CN110372387B - 一种碳化硅石墨烯复合材料制备方法 - Google Patents

一种碳化硅石墨烯复合材料制备方法 Download PDF

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CN110372387B
CN110372387B CN201910722666.0A CN201910722666A CN110372387B CN 110372387 B CN110372387 B CN 110372387B CN 201910722666 A CN201910722666 A CN 201910722666A CN 110372387 B CN110372387 B CN 110372387B
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贺刚
封立杰
封立征
刘岩
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Abstract

本发明属于陶瓷复合材料领域，具体涉及一种碳化硅石墨烯复合材料制备方法，本发明的一种碳化硅石墨烯复合材料制备方法，其特征在于将SiC、Al2O3、Mg的混合粉体压制成块体，在二氧化碳气氛下进行两步烧结，冷却后得到碳化硅‑石墨烯复合材料，本发明的碳化硅石墨烯复合材料制备方法，具有工艺简单、制备周期短、成本低等优点。

Description

一种碳化硅石墨烯复合材料制备方法
技术领域
本发明属于陶瓷复合材料技术领域，具体涉及一种碳化硅石墨烯复合材料制备方法。
背景技术
碳化硅 ( SiC ) 是结构陶瓷材料的典范，具有高温强度大、抗氧化性强、耐磨损性好、热膨胀系数小、热导率大、硬度高以及抗热震和耐化学腐蚀等优良特性，被广泛应用于航空航天、机械工业、石油化工等领域。相较于氮化硅、氧化锆陶瓷而言，较低的断裂韧性限制了碳化硅陶瓷的高端应用。氮化硅陶瓷因晶须互锁微结构特征，典型的断裂韧性值>7MPa·m1/2。氧化锆因其特有的相变增韧机制，其断裂韧性值>10MPa·m1/2。而碳化硅陶瓷典型的断裂韧性值为3~5MPa·m1/2。
为提高碳化硅陶瓷的韧性，国际范围内开展了广泛的研究，主要对策包括：纤维增韧、复相增韧和微结构调控等机制。其中碳纤维增韧碳化硅陶瓷，已表现出显著的优化效果，在飞机刹车片、超高温结构部件和核电材料领域获得高度关注，但较高的制备成本限制了其规模应用。近年来，兴起的石墨烯材料，在陶瓷材料领域也引发了研究热潮。石墨烯其优异的机械性能，被视为提升陶瓷材料韧性的一个理想选择。将石墨烯引入碳化硅陶瓷，通过石墨烯的拔出和裂纹偏转，有望实现碳化硅陶瓷材料韧性的显著提高。
目前，主要通过粉末冶金工艺路线来制备碳化硅-石墨烯复合材料。在SiC与石墨烯研磨混合过程中，不可避免破坏石墨烯结构，并存在团聚混合不均的现象，最终不能发挥石墨烯的增韧效果，且该制备方法周期长、工艺复杂、成本高。已报道燃烧合成的方法[CN201711308507.3]，虽然能够原位反应生成石墨烯，但燃烧波蔓延的非平衡特征，使得无法获得稳定的温度场，导致生成的石墨烯均匀性差，影响制得复合材料的性能。此外，由于石墨烯抑制晶界扩散传质的作用，常规烧结方法难以获得致密的碳化硅-石墨烯复合材料。
为解决以上技术难题，本发明提供一种碳化硅石墨烯复合材料制备方法，实现高韧性碳化硅-石墨烯复合材料的制备。
发明内容
本发明的目的是提供一种碳化硅石墨烯复合材料制备方法。
本发明的一种碳化硅石墨烯复合材料制备方法为：将SiC、Al2O3、Mg的混合粉体压制成块体，在二氧化碳气氛下进行两步烧结，冷却后得到碳化硅-石墨烯复合材料。
优选的，按重量份数计，所述混合粉体中SiC粉为80~90份，Al2O3粉为5~10份，Mg粉为5~10份。
优选的，所述压制块体的压力为100~200MPa。
优选的，所述二氧化碳气氛的压力为0.1~1MPa。
优选的，所述两步烧结为：先从室温升温至2100℃后，保温20-30min，然后降温至1800~2000℃，保温时间4~8h。
优选的，所述碳化硅-石墨烯复合材料的相对密度为99.1-99.5%，抗弯强度为450~550MPa，断裂韧性为5~7 MPa·m1/2。
另外，如无特殊说明，本发明所记载的任何范围包括端值以及端值之间的任何数值以及端值或者端值之间的任意数值所构成的任意子范围。
本发明的有益效果在于：本发明的碳化硅石墨烯复合材料制备方法，使用单质Mg粉为原料，在二氧化碳气氛中，均匀的温度场下原位反应生成石墨烯和氧化镁，石墨烯均匀分散于陶瓷基体，氧化镁作为碳化硅的烧结助剂，采用两步烧结首先在高温下激活晶界传质，在降低温度保温烧结，实现碳化硅-石墨烯复合材料的致密化。该制备方法具有工艺简单、制备周期短、成本低等优点。
附图说明
图1为实施例1的碳化硅-石墨烯复合材料的Raman图谱。
具体实施方式
下面结合实施例及附图对本发明做进一步的说明，但本发明并不局限于下面所述的内容。
实施例1
将SiC、Al2O3、Mg原料粉末分别按90、5、5的重量份数称量混合后，在100MPa压力下压制成块体，在0.1MPa的二氧化碳气氛下升温至2100℃后降温至2000℃烧结保温8h，冷却后得到碳化硅-石墨烯复合材料。
对得到的块体进行Raman光谱测试，结果如图1所示，结果表明，产物中生成了石墨烯。采用排水法测得块体样品相对密度为99.5%，对块体样品加工后，采用三点抗弯法测得强度其为550MPa，采用单边切开梁法测得起断裂韧性为5.0MPa·m1/2。
实施例2
将SiC、Al2O3、Mg原料粉末分别按85、8、7的重量份数称量混合后，在150MPa压力下压制成块体，在0.5MPa的二氧化碳气氛下升温至2100℃后降温至1900℃烧结保温6h，冷却后得到碳化硅-石墨烯复合材料。
对得到的块体进行Raman光谱测试，结果表明，产物中生成了石墨烯。采用排水法测得块体样品相对密度为99.2%，对块体样品加工后，采用三点抗弯法测得强度其为500MPa，采用单边切开梁法测得起断裂韧性为6.0MPa·m1/2。
实施例3
将SiC、Al2O3、Mg原料粉末分别按80、10、10的重量份数称量混合后，在200MPa压力下压制成块体，在1.0MPa的二氧化碳气氛下升温至2100℃后降温至1800℃烧结保温4h，冷却后得到碳化硅-石墨烯复合材料。
对得到的块体进行Raman光谱测试，结果表明，产物中生成了石墨烯。采用排水法测得块体样品相对密度为99.1%，对块体样品加工后，采用三点抗弯法测得强度其为450MPa，采用单边切开梁法测得起断裂韧性为5.5MPa·m1/2。
实施例4
将SiC、Al2O3、Mg原料粉末分别按85、5、10的重量份数称量混合后，在100MPa压力下压制成块体，在1.0MPa的二氧化碳气氛下升温至2100℃后降温至1900℃烧结保温6h，冷却后得到碳化硅-石墨烯复合材料。
对得到的块体进行Raman光谱测试，结果表明，产物中生成了石墨烯。采用排水法测得块体样品相对密度为99.3%，对块体样品加工后，采用三点抗弯法测得强度其为520MPa，采用单边切开梁法测得起断裂韧性为7.0MPa·m1/2。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定，对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动，这里无法对所有的实施方式予以穷举，凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。

Claims (3)

1.一种碳化硅石墨烯复合材料制备方法，其特征在于：将SiC、Al2O3、Mg的混合粉体压制成块体，在二氧化碳气氛下进行两步烧结，冷却后得到碳化硅-石墨烯复合材料，所述压制块体的压力为100~200MPa，所述两步烧结为：先从室温升温至2100℃后，保温20-30min，然后降温至1800~2000℃，保温时间4~8h，按重量份数计，所述混合粉体中SiC粉为80~90份，Al2O3粉为5~10份，Mg粉为5~10份。
2.根据权利要求1所述的碳化硅石墨烯复合材料制备方法，其特征是：所述二氧化碳气氛的压力为0.1~1MPa。
3.根据权利要求1所述的碳化硅石墨烯复合材料制备方法，其特征是：所述碳化硅-石墨烯复合材料的相对密度为99.1-99.5%，抗弯强度为450~550MPa，断裂韧性为5~7 MPa·m1 /2。
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