Formation of Tough Composite Joints

Joints that exhibited tough fracture behavior were formed in a Si/SiC matrix reinforced with Textron SCS-6 fibers with either boron nitride or silicon nitride fiber coatings. Lapped joints (joints with overlapping 'fingers') were necessary to obtain tough behavior. Geometrical requirements necessary to avoid brittle joint failure were proposed. Joints with a simple overlap geometry (only a few fingers) had to be very long in order to prevent brittle failure. Joints with an optimized stepped sawtooth geometry produced composite-like failures with the stress/strain curves containing an elastic region followed by a region of rising stress with an increase of strain. Increasing the fiber/matrix interfacial strength, by changing the fiber coating, significantly increased matrix cracking and ultimate strength of the joints. The best joints had matrix cracking stress and ultimate strength of 138 and 240 MPa, respectively. Joint failure was preceded by multiple matrix cracking in the entire composite. The high strength of the joints should permit building of structures containing joints with only a minor reduction of design stresses.     

静载多点压痕对氮化硅陶瓷强度的影响

本文在对XJM－1型磨片机进行改装的基础上研究了静载多点压痕对氮化硅陶瓷强度的影响。实验发现：与原始强度相比，静载多点压痕后的氮化硅强度有所降低；强度与多点压痕荷载之间的关系曲线出现一极大值。分析后表明：表面残余应力与裂纹尺寸是影响陶瓷材料强度的两个主要因素，它们的变化将对陶瓷材料强度产生直接影响。     

Structural Reliability of Yttria-Doped Hot-Pressed Silicon Nitride at Elevated Temperatures

The strength of yttria-doped hot-pressed silicon nitride was investigated as a function of temperature, time, and applied load. Data collected at 1200°C are presented in the form of a strength-degradation diagram for an applied stress of 350 MPa. At this temperature, the behavior of yttria-doped hot-pressed silicon nitride is found to be superior to that of magnesia-doped hot-pressed silicon nitride, in which creep results in the formation of microcracks that lead to strength degradation. By contrast, the yttria-doped material does not suffer from microcrack formation or strength degradation at 1200°C. Strength degradation does occur at higher temperatures and, as a consequence, an upper limit of 1200°C is recommended for yttria-doped hot-pressed silicon nitride in structural applications.     

Excellent corrosion protection performance of epoxy composite coatings filled with silane functionalized silicon nitride

Silicon nitride was firstly used as anticorrosive pigment in organic coatings. An effective strategy by combining inorganic fillers and organosilanes was used to enhance the dispersibility of silicon nitride in epoxy resin. The formed nanocomposites were applied to protect Q235 carbon steel from corrosion. The anticorrosive performance of modified silicon nitride with silane (KH-570) was investigated by electrochemical impedance spectroscopy (EIS), water absorption and pull-off adhesion methods. With the increase of immersion time, the corrosion resistance as well as adhesion strength of epoxy resin coating and unmodified silicon nitride coating decreased significantly. However, for the modified silicon nitride coating, the corrosion resistance and adhesion strength still maintained 5.7×10¹⁰ Ω cm² and 7.6 MPa after 2400-h and 1200-h immersion, respectively. The excellent corrosion resistance performance could be attributed to the chemical interactions between KH-570 functional groups and silicon nitride powders, which mainly came from the easy formation of Si-O-Si bonds. Furthermore, the modified silicon nitride coating formed a strong barrier to corrosive electrolyte due to the hydrophobic of modified silicon nitride powder and increased bonds.     

Assessment of Strength by Young's Modulus and Porosity: A Critical Evaluation

Literature data on strength, porosity, and Young's modulus at room temperature of reaction-bonded silicon nitride, sintered silicon nitride, and hot-pressed silicon nitride have been fitted into available and proposed strength-porosity relationships. In general, the Lewis method of iterative least-squares fitting in these relationships has been found to be better than conventional linearized least-squares fitting. Further a semiempirically proposed strength–Young's modulus relationship has been found to predict strength more precisely than the conventional strength-porosity relationship.     

High performance porous Si3N4 ceramics prepared by coated pore-forming agent method

Coated pore-forming agent method (CPFAM) was introduced to improve the pore-forming agent method (PFAM) for the preparation of porous silicon nitride ceramics. Using SEM in combination with measurements of porosity and flexural strength, it has been found that the flexural strength of the porous silicon nitride ceramics produced with the CPFAM method is significantly higher than those without the coating process: a 100% increase in flexural strength for samples with a porosity of 50%. The porous silicon nitride ceramics also have a very low dielectric constant, which is ideal for applications in wave-transmitting systems. The enhanced mechanical strength of the silicon nitride made by the CPFAM method is a result of a more uniform distribution of the spherical pores and the formation of a dense layer of rod-like microstructures near the surface of the pores.     

Surface strength of balls made of five structural ceramic materials evaluated with the Notched Ball Test (NBT)

In high performance hybrid bearings the balls are conventionally made of silicon nitride ceramics. There are some disadvantages such as costs or the higher stiffness of silicon nitride compared to steel. Therefore, alternative materials are under investigation. The surface strength is one of the most important criteria for the qualification of the spherical components in the application. It has to be evaluated for each new material (or new surface finish).The recently standardised Notched Ball Test (NBT) enables one to determine the surface strength (tensile strength) of balls, which is strongly influenced by the surface finish and volume flaw populations. In this paper the NBT strength of five candidate materials for rolling elements (silicon carbide, silicon nitride, alumina, zirconia and zirconia toughened alumina) is investigated. Fractography is performed to evaluate the direct correlation between the defects found at the surface and the measured strength.     

烧结助剂对多孔氮化硅陶瓷的力学性能及介电性能的影响

通过添加烧结助剂,采用常压烧结工艺制备出不同气孔率(19%～54%)的氮化硅陶瓷.采用Archimedes法、三点弯曲法和Vickers硬度测试法测量了材料的密度、气孔率、抗弯强度及硬度.用X射线衍射及扫描电镜检测了相组成和显微结构.用谐振腔法测试了氮化硅陶瓷在10.2 GHz的介电特性.结果表明:材料具有优良的介电性能.随着烧结助剂的减少,样品中气孔率增加,力学性能有所下降,介电常数和介电损耗降低.添加Lu2O3所制备的氮化硅陶瓷的力学性能和介电性能优于添加Eu2O3或Y2O3制备的氮化硅陶瓷.当气孔率高于50%时,多孔氮化硅陶瓷(添加入5%的Y2O3或Lu2O3,或Eu2O3,质量分数)的抗弯强度可达170 MPa,介电常数为3.0～3.2,介电损耗为0.000 6～0.002.     

氮化硅陶瓷的制备及性能研究进展

氮化硅陶瓷是一种具有广阔发展前景的高温、高强度结构陶瓷,它具有强度高、抗热震稳定性好、疲劳韧性高、室温抗弯强度高、耐磨、抗氧化、耐腐蚀性能好等高性能,已被广泛应用于各行业。本文介绍了氮化硅陶瓷的基本性质．综述了氮化硅陶瓷的制备工艺和提高其高温性能的方法以及增韧的途径,并展望了氮化硅陶瓷的发展前景。     

Hierarchical Structure of Porous Silicon Nitride Ceramics with Aligned Pore Channels Prepared by Ice‐Templating and Nitridation of Silicon Powder

A unique hierarchical porous structure of silicon nitride ceramic with 76.5% porosity is fabricated by combining an ice‐templating method and nitridation for a silicon powder. The porous silicon nitride ceramics were composed of a lamellar structure with aligned pore channels and ceramic walls filled with fibrous whiskers. This study is focused on the influences of freezing rate on the microstructures and properties of the silicon nitride ceramics. The properties were characterized by compressive strength and gas permeability, which were shown to vary with controlled microstructure. The compressive strength and the permeability reached up to 32.2 MPa and 0.035^?12 m², respectively.     

Evaluation of Mechanical Stability of a Commercial Sn88 Silicon Nitride at Intermediate Temperatures

Dynamic fatigue and stress rupture tests in four-point bending were conducted on a commercially available SN88 silicon nitride ceramic at temperatures in the range 700°–1000°C in air. The objective of the present study was to elucidate the failure of SN88 silicon nitride ceramic nozzles arising from a critical crack initiated at the intermediate temperature airfoil region during an engine field test. Results of dynamic fatigue tests indicated that SN88 silicon nitride tested at a stressing rate of 30 MPa/s exhibited little change in characteristic strength at the various test temperatures. However, SN88 silicon nitride exhibited a significant degradation in mechanical strength when tested at 0.003 MPa/s at temperatures indicative of a great susceptibility to slow crack growth, especially at 850°C. SEM and XRD analyses indicated that the mechanical instability of SN88 silicon nitride at intermediate temperatures resulted from the transformation of secondary phase(s) from oxidation. These phase transformations were accompanied by a large volume change, which led to the generation of large local residual tensile stresses. As a result, extensive damage zones were formed, which led to a substantial degradation of mechanical strength and reliability. Microstructural examination of failed SN88 airfoils indicated that a similar damage zone was formed in the regions exposed to intermediate temperatures during engine testing. Consequently, the ultimate failure of these vanes was attributed to the loss in mechanical strength from the damage zone formation.     

High-Temperature Strength of Sinter-Forged Silicon Nitride with Lutetia Additive

A sinter-forging technique was successfully applied to fabricate a silicon nitride with a lutetia (Lu₂O₃) additive. The sinter-forged specimen had a strongly anisotropic microstructure where rodlike silicon nitride grains preferentially aligned perpendicular to the forging direction. The specimen exhibited superior strength of ∼700 MPa at 1500°C. This strength was highest when compared with previous silicon nitrides at temperatures >1400°C. Such superior high-temperature strength was attributed to grain alignment as well as to the refractory grain-boundary glassy phase and the existence of glass-free grain boundaries.     

Fabrication and Characteristic of Nextel 720 Fiber‐Reinforced Silicon Nitride Matrix Composites by Chemical Vapor Infiltration Process

Most current processes for fiber‐reinforced silicon nitride composites are conducted at very high temperature, which is not possible to use oxide fiber as reinforcement. Here, low‐temperature process of chemical vapor infiltration (CVI) was utilized to fabricate Nextel 720 oxide fiber tow‐reinforced silicon nitride matrix composite with PyC as interphase. The tensile strength was analyzed by Weibull distribution. The microstructure showed that there were two types of interface bonding. The strong interface bonding determined the unexpected low strength of the composites. This indicated that the suitable interface design is the urgent issue for oxide fiber‐reinforced silicon nitride composite by CVI.     

Fabrication and properties of in situ silicon nitride nanowires reinforced porous silicon nitride (SNNWs/SN) composites

The in situ silicon nitride nanowires reinforced porous silicon nitride (SNNWs/SN) composites were fabricated via gelcasting followed by pressureless sintering. SNNWs were well distributed in the porous silicon nitride matrix. The tip-body appearance suggested a VLS growth mechanism. The flexural strength and elastic modulus of the prepared composites can achieve 84.3?±?3.9?MPa and 23.3?±?2.0?GPa respectively (25?°C), while the corresponding porosity was 40.7?vol.%. Remarkably, the strength retention rate of the composites at 1400?°C was up to 66.1%. This is due to the excellent thermal stability of SNNWs and silicon nitride matrix. Also, the fracture toughness of the composites was improved to ～42% larger than pure porous silicon nitride ceramics because of the bridging effect of the NWs and the interlocking effect of β-Si₃N₄ crystals. In addition, a good thermal shock resistance and dielectric properties were indicated. The good overall performance made SNNWs/SN composites promising candidate for advanced high-temperature applications.     

Effect of Powder Surface Modifications on the Properties of Silicon Nitride Ceramics

The effect of surface oxygen concentration of silicon nitride powders on the properties of resulting ceramics was studied. A high-purity silicon nitride powder was treated physically and chemically to modify its surface oxygen content. The resulting powders were hot-pressed into dense ceramics using 6 wt% yttria as a sintering aid. Strength and oxidation resistance of these ceramics were measured and correlated with the powder and ceramic compositions as well as the resulting intergranular phases. Results show that the phases developed in yttria-containing silicon nitride ceramics vary with slight changes in the initial powder oxygen content, as predicted, and that strength can be correlated to initial oxygen concentration. The mechanical strength vs oxygen content curve has a definite maximum; i.e., there is a small oxygen concentration range at which optimum ceramic strength is realized. Best results are obtained when the oxygen content is increased by thermal oxidation; other techniques such as chemical oxidation or addition of silica are not as effective, particularly in attaining high strength at elevated temperatures.     

Features of adhesive technology for silicon nitride ceramic components

A method is provided for joining (gluing) individual silicon nitride components used in the preparation of structural objects of different types of silicon nitride ceramic with a broad range of porosity (from zero to ~23%). The method includes preparation of an adhesive mixture based on silicon nitride, successive application of the mixture to component surfaces being joined, and firing of the joined object at 1000°C with exposure for 2 h. The glued joint is distinguished by high adhesive strength, which makes it possible to prepare objects of complex structure by this method.     

High-Temperature Environmental Strength Degradation of a Hot-Pressed Silicon Nitride: An Experimental Test

High-temperature environmental strength degradation of hot-pressed silicon nitride ceramics is postulated to occur as a consequence of the properties of the noncrystalline inter-granular phase being altered by cation diffusion from the environment. The model proposed is tested by comparing the strength before and after prolonged high-temperature exposures to a calcium-rich magnesium silicate. Two high-temperature degradation regimes are identified, one in which the intergranular phase alone is affected, and the other, at still higher temperatures, where actual corrosion of the silicon nitride grains occurs.     

Diffusion Bonding of Silicon Nitride Using a Superplastic β-SiAlON Interlayer

A superplastic β-SiAlON was used as an interlayer to diffusionally bond a hot-pressed silicon nitride to itself. The bonding was conducted in a graphite furnace under a constant uniaxial load of 5 MPa at temperatures varying from 1500° to 1650°C for 2 h, followed by annealing at temperatures in the range of 1600° to 1750^oC for 2 h. The bonds were evaluated using the four-point-bend method at both room temperature and high temperatures. The results indicate that strong, void-free joints can be produced with the superplastic β-SiAlON interlayer, with bond strengths ranging from 438 to 682 MPa, and that the Si₃N₄ joints are heat resistant, being able to retain their strength up to 1000°C (635 MPa), and therefore have potential for high-temperature applications.     

X-ray Diffraction Study of the Structure of Silicon Nitride Fiber Made from Perhydropolysilazane

Continuous stoichiometric silicon nitride fiber was produced by the pyrolysis of perhydropolysilazane. This high-purity silicon nitride fiber is colorless and has high strength, modulus of elasticity, and thermal stability which are properties suitable for reinforcing plastics, metals, glasses, and even ceramics. The structures of three kinds of amorphous silicon nitride fibers (with stoichiometric, Si-excess and O-excess composition) were investigated by X-ray diffraction followed by calculating the radial distribution functions. Radial distribution functions were calculated from several possible crystal structures and compared with observed radial distribution functions.     

Mechanical reliability evaluation of silicon nitride ceramic components after exposure in industrial gas turbines

Several studies have recently been undertaken to examine the mechanical reliability and thermal stability of silicon nitride ceramic components that are currently being considered for structural application in industrial gas turbines. Specifically, ceramic components evaluated included a bow-shaped silicon nitride nozzle evaluated in an engine test rig, silicon nitride vanes exposed in an engine field test, and an air-cooled silicon nitride vane that is currently under development. Despite the differences in field test conditions all of the exposed silicon nitride ceramic components exhibited a significant material recession arising from the oxidation of silicon nitride and subsequent volatilization of the oxide (i.e., silica). The fracture strength of exposed airfoils was also decreased due to the formation of a subsurface damage zone induced by the turbine environments. In addition, studies indicated that the properties of as-processed ceramic components, especially in airfoil regions, were not always comparable to those generated from the standard specimens with machined surface extracted from production billets. The component characterization efforts provided an important insight into the effect of gas turbine environments on the material recession and mechanical reliability of materials as functions of exposure time and conditions, which were very difficult to obtain from a laboratory scale test.