原位转化碳纤维增韧氧化铝复合材料的制备工艺
Preparation process of in situ carbon reinforced alumina composites
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摘要: 以聚丙烯腈预氧化纤维为先驱纤维,使其在真空烧结过程中原位转化生成碳纤维来增韧氧化铝陶瓷材料.利用热重–差热分析和X射线衍射研究了聚丙烯腈预氧化纤维的相结构和化学结构以确定制备复合材料的升温烧结工艺,并探讨了加压方式和聚丙烯腈预氧化纤维含量对复合材料组织结构和性能的影响.研究发现聚丙烯腈预氧化纤维在差热曲线上444℃左右的放热峰和X射线衍射图谱中17左右的衍射峰是由预氧化阶段残留的未充分氧化的聚丙烯腈分子引起的;而1073℃左右的吸热峰和25.5左右的衍射峰说明预氧化纤维在加热烧结过程中已开始向碳纤维转变.热压烧结制备的复合材料的力学性能明显优于无压烧结.随着聚丙烯腈预氧化纤维含量的增加,复合材料的密度和显微硬度降低,而断裂韧性则先升高后降低,当聚丙烯腈预氧化纤维体积分数为20%时,复合材料的断裂韧性最大,达9.39MPa·m1/2,说明原位碳纤维的生成提高了复合材料的断裂韧性,其增韧机制主要为纤维拔出和脱黏.Abstract: Pre-oxidized polyacrylonitrile (PAN) fibers were used as a precursor and they were in situ transformed into carbon fibers to toughen alumina ceramics in vacuum sintering. The chemical structure and phase of the pre-oxidized PAN fibers were studied by thermogravimetric/differential thermal analysis (TG/DTA) and X-ray diffraction to determine a suitable sintering process of the composites. The effects of pressing ways and pre-oxidized PAN fiber content on the microstructure and properties of the composites were explored. It is found that the exothermic peak around 444~C in the DTA curve and the diffraction peak around 17~in the XRD pattern of the pre-oxidized PAN fibers are due to incompletely oxidized PAN molecules during pre-oxidation, while the endothermic peak at 1073~C and the diffraction peak around 25.5~show the pre-oxidized PAN fibers having begun to transform into carbon fibers during the sintering. The mechanical properties of the composites prepared by hot pressing are superior to those by pressureless sintering. With the pre-oxidized PAN fiber content increasing, the density and microhardness of the composites decline, however the fracture toughness increases first and then decreases. When the volume fraction of the pre-oxidized PAN fibers is 20%, the fracture toughness of the composites is up to 9.39 MPa·m1/2. It illustrates that the in situ transformation carbon fibers improve the fracture toughness of the composites. The toughening mechanism is mainly fiber pulling-out and deboning.