VAMAS Round Robin on Fracture Toughness of Silicon Nitride

Eight laboratories in Germany, Japan, U.K., and U.S. participated in the VAMAS round robin. The fracture toughness of silicon nitride at room temperature and at 1200^deg;C was measured by three methods: the single-edge V-notched beam (SEVNB), single-edge precracked beam (SEPB), and chevron notched beam (CNB). The obtained values show hardly any crosshead speed dependence, irrespective of test temperature and atmosphere. Results may have been influenced by a small amount of slow crack growth, but distinct R -curve behavior could not be detected within the scope of the tests. The values at 1200^deg;C in N₂ can be measured by the SEVNB and SEPB methods with small scatters. The oxidation of silicon nitride, caused by heating in air, increases the SEVNB and SEPB values. The CNB values are free from the effects of test temperature and atmosphere, but they show a large scatter between laboratories. However, the chevron V-notched beam (CVNB) method, which is an improved CNB method, shows values with a small scatter, irrespective of the measurement conditions. The SEVNB and SEPB measurements in N₂ and the CVNB measurement under any conditions are recommended for the measurement of high-temperature fracture toughness.     

Grain Boundary Films in Rare-Earth-Glass-Based Silicon Nitride

The thickness of the intergranular films in Si₃N₄ densified with lanthanide oxides has been systematically investigated using high-resolution transmission electron microscopy. Four lanthanide oxides—La₂O₃, Nd₂O₃, Gd₂O₃, and Yb2O3—as well as Y₂O₃ are chosen so that the results will reflect the overall trend in the effect of the lanthanide utilized. The film thicknesses increase with increasing ionic radius of the lanthanide. In addition, Si₃N₄ particles flocculated into isolated clusters in the lanthanide-based glasses are also characteristically separated by an amorphous film whose thickness is similar to that in the comparable polycrystalline ceramics, demonstrating that the film thickness is dictated entirely by the composition and not by the amount of the glass phase present.     

Fracture Toughness and Thermal Shock Behavior of Silicon Nitride–Boron Nitride Ceramics

Fracture toughness behavior, stress–strain behavior, and flaw resistance of pressureless-sintered Si₃N₄-BN ceramics are investigated. The results are discussed with respect to the reported thermal shock behavior of these composites. Although the materials behave linear-elastic and exhibit no R -curve behavior, their flaw resistance is different from that of other linear-elastic materials. Whereas the critical thermal shock temperature difference (Δ T _c) is enhanced by adding BN, the content of BN has no influence on the strength loss during severe thermal shocks.     

Fracture Toughness of High-Pressure-Sintered Diamond/Silicon Nitride Composites

Diamond particles were dispersed in silicon nitride, sintered at 6 GPa and 1600°C for 30 min, and heat-treated under vacuum at 1300°C to induce graphitization of the diamond. Improved fracture toughness values up to 7.5 MN/m³¹² were achieved for these composites. Stress-induced microcrack toughening is considered to be a plausible toughening mechanism. Comparisons with diamondlalumina ceramics were made.     

Crack Stability and Its Effect on Fracture Toughness of Hot-Pressed Silicon Nitride Beam Specimens

The effect of stable crack extension on fracture toughness test results was determined using single-edge precracked beam specimens. Crack growth stability was examined theoretically for bars loaded in three-point bending under displacement control. The calculations took into account the stiffness of both the specimen and the loading system. The results indicated that the stiffness of the testing system played a major role in crack growth stability. Accordingly, a test system and specimen dimensions were selected which would result in unstable or stable crack extension during the fracture toughness test, depending on the exact test conditions. Hot-pressed silicon nitride bend bars (NC132) were prepared with precracks of different lengths, resulting in specimens with different stiffnesses. The specimens with the shorter precracks and thus higher stiffness broke without stable crack extension, while those with longer cracks, and lower stiffness, broke after some stable crack extension. The fracture toughness values from the unstable tests were 10% higher than those from the stable tests. This difference, albeit small, is systematic and is not considered to be due to material or specimen-to-specimen variation. It is concluded that instability due to the stiffness of test system and specimen must be minimized to ensure some stable crack extension in a fracture toughness test of brittle materials in order to avoid inflated fracture toughness values.     

Grain Boundary Film Thicknesses in Superplastically Deformed Silicon Nitride

The thickness of intergranular films in polycrystalline β-Si₃N₄ ceramics, both before and after superplastic deformation, has been systematically investigated using high-resolution transmission electron microscopy. In characterizing the film thickness, care was taken to correlate the grain boundary orientation with the direction of the compressive stress applied during the hot-pressing and the superplastic deformation. The film thickness shows a dependence on the intersection angle between the grain boundary and the applied force direction, typically ranging from around a characteristic value for most of the boundaries to zero for a boundary which has an overall short length and is perpendicular to the applied force direction. The film thicknesses in the deformed material, as compared with those before deformation, are marked by a wider distribution and an increased fraction of boundaries free of films, unequivocally demonstrating that during the superplastic deformation the liquid phase is redistributed within short ranges, a process governed by the local stress level as well as kinetic factors. Possible consequences of the liquid-phase redistribution on the deformation behavior are also discussed.     

Fracture Toughness of a Toughened Silicon Nitride by ASTM C 1421

The fracture toughness of a sintered reaction-bonded silicon nitride was measured by the single-edge precracked beam and surface crack in flexure methods, which are two of the three complementary test methods in ASTM C 1421. Results were compared with chevron-notched beam results that were available from another source. Precracks ranged from tiny artificial flaws introduced by Knoop indentation to millimeter-long precracks in single-edge precracked beams. The fracture toughness values from the three methods were in good agreement at 5.6 MPa·m^1/2.     

Microstructural Design of Silicon Nitride with Improved Fracture Toughness: I, Effects of Grain Shape and Size

The use of self-reinforcement by larger elongated grains in silicon nitride ceramics requires judicious control of the microstructure to achieve high steady-state toughness and high fracture strength. With a distinct bimodal distribution of grain diameters, such as that achieved by the addition of 2% rodlike seeds, the fracture resistance rapidly rises with crack extension to steady-state values of up to 10 MPam^1/2 and is accompanied by fracture strengths in excess of 1 GPa. When the generation of elongated reinforcing grains is not regulated, a broad grain diameter distribution is typically generated. While some toughening is achieved, both the plateau (steady-state) toughness and the R -curve response suffer, and the fracture strength undergoes a substantial reduction. Unreinforced equiaxed silicon nitride exhibits the least R -curve response with a steady-state toughness of only 3.5 MPam^1/2 coupled with a reduced fracture strength.     

Fracture Toughness of a Silicon Nitride/Silicon Carbide Nanocomposite at 1350°C

The fracture toughness of a hot-pressed silicon nitride/silicon carbide (Si₃N₄/SiC) nanocomposite and reference monolithic Si₃N₄ has been investigated in four-point bending at 1350°C in air, using different loading rates (0.01-1 mm/min). Single-edge V-notched bend specimens that were prepared by polishing the notch tip to a radius of <10 µm, using 1 µm diamond paste, were used for the fracture toughness measurement. Slow crack growth (SCG) prior to catastrophic failure was detected at all applied loading rates at 1350°C. The fracture toughness at 1350°C, as calculated using the actual crack size measured on the fracture surface after the bend test, increased in both ceramics with decreasing loading rate and increasing area of the SCG region.     

Effect of Grain Growth of β-Silicon Nitride on Strength, Weibull Modulus, and Fracture Toughness

β-Si₃N₄ powder containing 1 mol% of equimolar Y₂O₃–Nd₂O₃ was gas-pressure sintered at 2000°C for 2 h (SN2), 4 h (SN4), and 8 h (SN8) in 30-MPa nitrogen gas. These materials had a microstructure of " in-situ composites" as a result of exaggerated grain growth of some β Si₃N₄ grains during firing. Growth of elongated grains was controlled by the sintering time, so that the desired microstructures were obtained. SN2 had a Weibull modulus as high as 53 because of the uniform size and spatial distribution of its large grains. SN4 had a fracture toughness of 10.3 MPa-m^1/2 because of toughening provided by the bridging of elongated grains, whereas SN8 showed a lower fracture toughness, possibly caused by extensive microcracking resulting from excessively large grains. Gas-pressure sintering of β-Si₃N₄ powder was shown to be effective in fostering selective grain growth for obtaining the desired composite microstructure.     

Effect of Grain Contiguity on the Thermal Diffusivity of Aluminum Nitride

Thermal diffusivity of AlN-based ceramics was studied as a function of second-phase amount and heat-treatment time. The Y₂O₃·Al₂O₃ contents varied over the range of 13-31 vol%. The thermal diffusivity decreased as the amount of second phase increased. After sintering at 1850°C, the AlN ceramics consisted of rounded, largely isolated grains. Heat treatment of these samples for 5-50 h at 1800°C resulted in microstructures that consisted of largely contiguous AlN grains. There was a substantial increase in the thermal diffusivity after the heat-treatment step, and the incremental improvement was essentially constant for the three compositions that have been studied. The amount of second phase was unchanged during heat treatment; therefore, the increase in thermal diffusivity is assumed to be a direct result of the enhanced contiguity of AlN grains.     

Relationship between Microstructure, Toughening Mechanisms, and Fracture Toughness of Reinforced Silicon Nitride Ceramics

Different microstructures in Si₃N₄ ceramics containing Y₂O₃and Al₂O₃ as sintering additives were prepared by two-step sintering. Pull-out and elastic bridging were most frequently observed as the toughening mechanisms in samples with fine-grained microstructures having needlelike β-Si₃N₄grains with diameters of <1 μm. Crack deflection was the main toughening mechanism observed in samples with coarse-grained microstructures having grains with diameters of >1 μm. The values of fracture toughness were varied from 6.1 to 8.2 MPa·m^1/2 with respect to the microstructural characteristics, characterized by the volume fraction of needlelike grains and their diameter.     

Short-Crack Fracture Toughness of Silicon Carbide

The fracture toughness of four different silicon carbides was measured using single-edge precracked beam (SEPB) and indentation/strength techniques. Two were development grades with similar microstructures and chemistries, and yet exhibited different fracture modes. The grade that exhibited a predominantly intergranular fracture had an SEPB fracture toughness (6.4 MPa√m) 88% higher than the one that showed primarily a transgranular fracture (3.4 MPa√m). The higher fracture toughness was associated with a modest increase in average strength (25%), although there was a significant increase in the Weibull modulus (11–32). Fracture toughness at short crack lengths was assessed by an indentation method that used fracture strengths, crack lengths at fracture, and a new method of estimating the constant δ that characterizes the residual driving force of the plastic zones based on the stable growth of the indentation cracks from the initial ( c ₀) to the instability ( c ^*) lengths. The results showed a rising crack-growth-resistance behavior for the grade exhibiting intergranular fracture, while the grade showing transgranular fracture had a flat crack-growth resistance. Tests on two commercial grades of silicon carbide showed similar behaviors associated with the respective fracture modes.     

Short-Crack Toughness and Abrasive Machining of Silicon Nitride

Hardness and toughness are often used to analyze the abrasive machining behavior of ceramic materials. However, toughness values of silicon nitride ceramics with microstructures containing elongated grains increase with crack extension. The present study investigates the effect of toughness on the process of abrasive machining to determine which value of toughness should be used in the analysis. The toughness curves (i.e., toughness as a function of crack length) of ten different silicon nitride materials are characterized by an indentation-strength technique and an indentation technique. The forces in surface grinding are measured as a function of the depth of cut. Examination of ground surfaces by scanning electron microscopy indicates that the material-removal processes in grinding follows the formation of short cracks (i.e., microcracks) and grain-scale material dislodgement. An indentation fracture model for material removal in abrasive machining is used to correlate the grinding forces with toughness and hardness of the materials. An agreement is obtained between the experimental results and the indentation model only when the toughness associated with short cracks is used. This study shows the importance of using appropriate toughness values corresponding to the microfracture processes in analyzing abrasive machining results for materials possessing rising toughness curves.     

Effect of Silicon Dioxide on the Thermal Diffusivity of Aluminum Nitride Ceramics

The thermal diffusivity of AlN ceramics was significantly decreased by the addition of SiO₂. The AlN ceramics with 4 wt% SiO₂ could not be densified by pressureless sintering in the temperature range 1400° to 1800°C. The thermal diffusivity of these samples was very low because of their porous structure. The AlN ceramics containing 2, 4, and 8 wt% SiO₂ were densified by hot-pressing and also had low thermal diffusivity. In these samples, the grains of the 27R polytype that resulted from the reaction between AlN and SiO₂ were dispersed, obstructing the conduction of heat. The relation between the amount of 27R polytype and the thermal diffusivity of the AlN ceramics was determined.     

缺陷对氮化硅导热性能影响的模拟研究

通过反应或热压烧结制备氮化硅器件过程中,产生的晶格空位和杂质氧等缺陷会严重影响氮化硅材料的导热性能。为了探究空位和氧杂质对氮化硅材料导热性能的影响规律,利用分子动力学模拟方法设计了多种不同缺陷状态的氮化硅模型,分析了空位/氧杂质的比例、分布状态、晶格位置以及温度对氮化硅材料导热性能的影响。研究结果表明:随着空位/氧杂质比例的增加以及温度的升高,氮化硅体系的热导率都呈明显的下降趋势;当空位/氧杂质由原本随机分布逐渐向导热通路中间聚集时,氮化硅的热导率急剧降低;空位/氧杂质所处不同晶格位置,体系热导率有明显差异。另外,通过计算氮化硅模型的声子态密度,进一步验证了空位/氧杂质比例以及温度对体系导热性能的影响规律。研究结果为制备具有高导热性的氮化硅陶瓷提供了重要的指导。