CN107382351A - 一种热解碳增韧的C/SiC陶瓷基复合材料及制备方法 - Google Patents

一种热解碳增韧的C/SiC陶瓷基复合材料及制备方法 Download PDF

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CN107382351A
CN107382351A CN201710604509.0A CN201710604509A CN107382351A CN 107382351 A CN107382351 A CN 107382351A CN 201710604509 A CN201710604509 A CN 201710604509A CN 107382351 A CN107382351 A CN 107382351A
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Abstract

一种包括石墨烯的多相增韧碳化硅陶瓷的制备方法,其特征在于下述顺序的步骤:(1)的碳化硅粉末和氧化铝颗粒以及碳化硅粉,碳黑粉末,聚乙烯醇和石墨烯粉混合;(2)将粉体进行球磨混合,加入水均匀混合制成浆料,注入到压力为0.01MPa~1MPa的真空压力罐中处理;(3)处理好的浆料放置到模具中,模压成型制成胚体,在70℃~90℃炉中进行干燥;(4)将干燥好的胚体放入真空烧结炉中,炉内压强为0.01MPa~0.1MPa,将炉内温度升至1200℃~2000℃,保温时间为1h~4h,然后降温至100℃~200℃取出;(5)烧制完成的产品进过一系列的后加工,制成成品。该方法制得的碳化硅陶瓷增韧效果高于单一氧化铝颗粒增韧,增韧效果与石墨烯增韧效果相当显著高于一般陶瓷材料,制作成本降低。

Description

一种热解碳增韧的C/SiC陶瓷基复合材料及制备方法
技术领域
本发明涉及一种包括石墨烯的多相增韧碳化硅陶瓷制备方法,特别是涉及一种包括石墨烯和氧化铝颗粒增韧碳化硅陶瓷的制备方法。
背景技术
碳化硅陶瓷材料具有高温强度大、高温抗氧化性强、耐磨损性能好、热稳定性佳、热膨胀系数小、热导率大、硬度高、抗热震和耐化学腐蚀等优良特性,在汽车、机械化工、环境保护、空间技术、信息电子、能源等领域有着日益广泛的应用,已经成为一种在很多工业领域性能优异的其他材料不可替代的结构陶瓷。
航空航天、原子能工业等需要耐受超高温度的场合如核裂变和核聚变反应堆中需要的可承受2000℃左右高温的耐热材料火箭和航天飞行器表面用于耐受与大气剧烈摩擦中产生的高达数千温度的隔热瓦火箭发动机燃烧室喉衬和内衬材料,燃气涡轮叶片高温炉的顶板、支架,以及高温实验用的卡具等高温构件也普遍采用碳化硅陶瓷构件。碳化硅陶瓷在石油化学工业中还被广泛地用作各种耐腐蚀用容器和管道。要进一步提高碳化硅陶瓷的性能,如何解决脆性问题,是一个关注的焦点。
公开号为CN101172875A的中国专利公开了一种多形态氧化铝颗粒组合增韧碳化硅陶瓷的制备方法。所述碳化硅陶瓷增韧的方法是利用多种形态氧化铝颗粒的组合作为增韧料,通过片状增韧颗粒拔出效应以及棒状增韧颗粒拔出效应达到有益的增韧。该多形态氧化铝颗粒组合增韧碳化硅陶瓷的制备方法,具有一定的陶瓷增韧效果,增韧料价格便宜,可用于较高压力应变较低的场合。
公开号CN105801154A的中国发明专利公开了一种石墨烯增韧碳化硅陶瓷复合材料的制备方法。所述碳化硅陶瓷增韧的方法是通过碳热还原反应,原位生长碳化硅晶须及颗粒,提高界面强度和抗氧化能力,产生界面强化作用,增加裂纹扩展阻力,进一步改善陶瓷断裂韧性。但由于石墨烯价格昂贵,限制应用范围。
以上两个专利,在多相增韧碳化硅陶瓷制备的成本和增韧效果的控制中,不能有效的降低石墨烯的使用量减少成本,提高碳化硅陶瓷的韧性,难以制备出一种符合现代高压环境下使用的增韧碳化硅陶瓷,因此急需一种新型低成本的可应用于高压环境的增韧碳化硅陶瓷制备方法。
发明内容
本发明的目的旨在克服现有技术的不足,提供一种包括石墨烯的多相增韧碳化硅陶瓷制备方法,制作成本降低,碳化硅陶瓷增韧效果高于单一氧化铝颗粒增韧,增韧效果与石墨烯增韧效果相当。
为实现本发明的目的所采用的技术方案是:一种包括石墨烯的多相增韧碳化硅陶瓷制备方法,该制造方法的原料是碳化硅粉、烧结助剂、增韧料以及结合剂,经混合、成型、固化、高温烧结等主要工艺步骤,形成碳化硅陶瓷产品,原料中含有的增韧料是为增加碳化硅陶瓷的韧性而加入的物料,所述高温烧结工艺步骤的烧结方式是反应烧结。
一种包括石墨烯的多相增韧碳化硅陶瓷的制备方法,其特征在于下述顺序的步骤:
(1)将4%~6%质量粒度为1~10μm的碳化硅粉末纯度>99%和3%~10%质量粒度为0.1~2μm的氧化铝颗粒以及65%~80%质量粒度为20~80μm的碳化硅粉,粉末纯度>99%;1%~2%质量的碳黑粉末,0.2%~0.6%质量的聚乙烯醇浓度为55%~70%和2%~12%质量粒度为2~10μm的石墨烯粉混合;
(2)将粉体进行球磨混合,加入粉末质量20%~35%的水均匀混合制成浆料,注入到压力为0.01MPa~1MPa的真空压力罐中处理;
(3)处理好的浆料放置到模具中,模压成型制成胚体,在70℃~90℃炉中进行干燥;
(4)将干燥好的胚体放入真空烧结炉中,炉内压强为0.01MPa~0.1MPa,以4~8℃/min的速度将炉内温度升至1200℃~2000℃,保温时间为1h~4h,然后降温至100℃~200℃取出;
(5)烧制完成的产品进过一系列的后加工,制成成品。
本发明的有益效果是:碳化硅陶瓷增韧效果高于单一氧化铝颗粒增韧,增韧效果与石墨烯增韧效果相当显著高于一般陶瓷材料,断裂韧性提高到7.0 MPa·m1/2制作成本降低。
具体实施方式
下面结合具体实施例,进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。
实施例1
一种包括石墨烯的多相增韧碳化硅陶瓷的制备方法,该制造方法的原料是碳化硅粉、烧结助剂、增韧料以及结合剂,经混合、成型、固化、高温烧结等主要工艺步骤,形成碳化硅陶瓷产品,原料中含有的增韧料是为增加碳化硅陶瓷的韧性而加入的物料,所述高温烧结工艺步骤的烧结方式是反应烧结,其特征在于下述顺序的步骤:
(1)将6%质量粒度为2μm的碳化硅粉末纯度>99%和10%质量粒度为0.8μm的氧化铝颗粒以及70%质量粒度为25μm的碳化硅粉,粉末纯度>99%;1.4%质量的碳黑粉末,0.6%质量的聚乙烯醇浓度为55%~70%和12%质量粒度为2~10μm的石墨烯粉混合;
(2)将粉体进行球磨混合,加入粉末质量35%的水均匀混合制成浆料,注入到压力为0.08MPa的真空压力罐中处理;
(3)处理好的浆料放置到模具中,模压成型制成胚体,在80℃炉中进行干燥;
(4)将干燥好的胚体放入真空烧结炉中,炉内压强为0.1MPa,以6℃/min的速度将炉内温度升至1800℃,保温时间为3h,然后降温至150℃取出;
(5)烧制完成的产品进过一系列的后加工,制成成品。
实施例2
一种包括石墨烯的多相增韧碳化硅陶瓷的制备方法,该制造方法的原料是碳化硅粉、烧结助剂、增韧料以及结合剂,经混合、成型、固化、高温烧结等主要工艺步骤,形成碳化硅陶瓷产品,原料中含有的增韧料是为增加碳化硅陶瓷的韧性而加入的物料,所述高温烧结工艺步骤的烧结方式是反应烧结,其特征在于下述顺序的步骤:
(1)将4%质量粒度为2μm的碳化硅粉末纯度>99%和8%质量粒度为0.8μm的氧化铝颗粒以及74%质量粒度为25μm的碳化硅粉,粉末纯度>99%;1.5%质量的碳黑粉末,0.5%质量的聚乙烯醇浓度为55%~70%和10%质量粒度为2~10μm的石墨烯粉混合;
(2)将粉体进行球磨混合,加入粉末质量28%的水均匀混合制成浆料,注入到压力为0.1MPa的真空压力罐中处理;
(3)处理好的浆料放置到模具中,模压成型制成胚体,在70℃炉中进行干燥;
(4)将干燥好的胚体放入真空烧结炉中,炉内压强为0.08MPa,以7℃/min的速度将炉内温度升至1600℃,保温时间为4h,然后降温至180℃取出;
(5)烧制完成的产品进过一系列的后加工,制成成品。
上述仅为本发明的两个具体实施方式,但本发明的设计构思并不局限于此,凡利用此构思对本发明进行非实质性的改动,均应属于侵犯本发明保护的范围的行为。但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何形式的简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。

Claims (4)

1.一种包括石墨烯的多相增韧碳化硅陶瓷的制备方法,其特征在于下述顺序的步骤:
将4%~6%质量粒度为1~10μm的碳化硅粉末纯度>99%和3%~10%质量粒度为0.1~2μm的氧化铝颗粒以及65%~80%质量粒度为20~80μm的碳化硅粉,粉末纯度>99%,1%~2%质量的碳黑粉末,0.2%~0.6%质量的聚乙烯醇浓度为55%~70%和2%~12%质量粒度为2~10μm的石墨烯粉混合;
将粉体进行球磨混合,加入粉末质量20%~35%的水均匀混合制成浆料,注入到压力为0.01MPa~1MPa的真空压力罐中处理;
处理好的浆料放置到模具中,模压成型制成胚体,在70℃~90℃炉中进行干燥;
将干燥好的胚体放入真空烧结炉中,炉内压强为0.01MPa~0.1MPa,以4~8℃/min的速度将炉内温度升至1200℃~2000℃,保温时间为1h~4h,然后降温至100℃~200℃取出;
烧制完成的产品进过一系列的后加工,制成成品。
2.根据权利要求书1所述的增韧碳化硅陶瓷的制备方法,其特征在于所述的烧结方法不仅限于真空烧结,还包括其他陶瓷材料烧结方式。
3.根据权利要求书1所述的增韧碳化硅陶瓷的制备方法,其特征在于所述的陶瓷胚体干燥时间要根据陶瓷胚体的具体尺寸厚度进行确定。
4.根据权利要求书1所述的增韧碳化硅陶瓷的制备方法,其特征在于所述的粉体混合不仅限于球磨混合,只要求将粉末混合均匀。
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