Relationship between fracture toughness determined by surface crack in flexure and fracture resistance measured by indentation fracture for silicon nitride ceramics with various microstructures

The reliability of the Vickers indentation fracture (IF) method for various types of silicon nitride (Si₃N₄) ceramics was assessed by comparing the fracture resistance, K_R obtained from the IF test with the fracture toughness, K_Ic from the surface crack in flexure (SCF) technique in the same crack depth region. The K_R of a fine-grained and equiaxed Si₃N₄ matched with the K_Ic from the SCF test when Miyoshi's equation was used, while the K_Ic of a bearing-grade Si₃N₄ was found to lie between K_R values calculated with Niihara's equation (higher side) and Miyoshi's equations (lower side). In the case of coarse Si₃N₄ with elongated grains, the K_R determined using Niihara's equation gave the best fit with K_Ic. The inconsistent outcomes were explained by the probable mechanisms, indicating that the K_R from the IF test cannot be correlated directly with the K_Ic unless the effective crack length for the IF test was clarified.     

Low temperature densification of silicon nitride using Li2O-based surface coatings

For better control of the mechanical properties of Si₃N₄ ceramics, it is necessary to generate homogeneous microstructures, and for this purpose, chemical heterogeneities must be minimised, by careful control of powder processing and the subsequent consolidation steps. Coating of the starting silicon nitride powder is a convenient way of incorporating a liquid forming sintering aid more homogeneously than can be achieved by current commercial methods such as ball-milling.Thin layers of oxides, corresponding to additions of up to 5 w/o Li₂O have been deposited on the surface of grains of a commercial silicon nitride powder using alcoholic solutions containing appropriate amounts of the metal alkoxide. The resulting powders have been densified by pressurelesss sintering techniques, and their sintering characteristics identified in comparison with equivalent materials produced by adding the oxide in particulate form. In every case, a better sintering performance was observed at lower temperatures for the oxide-coated materials, with fully dense pressureless-sintered materials being obtained at temperatures as low as 1250 °C. An added observation was that for the coated samples, the final microstructure was more uniform, and showed an absence of large pores.     

Effect of monomer content on physical properties of silicon nitride ceramic green body prepared by gelcasting

The gelcasting technique was employed to prepare Si₃N₄ green body. The monomers used in the research were acrylamide (AM) and N,N′-methylenebisacrylamide (MBAM). The influences of the monomer content (AM and MBAM) and the ratio of monomers (AM/MBAM) on the warpage rate, shrinkage rate, and the flexural strength of Si₃N₄ ceramics green body were investigated. Both warpage rate and shrinkage rate of green body were found to decrease with the increase of monomer content, and monotonically increase with the ratio of monomers after drying. The variation of warpage rate with the ratio of monomers is evident when monomer content is 20 wt.%, but the variations are not evident when monomer contents are 40 and 55 wt.%. The flexural strength of the green body is highest at an optimum value of the monomers ratio, and increases with increasing monomer content, reaching 50–90 MPa when monomer contents are 40 and 55 wt.%.     

Indentation fracture resistance test round robin on silicon nitride ceramics

Reproducibility of indentation fracture resistance of three commercial silicon nitrides including bearing balls was evaluated by an international round robin with six laboratories. The between-laboratory standard deviations for indentations at 196 N on the perfectly mirror-finished surfaces were in the range of 0.2–0.5 MPa m^1/2, demonstrating an excellent precession of the test results. The scatter in the fracture resistance increased as the indentation load decreased from 196 to 98 N. The errors in measuring crack lengths deduced from the deviation of each laboratory's readings from author's reading for the same indentations tended to increase with a decrease in the magnification of the lab's microscope, which suggested that finding exact crack tips with lower magnification was difficult especially for those samples with insufficiently mirror-finished surfaces indented at 98 N. Observation of indentations at the load of 196 N with powerful optics was advised to ensure the validity of the indentation technique which is used as the quality assessment of Si₃N₄ bearing balls.     

Fabrication and characteristic of non-oxide fiber tow reinforced silicon nitride matrix composites by low temperature CVI process

Non-oxide fiber tow reinforced silicon nitride matrix composite was fabricated by low temperature CVI process with PyC as interphase. The tensile strength of the C and SiC fiber tow composites were 547 MPa and 740 MPa, respectively. The difference in tensile strength was analyzed based on the length, amount of pull-out fiber and also interface bonding. The infiltration uniformity of CVI silicon nitride (SiN) matrix within SiC fiber tow was comparable with that of CVI SiC matrix. These results suggested that the low temperature CVI process is suitable for the fabrication of fiber reinforced SiN matrix composites with proper interface bonding and high strength.     

Morphology control of a silicon nitride thick film derived from polysilazane precursor using UV curing and IR heat treatment

Silicon nitride (Si₃N₄) has excellent thermo-mechanical properties, and can be used as heat dissipation substrate for various devices. Si₃N₄ thin films are generally synthesised by chemical vapour deposition (CVD) or plasma-enhanced CVD. The use of polysilazanes (PSZs) as a precursor to the synthesis of Si₃N₄ has attracted significant attention because of their high mouldability and processability. In this study, Si₃N₄ thick films were prepared on silicon wafers or aluminium substrates by a spin- or dip-coating liquid PSZ, followed by UV curing and IR heat treatment under various conditions. The effects of the heat treatment conditions on the Si₃N₄ thick film surface were analysed by optical microscopy, X-ray diffraction, and scanning electron microscopy. An almost single phase of Si₃N₄ was synthesised successfully on the single crystalline silicon with UV curing at 400°C for 30 min and IR heating at 800°C in N₂ atmosphere.     

Porous Si3N4 ceramics prepared via slip casting of Si and reaction bonded silicon nitride

Slip casting process combined with reaction bonded silicon nitride (RBSN) was used to prepare porous Si₃N₄ ceramic with near-net and complex shape. A butyl stearate (BS) coated process was introduced to restrain the hydrolysis of Si, and ammonium polyacrylate (NH₄PAA) was used to enhance the dispersion of coated Si. The measured oxygen content showed that the hydrolysis of Si was strongly prohibited by BS coating, and relatively low viscosity was obtained with the addition of 0.25-1.5 wt% NH₄PAA to the 60 wt% solid load slurry. 40-60 wt% solid load slurries were used for slip casting in the experiment. After vacuum degassing, slip casting, debindering and nitridation, a density of 1.57-1.92 g/cm³ (porosity 50.9-40%) and a flexural strength of 47-108 MPa were obtained. The samples without vacuum degassing showed a large number of nanowires grown in the large pores.     

Processing of micro-components made of sintered reaction-bonded silicon nitride (SRBSN). Part 1: Factors influencing the reaction-bonding process

In order to establish a process for the manufacturing of injection moulded micro-components of sintered reaction-bonded silicon nitride (SRBSN) several process parameters were investigated with regard to their influence on the reaction-bonding step. One question to be answered was how the sintering aids affect the nitridation behaviour of a silicon green body. For the processing of micro-components it was of special interest to study, how a decreasing sample size and wall thickness would influence the rate of Si₃N₄ formation. By varying the added amounts of the sintering aids, it was found that increasing the Y₂O₃ and MgO contents both improved the nitridation rate, whereas an increase of Al₂O₃ content resulted in reduced nitridation rates. Within the investigated range of sample dimensions (0.2–4.0 g) the unexpected observation was made, that with decreasing sample weight the nitridation rate also decreased. This was explained by the exothermic nature of the reaction between Si and N₂ and the fact that small samples with a large surface-to-volume ratio attain thermal equilibrium with their environment better than large samples which may be subject to local overheating.     

An algorithm for the generation of silicon nitride structures

Silicon nitride is used for demanding tasks due to its high stiffness, strength and, especially, its high fracture toughness. Examples include cutting tools, forming rolls and ball bearings. The microstructure is characterized by elongated β-Si₃N₄ grains of different size and shape, which lead to the increased fracture toughness. Consequently, the paper will present an algorithm for the generation of three-dimensional and periodic silicon nitride-like microstructures, which will be used for micromechanical finite element simulations. The structure generation algorithm enhances the sequential adsorption technique with growth of particles and steric hindrance, which are motivated by experimental results. Results of the structure generator, such as the pseudo-time evolution and its statistical geometric distributions are presented and compared to literature data. With the finite element simulations, using a periodic unit cell, a validation of the model with literature values for Young's modulus and Poisson's ratio was possible.     

Silicon nitride based nanocomposites produced by two different sintering methods

This research explores the use of a variety of carbon nanostructures as reinforcing agents for Si₃N₄ matrix composites. We have chosen highly promising families of carbon materials: multiwall, singlewall carbon nanotubes (MWCNTs, SWCNTs), graphene, carbon black nanograins and graphite micrograins for use as fillers. These materials were dispersed with a concentration of 3 wt% in silicon nitride matrices. A high efficiency attritor mill has also been used for effective dispersion of second phases in the matrix. In the present work the development of sintering processes (hot isostatic pressing (HIP) and spark plasma sintering (SPS)) has been performed to consolidate and tailor the microstructure of Carbon nanotube (CNT)-reinforced silicon nitride-based ceramic composites. The silicon nitride nanocomposite systems retained the mechanical robustness of the original systems. Elastic modulus measurements and micro-indentation investigations of the hardness and fracture toughness have been performed as well as scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction in order to characterize the composites produced by the two sintering methods.