, a microstructure with GBs present is stronger than the corresponding microstructure with GBs removed. However, in cases where the second phase SiC particles are in the wake of microcracks the microstructure without GB becomes stronger against fracture in comparison to the corresponding one with GBs owing to the crack bridging effect caused by the second phase SiC particles.     

Reactive and dense sintering of reinforced-toughened B4C matrix composites

Reactive hot-press (1800-1880 °C, 30 MPa, vacuum) is used to fabricate relatively dense B₄C matrix light composites with the sintering additive of (Al₂O₃ +Y₂O₃). Phase composition, microstructure and mechanical properties are determined by methods of XRD, SEM and SENB, etc. These results show that reactions among original powders B₄C, Si₃N₄ and TiC occur during sintering and new phases as SiC, TiB₂ and BN are produced. The sandwich SiC and claviform TiB₂ play an important role in improving the properties. The composites are ultimately and compactly sintered owing to higher temperature, fine grains and liquid phase sintering, with the highest relative density of 95.6%. The composite sintered at 1880 °C possesses the best general properties with bending strength of 540 MPa and fracture toughness of 5.6 MPa m^1/2, 29 and 80% higher than that of monolithic B₄C, respectively. The fracture mode is the combination of transgranular fracture and intergranular fracture. The toughening mechanism is certified to consist of crack deflection, crack bridging and pulling-out effects of the grains.     

Microstructure and mechanical properties of silicon nitride-titanium nitride composites prepared by spark plasma sintering

Si₃N₄-TiN composites were prepared by spark plasma sintering (conventional sintering (SPS1) and in situ reaction sintering (SPS2)). Homogeneous distribution of equiaxed TiN grains in Si₃N₄ matrix results in the highest microhardness (21.7 GPa) and bending strength (621 MPa) of sample SPS1 sintered at 1550 °C. Dispersion of elongated TiN grains in Si₃N₄ matrix results in the highest fracture toughness (8.39 MPa m^1/2) of sample SPS2 sintered at 1300 °C.     

Fabrication and mechanical properties of silicon carbide–silicon nitride nanocomposites

A powder mixture of ultrafine –SiC–35 wt% –Si₃N₄ containing 6 wt% Al₂O₃ and 4 wt% Y₂O₃ as sintering additives were liquid–phase sintered at 1800°C for 30 min by hot–pressing. The hot–pressed composites were subsequently annealed at 1920°C under nitrogen–gas–pressure to enhance grain growth. The average grain–size of the sintered bodies were ranged from 96 to 251 nm for SiC and from 202 to 407 nm for Si₃N₄, which were much finer than those of ordinary sintered SiC–Si₃N₄ composites. Both strength and fracture toughness of fine–grained SiC–Si₃N₄ composites increased with increasing grain size. Such results suggested that a small amount of grain growth in the fine–grained region (250 nm for SiC and 400 nm for Si₃N₄) was beneficial for mechanical properties of the composites. The room–temperature flexural strength and fracture toughness of the 8–h annealed composites were 698 MPa and 4.7 MPa · m^1/2, respectively.     

In Situ synthesis of TiN-reinforced Si3N4 matrix composites using Si and sponge Ti powders

Dense Si₃N₄-TiN composites from Si and sponge Ti (0–40 wt %) powders were produced by in situ reaction-bonding and post-sintering under N₂ atomosphere. The fracture strength and toughness of Si₃N₄-17% TiN composite were found to be 537.9 MPa and 10.4 MPam^1/2, respectively. In the reaction-bonded bodies, Si₃N₄ grains were constructed with - and -Si₃N₄ structure as well as TiN and some amounts of residual Si phase. After post-sintering, the residual Si and -Si₃N₄ grains were transformed to -Si₃N₄ grains with rod-like shape. No intermetallic compounds (e.g., TiSi₂, Ti₅Si₃ and Ti₅Si₄) were formed at the interfaces between Si₃N₄ and TiN grains. The main toughening mechanisms were crack deflection and crack bridging caused by rod-like Si₃N₄ grains which were randomly dispersed in sintered body. Microcracking due to the dispersion of in situ formed TiN particles also contributed to the toughening of the sintered body.     

Microstructural characterization of electroconductive Si3N4–TiN composites

Electroconductive Si₃N₄–TiN composites from Si and TiN powders have been fabricated by in situ reaction-bonding and post-sintering under N₂ atomosphere. The values of fracture strength and electrical resistivity in the Si₃N₄–50 wt.% TiN composite were 531 MPa and 2.5×10⁻² Ω cm, respectively. The dispersion of TiN particles inhibited the abnormal growth of rod-like Si₃N₄ grains with large size in diameter. An amorphous phase observed in most grain boundaries and triple points is attributed to liquid phase sintering. Many dislocations formed by the difference of thermal expansion coefficients were observed in Si₃N₄ and TiN grains.     

Fabrication,mechanical properties and microstructure analysis of Si3N4/SiC nanocomposite

Ceramic nanocomposites, Si₃N₄ matrix reinforced with nano-sized SiC particles, were fabricated by hot pressing the mixture of Si₃N₄ and SiC fine powders with different sintering additives. Distinguishable increase in fracture strength at low and high temperatures was obtained by adding nano-sized SiC particles in Si₃N₄ with Al₂O₃ and/or Y₂O₃. Si₃N₄/SiC nanocomposite added with Al₂O₃ and Y₂O₃ demonstrated the maximum strength of 1.9 GPa with average strength of 1.7 GPa. Fracture strength of room temperature was retained up to 1400 as 1 GPa in the sample with addition of 30 nm SiC and 4 wt% Y₂O₃. Striking observation in this nanocomposite is that SiC particles at grain boundary are directly bonded to Si₃N₄ grain without glassy phases. Thus, significant improvement in high temperature strength in this nanocomposite can be attributed to inhibition of grain boundary sliding and cavity formation primarily by intergranular SiC particles, besides crystallization of grain boundary phase.     

Mechanical properties Of Si3N4 cerarnics reinforced with SiC whiskers and SiC platelets

Silicon nitride ceramics reinforced with SiC whiskers and SiC platelets were fabricated by hot pressing and their mechanical properties were studied. They showed higher fracture energy than conventional composites, particularly when they were consolidated by gas-pressure hot pressing at high temperature. A high fracture toughness (10.7 MPa m^1/2) which was measured by the single-edge pre-cracked beam method was achieved. Furthermore, a unique method to observe the crack propagation behaviours directly in a scanning electron microscope with loading devices was developed. As a result, much bridging and pull-out of the whiskers and the elongated Si₃N₄ grains, and crack deflection along the platelets, were observed behind the crack tip. This means that these grains are effective in enhancing the fracture resistance during crack propagation.     

Influence of SiC, Si3N4 and Al2O3 particles on the structure and properties of electrodeposited Ni

The structure and properties of electrodeposited nickel composites reinforced with inert particles like SiC, Si₃N₄ and Al₂O₃ were compared. A comparison was made with respect to structure, morphology, microhardness and tribological behaviour. The coatings were characterized with optical microscopy, Scanning electron microscopy (SEM), Energy dispersive X-ray analysis (EDX) and X-ray diffraction (XRD) technique. The cross-sectional microscopy studies revealed that the particles were uniformly distributed in all the composites. However, a difference in the surface morphology was revealed from SEM studies. The microhardness studies revealed that Si₃N₄ reinforced composite showed higher hardness compared to SiC and Al₂O₃ composite. This was attributed to the reduced crystallite size of Ni — 12 nm compared to 16 nm (SiC) and 23 nm (Al₂O₃) in the composite coating. The tribological performance of these coatings studied using a Pin-on-disk wear tester, revealed that Si₃N₄ reinforced composite exhibited better wear resistance compared to SiC and Al₂O₃ composites. However, no significant variation in the coefficient of friction was observed for all the three composites.     

Synthesis and properties of model SiC-Si3N4 interfaces

Microscopic and macroscopic SiC-Si₃N₄ interfacial structures were synthesized and their properties examined. Microscopic interfaces were produced by hot isostatic pressing vapour-liquid-solid SiC whisker-polycrystalline Si₃N₄ matrix composites without densification aids. Macroscopic interfaces were formed by the chemical vapour deposited Si₃N₄ coating of large SiC single crystals. The characteristics of these model interfaces were investigated using transmission electron microscopy and indentation fracture. Results showed the microscopic interfaces to contain a small amount of second phase, while the macroscopic interfaces were pristine in nature with no second phase present. Pristine SiC-Si₃N₄ interfaces were strongly bonded at room temperature, but interfacial strength decreased at elevated temperatures.     

Si<Subscript>3</Subscript>N<Subscript>4</Subscript>/TiN composites produced from TiO<Subscript>2</Subscript>-Modified Si<Subscript>3</Subscript>N<Subscript>4</Subscript> powders

Si₃N₄/TiN composites have been produced by hot pressing at temperatures from 1600 to 1800°C in a nitrogen atmosphere, using silicon nitride powders prepared by self-propagating high-temperature synthesis and surface-modified with titanium dioxide nanoparticles. We examined the effect of TiO₂ content on the microstructure, phase composition, and mechanical strength of the ceramics. It is shown that titanium nitride can be formed by the reaction Si₃N₄ + TiO₂ → TiN + NO + N₂O + 3Si. The Si₃N₄/TiN composites containing 5–20% TiN have a low density, high porosity, and a bending strength of 60 MPa or lower. In Si₃N₄/TiN ceramics produced using calcium aluminates as sintering aids, the silicon nitride grains are densely packed, which ensures an increase in strength to 650 MPa.     

Residual stresses in particle-reinforced ceramic composites using synchrotron radiation

Residual stresses were determined in particle-reinforced ceramic composites using synchrotron based x-ray diffraction. The baseline Si₃N₄ and the Si₃N₄-TiN composites were processed by turbomilling, pressure casting, and isopressing. They were then continuously sintered to full density, under a pressureless, flowing nitrogen atmosphere. The flexural strength, fracture toughness, and residual stress were measured for as-machined samples and following quenching in water from 1000°C, 1100°C, and 1200°C. The residual stresses for both the baseline Si₃N₄ and the Si₃N₄-TiN composites were determined from the (441) and (531) reflections, by applying the 2-sin² method. The measured residual stresses were compared with the flexural strength and fracture toughness results to determine the effects of residual stress and thermal shocking on the mechanical properties of each material. In both the baseline Si₃N₄ and Si₃N₄-TiN composites, after thermal shocking, the compressive residual stresses were developed in directions both parallel and perpendicular to the sample surface. The residual compressive stresses for the Si₃N₄-TiN composites were much higher than the baseline Si₃N₄. As a result, both fracture toughness and flexural strength of the Si₃N₄-TiN composites were improved. In addition, the addition of the TiN appears to improve both the strength and toughness of the baseline Si₃N₄.     

Fracture toughness of Si3N4 and its Si3N4 whisker composite without sintering aids

Si₃N₄ without sintering aids is studied with special interest to the fracture behaviour and its relation to microstructure. Cracks propagated almost transgranularly and no rising R-curve behaviour was found, because crack-wake region gave no contribution on toughening due to very high grain-boundary bonding strength. Microstructure with highly elongated grains was obtained by addition of 20%Si₃N₄ whisker, but fracture toughness was found to be similar to that of the monolithic Si₃IM₄ with equiaxed grains. It is recognized that fracture toughness is not determined simply by apparent microstructural parameters such as mean aspect ratio of grains when grain-boundary bonding is sufficiently strong. Detailed examination of microfracture behaviour is, therefore, necessary for the analysis of toughening in this kind of composites.     

Effect of a silicon sintering additive on solid state bonding of SiC to Nb

Pressureless-sintered (PLS) SiC was joined to Nb by solid state bonding in a vacuum. The joining strength of the PLS SiC/Nb joint increases to the saturated value of 108 MPa with increasing joining pressure at a joining condition of 1673 K and 7.2 ks. This saturated value of PLS SiC/Nb joint is higher than that of the reaction sintered (RS) SiC/Nb joint. The strength of SiC itself affects the strength of the SiC/Nb joint. The high stability of the intermediate phase Nb₅Si₃ in the interface at elevated temperature leads to the high heat resistance of the joint. The thickness of the intermediate phase Nb₅Si₃ in the PLS SiC/Nb system is lower than that of the RS SiC/Nb system at a constant joining time, although the activation energy, 452 kJ mol^–1, of growth for the phase in the PLS SiC/Nb system is almost the same as the RS SiC/Nb system, 456 kJ mol^–1. The rate constant of the growth for the phase in the PLS SiC/Nb system is lower than that in the RS SiC/Nb system. The excess silicon in RS SiC promotes the formation of the Nb₅Si₃ phase at the interface between SiC and Nb.     

Effect of grain width and aspect ratio on mechanical properties of Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramics

Sintering additives Y₂O₃ and Al₂O₃ with different ratios ((Y₂O₃/Al₂O₃) from 1 to 4) were used to sinter Si₃N₄ to high density and to induce microstructural changes suitable for raising mechanical properties of the resultant ceramics. The sintered Si₃N₄ ceramics have bi-modal microstructures with elongated β-Si₃N₄ grains uniformly distributed in a matrix of equiaxed or slightly elongated grains. Pores were found within the grain boundary phase at the junction regions of Si₃N₄ grains. The highest average aspect ratio (length/width of the grains) of ∼4.92 was found for Y₂O₃/Al₂O₃ ratio of 2.33 with fracture toughness and strength values of ∼7 MPam^1/2 and 800 MPa, respectively. The effect of microstructure, specifically grain morphology, on mechanical properties of sintered Si₃N₄ were investigated and found that the aspect ratio of the elongated grains is the most important microstructural feature which controls mechanical properties of these ceramics.     

Fabrication of SiC particles-reinforced magnesium matrix composite by ultrasonic vibration

Magnesium matrix composites reinforced with two volume fractions (1 and 3%) of SiC particles (1 μm) were successfully fabricated by ultrasonic vibration. Compared with as-cast AZ91 alloy, with the addition of the SiC particles grain size of matrix decreased, while most of the phase Mg₁₇Al₁₂ varied from coarse plates to lamellar precipitates in the SiCp/AZ91 composites. With increasing volume fraction of the SiC particles, grains of matrix in the SiCp/AZ91 composites were gradually refined. The SiC particles were located mainly at grain boundaries in both 1 vol% SiCp/AZ91 composite and 3 vol% SiCp/AZ91 composite. SiC particles inside the particle clusters may be still separated by magnesium. The study of the interface between the SiC particle and the alloy matrix suggested that SiC particles bonded well with the alloy matrix without interfacial reaction. The ultimate tensile strength, yield strength, and elongation to fracture of the SiCp/AZ91 composites were simultaneously improved compared with that of the as-cast AZ91 alloy.     

Effect of size and morphology of particulate SiC dispersions on fracture behaviour of Si3N4 without sintering aids

The relation between microstructural characteristics and fracture behaviour of Si₃N₄/SiC-particle composites were evaluated for a series of materials containing a 25 vol% dispersion, with mean size in the range 7–106m. All the composites were fabricated by hot isostatic pressing without external addition of sintering aids via glass encapsulation. Quantitative image analysis techniques were employed to assess the microstructural parameters, dealing with morphology and distribution of the SiC particles. A fracture mechanics analysis based on the determination of fracture strength, toughness, work of fracture and rising R-curve behaviour provided the basis for discussion of the effectiveness of the SiC dispersions.The results of mechanical tests are compared with those obtained on the monolithic material fabricated by the same process. The microfracture mechanisms in composites are discussed by relating microstructural data, obtained by image analysis, to toughness data.     

Behaviour of SiC+Si3N4 mixtures during heating

This article discusses the behavior of the Si₃N₄+SiC mixture during sintering. The purpose of this study was to obtain data on sintered Si₃N₄/SiC composites. The proportion of Si₃N₄ and SiC powders in the initial mixtures varied from 0% to 100%, while the molar ratio of SiO₂/Y₂O₃ was 2:1 and the total amount of additives (14 wt.%) was kept constant. Samples of the powders were pressed under 300 MPa and heated to 1600, 1650, 1700, 1750, 1800, 1850, 1900, 1950 and 2000 °C, in a nitrogen atmosphere, and allowed to cool as soon as this temperatures were reached. After the heating step, the samples were characterized according to their final density, crystalline phases, microstructures and weight loss. The samples displayed little weight loss, but their density decreased with increasing amounts of SiC, particularly at temperatures above 1750 °C. All the mixtures showed the formation of liquid phase between 1650 and 1750 °C, regardless of their composition.