SiC/SiC复合材料高温力学性能研究

以聚碳硅烷为连续SiC陶瓷基体相的先驱体,三维四向SiC纤维预制体为增强相,采用聚合物先驱体浸渍裂解工艺制备了SiC纤维增强SiC陶瓷基(SiC/SiC)复合材料,分析表征了复合材料的组成、结构和力学性能.结果表明,SiC/SiC复合材料室温弯曲强度和断裂韧性分别为400 MPa和16.5 MPa·m1/2,优异的室温力学性能可以保持到1350℃.随着温度增加,弯曲强度基本不变,1350℃时因界面层受到破坏而断裂韧性稍有下降.     

Al2O3-SiO2-TiO2表面涂层对3D-Cf/SiC复合材料力学性能的影响

采用溶胶凝胶法在三维碳纤维预制体(3D-Cf)表面形成Al2O3-SiO2-TiO2涂层,而后采用先驱体浸渍裂解工艺(PIP)制备了3D-Cf/SiC复合材料,通过SEM、XRD等分析测试手段以及三点弯曲等试验方法,研究了碳纤维的界面对复合材料的微观结构、力学性能的影响.结果表明,Al2O3-SiO2-TiO2涂覆处理后的碳纤维的强度约为原始碳纤维的96.8;,涂层碳纤维在复合材料断裂过程中起到了较好的增韧作用,涂层处理后的3D-Cf/SiC复合材料的抗弯强度达303 MPa,断裂韧度达6.5 MPa/m1/2.     

浸渍工艺对ZrO2纤维布结构及性能的影响

采用前驱体浸渍工艺制备ZrO2纤维布.利用SEM、XRD研究粘胶织物及ZrO2纤维布的微观结构;测试了ZrO2纤维布的横向抗张强度,研究了浸渍工艺对ZrO2纤维布微观结构、面密度和抗张强度的影响.结果表明:粘胶织物是制备ZrO2纤维布的理想前驱体材料;改善浸渍方式、提高浸渍溶液浓度和温度均能提高ZrO2纤维布的面密度;浸渍方式显著影响单根纤维的致密程度,残液去除方式显著影响纤维的分散程度,采用辊压浸渍和离心甩干去除残液的方式能够显著提高ZrO2纤维布的抗张强度.     

碳化硅粉体对熔融渗硅法制备C_f/SiC复合材料结构的影响

以三维针刺碳纤维为预制体,含有微米级碳化硅粉体的酚醛树脂浆料为碳源,采用熔融渗硅(Molten Silicon Infiltration)法制备Cf/SiC复合材料,研究了碳化硅粉体的存在对制备Cf/SiC复合材料结构的影响。结果表明:预成型体中,微米级碳化硅粉体能有效的浸渍至纤维束中,并在裂解过程中因与基体碳热膨胀系数差异产生与粉体粒径相当的微裂纹,形成裂纹孔道结构,预成型体密度为1.32 g/cm3,开口气孔率为25%;复合材料中,裂纹的引入为熔融渗硅提供通道,但裂纹孔道尺寸过大影响了复合材料的进一步致密化,SEM表明在碳化硅颗粒周围形成闭气孔,复合材料密度为1.93 g/cm3,开口气孔率为7%。     

浸渍-裂解工艺对无压烧结制备六方氮化硼陶瓷性能的影响

以硼酸-尿素混合水溶液作为h-BN先驱体,对无压烧结制备的高纯h-BN陶瓷进行了浸渍-裂解-二次无压烧结处理,以提高其致密度和性能.研究了先驱体溶液浓度和循环次数对浸渍-裂解-烧结后h-BN陶瓷的显微结构及性能的影响.结果表明,随着先驱体溶液浓度的增大,h-BN陶瓷的密度、弯曲强度、断裂韧性和热导率均先升高后降低,浓度为68wt;时均达到最大.浓度过高会导致先驱体溶液在浸渍过程中发生析出,反而不利于浸渍.随着循环次数的增加,h-BN陶瓷的致密度、弯曲强度、断裂韧性及热导率均逐渐增大,但趋势逐渐变缓.循环6次得到的h-BN陶瓷的密度、弯曲强度、断裂韧性和热导率分别为1.465 g./cm3、84.1 MPa、1.52 MPa·m1/2、44.36 W·m-1·k-1,相对于未处理的h-BN陶瓷分别提高4.7;、31.6;、63.7;、31.2;.     

Ti3Al含量对TiC/(Ti3Al+ZrO2)陶瓷复合材料晶粒生长及性能的影响

采用机械合金化和热压烧结制备了TiC/(Ti3Al+ZrO2)复合材料.研究了1550℃烧结温度下,不同Ti3Al含量(10、15、20、25;质量分数)对复合材料烧结及力学性能的影响.结果表明:随着Ti3Al含量的增加,烧结体致密化程度提高,抗弯强度和硬度相应提高,但当Ti3Al超过一定量时,强度、硬度又有所降低.     

透辉石增韧补强氧化铝基陶瓷材料烧结动力学和烧结机制

研究了透辉石增韧补强Al2O3,基陶瓷材料的无压烧结致密化过程,根据压坏烧结时烧结温度和保温时间对线收缩率的影响,计算了复合材料液相烧结的表观激活能Q,得出其致密化机理为扩散机制控制.建立了透辉石增韧补强Al2O3,基陶瓷材料的烧结动力学方程,并由特征指数n值对比研究了它们的烧结致密化机制.纯Al2O3陶瓷材料烧结过程中的物质迁移机制由体扩散控制;透辉石增韧补强Al2O3基陶瓷材料烧结过程中的物质迁移机制既有体扩散,也有晶界扩散.     

滴定方式对纳米NH4AlO(OH)HCO3先驱体制备的影响

本文以NH4Al（SO4）2和NH4HCO3为主要原料,采用均相沉淀法制备纳米NH4AlO（OH）HCO3（AACH）先驱体,利用X射线衍射仪和透射电镜研究了滴定方式对其制备的影响。结果表明：将碳酸氢铵溶液滴入剧烈搅拌的硫酸铝铵溶液中,可获得勃姆石,将硫酸铝铵溶液滴入剧烈搅拌的碳酸氢铵溶液中,则可获得呈纤维状的纳米NH4AlO（OH）HCO3先驱体,分散较好且无明显团聚。     

成型压力对SiCnf增韧SiC陶瓷基复合材料微观结构和性能的影响

研究采用不同成型压力制备不同体积分数的SiC纳米纤维预制体,并通过前驱体浸渍裂解和反应熔渗联用工艺制备了SiC纳米纤维增韧SiC陶瓷基复合材料。研究了成型压力对SiC陶瓷基复合材料结构和性能的影响。结果表明,通过模压成型可实现高体积分数的SiC纳米纤维预制体的制备。当成型压力为40 MPa时,预制体SiC纳米纤维体积分数高达22.13%,但过高的成型压力也会导致SiC纳米纤维断裂。相较于单一前驱体浸渍裂解工艺,采用前驱体浸渍裂解和反应熔渗联用工艺制备的复合材料孔隙率显著降低,材料平均孔隙率从14.19%降至1.43%。当成型压力为30 MPa时,复合材料中游离硅含量低且SiC纳米纤维断裂少,材料抗弯强度和断裂韧性分别达到最大值178 MPa和21.6 MPa·m^1/2。     

无压烧结制备透辉石/AlTiB增韧补强氧化铝基结构陶瓷材料

采用温度梯度无压烧结工艺制备了透辉石/AlTiB增韧补强Al2O3基结构陶瓷材料,探讨了其致密化烧结特性,并对其力学性能进行了测试和分析.研究了透辉石/AlTiB增韧补强Al2O3基结构陶瓷材料的微观结构,并分析了其力学性能和微观结构与透辉石含量的关系.结果表明:与纯Al2O3相比,透辉石/AlTiB增韧补强Al2O3基结构陶瓷材料的力学性能得到明显提高,其中添加6;(体积百分含量,下同)透辉石和4;AlTiB的Al2O3基结构陶瓷材料获得较好的综合力学性能,其硬度、抗弯强度和断裂韧性分别达到16.02 GPa、370 MPa和5.11 MPa·m1/2.力学性能提高的主要原因为:添加相与Al2O3基体之间界面反应的发生以及透辉石和AlTiB对复合材料的协同晶粒细化效应.     

Moisture behavior and effects on the mechanical properties and the microstructures of SiO2f/Si3N4–BN amorphous composites

Water diffusion in fiber reinforced ceramic composites could reduce the flexural strength as a result of weakened fiber/matrix binding. In the paper, the braided silica fiber reinforced silicon nitride and boron nitride amorphous composites (SiO_2f/Si₃N₄–BN) was prepared through repeated infiltration of hybrid preceramic precursor and pyrolysis at high temperature in ammonia atmosphere. The moisture behavior of the SiO_2f/Si₃N₄–BN composites and moist effects on the mechanical properties and the microstructures of composites were studied. The results showed that the water absorption characteristic of amorphous composites could be described by using the Fick’ law. The flexural strength could be adjusted and the maximal value of that reached 161.7 MPa by controlling moderate relative humidity, which is 58.8% higher more than that of the as-received composites. SEM indicated that good mechanical properties is on the ground of the interface structure change between fiber and matrix and more fibers were pulled out which absorbing much more fracture energy.     

SiC crystal growth from transition metal silicide fluxes

SiC crystal growth in transition metal silicide melts was investigated by using spontaneous infiltration and solution methods. In the infiltration experiments, SiC powder preforms were infiltrated with Fe_xSi_y (Fe₃Si, Fe₅Si₃ and FeSi) and CoSi melts. The dissolution and precipitation of SiC led to SiC crystals growth in the infiltrated Fe₅Si₃ and CoSi melts, SiC particles coalescing in FeSi and free carbon precipitation in Fe₃Si. In the solution experiments, carbon from the graphite crucible dissolved in and reacted with FeSi₂ and Ti_2.3Si_7.7 to form SiC crystals. Scanning electron microscopy (SEM), X‐ray diffraction (XRD) and Raman scattering spectrometer were employed to investigate SiC crystals growth. Based on the investigation, the effect of solution content on the SiC crystal growth, the growth mechanisms in both methods and prototypes of the SiC crystals are also discussed. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization behaviors of carbon fiber reinforced BN‐Si3N4 matrix composite

The crystallization behaviors of a new carbon fiber reinforced composite with a hybrid matrix comprising BN and Si₃N₄ prepared by precursor infiltration and pyrolysis were investigated by Fourier transform infrared spectroscopy, X‐ray diffraction and scanning electron microscopy. The results show that the as‐received composite is almost amorphous, and its main composition is BN and Si₃N₄. When heat treated at 1600°C, the composite is crystallized and shows a much better crystal form. When heat treated at 2100°C, Si₃N₄ in the matrix is decomposed, and BN exhibits a relatively complete crystallization. The existence of B₄C and SiC is detected, which indicates the interfacial chemical reactions between nitride matrices and carbon fibers. The surface morphology of carbon fibers in the composite changed significantly when heated from 1600 to 2100°C, which also proved the occurrence of interfacial chemical reactions. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

硅树脂转化制备硅氧碳多孔陶瓷

采用硅树脂RSN-6018为陶瓷先驱体,并引入一定比例的预固化硅树脂,在N2气氛下于1200 ℃裂解转化制备组分单一、孔结构可控以及陶瓷产率高的硅氧碳(Si-O-C)多孔陶瓷,研究了预固化硅树脂含量对Si-O-C多孔陶瓷微观形貌和性能的影响.结果表明:预固化硅树脂的加入可有效调节Si-O-C多孔陶瓷的孔形貌、孔径以及气孔率,当预固化硅树脂含量低于90wt;时,随着预固化硅树脂含量的增加,孔结构从贯通圆孔变为颗粒"搭接"贯通孔,再变为颗粒堆积孔,且气孔率增大;而体积收缩减小,陶瓷产率提高;耐压强度在27.9~17.5 MPa之间.     

TiB2、CNT双相增韧碳化硼复合陶瓷及其性能研究

在1 500 ℃的真空条件下,通过液相渗硅法(liquid silicon infiltration, LSI)制备了碳化硼/二硼化钛-碳纳米管(B₄C-TiB₂-CNT)陶瓷复合材料,对其成分、形貌、性能和增韧机理进行了分析表征和研究。结果表明:复合材料的主要组成相为B₁₂(C, Si, B)₃、SiC和Si。二硼化钛和碳纳米管显著提高了液相渗硅烧结碳化硼陶瓷的力学性能,在TiB₂和CNT的添加量分别为10%和0.4%时,复合陶瓷的弯曲强度和断裂韧性达到了(390±18) MPa和(5.38±0.38) MPa·m^1/2,分别比B₄C陶瓷高了31%和53%。本文的研究从片状SiC颗粒和CNT的拔出、TiB₂的颗粒增韧以及裂纹的偏转等方面解释了B₄C-TiB₂-CNT复合材料的增韧机理。     

Preparation of amorphous composites with polymer-derived silicon nitride matrix reinforced by three-dimensional silica fiber

Perhydropolysilazane, a low viscosity preceramic polymer with good infiltration efficiency and high char yield, was used to prepare amorphous composites with polymer-derived silicon nitride matrix reinforced by three-dimensional silica fiber, and the mechanical properties and microstructures were investigated. The composites without fiber coating showed a typical brittle fracture behavior with a smooth fracture surface, and a flexural strength of just 33.5 MPa. While the composites with fiber coating exhibited a non-brittle fracture behavior with distinct fiber pull-out in the fracture surface, and a high flexural strength of 144.9 MPa. It was the controlled fiber/matrix interface by precoating treatment that contributed to the high mechanical property of the composites.     

SiC/Al复合材料的热导率研究

用无压浸渗法制备了高导热的SiC/Al电子封装材料.采用光学显微镜、X射线衍射仪、扫描电镜和激光热导仪对复合材料导热率、晶体结构和微观形貌进行了分析,研究了SiC颗粒大小、形状、体积分数、基体中Mg的含量和预氧化等参数对SiC/Al复合材料的导热率的影响.结果表明,选择适当的原料参数和工艺参数可制得导热率高达172.27 W/(m·k)的SiC/Al复合材料,满足电子封装材料的要求.     

陶瓷纤维/莫来石晶须原位增强堇青石-莫来石轻质隔热材料

以蓝晶石、粘土、氧化镁粉为原料,以淀粉为造孔剂和固化剂,引入适量的硅酸铝陶瓷纤维或多晶莫来石纤维和AlF3,通过莫来石晶须在陶瓷纤维表面的原位形成,制备了具有陶瓷纤维/莫来石晶须互锁结构的堇青石-莫来石轻质隔热材料.研究了陶瓷纤维在AlF3的作用下对材料显微结构观察、常温力学性能和导热系数的影响.研究表明:在AlF3的作用下,莫来石晶须在硅酸铝纤维表面垂直生长,部分穿插在发育良好的堇青石晶粒中;这种具有陶瓷纤维/莫来石晶须互锁结构的的陶瓷材料,其力学性能得以提高并降低了材料的导热系数.     

基于单体石墨纤维的场发射特性研究

利用化学气相沉积(CVD)法,以甲烷为碳源在管式炉中合成了单体石墨纤维(MGF)。选取长度为3.426 mm,顶端球面半径为11.26 μm的单体石墨纤维直立于圆铜片上作为阴极,以导电ITO玻璃作为阳极,采用二极管结构在真空室中进行直流场发射测试,证实MGF的开启场强为0.477 5 V/μm。基于有限元仿真软件ANSYS进行电磁场分析,计算了MGF在不同电压下的有效发射面积。结果表明,当电压为5.36 kV时,MGF达到最大发射面积为796.226 μm²,在实验测量电压范围内,平均发射电流密度可以达到46.069 A/cm²,单体石墨纤维具有良好的场发射特性。