氮化硼纳米管增强氮化硅复合材料的裂纹扩展阻力行为

用氮化硼纳米管(BNNT)增强氮化硅(Si₃N₄)陶瓷制备了BNNT/Si₃N₄复合材料, 利用三点弯曲强度及单边切口梁(SENB)法测定了BNNT/Si₃N₄复合材料的弯曲强度和断裂韧性。通过SEM观察了BNNT/Si₃N₄复合材料微观形貌。基于BNNT增强Si₃N₄陶瓷复合材料的裂纹扩展阻力计算公式, 构建了BNNT对Si₃N₄陶瓷裂纹屏蔽区的裂纹扩展阻力的数学模型。用该模型的计算结果与Si₃N₄陶瓷的裂纹扩展阻力进行了对比。结果表明: BNNT/Si₃N₄复合材料的弯曲强度和断裂韧性明显高于Si₃N₄陶瓷, 说明BNNT对Si₃N₄陶瓷的裂纹扩展有阻力作用, 摩擦拔出是Si₃N₄陶瓷抗裂纹扩展能力提高的主要原因; BNNT对Si₃N₄陶瓷有明显的升值阻力曲线行为。通过有限元模拟裂纹尖端应力分布, 发现BNNT使Si₃N₄陶瓷裂纹尖端的最大应力转移到纳米管上, 而且BNNT降低了Si₃N₄陶瓷裂纹尖端的应力, 对Si₃N₄陶瓷尖端的裂纹有屏蔽作用, 从而提高了Si₃N₄陶瓷的裂纹扩展阻力。     

An investigation into a multilayered BN/Si3N4/BN interfacial coating

In order to prevent environmental degradation of the interface, a triplex coating was employed as the interface in ceramic matrix composites (CMC). This interface consists of an initial BN layer followed by a Si₃N₄ layer and lastly another BN layer. Single strand unidirectional mini-composites using BN/Si₃N₄/BN coated ceramic grade Nicalon? fibers as the reinforcement and chemical vapor infiltrated (CVI) SiC as the matrix were fabricated to understand the initial properties of the interfacial coating. Field emission scanning electron microscopy (FE-SEM) confirmed the thickness of the triplex coating before and after mini-composite fabrication. FE-SEM micrographs after mechanical and environmental testing of the single strand unidirectional mini-composites showed the consequences of using the triplex interfacial coating. Finally, eight ply continuous fiber reinforced (CFR) CMCs with the BN/Si₃N₄/BN triplex interface and the traditional BN/Si₃N₄ duplex interface were fabricated using the polymer impregnation and pyrolysis (PIP) process. The PIP process has gained popularity in recent years and this allows for the fabrication of larger CMC panels as compared with the CVI process. Mechanical testing for the PIP-fabricated CFR-CMC panels showed that the composites using the triplex interface had better mechanical properties than those fabricated with a BN/Si₃N₄ duplex interface after environmental testing.     

烧结助剂对Si3N4/BN层状复合陶瓷结构与性能的影响

研究了MgO-Y₂O₃-Al₂O₃体系(相应的层状复合陶瓷试样记为A)、Y₂O₃-Al₂O₃体系(相应的层状复合陶瓷试样记为B)及La₂O₃-Y₂O₃-Al₂O₃体系(相应的层状复合陶瓷试样记为C)烧结助剂对Si₃N₄/BN层状复合陶瓷结构与性能的影响.研究表明:在相同的烧结工艺下,试样A、B、C的抗弯强度分别为700、630、610MPa,断裂功分别为2100、1600、3100J/m².试样A、B以脆性断裂为主,裂纹偏转现象不明显,而试样C的载荷-位移曲线显示了明显的“伪塑性”特征,裂纹的偏转与扩展现象明显.试样A中Si₃N₄晶粒大小不均且长径比较小,而试样C中长柱状Si₃N₄晶粒发育完善,有较大的长径比.     

ICVI法制备Si3N4P/ Si3N4 复合材料致密化行为数值模拟

根据Si₃N₄ 颗粒增强体的结构特点及等温化学气相法( ICVI) 的工艺特点, 对Si₃N₄ 颗粒增强Si₃N₄ 复合材料的致密化过程进行了数值模拟。用球形孔隙模型表征Si₃N₄ 颗粒增强体的结构特征, 用传质连续方程表征先驱体在预制体中的浓度分布。为了检验模型的准确性和适用性, 进行了相应的实验验证。模拟结果与实验结果具有相似的致密化规律, 预测的渗透时间和孔隙率与实验结果均十分接近, 表明本文中建立的数学模型可以较好地表征Si₃N₄P / Si₃N₄ 复合材料的ICVI 过程。     

Texture development in Si3N4/BN fibrous monolithic ceramics

Preferred orientation was measured in Si₃N₄/BN fibrous monolithic ceramics using x-ray diffraction. The materials were manufactured by co-extrusion of polymer binder/ceramic blends which were subsequently pyrolized and then hot-pressed to produced a fully dense ceramic composite. A very strong modified wire texture was present in the BN with the basal planes aligned parallel to the axis of extrusion due to shear-induced reorientation of the platelet-shaped BN particles during co-extrusion. Texture was also observed in the Si₃N₄ and was attributed to a combination of co-extrusion and hot-pressing. After hot pressing, the basal planes of the rod-shaped -Si₃N₄ were observed to be preferentially aligned perpendicular to the extrusion direction. Measurements prior to hot-pressing revealed that a small amount (5%) of -Si₃N₄ was present in the -Si₃N₄ starting powder. Although texturing of the predominant -Si₃N₄ did not occur during co-extrusion, significant texturing of the -Si₃N₄ was observed. During subsequent hot-pressing, the pre-existing textured -Si₃N₄ particles appeared to act as seeds for transformation and preferred growth of rod-shaped grains parallel to the axis of extrusion.     

Si3N4/BN纤维独石陶瓷阻力曲线的研究

通过压痕小裂纹直接测量法获得Si3N4/BN纤维独石陶瓷的阻力曲线,采用指数经验公式拟合了实验数据,对纤维独石陶瓷阻力曲线具有的独特的阶梯状进行分析,并对纤维独石陶瓷具有高韧性的机理作了研究。     

无压浸渗制备梯度Si3N4/Al复合材料

采用Al-Mg合金无压渗入具有梯度孔隙分布的Si3N4多孔预制体,制得大尺寸、梯度Si3N4/Al复合材料;对复合材料的显微组织,相组成,硬度进行了观察和测定,分析了层间铝合金薄层在释放梯度层间应力的作用,并采用SHPB装置对梯度复合材料进行动态压缩试验.试验结果表明梯度复合材料层间结合紧密,硬度从HRA80.5逐层过渡到HRA61.5,主要组成相为Al,Si3N4,AlN和Mg2Si;梯度复合材料在动态压缩过程中表现出较高韧性.     

原位引入BN-SiC燃烧合成Si3N4-BN-SiC复合材料

Si₃N₄-BN-SiC复合材料以其良好的力学性能和抗氧化性能而具有良好的工程应用前景。本研究以Si、Si₃N₄稀释剂、B₄C和Y₂O₃为原料, 采用燃烧合成法成功制备了Si₃N₄-BN-SiC复合材料。通过Si、B₄C和N₂气之间的反应, 在Si₃N₄陶瓷中原位引入BN和SiC, 制备的Si₃N₄-BN-SiC复合材料由长棒状的β-Si₃N₄和空心球形复合材料组成。实验研究了空心球微结构的形成机理, 结果表明, 生成的SiC、BN颗粒及玻璃相覆盖在原料颗粒上, 当原料颗粒反应完全时, 形成空心球形微结构。并进一步研究了B₄C含量对Si₃N₄-BN-SiC复合材料力学性能的影响。原位引入SiC和BN在一定程度上可以提高复合材料的力学性能。当B₄C添加量为质量分数0~20%时, 获得了抗弯强度为28~144 MPa、断裂韧性为0.6~2.3 MPa·m ^1/2, 杨氏模量为17.4~54.5 GPa, 孔隙率为37.7%~51.8%的Si₃N₄-BN-SiC复合材料。     

Microstructure and infiltration kinetics of Si3N4/Al–Mg composites fabricated by pressureless infiltration

Si₃N₄/ Al–Mg composites reinforced by ceramic interpenetrating network structure had been fabricated via pressureless infiltration technology. The matrix and the reinforcement phase, form an interconnected interpenetrating network structure. The Al–Mg/Si₃N₄ system exhibits an excellent wettability under moderate conditions. The increasing of Mg content (2–10 wt%) resulted in an increased amount of infiltration, once Mg content beyond 10 wt% has an adverse effect. Light chemical reaction occurs in the interface of Al–Mg/Si₃N₄ system and the reaction productions reduce the surface tension of melt and impulse the advance of infiltration. Infiltration temperature and infiltration time were the key parameters, which turn into the infiltration impetus. The appropriate infiltration temperature is 1050 °C and the corresponding infiltration time is 15 min, prolonging the infiltration time continuously has no significance.     

Field nanoemitters: ultrathin BN nanosheets protruding from Si3N4 nanowires

Field emitters in nanoscale are important in micro/nanoelectronic devices. Here, we report a large scale synthesis and effective field emission of field nanoemitters. The integrated nanostructures of ultrathin BN nanosheets aligned on Si3N4 nanowires are prepared through a two-stage process. Si3N4 nanowires were previously synthesized through heating Si powder at 1500 degrees C under a N2 atmosphere. Ultrathin BN nanosheets were then deposited on Si3N4 nanowires by heating a homemade B-N-O precursor under a N2/NH3 atmosphere. The as-prepared nanofilaments act as cold electron emitters displaying excellent field emission performance owing to the untrathin and sharp edges of the protruding BN nanosheets.     

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.     

Mechanical properties of Si3N4/BN fibrous monolithic ceramics at elevated-temperature

The mechanical properties at high temperature of Si₃N₄/BN fibrous monolithic ceramics were tested. The flexural strength of SiC whisker reinforced Si₃N₄/BN fibrous monolithic ceramics from 25°C to 1200°C were investigated. The strength degraded slowly from 1000°C to 1200°C which was different to Si₃N₄ monolithic ceramics. The creep behaviors of the material at different temperatures were characterized. Si₃N₄/BN fibrous monolithic ceramics possess high creep resistance. The chemical composition and microstructure of the composites were analyzed by XRD and SEM.     

Super-lyophobicity of porous Si3N4/BN ceramics with nanopores and nanowires by molten copper

Porous Si₃N₄/BN ceramics (PSBC) with a microstructure containing nanopores and nanowires were prepared by reaction bonding of silicon nitride (RBSN) technique. The phase composition and microstructure of PSBC were characterized by X-ray diffractometry (XRD) and field emission scanning electronic microscope (FE-SEM). The porosity of PSBC was 52.6%, the pore size was in the range of 60 to 300 nm. The wettability of PSBC by molten Cu at 1300 °C was investigated by the sessile drop method. The ceramics exhibit super-lyophobicity by molten Cu. The nanopores and nanowires embodied in PSBC increased the heterogeneity and surface roughness, resulting in the super-lyophobicity of the ceramics by molten Cu.     

放电等离子快速烧结SiC晶须增强Si3N4BN层状复合材料

采用放电等离子烧结技术(SPS)快速烧结了SiC晶须增强的Si₃N₄/BN层状复合材料.利用SPS技术,在烧结温度为1650℃、保温15min的条件下,材料的密度可达3.18g/cm³,抗弯强度高达600MPa,断裂功达到3500J/m².研究表明:特殊的层状结构、SiC晶须的拔出与折断是材料断裂功提高的主要原因.X射线衍射及扫描电子显微镜研究表明:α-Si₃N₄已经在短短的烧结过程中全部转变成长柱状的β-Si₃N₄,并且长柱状的β-Si₃N₄和SiC晶须具有明显的织构.     

Sintering process of Y2O3-added Si3N4

The sintering process of Y₂O₃-added Si₃N₄ has been investigated by dilatometry and microstructural observations. Densification was promoted above 1440 ° C by the formation of eutectic melts in the Y₂O₃-SiO₂-Si₃N₄ triangle. However, the dilatometric curves indicated no shrinkage corresponding to the rearrangement process, despite liquid-phase sintering. The kinetic order for The Initial-stage sintering was 0.47 to 0.49. These values indicated that the phase-boundary reaction was rate controlling. The apparent activation energy (323 kJ mol^–1) was smaller than the dissociation energy for the Si-N bond (435 kJ mol^–1). ESR data and lattice strain indicated that the disordered crystalline structure of the Si₃N₄ starting powder promoted the reaction of Si₃N₄ with eutectic melts. After a period of initial-stage sintering, the formation of fibrous -Si₃N₄ grains resulted in interlocked structures to interrupt the densification.     

Development of microstructure during the fabrication of Si3N4 by nitridation and pressureless sintering of Si:Si3N4 compacts

The technique for the fabrication of Si₃N₄ which was investigated involves the nitridation of Si:Si₃N₄ powder compacts containing additions of sintering aids (e.g. Y₂O₃ and Al₂O₃) followed by pressureless sintering. The development of microstructure during fabrication by this method has been followed by X-ray diffraction and analytical electron microscopy. As well as being important for the sintering process, it was found that the sintering aids promote nitridation through reaction with the surface silica on the powder particles. During nitridation extremely fine grained Si₃N₄ forms at silicon powder particle surfaces and at tunnel walls extending into the interior of these powder particles. Secondary crystalline phases which form during nitridation are eliminated from the microstructure during sintering. The- to-Si₃N₄ phase transformation is completed early in the sintering process, but despite this the fully sintered product contains fine-Si₃N₄ grains. The grains are surrounded by a thin intergranular amorphous film.