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CN113307644A - 一种氮化改性反应烧结碳化硅陶瓷表面的方法 - Google Patents

一种氮化改性反应烧结碳化硅陶瓷表面的方法 Download PDF

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CN113307644A
CN113307644A CN202110669667.0A CN202110669667A CN113307644A CN 113307644 A CN113307644 A CN 113307644A CN 202110669667 A CN202110669667 A CN 202110669667A CN 113307644 A CN113307644 A CN 113307644A
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silicon carbide
reaction
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马丽
孙珊
龚红宇
马坤
龚志刚
李志涛
龚星宇
袁洪峰
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Shantian Abrasive Co ltd
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Abstract

本发明涉及一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法，反应烧结碳化硅陶瓷包括碳化硅、炭黑、碳纤维、粘结剂、分散剂、去离子水；所述粘结剂为羧甲基纤维素和PAF‑Ⅱ型粉状粘结剂以任意比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以任意比混合。制备方法包括混料、醒料、烧结和表面处理。本发明是在一定压力下通入流动的氮气，使氮气与游离硅反应生成硅和氮的化合物，提高反应烧结碳化硅的使用寿命和耐腐蚀能力。

Description

一种氮化改性反应烧结碳化硅陶瓷表面的方法
技术领域
本发明涉及一种氮化改性反应烧结碳化硅陶瓷表面的方法，属于碳化硅改性技术领域。
背景技术
碳化硅具有高硬度、高温强度大、抗氧化性好、热稳定性好、热膨胀系数低、热导率大及耐腐蚀性好等优良特性，因此，可以用作密封环、研磨介质、研磨盘、防弹板、喷嘴、磁力泵泵件、窑炉中的辊棒等。对于碳化硅陶瓷的制备有无压烧结、热压烧结、热等静压烧结、放电等离子烧结、反应烧结等，其中反应烧结制备碳化硅陶瓷，其烧结温度低、制品的尺寸收缩小、致密度高、经济效益好、工业成本较低，但是由于反应烧结需利用熔融硅浸渗含碳的碳化硅陶瓷素坯，使所制得的陶瓷制品中含有游离硅。由于硅的熔点为1400℃，因此游离硅在反应烧结碳化硅中的存在缩短了反应烧结碳化硅在高温下的使用寿命而且其耐腐蚀性能也大幅度下降。
专利文献CN110304933A公开了PyC-SiCW表面的热解碳涂层在反应烧结过程中与液硅发生反应在PyC-SiCW表面原位生成一层SiC涂层，SiC涂层将SiCW与高温液硅相互隔离，避免了高温下液硅对SiCW的侵蚀损伤。本发明采用的是在陶瓷的表面形成SiC涂层来增加其陶瓷的抗侵蚀性；而本发明的目的是减少游离硅的含量，提高反应烧结碳化硅的耐腐蚀性，就是将反应烧结碳化硅陶瓷中的游离硅和氮气反应生成氮化硅。目前对于反应烧结碳化硅表面处理的文献很少，尤其是采用氮气来处理反应烧结碳化硅陶瓷的表面。
发明内容
本发明针对反应烧结碳化硅作为窑炉辊棒，在高温下抗锂电腐蚀性差的问题，提出一种低成本、易实现的一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法。本发明的技术方案如下：
一种表面氮化改性的反应烧结碳化硅陶瓷，包括以下按重量份数计的原料：
碳化硅5-40份、炭黑2-7份、碳纤维3-8份、粘结剂2-6份、分散剂0.1-0.4份、去离子水10-40份；
所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以任意比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以任意比混合。
优选的，所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物。
优选的，所述F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的重量比为1:2:1:2；所述羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合；所述聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合；所述炭黑和碳纤维的粒径分别为0.5-1μm和7-8μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料8-20h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料10-24h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1500-1850℃下烧结5-12h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，在加热同时通入流动的高纯氮气，进而生成表面氮化改性的反应烧结碳化硅陶瓷；氮气在高温下与反应烧结碳化硅表面的游离硅反应生成氮和硅的化合物，以增加反应烧结碳化硅耐锂电腐蚀的性能。
进一步的，所述步骤（4）中将反应烧结碳化硅放置到高温炉中，以流量为15-25m3/h向高温炉中通入流动性的高纯氮气，加热温度为1250-1350℃，保温时间为4-8h。
本发明与现有技术相比具有以下优点：
本发明通过复合粘结剂、复合分散剂、复合碳源、不同粒径的碳化硅及去离子水为原料，进行混料、醒料、烧结、表面处理，制得反应烧结的碳化硅陶瓷。将制得的反应烧结陶瓷放入高温炉中在一定压力下通入流动的氮气，在一定的热处理温度和时间下，使氮气和游离硅反应生成氮和硅的化合物，提高反应烧结碳化硅的使用寿命和耐腐蚀能力。
附图说明
图1为1350℃氮化处理的反应烧结碳化硅的XPS图；
图2 为电池材料腐蚀图片，其中，2A为未处理碳化硅烧结锂电池材料的腐蚀图片；2B为为本发明氮化处理的碳化硅烧结锂电池材料的腐蚀图片。
具体实施方式
下面结合具体实施例来进一步描述本发明，本发明的优点和特点将会随着描述而更为清楚。但实施例仅是范例性的，并不对本发明的范围构成任何限制。本领域技术人员应该理解的是，在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换，但这些修改和替换均落入本发明的保护范围内。
实施例1：一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法
表面氮化改性的反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅30份、炭黑5份、碳纤维5份、粘结剂4份、分散剂0.3份、去离子水20份；
所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物，其重量比为1:2:1:2；所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合；所述炭黑和碳纤维的粒径分别为0.7μm和7μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料10h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料18h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1600℃下烧结10h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，以流量为15m3/h向高温炉中通入流动性的高纯氮气，加热温度为1250℃，保温时间为8h，获得表面氮化改性的反应烧结碳化硅陶瓷。
经检测，该实施例获得表面氮化改性的反应烧结碳化硅陶瓷的弯曲强度为317MPa，断裂韧性为3MPa·m1/2。
实施例2：一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法
表面氮化改性的反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅15份、炭黑4份、碳纤维6份、粘结剂4份、分散剂0.2份、去离子水15份；
所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物，其重量比为1:2:1:2；所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以2:1的重量比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合；所述炭黑和碳纤维的粒径分别为0.6μm和8μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料15h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料15h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1750℃下烧结7h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，以流量为20m3/h向高温炉中通入流动性的高纯氮气，加热温度为1300℃，保温时间为6h，获得表面氮化改性的反应烧结碳化硅陶瓷。
经检测，该实施例获得表面氮化改性的反应烧结碳化硅陶瓷的弯曲强度为379MPa，断裂韧性为3.24MPa·m1/2。
实施例3：一种表面氮化改性的反应烧结碳化硅陶瓷及其制备方法
表面氮化改性的反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅35份、炭黑7份、碳纤维7份、粘结剂5份、分散剂0.4份、去离子水40份；
所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以1:1的重量比混合；所述碳化硅为F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅以重量比为1:1:1:1的比例混合；所述炭黑和碳纤维的粒径分别为0.5μm和7μm。
上述表面氮化改性的反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料18h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料20h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1800℃下烧结5-12h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，以流量为23m3/h向高温炉中通入流动性的高纯氮气，加热温度为1350℃，保温时间为4h，改性的反应烧结碳化硅陶瓷的弯曲强度为425MPa，断裂韧性为3.76MPa·m1/2。

Claims (8)

1.一种表面氮化改性的反应烧结碳化硅陶瓷，其特征在于，所述反应烧结碳化硅陶瓷包括以下按重量份数计的原料：
碳化硅5-40份、炭黑2-7份、碳纤维3-8份、粘结剂2-6份、分散剂0.1-0.4份、去离子水10-40份；
所述粘结剂为羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以任意比混合；所述分散剂为聚乙二醇和聚乙烯吡咯烷酮以任意比混合。
2.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述碳化硅选自F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的混合物。
3.根据权利要求2所述的反应烧结碳化硅陶瓷，其特征在于，所述F90的碳化硅、F120的碳化硅、F180的碳化硅和F1200的碳化硅的重量比为1:2:1:2。
4.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述羧甲基纤维素和PAF-Ⅱ型粉状粘结剂以1:1的重量比混合。
5.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述聚乙二醇和聚乙烯吡咯烷酮以2:1的重量比混合。
6.根据权利要求1所述的反应烧结碳化硅陶瓷，其特征在于，所述炭黑和碳纤维的粒径分别为0.5-1μm和7-8μm。
7.如权利要求1-6任一项所述反应烧结碳化硅陶瓷的制备方法，步骤如下：
（1）混料
取去离子水，将分散剂和粘结剂充分溶解，再称取F90的碳化硅、F120的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、碳纤维，在常温下利用滚筒混料机混料8-20h，将各组分混合均匀，获得混合物A；
（2）醒料
将步骤（1）所制得的混合物A放置到塑料膜内常温醒料10-24h，将醒好的混合物A放入挤出机中挤出所需陶瓷坯体；
（3）烧结
将步骤（2）制得的陶瓷素坯放置于真空反应烧结炉中，在1500-1850℃下烧结5-12h，制得碳化硅陶瓷；
（4）表面处理
将反应烧结碳化硅放置到高温炉中，在加热同时通入流动的高纯氮气，进而生成表面氮化改性的反应烧结碳化硅陶瓷。
8.根据权利要求7所述的制备方法，其特征在于，所述步骤（4）中将反应烧结碳化硅放置到高温炉中，以流量为15-25m3/h向高温炉中通入流动性的高纯氮气，加热温度为1250-1350℃，保温时间为4-8h。
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