Fabrication of SiC whisker reinforced Al2O3 composites

It is reported that SiC whiskers and alumina powder can be mixed in water medium when the whiskers are flocculated and the powder deflocculated, and that the composite slip can be cast to high green density. However, sintering of the composite to fully dense material was found to be difficult. The reasons were the formation of whisker networks and the development of the differential sintering stresses in the matrix around the whiskers. Hot pressing was subsequently employed, and the use of the computerized dilatometer allowed the establishment of a quantitative relationship of the densification rate with pressure, temperature and SiC whisker content. The present results help provide a useful basis for the effective design, development and fabrication of the whisker-reinforced ceramic composite.     

Interfacial structure of Si3N4 whisker reinforced 7064 aluminium composite

Abstracts are not published in this journal This revised version was published online in November 2006 with corrections to the Cover Date.     

Influence of whisker toughening and microstructure on the wear behavior of Si3N4- and Al2O3-matrix composites reinforced with SiC

A comparative study of the influence of randomly-oriented SiC whiskers on the abrasive wear behavior of several commercially-produced Si₃N₄- and Al₂O₃-based ceramics suggested that the residual stress states present within the materials can be important in predicting their wear resistance. The addition of SiC whiskers to the Si₃N₄ matrix created residual tensile stresses at the whisker-matrix interfaces which led to enhanced bulk fracture toughness, but which degraded the fracture toughness at the microstructural level, and thus the abrasive wear resistance, by promoting easier whisker debonding and removal by the abrasive particles. The addition of SiC whiskers to an alumina matrix, on the other hand, led to the creation of residual compressive stresses at whisker-matrix interfaces, producing a locally tougher interface that was more able to withstand the rigors of the abrasive wear environment. These results indicate that in brittle materials, improved bulk mechanical properties do not always translate directly to improved performance in a tribological environment.     

Quantitative determination of the stability of SiC whisker in reaction-bonded/hot-pressed Si3N4 composites by X-ray diffraction

A method was developed for the quantitative determination of weight fractions of the phases in SiC whisker-reinforced reaction-bonded Si₃N₄ composites using X-ray diffraction. Composites with different amounts of sintering additives and whiskers were fabricated using reaction bonding followed by hot pressing. The amount of whiskers remaining in each composite after each processing stage was determined. In order to study the degradation mechanism, the microstructural development after each processing step was examined using scanning and transmission electron microscopy. Finally, the effect of sintering additives on the microstructural development and whisker stability was also investigated.     

Si_3N_4原位增强Cu基复合材料的制备

采用感应炉熔炼及水雾化工艺制得了Cu-Si合金粉末,经N2、H2混合气体选择氮化和真空放电等离子烧结(SPS)成型,制备得到了Si3N4原位增强Cu基复合材料(Si3N4/Cu),利用萃取法研究了选择性氮化产物及其晶体结构。结果表明:复合粉末中N含量随氮化温度的升高和氮化时间的延长而增大。在1 000℃下氮化,持续时间大于60h时,粉末中的N含量明显提高;Cu的衍射峰出现整体向大角度方向的明显偏移,同时晶格常数变小,表明Si从Cu基体中脱溶,与N反应生成Si3N4;Si3N4/Cu复合材料的增强体以β-Si3N4为主;随着氮化温度的升高和氮化时间的延长,Si3N4/Cu复合材料的电导率和硬度逐步提高。     

Microstructure and properties of SiC whisker reinforced ceramic composites

Microstructures of SiC whisker reinforced alumina and tetragonal zirconia polycrystals (TZP) were investigated using analytical electron microscopy. In the Al₂O₃-SiC system, amorphous phases between the whisker and matrix were observed; these amorphous phases were virtually eliminated when the whiskers were leached with HF acid before being incorporated into the matrix. In the TZP/SiC system, reaction between the whisker and matrix had taken place during fabrication and resulted in the formation of a glassy phase. This reaction appeared to be associated with the presence of SiO₂ impurity present in the TZP matrix.Mechanical properties of the composites were measured both at ambient and elevated temperatures and fracture surfaces were examined. The results indicated that fracture of the composites was sensitively influenced by the whisker-matrix interface. The presence of amorphous interfacial phases was detrimental to the properties of the composites and caused a reduction in fracture energy. High temperature tests showed that the TZP composite had a structural transition with extensive cracking occurring at 1000 °C, whilst the alumina composites retained their properties up to 1200 °C, whereupon they deteriorated rapidly.     

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.     

Slurry processing for fabrication of SiC whisker-reinforced Si3N4 composites

In order to solve the major problems of processing whisker-reinforced ceramic composites, such as agglomeration of whiskers, correlation between pH and viscosity has been carefully investigated in a mixed slurry of whiskers and matrix powder. SiC whiskers and Si₃N₄ powder were dispersed homogeneously by controlling pH in aqueous suspension, and the state was successfully fixed by a sudden change of pH to make the slurry more viscous. The slurry was then filtrated rapidly and dried. The strength of hot pressed composites obtained by this procedure was scarcely lowered, with increased whisker loading in the range 0–30 wt% and fracture toughness increased more than 75%.     

Creep properties of (Si–Al–O–N)SiC whisker composites

(Si–Al–O–N) (sialon)–SiC whisker (SiC_w) composites containing up to 10 mass% SiC_w were prepared by hot isostatic pressing. The strengths and the fracture toughness of composites remained relatively unchanged with the amount of SiC_w. The addition of SiC_w enabled us to improve the creep properties of sialon ceramics. The total creep strain and steady-state creep rate at 1473 K under a stress of 400–500 MPa decreased with increasing the amount of SiC_w. The experimental creep exponent values of monolithic sialon and sialon–SiC_w composites were nearly 1. It is supposed that the creep of both monolithic sialon and sialon–SiC_w composites are dominated by the viscous flow of the interglanular glassy phase.     

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.     

网状结构Si3N4陶瓷增强金属基复合材料的研究

利用有机前驱体浸渍法制备了Si3N4网络陶瓷预制体,利用液态金属浸渗法制备出Al基、Mg基复合材料.分析了在浸渗过程中浸渗温度、润湿角、浸渗时间、浸渗高度的相互关系.在压力下金属液克服浸渗阻力,使浸渗得以完成.网络陶瓷骨架孔筋表面覆盖一层氧化膜有利于自发浸渗的进行.合金中适量镁元素的存在使界面上发生轻微化学放热反应,对浸渗有利.指出压力浸渗制备铝基复合材料与无压浸渗制备镁基复合材料的特点.探讨了这种复合材料抗压强度和摩擦磨损性能特点.指出Si3N4/Al复合材料,Si3N4/Mg复合材料抗磨擦性能明显优于基体,抗拉强度大大高于基体.     

网状结构Si3N4陶瓷增强金属基复合材料的研究

利用有机前驱体浸渍法制备了Si3N4网络陶瓷预制体,利用液态金属浸渗法制备出Al基、Mg基复合材料：分析了在浸渗过程中浸渗温度、润湿角、浸渗时间、浸渗高度的相互关系。在压力下金属液克服浸渗阻力．使浸渗得以完成。网络陶瓷骨架孔筋表面覆盖一层氧化膜有利于自发娄渗的进行。合金中适量镁元素的存在使平面上发生轻微化学放热反应．对浸渗有利。指出压力浸渗制备铝基复合材料与无压浸渗制备镁基合材料的特点。探计了这种复合材料抗压强度和摩擦磨损性能特点。指出Si3N4／Al复合材料，Si3N4/Mg复合材料抗磨擦性能明显优于基休．抗拉强度大大高于基体。     

纳米SiC纤维改性短切碳纤维增强Si_3N_4陶瓷介电响应及吸波性能

以甲基三氯硅烷为原料,采用催化化学气相沉积(CCVD)工艺在短切碳纤维(C_(fd))表面制备了纳米SiC纤维(nano SiC_f)改性层,并采用凝胶注模-无压烧结工艺制备了nano SiC_f-C_(fd)/Si_3N_4和C_(fd)/Si_3N_4复合材料。使用矢量网络分析仪研究了nano SiC_f-C_(fd)和C_(fd)对Si_3N_4陶瓷在X波段(8.2~12.4GHz)的介电响应和吸波性能的影响。结果表明:nano SiC_f-C_(fd)/Si_3N_4和C_(fd)/Si_3N_4复合材料的复介电常数和介电损耗角正切值(tanδ)均随纤维添加量增加而增大;相同纤维含量时,nano SiC_f-C_(fd)/Si_3N_4复合材料的介电常数实部比C_(fd)/Si_3N_4复合材料有所降低,但损耗角正切升高。反射损耗结果表明:nano SiC_f-C_(fd)/Si_3N_4复合材料拥有更优的电磁波吸收效果。nano SiC_f-C_(fd)含量为2wt%、d=2.5mm时,出现最大吸收峰-14.95dB,反射损耗优于-5dB,波段频宽达3.5GHz。nano SiC_f界面改性能有效提高C_(fd)/Si_3N_4复合材料的吸波性能。     

氮化硅晶须的研究现状

介绍了晶须的生长机理、氮化硅晶须的制备方法以及影响其生长的因素。阐述了氮化硅晶须增强复合材料的现状,指出加强晶须的基础研究,改进制备技术和降低成本是今后的发展方向。     

Thermomechanically induced embrittlement in hot isostatically pressed Si3N4/SiC composites

The macroscopic fracture properties of an Si₃N₄/SiC-platelet composite fabricated by hot isostatic pressing (HIP) without sintering aids were measured by the chevron-notch technique in bending and related to micromechanisms of fracture by means of a quantitative profilometric analysis of the fracture surfaces. Compositional and processing parameters were varied systematically in order to maximize both the fracture toughness and the work of fracture of the composite. Data were compared with those of monolithic Si₃N₄ fabricated by the same process. Cooling-rate from the HI Ping temperature was indicated as a critical parameter especially when cooling was performed under high pressure. A marked embrittlement of the composite body was found by cooling at around 650 °C h^–1 and it could not be completely recovered by successive annealing even up to temperatures above 1700 °C. The highest fracture toughness and work of fracture in the composite (obtained at a cooling rate of about 100 °C h^–1), were measured as 4.6 MPa m^1/2 and 58.6 J m^–2, respectively. In agreement with fractal analysis results, they were estimated to be about 60%–70% of the maximum values, respectively, obtainable in the present composite system, provided that a complete debonding at the platelet/matrix interface can occur.     

SiC-nanoparticle-reinforced Si3N4 matrix composites

Hot-pressed nanosized SiC-particle (SiC_p-reinforced Si₃N₄ composites have been studied with respect to their microstructures, room temperature mechanical properties and thermal shock resistance. The experimental results indicate that the flexural strength, fracture toughness and thermal shock resistance are all increased by the addition of 5 vol% SiC_p. Further additions of SiC_p, however, have a detrimental effect on these properties. These changes are closely related to the effects of SiC_p on the matrix grain morphology. The mechanisms of nucleation and growth of -Si₃N₄ grains in the presence of SiC nano-particles are discussed.     

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。