CN108178636A - 一种Si3N4/SiC复合吸波陶瓷及其制备方法 - Google Patents
一种Si3N4/SiC复合吸波陶瓷及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 54
- 229910003465 moissanite Inorganic materials 0.000 claims abstract description 52
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- 229910021389 graphene Inorganic materials 0.000 claims abstract description 23
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- 239000011268 mixed slurry Substances 0.000 claims description 8
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
本发明涉及一种Si3N4/SiC复合吸波陶瓷及其制备方法，属于吸波透波陶瓷复合材料制备技术领域，该复合吸波陶瓷物相组成为Si3N4、SiC和石墨烯；所述Si3N4、SiC和石墨烯的质量比为95：5：0‑0.3。本发明采用石墨烯对Si3N4/SiC复合吸波陶瓷进行改性，得到了性能优良的Si3N4/SiC复合吸波陶瓷材料；本发明相较于其他烧结工艺制备的Si3N4/SiC复合吸波陶瓷的过程中，原材料之间没有发生任何反应；通过严格控制原料配比及烧结制备条件，避免了石墨烯的石墨化。
Description
技术领域
本发明涉及一种Si3N4/SiC复合吸波陶瓷及其制备方法，属于吸波透波陶瓷复合材料制备技术领域。
背景技术
SiC粉体吸波剂具有吸收频带宽、抗氧化性好、高温性能稳定的特性，是一种介电损耗型吸波剂。在SiC粉体中掺杂N后，SiC 晶格中固溶的N原子取代C原子形成晶格缺陷，由于N为三价，只能与三个Si原子成键，另一个Si原子将剩余一个不能成键的价电子，形成一个带负电的缺陷。这个电子可在 N原子周围的四个Si原子上运动，在电磁场中该电子的位置也会随电磁场方向变化而发生位移。随电磁场频率增加，电子位移运动滞后于电场出现强烈极化弛豫，该强烈极化弛豫能显著提高SiC对电磁波的损耗能力。
近年来，对于以 Si3N4为基本组成的复合陶瓷材料，一方面继续改进热压、反应烧结制备工艺和技术，另一方面也在无压烧结工艺和材料的基础组成方面进行了大量的研究工作。但是对Si3N4/SiC复合吸波陶瓷的研究相对较少，且制备的复合材料性能有待进一步的提高。
发明内容
本发明的目的在于提供一种Si3N4/SiC复合吸波陶瓷。
本发明还提供了一种Si3N4/SiC复合吸波陶瓷的制备方法，该方法利用冷等静压和气氛压力烧结的制备工艺，制备的复合吸波陶瓷，具有良好的微观结构、力学性能。
本发明为了实现上述目的所采用的技术方案为：
本发明提供了一种Si3N4/SiC复合吸波陶瓷，该复合吸波陶瓷物相组成为Si3N4、SiC和石墨烯；
所述Si3N4、SiC和石墨烯的质量比为95：5：0-0.3。
本发明还提供了一种Si3N4/SiC复合吸波陶瓷的制备方法，包括以下步骤：
（1）制备Si3N4/SiC复合吸波陶瓷的生坯：将Si3N4粉末、SiC粉体、石墨烯和无水乙醇混合，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氮化硅球，分散剂为1wt%聚乙二醇；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过造粒、陈腐24h后过200目筛备用；将混合粉末利用压片机预成型样品，再利用冷等静压机制备Si3N4/SiC生坯；
（2）烧结：生坯于高纯氮气气氛中高温烧结，得Si3N4/SiC复合吸波陶瓷。
进一步的，所述Si3N4粉末、SiC粉体、石墨烯及无水乙醇的质量比为95：5：0～0.3：20。
进一步的，所述Si3N4粉末的平均粒径为300nm；所述SiC粉体的平均粒径为200nm。
进一步的，所述压片机的成型压力为10MPa，保压时间2min。
本发明步骤（1）中，利用冷等静压机制备Si3N4/SiC生坯为200MPa下保压2min。
进一步的，所述高温烧结为1650-1750℃、0.1-4MPa条件下烧结1-2h，升温速度为10℃/分钟。
通过本发明提供的制备方法制备的Si3N4/SiC复合吸波陶瓷，在氮化硅、碳化硅和石墨烯在烧结过程中，在压力的作用下坯体达到致密烧结；由于石墨烯在高温压力作用下可能会发生石墨化，从而对材料的性能起到降低的作用。本发明制备的Si3N4/SiC复合吸波陶瓷，相对密度为97.66-99.63%；抗弯强度为329.11-443.19MPa。而且原材料之间没有发生任何反应，石墨烯也没有发生石墨化。
本发明相比现有技术的优越性在于：
（1）本发明采用石墨烯对Si3N4/SiC复合吸波陶瓷进行改性，得到了性能优良的Si3N4/SiC复合吸波陶瓷材料；
（2）本发明相较于其他烧结工艺制备的Si3N4/SiC复合吸波陶瓷的过程中，原材料之间没有发生任何反应；通过严格控制原料配比及烧结制备条件，避免了石墨烯的石墨化。
附图说明
图1为实施例1中添加石墨烯之后Si3N4/SiC混合粉料的SEM照片；
图2为实施例1中Si3N4/SiC复合吸波陶瓷的XRD图谱；
图3为实施例1中Si3N4/SiC复合吸波陶瓷的断面低倍SEM图；
图4为实施例1中Si3N4/SiC复合吸波陶瓷的TEM图；
具体实施方式
下面通过具体的实施例对本发明的技术方案作进一步的解释和说明。
实施例1
将Si3N4粉末（平均粒径为300nm）、SiC粉体（平均粒径为200nm）、石墨烯和无水乙醇按照一定（95: 5: 0.3: 20）的质量比进行混合，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氮化硅球，分散剂为1wt%聚乙二醇；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过造粒、陈腐24h后过200目筛备用；称取一定质量的混合粉末，利用压片机预成型样品，再利用冷等静压机在200 MPa下保压2min；制备Si3N4/SiC生坯。生坯于高纯氮气气氛保护条件下、1750℃、4MPa条件下烧结2h，得产品；升温速度为10℃/分钟。其相对密度为99.63%；抗弯强度为443.18MPa。图1中为氮化硅和碳化硅粉体添加石墨烯之后的SEM照片，由此可以看出，本发明添加石墨烯后的混合粉料可以得到石墨烯混合均匀的粉料。图2为制得的Si3N4/SiC复合吸波陶瓷的样品XRD图谱，其物相组成主要为氮化硅、碳化硅和石墨烯，原材料之间没有发生反应；图3为样品断面的SEM图片，基本实现了致密化烧结，而且断面中呈现出片层状石墨烯结构；图4为Si3N4/SiC复合吸波陶瓷的TEM照片，石墨烯包裹在颗粒表面以及存在于颗粒之间的空隙之中，在其界面处形成包覆层，从而提高了其力学性能。
对比例1
将Si3N4粉末（平均粒径为300nm）、SiC粉体（平均粒径为200nm）和无水乙醇按照一定（95: 5: 20）的质量比进行混合，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氮化硅球，分散剂为1wt%聚乙二醇；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过造粒、陈腐24h后过200目筛备用；称取一定质量的混合粉末，利用压片机预成型样品，再利用冷等静压机在200 MPa下保压2min；制备Si3N4/SiC生坯。生坯于高纯氮气气氛保护条件下、1750℃、4MPa条件下烧结2h，得产品；升温速度为10℃/分钟。其相对密度为97.66%；抗弯强度为329.11MPa。
Claims (7)
1.一种Si3N4/SiC复合吸波陶瓷，其特征在于，该复合吸波陶瓷物相组成为Si3N4、SiC和石墨烯；
所述Si3N4、SiC和石墨烯的质量比为95：5：0-0.3。
2.一种Si3N4/SiC复合吸波陶瓷的制备方法，其特征在于，包括以下步骤：
（1）制备Si3N4/SiC复合吸波陶瓷的生坯：将Si3N4粉末、SiC粉体、石墨烯和无水乙醇混合，在室温下进行磁力搅拌及超声分散20min得到混合浆料；随后将混合浆料放入聚四氟乙烯罐中进行行星式球磨12小时，球磨介质为氮化硅球，分散剂为1wt%聚乙二醇；球磨后的浆料放入真空干燥箱中在80℃下干燥2h得混合粉体；然后经过造粒、陈腐24h后过200目筛备用；将混合粉末利用压片机预成型样品，再利用冷等静压机制备Si3N4/SiC生坯；
（2）烧结：生坯于高纯氮气气氛中高温烧结，得Si3N4/SiC复合吸波陶瓷。
3.根据权利要求2所述的制备方法，其特征在于，所述Si3N4粉末、SiC粉体、石墨烯及无水乙醇的质量比为95：5：0～0.3：20。
4.根据权利要求2所述的制备方法，其特征在于，所述Si3N4粉末的平均粒径为300nm；所述SiC粉体的平均粒径为200nm。
5.根据权利要求2-4任一项所述的制备方法，其特征在于，所述压片机的成型压力为10MPa，保压时间2min。
6.根据权利要求2-5任一项所述的制备方法，其特征在于，所述利用冷等静压机制备Si3N4/SiC生坯为200MPa下保压2min。
7.根据权利要求2、5或6所述的制备方法，其特征在于，所述高温烧结为1650-1750℃、0.1-4MPa条件下烧结1-2h，升温速度为10℃/分钟。
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