CN107827465A - 一种碳化硅陶瓷材料的制备方法 - Google Patents

一种碳化硅陶瓷材料的制备方法 Download PDF

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CN107827465A
CN107827465A CN201711410801.5A CN201711410801A CN107827465A CN 107827465 A CN107827465 A CN 107827465A CN 201711410801 A CN201711410801 A CN 201711410801A CN 107827465 A CN107827465 A CN 107827465A
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Abstract

本发明公开了一种碳化硅陶瓷材料的制备方法，涉及陶瓷材料技术领域，包括以下步骤：（1）碳化硅处理；（2）制备毛坯；（3）制得碳化硅陶瓷材料；本发明通过采用氧化铋包覆纳米石墨烯添加到陶瓷烧制中，能够有效的降低陶瓷材料的烧结温度，提高陶瓷材料的硬度和耐磨性，通过对碳化硅的处理，能够有效的降低陶瓷材料的体积密度以及耐磨性，通过添加氧化铋包覆纳米石墨烯的作用，能够使得陶瓷晶粒大小分布更加均匀，陶瓷孔隙率显著降低，孔径较小，晶界结合更加紧密，说明添加的氧化铋包覆纳米石墨烯能够有效的改善陶瓷材料内部微观结构。

Description

一种碳化硅陶瓷材料的制备方法
技术领域
本发明属于陶瓷材料技术领域，具体涉及一种碳化硅陶瓷材料的制备方法。
背景技术
目前主要的碳化硅烧结方法为反应烧结和无压烧结。反应烧结碳化硅陶瓷：处理温度低、时间短、不需特殊及昂贵设备；反应烧结坯件不收缩，尺寸不变；成型方法多，烧结过程无需加压，可制备大尺寸、形状复杂的制品。但碳化硅的密度高，制品较沉重，由于制品中较高的游离硅含量会增加制品的脆性，降低制品的强度，严重影响反应烧结碳化硅的力学性能。
发明内容
本发明的目的是针对现有的问题，提供了一种碳化硅陶瓷材料的制备方法。
本发明是通过以下技术方案实现的：
一种碳化硅陶瓷材料的制备方法，包括以下步骤：
（1）将海藻酸钠溶于乙醇溶液中，配制成质量分数为10%的海藻酸钠溶液，将碳化硅添加到海藻酸钠溶液中，进行研磨1.5-2小时，然后再添加到真空反应釜中，添加碳化硅质量3.5-3.8%的偶联剂，处理40-50min，然后进行过滤，烘干至恒重；
（2）将氧化铋包覆纳米石墨烯与炭黑、纳米氧化铝、碳化硅按:3-5:1-3：0.3-0.5：50-60质量比例混合均匀，并压制成型，制成素坯，将素坯在600-650℃下烧结30-40min，得到毛坯；
（3）将烧结后的毛坯在氮气气氛下，温度为1350-1450℃、2.5-4.5MPa压力下保温1.5-2.5小时后制得碳化硅陶瓷材料。
进一步的，所述步骤（1）中乙醇溶液质量分数为15%。
进一步的，所述步骤（1）中真空反应釜中真空度为0.025MPa。
进一步的，所述步骤（1）中偶联剂为有机硅烷偶联剂。
进一步的，所述步骤（2）中压制成型，成型压制的压力为10.5MPa。
进一步的，所述步骤（2）中氧化铋包覆纳米石墨烯制备方法为：
（1）按3:15.5的质量比例将纳米石墨烯、硝酸铋放入球磨罐，控制球料比为120：1，然后添加纳米石墨烯质量3.5倍的无水乙醇，球磨40min，然后进行干燥去除无水乙醇，得到固体混合物；
（2）向固体混合物中添加其质量0.38%的碳酸钠，然后再添加固体混合物质量0.5%的柠檬酸，搅拌均匀，继续球磨55min，得到混合物料；
（3）将混合物料置于马弗炉里，加热至780℃，保温35min，然后冷却至320℃，保温1小时，然后再自然冷却至室温，得到固体粉末，将固体粉末按1：5质量比例添加到无水乙醇中，以2000r/min转速搅拌50min，然后在30kHz超声波下处理10min，最后真空干燥至室温，再研磨，即得。
本发明相比现有技术具有以下优点：本发明通过采用氧化铋包覆纳米石墨烯添加到陶瓷烧制中，能够有效的降低陶瓷材料的烧结温度，提高陶瓷材料的硬度和耐磨性，通过对碳化硅的处理，能够有效的降低陶瓷材料的体积密度以及耐磨性，通过添加氧化铋包覆纳米石墨烯的作用，能够使得陶瓷晶粒大小分布更加均匀，陶瓷孔隙率显著降低，孔径较小，晶界结合更加紧密，说明添加的氧化铋包覆纳米石墨烯能够有效的改善陶瓷材料内部微观结构，有细化晶粒，促进气体排出，强化晶界结合强度的作用，降低陶瓷材料的脆性，良好的微观结构能够大幅度的改善陶瓷材料的性能。
具体实施方式
实施例1
一种碳化硅陶瓷材料的制备方法，包括以下步骤：
（1）将海藻酸钠溶于乙醇溶液中，配制成质量分数为10%的海藻酸钠溶液，将碳化硅添加到海藻酸钠溶液中，进行研磨1.5小时，然后再添加到真空反应釜中，添加碳化硅质量3.5%的偶联剂，处理40min，然后进行过滤，烘干至恒重；
（2）将氧化铋包覆纳米石墨烯与炭黑、纳米氧化铝、碳化硅按:3:1：0.3：50质量比例混合均匀，并压制成型，制成素坯，将素坯在600℃下烧结30min，得到毛坯；
（3）将烧结后的毛坯在氮气气氛下，温度为1350℃、2.5MPa压力下保温1.5小时后制得碳化硅陶瓷材料。
进一步的，所述步骤（1）中乙醇溶液质量分数为15%。
进一步的，所述步骤（1）中真空反应釜中真空度为0.025MPa。
进一步的，所述步骤（1）中偶联剂为有机硅烷偶联剂。
进一步的，所述步骤（2）中压制成型，成型压制的压力为10.5MPa。
进一步的，所述步骤（2）中氧化铋包覆纳米石墨烯制备方法为：
（1）按3:15.5的质量比例将纳米石墨烯、硝酸铋放入球磨罐，控制球料比为120：1，然后添加纳米石墨烯质量3.5倍的无水乙醇，球磨40min，然后进行干燥去除无水乙醇，得到固体混合物；
（2）向固体混合物中添加其质量0.38%的碳酸钠，然后再添加固体混合物质量0.5%的柠檬酸，搅拌均匀，继续球磨55min，得到混合物料；
（3）将混合物料置于马弗炉里，加热至780℃，保温35min，然后冷却至320℃，保温1小时，然后再自然冷却至室温，得到固体粉末，将固体粉末按1：5质量比例添加到无水乙醇中，以2000r/min转速搅拌50min，然后在30kHz超声波下处理10min，最后真空干燥至室温，再研磨，即得。
实施例2
一种碳化硅陶瓷材料的制备方法，包括以下步骤：
（1）将海藻酸钠溶于乙醇溶液中，配制成质量分数为10%的海藻酸钠溶液，将碳化硅添加到海藻酸钠溶液中，进行研磨2小时，然后再添加到真空反应釜中，添加碳化硅质量3.8%的偶联剂，处理50min，然后进行过滤，烘干至恒重；
（2）将氧化铋包覆纳米石墨烯与炭黑、纳米氧化铝、碳化硅按:5:3：0.5：60质量比例混合均匀，并压制成型，制成素坯，将素坯在600-650℃下烧结40min，得到毛坯；
（3）将烧结后的毛坯在氮气气氛下，温度为1450℃、4.5MPa压力下保温2.5小时后制得碳化硅陶瓷材料。
进一步的，所述步骤（1）中乙醇溶液质量分数为15%。
进一步的，所述步骤（1）中真空反应釜中真空度为0.025MPa。
进一步的，所述步骤（1）中偶联剂为有机硅烷偶联剂。
进一步的，所述步骤（2）中压制成型，成型压制的压力为10.5MPa。
进一步的，所述步骤（2）中氧化铋包覆纳米石墨烯制备方法为：
（1）按3:15.5的质量比例将纳米石墨烯、硝酸铋放入球磨罐，控制球料比为120：1，然后添加纳米石墨烯质量3.5倍的无水乙醇，球磨40min，然后进行干燥去除无水乙醇，得到固体混合物；
（2）向固体混合物中添加其质量0.38%的碳酸钠，然后再添加固体混合物质量0.5%的柠檬酸，搅拌均匀，继续球磨55min，得到混合物料；
（3）将混合物料置于马弗炉里，加热至780℃，保温35min，然后冷却至320℃，保温1小时，然后再自然冷却至室温，得到固体粉末，将固体粉末按1：5质量比例添加到无水乙醇中，以2000r/min转速搅拌50min，然后在30kHz超声波下处理10min，最后真空干燥至室温，再研磨，即得。
实施例3
一种碳化硅陶瓷材料的制备方法，包括以下步骤：
（1）将海藻酸钠溶于乙醇溶液中，配制成质量分数为10%的海藻酸钠溶液，将碳化硅添加到海藻酸钠溶液中，进行研磨1.8小时，然后再添加到真空反应釜中，添加碳化硅质量3.6%的偶联剂，处理45min，然后进行过滤，烘干至恒重；
（2）将氧化铋包覆纳米石墨烯与炭黑、纳米氧化铝、碳化硅按:4:2：0.4：55质量比例混合均匀，并压制成型，制成素坯，将素坯在620℃下烧结36min，得到毛坯；
（3）将烧结后的毛坯在氮气气氛下，温度为1390℃、2.8MPa压力下保温1.8小时后制得碳化硅陶瓷材料。
进一步的，所述步骤（1）中乙醇溶液质量分数为15%。
进一步的，所述步骤（1）中真空反应釜中真空度为0.025MPa。
进一步的，所述步骤（1）中偶联剂为有机硅烷偶联剂。
进一步的，所述步骤（2）中压制成型，成型压制的压力为10.5MPa。
进一步的，所述步骤（2）中氧化铋包覆纳米石墨烯制备方法为：
（1）按3:15.5的质量比例将纳米石墨烯、硝酸铋放入球磨罐，控制球料比为120：1，然后添加纳米石墨烯质量3.5倍的无水乙醇，球磨40min，然后进行干燥去除无水乙醇，得到固体混合物；
（2）向固体混合物中添加其质量0.38%的碳酸钠，然后再添加固体混合物质量0.5%的柠檬酸，搅拌均匀，继续球磨55min，得到混合物料；
（3）将混合物料置于马弗炉里，加热至780℃，保温35min，然后冷却至320℃，保温1小时，然后再自然冷却至室温，得到固体粉末，将固体粉末按1：5质量比例添加到无水乙醇中，以2000r/min转速搅拌50min，然后在30kHz超声波下处理10min，最后真空干燥至室温，再研磨，即得。
对比例1：与实施例1区别仅在于不经过步骤（1）处理。
对比例2：与实施例1区别仅在于不添加氧化铋包覆纳米石墨烯。
对比例3：与实施例1区别仅在于将氧化铋包覆纳米石墨烯替换为等量的纳米石墨烯。
对实施例与对比例制备的陶瓷（10cm×5cm×0.5cm）的耐磨性据行业标准JC/T848.1-1999测试；
表1
由表1可以看出，本发明制备的陶瓷材料具有优异的耐磨性和抗压强度。

Claims (6)

1.一种碳化硅陶瓷材料的制备方法，其特征在于，包括以下步骤：
（1）将海藻酸钠溶于乙醇溶液中，配制成质量分数为10%的海藻酸钠溶液，将碳化硅添加到海藻酸钠溶液中，进行研磨1.5-2小时，然后再添加到真空反应釜中，添加碳化硅质量3.5-3.8%的偶联剂，处理40-50min，然后进行过滤，烘干至恒重；
（2）将氧化铋包覆纳米石墨烯与炭黑、纳米氧化铝、碳化硅按:3-5:1-3：0.3-0.5：50-60质量比例混合均匀，并压制成型，制成素坯，将素坯在600-650℃下烧结30-40min，得到毛坯；
（3）将烧结后的毛坯在氮气气氛下，温度为1350-1450℃、2.5-4.5MPa压力下保温1.5-2.5小时后制得碳化硅陶瓷材料。
2.如权利要求1所述的一种碳化硅陶瓷材料的制备方法，其特征在于，所述步骤（1）中乙醇溶液质量分数为15%。
3.如权利要求1所述的一种碳化硅陶瓷材料的制备方法，其特征在于，所述步骤（1）中真空反应釜中真空度为0.025MPa。
4.如权利要求1所述的一种碳化硅陶瓷材料的制备方法，其特征在于，所述步骤（1）中偶联剂为有机硅烷偶联剂。
5.如权利要求1所述的一种碳化硅陶瓷材料的制备方法，其特征在于，所述步骤（2）中压制成型，成型压制的压力为10.5MPa。
6.如权利要求1所述的一种碳化硅陶瓷材料的制备方法，其特征在于，所述步骤（2）中氧化铋包覆纳米石墨烯制备方法为：
（1）按3:15.5的质量比例将纳米石墨烯、硝酸铋放入球磨罐，控制球料比为120：1，然后添加纳米石墨烯质量3.5倍的无水乙醇，球磨40min，然后进行干燥去除无水乙醇，得到固体混合物；
（2）向固体混合物中添加其质量0.38%的碳酸钠，然后再添加固体混合物质量0.5%的柠檬酸，搅拌均匀，继续球磨55min，得到混合物料；
（3）将混合物料置于马弗炉里，加热至780℃，保温35min，然后冷却至320℃，保温1小时，然后再自然冷却至室温，得到固体粉末，将固体粉末按1：5质量比例添加到无水乙醇中，以2000r/min转速搅拌50min，然后在30kHz超声波下处理10min，最后真空干燥至室温，再研磨，即得。
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