Fe-Al/Al_2O_3陶瓷基复合材料的凝胶注模成型工艺研究
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摘要
Fe-Al/Al2O3陶瓷基复合材料是以Al2O3陶瓷为基体,以Fe-Al金属间化合物为增韧补强相的复合材料。Fe-Al金属间化合物增韧补强陶瓷克服了纤维、晶须、金属颗粒增韧补强氧化铝陶瓷的弊端,充分发挥了Fe-Al金属间化合物这种半陶瓷材料与氧化铝相容性好的优点,使二者优势得到互补。
     目前制备Fe-Al/Al2O3陶瓷基复合材料的主要方法是机械合金化-加压烧结,首先用机械合金化方法制得Fe-Al粉末,然后与Al2O3陶瓷粉末混合后再热压烧结成型。这种成型方法简单易行,但难以得到复杂的形状,且烧结零件需进行后加工,增加了生产成本。
     本文选择凝胶注模成型工艺作为本课题研究的对象,其原理是在高固相含量的陶瓷浆料中加入可聚合有机单体及交联剂,在引发剂和催化剂的作用下,引发单体聚合使陶瓷浆料原位成型。运用该原理,本文制备出高固相体积含量的Fe-Al/Al2O3浆料,制得坯体强度高,组织结构均匀,具有良好的可加工性。通过机械合金化-中温培烧法制备得到Fe-Al金属间化合物粉末,确定工艺条件为球磨40h,750℃下保温2h。X射线衍射图看出金属铝逐渐与铁发生反应形成金属间化合物,750℃保温2h的退火促使材料由无序态向有序态转变。晶粒呈棒状,粒度达纳米级。
     本课题主要研究了如何制得高固相体积含量的流动性能良好的浆料,讨论了固相含量、分散剂及pH等对浆料流动性能的影响,研究得出浆料中固相含量为58Vol%时,以MN为分散剂,在pH=7时,可获得800mPa·s的低粘度浓悬浮液。
     本文还进行了浆料固化、干燥及脱胶工艺的研究。从聚合反应角度探讨了凝胶固化原理为单体自由基聚合,分析了引发剂对聚合反应速率及聚合物分子量的影响,并用红外光谱对聚合物结构进行了表征。实验结果表明:反应受引发剂影响显著,浆料中引发剂(浓度为10wt%)加入量为浆料的1.0vol%时,固化时间最为适宜,保证了浆料在浇注前有一定流动性而不会很快固化。本文还分析了坯体干燥和脱胶过程中,水分和有机物的失去过程,通过控制加热温度和时间,缩短了工艺周期。本研究使用SEM等技术对坯体的显微结构进行了表征,测定了坯体的抗弯强度,并分析了影响其性能的因素和机理。实验结果和显微结构分析表明:高固相含量浆料可浇注各种复杂器件,所得坯体强度高(89MPa)、组织结构均匀。
     在Fe-Al/Al2O3复合材料中,随着Fe-Al含量的增加,浆料粘度变大,固相含量减小,也使粉料的分散变得困难。但是坯体强度不与Fe-Al的含量成正比,当Fe-Al的含量为10%时,所得坯体结构均匀紧密。
Fe-Al/Al2O3 composite is a material which is compounded by Al2O3 as matrix and iron-aluminized as toughnessing and strengthening phase. Ceramic strengthened and toughnessed by iron-aluminized don’t have the disadvantage of which by fiber, whisker and metallic grain. It shows the advantage of iron-aluminized as semi-ceramic material that it has good consistence with alumina.
     Now the major method of the preparation of Fe-Al/Al2O3 composite is mechanical alloying and pressing sintering. First of all, the Fe-Al inter-metallic compounds powder is prepared by mechanical alloying. And it is mixed with alumina. The mixed powder is formed by pressing sintering. This forming method is easy , but it can’t be used in complex formation. The sintering parts need later machining and this increases production cost.
     The forming process of gel-casting of Fe-Al/Al2O3 composite was provided, wherein, slurry of composite powder in good dispersion was casted in a mould with the organic system,which could be caused the polymerization and made the slurry in-situ formation. This process can promise the uniformity of the powder dispersion,which also gave the green body in high strength. Further, the process is optimized by decreasing the amount of organic substances so that a large amount of time was saving for giving away the organics.
     The Fe-Al inter-metallic compounds powder is prepared by mechanical alloying and sintering. The best techniques are the ball milling time is 40h and the holding time is 2h at 750℃.
     For the requirement of in-situ forming and machining process, the solid content of slurry more than 50%(by volume)is needed. Otherwise, the critical point is to obtain thick suspension in good fluidity. The effect of solid content,dispersant and pH to the fluidity were discussed in the present thesis. The study showed that Fe-Al/Al2O3 composite slurry of 58%(by volume)in solid content with viscosity 800mPa.s was obtained by adding the dispersant of MN with pH7, which gave the green body with good performance by casting, for example, the three point bending strength was more than 89MPa.By scanning on the broken surface,the SEM picture showed that the inner of the green body was well dispersed without co-aggregation. The effects of initiator and temperature on the gelation time were also discussed in the present study. The experiment showed after adding initiator 10%(by volume), the gelation time is suitable. The study also included the process of dryness and discussing how to reduce time and remove shortage.
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