Preparation process of in situ carbon reinforced alumina composites
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摘要: 以聚丙烯腈預氧化纖維為先驅纖維,使其在真空燒結過程中原位轉化生成碳纖維來增韌氧化鋁陶瓷材料.利用熱重–差熱分析和X射線衍射研究了聚丙烯腈預氧化纖維的相結構和化學結構以確定制備復合材料的升溫燒結工藝,并探討了加壓方式和聚丙烯腈預氧化纖維含量對復合材料組織結構和性能的影響.研究發現聚丙烯腈預氧化纖維在差熱曲線上444℃左右的放熱峰和X射線衍射圖譜中17左右的衍射峰是由預氧化階段殘留的未充分氧化的聚丙烯腈分子引起的;而1073℃左右的吸熱峰和25.5左右的衍射峰說明預氧化纖維在加熱燒結過程中已開始向碳纖維轉變.熱壓燒結制備的復合材料的力學性能明顯優于無壓燒結.隨著聚丙烯腈預氧化纖維含量的增加,復合材料的密度和顯微硬度降低,而斷裂韌性則先升高后降低,當聚丙烯腈預氧化纖維體積分數為20%時,復合材料的斷裂韌性最大,達9.39MPa·m1/2,說明原位碳纖維的生成提高了復合材料的斷裂韌性,其增韌機制主要為纖維拔出和脫黏.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.
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Key words:
- ceramic matrix composites /
- alumina /
- carbon fibers /
- polyacrylonitrile /
- oxidation /
- toughening mechanism
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