CN106116592A - 耐高温陶瓷基复合涂层及其制备方法 - Google Patents

耐高温陶瓷基复合涂层及其制备方法 Download PDF

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CN106116592A
CN106116592A CN201610439845.XA CN201610439845A CN106116592A CN 106116592 A CN106116592 A CN 106116592A CN 201610439845 A CN201610439845 A CN 201610439845A CN 106116592 A CN106116592 A CN 106116592A
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刘键
林德苗
吴佩萱
王真
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Zhongwu Function Material Institute Co Ltd
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Abstract

一种耐高温陶瓷基复合涂层，包括以下重量份数的组分：含炔基树脂：1～99份；聚硼硅氮烷树脂或聚硅氮烷树脂：1～99份；及纳米级填料：1～99份；或包括以下重量份数的组分：含炔基聚硼硅氮烷或含炔基聚硅氮烷：1～99份；及纳米级填料：1～99份。还提供一种耐高温陶瓷基复合涂层的制备方法。上述耐高温陶瓷基复合涂层采用了炔基树脂、或含炔基聚硼硅氮烷或含炔基聚硅氮烷制备的耐高温陶瓷基复合涂层，从而该耐高温陶瓷基复合涂层可以实现在更低温度下的固化交联，形成的涂层具有更好的柔韧性。

Description

耐高温陶瓷基复合涂层及其制备方法
技术领域
本发明涉及陶瓷涂层材料领域，特别涉及一种耐高温陶瓷基复合涂层及其制备方法。
背景技术
陶瓷基复合材料是以陶瓷为基体与各种纤维复合的一类复合材料。陶瓷基复合材料能提供很好的综合性能，这是因为它们的共价键结合结构在高温下具有按照强度、刚度、硬度和耐磨性要求而调整结合的特殊能力，再加上这种材料的密度较低，从而很适合做高温材料。而其致命的弱点是具有脆性，即柔韧性较差，当材料处于应力状态时，会产生裂纹，甚至断裂导致材料失效。
发明内容
基于此，有必要提供一种柔韧性较好的耐高温陶瓷基复合涂层及其制备方法。
一种耐高温陶瓷基复合涂层，包括以下重量份数的组分：含炔基树脂：1～99份；聚硼硅氮烷树脂或聚硅氮烷树脂：1～99份；及纳米级填料：1～99份；
或包括以下重量份数的组分：含炔基聚硼硅氮烷或含炔基聚硅氮烷：1～99份；及纳米级填料：1～99份。
在其中一个实施例中，所述含炔基树脂为芳基乙炔树脂、乙炔基封端的聚酰亚胺树脂或含硅芳炔树脂、端炔基聚砜树脂、端炔基苯并吡啶树脂、乙炔基苯并噁嗪树脂或炔丙基酚醛树脂。
在其中一个实施例中，所述纳米级填料为Hf的氧化物、Hf的碳化物、Zr的氧化物或Zr的碳化物。
在其中一个实施例中，所述纳米级填料的粒径在50～500nm之间。
一种耐高温陶瓷基复合涂层的制备方法，包括：采用有机溶剂稀释含炔基树脂、聚硼硅氮烷树脂或聚硅氮烷树脂、及纳米级填料，充分研磨和分散后涂覆或浸渍在C/C复合材料上，然后固化交联，再裂解，形成所述耐高温陶瓷基复合涂层；其中：所述含炔基树脂1～99重量份，所述聚硼硅氮烷树脂或聚硅氮烷树脂1～99重量份，及纳米级填料1～99重量份；
或：
采用有机溶剂稀释含炔基聚硼硅氮烷或含炔基聚硅氮烷、及纳米级填料，充分研磨和分散后涂覆或浸渍在C/C复合材料上，然后固化交联，再裂解，形成所述耐高温陶瓷基复合涂层，其中所述含炔基聚硼硅氮烷或所述含炔基聚硅氮烷1～99重量份，及纳米级填料1～99重量份。
在其中一个实施例中，所述固化交联的固化温度为100℃～400℃。
在其中一个实施例中，所述裂解在惰性气体中进行。
在其中一个实施例中，所述惰性气体为氮气或氩气。
在其中一个实施例中，所述裂解的裂解温度为900℃～1800℃，且升温速度为5～10℃/min。
在其中一个实施例中，所述有机溶剂为甲苯、二甲苯、己烷、环己烷或正庚烷。
上述耐高温陶瓷基复合涂层采用了炔基树脂、或含炔基聚硼硅氮烷或含炔基聚硅氮烷制备的耐高温陶瓷基复合涂层，从而该耐高温陶瓷基复合涂层可以实现在更低温度下的固化交联，形成的涂层具有更好的柔韧性。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面对本发明的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本发明。但是本发明能够以很多不同于在此描述的其它方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似改进，因此本发明不受下面公开的具体实施的限制。
一实施方式的耐高温陶瓷基复合涂层，包括以下重量份数的组分：含炔基树脂：1～99份；聚硼硅氮烷树脂或聚硅氮烷树脂：1～99份；及纳米级填料：1～99份。优选地，含炔基树脂为50～99重量份。
一实施方式的耐高温陶瓷基复合涂层，包括以下重量份数的组分：含炔基聚硼硅氮烷或含炔基聚硅氮烷：1～99份；及纳米级填料：1～99份。优选地，含炔基聚硼硅氮烷或含炔基聚硅氮烷为50～99重量份。
含炔基聚硅氮烷是一种含-Si-N-重复单元的聚合物，高温裂解转化成SiCN、SiNO、SiCO等陶瓷。含炔基聚硼硅氮烷是一种含有B元素的以-Si-N-为重复单元的聚硅氮烷。含炔基聚硼硅氮烷或含炔基聚硅氮烷树脂一种含有-C≡C-的聚硅氮烷或聚硼硅氮烷。
上述耐高温陶瓷基复合涂层采用了炔基树脂、或含炔基聚硼硅氮烷或含炔基聚硅氮烷制备的耐高温陶瓷基复合涂层，成分中含有的炔基有助于低温固化交联，并且在裂解过程中形成自由碳，有助于形成难溶金属碳化物-SiC复合材料，增强涂层与碳材料、C/C或C-SiC等基材的结合能力，并同时发挥硅碳氮或硅硼碳氮高温陶瓷和金属碳化物-SiC复合材料的双重优势，从而该耐高温陶瓷基复合涂层可以实现在更低温度下的固化交联，形成的涂层具有更好的柔韧性。 该耐高温陶瓷基复合涂层增加基材在高温、冲蚀等恶劣环境中的使用寿命，可应用于航空航天等耐高温烧蚀领域。
在一实施方式中，含炔基树脂为芳基乙炔树脂、乙炔基封端的聚酰亚胺树脂或含硅芳炔树脂、端炔基聚砜树脂、端炔基苯并吡啶树脂、乙炔基苯并噁嗪树脂、或炔丙基酚醛树脂。
在一实施方式中，纳米级填料为Hf的氧化物、Hf的碳化物、Zr的氧化物或Zr的碳化物。在一实施方式中，纳米级填料的粒径在50～500nm之间。优选地，纳米级填料的粒径在100～300nm之间。
一种耐高温陶瓷基复合涂层的制备方法，包括：
采用有机溶剂稀释含炔基树脂、聚硼硅氮烷树脂或聚硅氮烷树脂、及纳米级填料，充分研磨和分散后涂覆或浸渍在C/C复合材料上，然后固化交联，再裂解，形成所述耐高温陶瓷基复合涂层；其中：所述含炔基树脂1～99重量份，所述聚硼硅氮烷树脂或聚硅氮烷树脂1～99重量份；及纳米级填料1～99重量份。优选地，含炔基树脂为50～99重量份。
或：
采用有机溶剂稀释含炔基聚硼硅氮烷或含炔基聚硅氮烷、及纳米级填料，充分研磨和分散后涂覆或浸渍在C/C复合材料上，然后固化交联，再裂解，形成所述耐高温陶瓷基复合涂层，其中所述含炔基聚硼硅氮烷或所述含炔基聚硅氮烷1～99重量份；及纳米级填料1～99重量份。优选地，含炔基聚硼硅氮烷或含炔基聚硅氮烷为50～99重量份。
在一实施方式中，纳米级填料为Hf的氧化物、Hf的碳化物、Zr的氧化物或Zr的碳化物。在一实施方式中，纳米级填料的粒径在50～500nm之间。优选地，纳米级填料的粒径在100～300nm之间。
在一实施方式中，在烘箱里进行固化交联。在一实施方式中，固化交联的固化温度为100℃～400℃。优选温度为150℃～350℃。
在一实施方式中，所述裂解在惰性气体中进行。优选地，所述惰性气体为氮气或氩气。在一实施方式中，在高温气氛炉中进行裂解，裂解温度为900℃～1800℃，且升温速度为5～10℃/min。
在一实施方式中，有机溶剂为甲苯、二甲苯、己烷、环己烷或正庚烷。
上述耐高温陶瓷基复合涂层采用了炔基树脂、或含炔基聚硼硅氮烷或含炔基聚硅氮烷制备的耐高温陶瓷基复合涂层，耐高温陶瓷基复合涂层的炔基含量较大时，在不同温度下，可形成不同难熔金属化合物结构的涂层，1200℃时难溶金属化合物Hf或Zr主要以氧化物的形式存在；大于1400℃时慢慢形成金属碳化物、SiC和SiBCN或SiCN多相陶瓷基涂层，多相陶瓷更有利于提高涂层的耐温值，其耐温性大于1700℃。上述含有的炔基不仅可以实现在更低温度下的固化交联，而且形成的涂层具有更好的柔韧性。
实施例
实施例1
将16.2g聚硅氮烷树脂、16.2g炔丙基酚醛树脂分别用甲苯稀释，混合均匀，然后加入事先研磨好200nm的ZrO2粉末4.1g，混合搅拌分散均匀，取一定量的碳纤维浸渍在混合液中，取出后在烘箱中150℃固化2h，采用Ar保护，然后在高温气氛炉中进行裂解，在1400℃(升温速度为10℃/min)热解2h，得到耐高温陶瓷基复合涂层。
XRD分析热解产物，发现产物中有SiBNC、ZrO2(t,m)和自由C生成。
实施例2
将15.7g聚硅氮烷树脂、2.6g芳基乙炔树脂分别用二甲苯稀释，混合均匀， 然后加入事先研磨好50nm的ZrC粉末2g，混合搅拌分散均匀，取一定量的碳纤维浸渍在混合液中，取出后在烘箱中200℃固化1.5h，Ar保护，在高温气氛炉中进行裂解，在900℃(升温速度为5℃/min)热解2h，得到耐高温陶瓷基复合涂层。
分析热解产物，除了ZrC之外，还有SiNC和自由C生成。
实施例3
将52.6g聚硼硅氮烷树脂、15.7g端炔基苯并吡啶树脂分别用环己烷稀释，混合均匀，然后加入事先研磨好100nm的氧化铪粉末20.5g，混合搅拌分散均匀，取一定量的碳纤维浸渍在混合液中，取出后在烘箱中250℃固化1h，Ar保护，在高温气氛炉中进行裂解，在1700℃(升温速度为8℃/min)热解2h，得到耐高温陶瓷基复合涂层。
分析热解产物，发现有HfC和SiBNC等耐高温相存在。
实施例4
将68.3g含炔基聚硼硅氮烷用环己烷稀释，混合均匀，然后加入事先研磨好500nm的氧化铪粉末31.5g，混合搅拌分散均匀，取一定量的碳纤维浸渍在混合液中，取出后在烘箱中400℃固化1h，N2保护，在高温气氛炉中进行裂解，在1800℃(升温速度为10℃/min)热解2h，得到耐高温陶瓷基复合涂层。
分析热解产物，发现有HfC和SiBNC等耐高温相存在。
实施例5
将70.6g含炔基聚硅氮烷用环己烷稀释，混合均匀，然后加入事先研磨好500nm的氧化铪粉末16.8g，混合搅拌分散均匀，取一定量的碳纤维浸渍在混合液中，取出后在烘箱中100℃固化1h，N2保护，在高温气氛炉中进行裂解，在1800℃(升温速度为10℃/min)热解2h，得到耐高温陶瓷基复合涂层。
分析热解产物，有SiNC和HfC等耐高温相存在。
上述含有的炔基不仅可以实现在更低温度下的固化交联，而且形成的涂层 具有更好的柔韧性。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (10)

1.一种耐高温陶瓷基复合涂层，其特征在于，
包括以下重量份数的组分：含炔基树脂：1～99份；聚硼硅氮烷树脂或聚硅氮烷树脂：1～99份；及纳米级填料：1～99份；
或包括以下重量份数的组分：含炔基聚硼硅氮烷或含炔基聚硅氮烷：1～99份；及纳米级填料：1～99份。
2.根据权利要求1所述的耐高温陶瓷基复合涂层，其特征在于，所述含炔基树脂为芳基乙炔树脂、乙炔基封端的聚酰亚胺树脂或含硅芳炔树脂、端炔基聚砜树脂、端炔基苯并吡啶树脂、乙炔基苯并噁嗪树脂或炔丙基酚醛树脂。
3.根据权利要求1所述的耐高温陶瓷基复合涂层，其特征在于，所述纳米级填料为Hf的氧化物、Hf的碳化物、Zr的氧化物或Zr的碳化物。
4.根据权利要求1所述的耐高温陶瓷基复合涂层，其特征在于，所述纳米级填料的粒径在50～500nm之间。
5.一种耐高温陶瓷基复合涂层的制备方法，其特征在于，包括：采用有机溶剂稀释含炔基树脂、聚硼硅氮烷树脂或聚硅氮烷树脂、及纳米级填料，充分研磨和分散后涂覆或浸渍在C/C复合材料上，然后固化交联，再裂解，形成所述耐高温陶瓷基复合涂层；其中：所述含炔基树脂1～99重量份，所述聚硼硅氮烷树脂或聚硅氮烷树脂1～99重量份，及纳米级填料1～99重量份；
或：
采用有机溶剂稀释含炔基聚硼硅氮烷或含炔基聚硅氮烷、及纳米级填料，充分研磨和分散后涂覆或浸渍在C/C复合材料上，然后固化交联，再裂解，形成所述耐高温陶瓷基复合涂层，其中所述含炔基聚硼硅氮烷或所述含炔基聚硅氮烷1～99重量份，及纳米级填料1～99重量份。
6.根据权利要求5所述的耐高温陶瓷基复合涂层的制备方法，其特征在于，所述固化交联的固化温度为100℃～400℃。
7.根据权利要求5所述的耐高温陶瓷基复合涂层的制备方法，其特征在于，所述裂解在惰性气体中进行。
8.根据权利要求7所述的耐高温陶瓷基复合涂层的制备方法，其特征在于，所述惰性气体为氮气或氩气。
9.根据权利要求7所述的耐高温陶瓷基复合涂层的制备方法，其特征在于，所述裂解的裂解温度为900℃～1800℃，且升温速度为5～10℃/min。
10.根据权利要求5所述的耐高温陶瓷基复合涂层的制备方法，其特征在于，所述有机溶剂为甲苯、二甲苯、己烷、环己烷或正庚烷。
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CN114031410A (zh) * 2021-11-30 2022-02-11 杭州清瓷新材料科技有限公司 一种耐1300℃高温的聚合物转化陶瓷涂层及制备方法
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CN107540399A (zh) * 2017-09-18 2018-01-05 中科院广州化学有限公司南雄材料生产基地 碳纳米管增韧SiBCN(O)金属基陶瓷涂层及其制法
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CN114031410A (zh) * 2021-11-30 2022-02-11 杭州清瓷新材料科技有限公司 一种耐1300℃高温的聚合物转化陶瓷涂层及制备方法
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CN116041073A (zh) * 2023-01-16 2023-05-02 哈尔滨工业大学 一种改性SiBCN陶瓷材料及其制备方法
CN116041073B (zh) * 2023-01-16 2023-11-10 哈尔滨工业大学 一种改性SiBCN陶瓷材料及其制备方法

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