Evaluating the effect of oxygen content in BN interfacial coatings on the stability of SiC/BN/SiC composites

Boron nitride was studied as a fiber–matrix interface coating for Nicalon™/SiC composites. The effect of initial O-impurity content within the as-processed BN coatings on the long-term interface stability was investigated at elevated temperatures in flowing oxygen. Two types of Nicalon™/SiC composites were used for this study; one composite had a BN coating with <2% oxygen (low-O BN) and another composite had BN with an oxygen concentration >11% (high-O BN) in the as-processed state. The high-O BN is actually most representative of BN coatings available commercially. The BN coatings in both the high-O and low-O BN containing composites were structurally similar. The samples used here were thinned to <200 μm before oxidation and the final preparation for electron microscopy examination of the interface region was done after the reactions were completed. Thin samples were used to simulate maximum corrosion effects that would occur at the surface of an actual part during service. Ech sample was exposed to flowing oxygen at temperatures as high as 950°C for times up to 400 h. After each oxidation experiment, the BN coatings were examined by TEM to quantify the extent of any reaction which occurred at either the fiber/BN and BN/SiC matrix interfaces. At 950°C for 100 h, there were no interface microstructural changes observed in the low-O BN but there was extensive silica formation at the fiber/BN interfaces in the high-O BN. After 400 h at 950°C, large voids formed at the fiber/BN interface in the high-O BN sample only. Oxygen present within the initial BN coating contributed significantly to the degradation of the interfacial properties of the composite. Several techniques, including transmission electron microscopy (TEM), Auger electron spectroscopy (AES), energy-dispersive spectrometry (EDS), and electron energy-loss spectroscopy (EELS) were used to characterize changes in structure and chemistry of the fiber–matrix interface region and to elucidate and quantify composite degradation mechanisms.     

SiC/BN层状陶瓷耐损伤性能

采用压痕法在SiC/BN层状陶瓷试样的表面引入不同尺寸的表面裂纹,利用三点弯曲测量含裂纹试样的极限断裂应力,研究了不同尺寸的表面裂纹对层状陶瓷断裂强度的影响;根据压痕载荷-强度实验结果,测定层状陶瓷的阻力曲线,并与单相SiC陶瓷对比。结果表明,层状陶瓷的压痕强度对压痕裂纹深度的变化不敏感,阻力曲线呈上升型;而单相SiC陶瓷的压痕强度随压痕裂纹深度的增加急剧下降,阻力曲线呈平稳型,说明层状陶瓷具有优异的耐损伤性能和升值R-曲线行为。分析认为,裂纹在弱界面处发生偏折是层状陶瓷具有优良耐损伤性能和升值R-曲线行为的主要原因。这为陶瓷材料在含有一定的制备和加工缺陷以及承受冲击、磨损等接触损伤的条件下保持高强度提供了可能。     

Influence of a multilayered matrix on the lifetime of SiC/BN/SiC minicomposites

The mechanical behaviour at room temperature and the lifetime in air at 700°C under static loading of SiC/BN/SiC minicomposites have been investigated. The minicomposites consisted of a single tow of Hi-Nicalon fibres coated with a BN interphase and a CVI-SiC matrix. For few of them, a BN layer was introduced within the matrix. All the minicomposites were heat treated at high temperature to improve the BN crystallinity. In some cases, the BN interphase was submitted to a specific treatment before the infiltration of the SiC matrix, to further improve its crystalline state. The differences in interfacial zone, as assessed by TEM, were correlated with those in mechanical properties. A significant improvement of the mechanical behaviour at room temperature and the lifetime of the minicomposites with a multilayered matrix was observed. The multilayered matrix is efficient when a silica layer on both sides of the BN layer within the matrix is present.     

Novel method to synthesize SiC nanowires and effect of SiC nanowires on flexural strength of Cf/SiC composite

The graphite fiber toughened silicon carbide (C_f/SiC) composite was annealed at 1500, 1600, 1700, 1750, 1800 and 1850 °C for 30 min and the flexural strength increased first and then decreased as annealing temperature increased. The maximum flexural strength was obtained for the sample annealed at 1750 °C. The microstructure observation indicated that the amount and length of in situ formed SiC nanowires increased as the annealing treatment time increased, which was very favorable to the improvement of flexural strength. The formation of SiC nanowires was attributed to the presence of the metal La and Al. The vapor–liquid–solid growth mechanism of the SiC nanowires along 〈1 1 1〉 direction is proposed. Furthermore, the purpose of this paper is to report novel method to synthesize SiC nanowires.     

Localized mechanical property assessment of SiC/SiC composite materials

SiC fiber-reinforced SiC matrix composites (SiC/SiC) are under consideration as a structural material for a range of nuclear applications. While these materials have been studied for decades, recently new small scale materials testing techniques have emerged which can be used to characterize SiC/SiC materials from a new perspective. In this work cross section nanoindentation was performed on SiC/SiC composites revealing that both the hardness and Young’s modulus was substantially lower in the fiber compared to the matrix despite both being SiC. Using scanning electron microscopy it was observed that the grain growth of the matrix during formation was radially out from the fiber with a changing grain structure as a function of radius from the fiber center. Focused ion beam machining was used to manufacture micro-cantilever samples and evaluate the fracture toughness and fracture strength in the matrix as a function of grain orientation in the matrix. Additionally microstructural characterization techniques like Raman spectroscopy, X-ray diffraction, and microtomography were used to evaluate differences in the matrix and fibers of the composite.     

超细氮化硼/环氧树脂复合材料的制备和性能影响

将超细高导热的氮化硼(简称BN)与环氧树脂(简称EP)进行复合制备了EP/超细BN复合材料.研究了超细BN的含量对EP/BN复合材料的导热性能及微观结构的影响.结果表明,当BN质量分数为90%时,EP/BN复合材料的热导率达到1.2447W/(m·K),约为纯EP的7倍.     

Microstructure and tensile properties of BN/SiC coated Hi-Nicalon, and Sylramic SiC fiber preforms

Batch to batch and within batch variations, and the influence of fiber architecture on room temperature physical and tensile properties of BN/SiC coated Hi-Nicalon and Sylramic SiC fiber preform specimens were determined. The three fiber architectures studied were plain weave (PW), 5-harness satin (5HS), and 8-harness satin (8HS). Results indicate that the physical properties vary up to 10 percent within a batch, and up to 20 percent between batches of preforms. Load-reload (Hysteresis) and acoustic emission methods were used to analyze damage accumulation occurring during tensile loading. Early acoustic emission activity, before observable hysteretic behavior, indicates that the damage starts with the formation of nonbridged tunnel cracks. These cracks then propagate and intersect the load bearing 0° fibers giving rise to hysteretic behavior. For the Hi-Nicalon preform specimens, the onset of ° bundle cracking stress and strain appeared to be independent of the fiber architecture. Also, the 0° fiber bundle cracking strain remained nearly the same for the preform specimens of both fiber types. TEM analysis indicates that the CVI BN interface coating is mostly amorphous and contains carbon and oxygen impurities, and the CVI SiC coating is crystalline. No reaction exists between the CVI BN and SiC coating.     

Compressive behaviour of SiC/ncsc reinforced Mg composite processed through powder metallurgy route

In this present work nano coconut shell charcoal (ncsc) and silicon carbide (SiC) particulates were reinforced with AZ31B Mg alloy and suitable magnesium composite was developed by using the powder metallurgy technique followed by hot extrusion. Density measurement of the Mg composites revealed that the addition of ncsc significantly improved the density of the composites and porosity measurement showed minimal porosity. The microstructure of the composites showed even distribution of the ncsc in the AZ31B/3SiC Mg composite. The compressive and impact behaviour of the samples were characterized, the results showed that on increasing the weight percentage of ncsc in AZ31B/3SiC/0.5ncsc Mg composites the mechanical properties such as ultimate compressive strength, 0.2% yield strength, ductility and impact strength decreased. The scanning electron microscope (SEM) analysis of fractured surface of AZ31B Mg alloy and AZ31B/3SiC/0.5ncsc Mg composites showed quasi-cleavage fracture. The presence of ncsc above 0.5 wt% composites revealed mixture of quasi cleavage planes and some dimples.     

Fabrication and characterisation of AZ91/SiC composite by pressureless infiltration method

Abstract

Since the spontaneous infiltration of molten AZ91 Mg alloy into the powder bed containing SiC particles occurred at 700°C for 1 h under a nitrogen atmosphere, it was possible to fabricate Mg alloy composites reinforced with SiC particles. Since the fabrication conditions (e.g. temperature, time and atmosphere) of the composite are different from those of the other fabrication route, reaction products formed during the composite fabrication were investigated in detail using field emission scanning electron microscopy and high resolution transmission electron microscopy. From the analysis of reaction products, the authors can identify the formation of MgO, MgAl₂O₄, Al₁₂Mg₁₇ and an AlN phase containing magnesium.     

SiC/BN层状陶瓷的抗热震性能研究

采用水中急冷法研究了SiC/BN层状陶瓷的抗热震性能,并同SiC块体陶瓷作比较.实验结果表明SiC/BN层状陶瓷的热震断裂临界温差ΔTc为300℃,略低于SiC块体陶瓷的抗热震断裂临界温差.当热震温差ΔT >ΔTc 时,SiC/BN层状陶瓷的热震剩余强度的下降趋势明显比块体陶瓷的下降趋势缓慢.这同热震断裂和热震损伤理论计算的热震参数R和R的结果相一致.这表明:与SiC块体陶瓷相比,SiC/BN层状陶瓷的热震裂纹形核阻力略有降低,但热震裂纹扩展阻力却大大提高.分析认为BN弱界面对裂纹的吸收和偏转是材料断裂能提高的主要原因,断裂能的提高有利于材料热震阻力的提高.     

BN/SiC复合界面层对SiC纤维和PIP-Mini复合材料力学性能的影响

采用化学气相渗透(CVI)工艺,在SiC纤维表面沉积BN和BN/SiC复合界面层,对沉积界面层前后纤维的力学性能进行了评价。采用聚合物浸渍裂解(PIP)工艺进行致密化,制得以原纤维、BN界面层和BN/SiC界面层纤维增强的三种Mini-SiCf/SiC复合材料,研究其微观结构和拉伸性能。结果表明:采用CVI工艺制得的界面层厚度均匀、结构致密,其中BN界面层中存在六方相,晶体尺寸为1.76 nm; SiC界面层结晶性较好,晶粒尺寸为18.73 nm;沉积界面层后SiC纤维的弹性模量基本保持不变,拉伸强度降低。与SiCf/SiC相比, PIP工艺制备的SiCf/BN/SiC和SiCf/(BN/SiC)/SiC-Mini复合材料所能承受的最大拉伸载荷和断裂应变明显提升, BN界面层起主要作用。由断面形貌分析可以看出, SiCf/BN/SiC和SiCf/(BN/SiC)/SiC复合材料的纤维拔出明显,说明在断裂时消耗的能量增加,可承受的最大载荷增大。     

聚硅氮烷/BN耐热复合涂层的制备及性能

采用聚硅氮烷作为树脂基体,h-BN作为功能粉体制备复合涂层,通过化学方法对BN进行接枝改性以改善其在复合涂层中的分散,利用FT-IR和TEM对改性前后BN的化学结构进行分析,采用SEM对复合涂层微观形貌结构进行表征,通过对不同树脂含量的复合涂层微观形貌的表征确定了复合涂层最优的树脂含量为50％(质量分数),并对复合涂层的性能进行初步测试分析.结果表明:化学改性的方法成功实现BN的表面接枝,改性后的BN在涂层中的分散性能得到了有效改善,复合涂层表现出较好的阻隔屏蔽性能和耐高温、抗氧化性能.     

Enhancement of dielectric and electrical properties in BT/SiC/PVDF three-phase composite through microstructure tailoring

A polymer composite with high dielectric permittivity was prepared by embedding silicon carbide (SiC) whisker with an average diameter of 500 nm–1 μm in poly(vinylidene fluoride) (PVDF). However, the high dielectric loss and electrical conductivity of the two-phase composite prohibits its potential applications. Barium titanate (BT) particles with average diameter of 100 nm and 1 μm were incorporated as a third phase to fabricate a three-phase composite. The morphology structure, dielectric and electrical properties before and after the addition of BT particles were investigated. The three-phase composite exhibits largely suppressed dielectric loss and electrical conductivity without sacrificing the high dielectric permittivity, which was extremely hard to be realized for two-phase composite. It is also found that the nano-size BT is more favorable in achieving high dielectric permittivity than the micro-size BT, where their dielectric loss and electrical conductivity are similar. Furthermore, electric modulus analysis confirms the largely suppressed electron conduction process which results in the enhanced dielectric and electrical properties in three-phase composite.     

2.5维C/SiC复合材料弹性参数不确定性识别方法研究

提出了一种2.5维C/SiC编织复合材料弹性参数不确定性识别方法。采用刚度平均法获得复合材料等效弹性参数理论预测值。选取对结构动态特性影响较大的3个弹性参数E11,E22和G12作为待识别参数;在确定性识别结果基础上,采用拉丁超立方体采样构造随机试验样本,开展不确定性参数识别方法仿真研究。仿真结果表明,针对考虑弹性参数不确定性的2.5维C/SiC复合材料,采用所提出的方法能够准确识别材料弹性参数的均值与标准差,建立反映实际结构动态特性统计意义的精确动力学模型。     

新型复式连通SiC/390Al复合材料的制备和性能

以空心多孔SiC泡沫陶瓷为增强体,用挤压铸造法制备了新型复式连通双连续相SiC/390Al复合材料,研究了泡沫陶瓷骨架筋的结构对复合材料的影响,以及复合材料中的界面对力学性能的影响.结果表明,SiC空心多孔泡沫陶瓷与390Al复合后形成了复式连通双连续相复合材料,具有独特的互穿式界面结构,材料界面的结合优异.随着复合材料界面结合的加强和泡沫增强体的复合韧化,复合材料的屈服强度、压缩强度和弯曲强度明显提高,韧性显著增强.     

BN/SiC复合涂层改性炭纤维的吸波性能研究

以尿素、硼酸为原料, 采用浸涂工艺先在炭纤维表面制备BN涂层, 再以三氯甲基硅烷为前驱体, 采用化学气相沉积工艺在纤维表面沉积SiC涂层, 制得了BN/SiC复合涂层改性炭纤维。对BN/SiC复合涂层改性炭纤维的微观结构、抗氧化性能、介电性能及吸波性能进行了研究。结果表明: 炭纤维表面BN涂层的厚度约为0.1 μm, SiC涂层的厚度约为0.7 μm。炭纤维经表面BN/SiC复合涂层改性后, 抗氧化性能明显提高, 开始明显氧化失重温度从560℃提高到790℃, 最终氧化温度从780℃提高到1200℃以上; 且介电性能得到有效改善, 吸波性能显著提高。相比于未改性炭纤维, 厚度为2 mm的BN/SiC复合涂层改性炭纤维的最小反射率减小到-13.3 dB, 小于-10 dB的带宽增加至2.5 GHz。     

Facile orientation of unmodified BN nanosheets in polysiloxane/BN composite films using a high magnetic field

Composite films consisting of highly oriented boron nitride (BN) nanosheets in polysiloxane were fabricated without modifying the BN surface by applying a high magnetic field generated by a superconducting magnet. The hexagonal BN nanosheets were dispersed by sonication in a prepolymer mixture of polysiloxane. The homogeneous suspension was then cast on a polyamide spacer of microscale thickness and a magnetic field was applied before the mixture became crosslinked. The BN nanosheets in the polysiloxane were aligned with high anisotropy either parallel or perpendicular to the composite film plane depending on the magnetic flux direction. The fabricated composite films exhibited enhanced thermal conductivity by controlling the anisotropy of the BN nanosheets in the film. The mechanisms for rotation of BN nanosheets and heat diffusion across the composite film are discussed.