IMR OpenIR
CVD SiC 纤维增强Al及TiAl基复合材料的制备新方法、界面及拉伸性能研究
其他题名Study on fabrication, interface and tensile strength of CVD SiC fiber reinforced Al and TiAl composites
冀鸰
学位类型博士
导师石南林
2008-05-23
学位授予单位中国科学院金属研究所
学位授予地点金属研究所
学位专业材料学
关键词复合材料 Sic纤维 Al Tial 真空热压 工艺 界面 拉伸性能
摘要本文使用不同的纤维表面涂层和复合材料成型工艺制备了SiCf/5A02基复合材料,并尝试采用一种新型的元素镀层法在800℃制备了SiCf/TiAl基复合材料,以改善复合材料的界面结构及拉伸性能。 采用阳极氧化法对富碳(C)表面涂层SiC纤维进行了表面处理,制备了表面富氧(O)的C涂层。扫描电子显微镜(SEM)和X射线光电子谱(XPS)表征结果表明,富C层表面生成了羟基、羰基和羧基等含氧官能团,氧含量升高了一倍左右。由于O原子的引入使涂层表面体积膨胀,产生了平行于纤维表面的压应力,缓解了纤维固有的表面张应力,而且纤维表面的粗糙结构被刻蚀掉,纤维表面损伤敏感性降低,拉伸强度得到了一定的提高,并且纤维性能分布离散度降低。 分别采用富C层、富氧C涂层和SiO2涂层SiC纤维制备了SiCf/5A02基复合材料。研究结果表明,涂层对复合材料界面微观结构及材料的拉伸性能都有很重要的影响。C涂层与基体在界面处生成了六角片状的Al4C3,以元素扩散与微量反应相连接的界面结合强度适中,复合材料拉断后纤维适当拔出,形成了损伤积累型破坏,强度最高。富氧C涂层中的O元素不但增加了纤维表面的反应活性,与基体在界面处生成了连续的MgO层,增强了界面连接强度,而且抑制了C元素的扩散与片状脆性相Al4C3的生成。但由于Mg向涂层中的扩散增加了C涂层表面的体积膨胀,在涂层内部或涂层与SiC柱状晶之间形成剪应力。因此当裂纹在涂层表面产生后,会在涂层内部或涂层与SiC柱状晶之间的结合较弱处偏转,形成脱粘型破坏,造成复合材料强度降低。SiO2涂层与基体生成了MgO与Al4C3混合生长的界面,界面结合较强,由于在脆性界面与SiC柱状晶之间没有缓冲层的保护,裂纹在SiC纤维表面生成并直接沿晶界扩展,形成脆性断裂,复合材料强度最低。 为了改善C涂层纤维与基体之间的界面状况,采用近熔态扩散法,即在合金固液线之间扩散结合的方法制备了C涂层SiCf/5A02基复合材料,并对比了不同的工艺条件下复合材料界面结构及断裂方式的变化。TEM 分析显示复合材料在固相线保温后,Al4C3密度及尺寸均比固态扩散法有所增加,并形成层状结构,界面结合强度增大,断口附近纤维均显示多次断裂,断口平齐;而在固液线之间保温处理后,Mg在基体冷却过程中偏聚到最后凝固的纤维周围, 并与界面处 的Al2O3薄膜发生氧化还原反应,形成细小的MgO颗粒,C的扩散受到阻碍,抑制了脆性相Al4C3的形核,减少了界面处Al4C3的数量,但制备温度的升高同时也促进了已形核的Al4C3的径向生长,增加了纤维表面损伤敏感性,使纤维容易在较低应力下产生表面裂纹,从而导致复合材料整体拉伸性能下降。缩短整体加热时间后,表面Al4C3尺寸减小,复合材料拉伸性能有所改善。 在论文的最后部分,采用磁控溅射法在SiC纤维表面交替溅射若干层厚约1μm的纯Ti和纯Al,制备了Ti-Al元素镀层SiC复合丝,并尝试利用单质镀层的良好变形能力在较低温度下制备了SiCf/TiAl基复合材料。复合材料的热压过程分四部分,即390℃/2h除胶+640℃/80MPa/2h热压成型+800℃/0MPa/2h基体均匀化+1.5℃/min控温冷却。制得的复合材料基体中热裂纹较少,界面反应程度轻微,元素镀层之间的扩散反应基本完成,生成了以TiAl为主的金属间化合物。实验证明该方法可以在较低温度下制得成分均匀的Ti-Al金属间化合物基复合材料,基体中的热裂纹及基体与纤维之间界面反应均能受到有效控制。
其他摘要In this paper, CVD SiCf/5A02 composites were prepared by different coatings of SiC fiber and manufacture processes, and SiCf/TiAl composite was made by a novel process called elemental coating method under 800℃ in order to improve the interface of the composites. Anodic oxidation method was used to treat the surface of carbon coated SiC fiber. The results of analysis by scan electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) indicated that hydroxy, carbonyl and carboxy were formed in the carbon coating and the oxygen (O) content on the surface of coating increased after the treatment. The dimension swelling of coating created a press stress on the surface of the fiber and the tensile stress on the surface of the fiber was reduced. Meanwhile,the damage sensitivity of the fiber relaxed since the surface of fiber was smoothed by the etching effect of the electrochemical treatment. As the result, the tensile strength of the fiber was improved in average and the dispersing ratio was reduced. SiCf/5A02 composite were prepared by the SiC fibers with carbon, O-rich carbon and SiO2 surface coatings respectively. The interface microstructure and tensile strength of the composites are affected greatly by coatings. The tensile strength of composite with carbon coating SiCf is the highest. Hexagonal Al4C3 plates formed by a mild diffusion reaction at the interface of composite,which resulted in a moderate bonding between the fiber and matrix. The fibers were lightly pulled out after composite broke under tensile stress. In the interface of O-rich carbon coating SiCf/5A02 composite, continuous MgO layer was formed, which restrict the diffusion of C and formation of Al4C3 and strengthen the bonding of interface. However, the volume of the coating swelled by the diffusion of Mg which increased a shear stress in coating or between coating and SiC columnar crystal. As the results, crack on the fiber surface can be deflected at weak bonding zone of the interface and the coating can be delaminated and fiber debonded. The tensile strength of the composite is lower ,the fibers were pulled out severely after the failure of the composite. In the interface of SiCf/5A02 composite with the SiO2 coating fiber, MgO and Al4C3 grew simultaneously and strong bonding interface formed. Because there is no buffer layer between SiC columnar crystal and the brittle interface, if a crack formed on the surface of fiber, it can be extend through grain boundary directly. The strength of the composite is the lowest. A novel processing called semi-solid diffusing (SSD) method was used to manufactured CVD SiCf /5A02 composite in order to improve the bonding between fiber and matrix, in which the diffusion bonding temperature is partly in the semi-solid zone of the Al alloy. SEM and TEM analysis shows after a treatment at solidas curve the size and density of Al4C3 in the interface of the composite is higher than that of prepared by soild diffusing method. The bonding of interface became stronger, so the fracture of the fiber shows multiple step cracks. After treating at semi-solid zone, Mg enriched around the surface of SiC fiber and reacted with Al2O3 film on the surface of Al alloy matrix to form fine MgO grains. The diffusion of C element and nucleation of brittle Al4C3 was restricted. But the size of Al4C3 was promoted by the increase of temperature, and the surface damage sensitivity of fiber was also increased as well. Crack tends to generate on the surface of fiber under the low stress. The tensile strength of composite is reduced. After shortenning the total heating time, the dimension of Al4C3 reduced and the strength of composite improved. At the last part of the paper, a SiCf/TiAl composite was made by a novel process called elemental coating method. Firstly, Ti and Al layers about 1μm in thickness were deposited on the SiC fiber alternately by magnetron sputtering to form a Ti-Al elemental coating SiC fiber. Then the SiCf/TiAl composite was prepared by diffusing bonding method at lower temperature with excellent plasticity of elemental coating. The preparation of composite has four steps: removing the glue at 390℃/2h+heat pressing at 640℃/80MPa/2h+uniform at 800℃/0MPa/2h+cooling with 1.5℃/min. The diffusion reaction between elemental coating is almost completed and TiAl intermetallic was formed. The experience shows that composite with uniform matrix could be prepared by this method, hot crack in the matrix and reaction in the interface can be controlled.
页数120
语种中文
文献类型学位论文
条目标识符http://ir.imr.ac.cn/handle/321006/17110
专题中国科学院金属研究所
推荐引用方式
GB/T 7714
冀鸰. CVD SiC 纤维增强Al及TiAl基复合材料的制备新方法、界面及拉伸性能研究[D]. 金属研究所. 中国科学院金属研究所,2008.
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