CN107805071B - 一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法 - Google Patents

一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法 Download PDF

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CN107805071B
CN107805071B CN201711016918.5A CN201711016918A CN107805071B CN 107805071 B CN107805071 B CN 107805071B CN 201711016918 A CN201711016918 A CN 201711016918A CN 107805071 B CN107805071 B CN 107805071B
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CN107805071A (zh
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胡春峰
朱德贵
许璐迪
张姬
李昌
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Southwest Jiaotong University
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Abstract

本发明公开了一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，包括以下步骤：（1）将Ti3AlC2粉和莫来石粉混合均匀，形成的混合物中莫来石体积分数为1～90%；（2）将步骤（1）中的混合物经模具冷压成胚体；（3）将步骤（2）得到胚体置于流动氩气环境中，在800～1600℃条件下反应0.5～5小时，冷却后既得所需Ti3AlC2/莫来石复合陶瓷；本发明制备工艺简单、生产成本低、易于工业化推广。

Description

一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法
技术领域
本发明涉及一种复合陶瓷的制备方法，具体涉及一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法。
背景技术
Ti3AlC2/莫来石复合陶瓷是一种新型耐热复合陶瓷材料，兼具Ti3AlC2陶瓷和莫来石的热稳定性和耐热震性能；可以在高温下重复使用，达到工业化生产玻璃制品作为托板的要求；某玻璃厂目前生产玻璃制品使用的陶瓷托板为氧化铝-莫来石陶瓷复合材料，全部从日本进口，价格昂贵，且使用寿命低，易于开裂；Ti3AlC2是一种三元层状陶瓷，具有很好地导热性能、导电性能和力学性能，同时具有高的熔点、高的热稳定性和热震性能，常应用在高温领域；莫来石耐火度高、导热率很低，是理想的高级耐火材料；本发明制备的低玻璃润湿性Ti3AlC2/莫来石复合陶瓷满足工业化生产玻璃制品的要求。
发明内容
本发明提供一种导热率低、耐热性好和耐热震性能好的低玻璃润湿性的钛三铝碳二/莫来石复合陶瓷的制备方法。
本发明采用的技术方案是：一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，包括以下步骤：
(1)将Ti3AlC2粉和莫来石粉混合均匀，形成的混合物中莫来石体积分数为1～90％；
(2)将步骤(1)中的混合物经模具冷压成胚体；
(3)将步骤(2)得到胚体置于流动氩气环境中，在800～1600℃条件下反应0.5～5小时，冷却后既得所需Ti3AlC2/莫来石复合陶瓷。
进一步的，得到Ti3AlC2/莫来石复合陶瓷后，将其进行高温热暴露氧化处理，处理温度在500～1500℃。
进一步的，所述步骤(1)中Ti3AlC2粉的粒径为200～400目，莫来石粉的粒径为200～400目。
进一步的，所述混合通过在滚筒式混料机上进行混合，混料5～20小时。
进一步的，所述步骤(2)中压力为3～12吨。
进一步的，所述步骤(3)升温速率为1～10℃/min，降温速率为1～10℃/min，氩气流量为50～250ml/min。
进一步的，所述高温热暴露氧化过程中升温速率为1～10℃/min，降温速率为1～10℃/min。
进一步的，所述高温热暴露氧化处理之前将Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光处理。
进一步的，所述高温热暴露氧化处理时间为4～24小时。
本发明的有益效果是：
(1)本发明通过混合烧结，即可获得Ti3AlC2/莫来石复合陶瓷，制备工艺简单、成本低，易于工业化推广；
(2)本发明获得的Ti3AlC2/莫来石复合陶瓷，烧结性好，在较低温度下即可烧结成形，远低于氧化铝-莫来石陶瓷高温烧结所需的1900℃，且力学性能优于氧化铝-莫来石陶瓷，抗热震性更好，使用寿命更长；
(3)本发明获得的Ti3AlC2/莫来石复合陶瓷在高温热暴露处理后，表面可获得一层厚厚的TiO2和Al2O3致密氧化膜，能增强Ti3AlC2/莫来石复合陶瓷的高温抗氧化性能和热稳定性能，同时可有效防止玻璃与Ti3AlC2/莫来石复合陶瓷发生粘结。
附图说明
图1为本发明实施例中制备的Ti3AlC2/莫来石复合陶瓷的X射线衍射图谱。
图2为本发明实施例中制备的Ti3AlC2/莫来石复合陶瓷的致密度曲线。
图3为本发明实施例中制备的Ti3AlC2/莫来石复合陶瓷的热导率曲线。
图4为本发明实施例1制备的Ti3AlC2/莫来石复合陶瓷的扫描电镜图。
图5为本发明实施例2制备的Ti3AlC2/莫来石复合陶瓷的扫描电镜图。
图6为本发明实施例3制备的Ti3AlC2/莫来石复合陶瓷的扫描电镜图。
图7为本发明实施例4制备的Ti3AlC2/莫来石复合陶瓷的扫描电镜图。
图8为本发明实施例5制备的Ti3AlC2/莫来石复合陶瓷的扫描电镜图。
具体实施方式
下面结合附图和具体实施例对本发明做进一步说明。
实施例1
一种低玻璃润湿性Ti3AlC2/莫来石复合陶瓷的制备方法，包括以下步骤：
(1)将200～400目的Ti3AlC2粉和200～400目的莫来石粉进行混合，混合粉中莫来石的体积分数为10％，在滚筒式混料机上混料5个小时；
(2)将步骤(1)得到的混合粉末经模具冷压成坯体；
(3)将步骤(2)得到的胚体置于流动氩气的管式炉中，在1300℃条件下保温处理1小时，得到反应产物；管式炉的升温速率为5℃/min，降温速率为5℃/min，氩气流量为200ml/min；
(4)将步骤(3)得到的Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光；
(5)将步骤(4)中粗磨、细磨和抛光后的Ti3AlC2/莫来石复合陶瓷置于箱式电阻炉中进行高温热暴露氧化处理，处理温度在500℃，时间为24h。
得到的Ti3AlC2/莫来石复合陶瓷表面喷涂BN涂层后，即可用作生产玻璃制品的托板。
实施例2
一种低玻璃润湿性Ti3AlC2/莫来石复合陶瓷的制备方法，包括以下步骤：
(1)将200～400目的Ti3AlC2粉和200～400目的莫来石粉进行混合，混合粉中莫来石的体积分数为20％，在滚筒式混料机上混料10个小时；
(2)将步骤(1)得到的混合粉末经模具冷压成坯体；
(3)将步骤(2)得到的胚体置于流动氩气的管式炉中，在1500℃条件下保温处理2小时，得到反应产物；管式炉的升温速率为5℃/min，降温速率为5℃/min，氩气流量为200ml/min；
(4)将步骤(3)得到的Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光；
(5)将步骤(4)中粗磨、细磨和抛光后的Ti3AlC2/莫来石复合陶瓷置于箱式电阻炉中进行高温热暴露氧化处理，处理温度在800℃，时间为20h。
得到的Ti3AlC2/莫来石复合陶瓷表面喷涂BN涂层后，即可用作生产玻璃制品的托板。
实施例3
一种低玻璃润湿性Ti3AlC2/莫来石复合陶瓷的制备方法，包括以下步骤：
(1)将200～400目的Ti3AlC2粉和200～400目的莫来石粉进行混合，混合粉中莫来石的体积分数为30％，在滚筒式混料机上混料15个小时；
(2)将步骤(1)得到的混合粉末经模具冷压成坯体；
(3)将步骤(2)得到的胚体置于流动氩气的管式炉中，在1500℃条件下保温处理4小时，得到反应产物；管式炉的升温速率为5℃/min，降温速率为5℃/min，氩气流量为200ml/min；
(4)将步骤(3)得到的Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光；
(5)将步骤(4)中粗磨、细磨和抛光后的Ti3AlC2/莫来石复合陶瓷置于箱式电阻炉中进行高温热暴露氧化处理，处理温度1000℃，时间为16h。
得到的Ti3AlC2/莫来石复合陶瓷表面喷涂BN涂层后，即可用作生产玻璃制品的托板。
实施例4
一种低玻璃润湿性Ti3AlC2/莫来石复合陶瓷的制备方法，包括以下步骤：
(1)将200～400目的Ti3AlC2粉和200～400目的莫来石粉进行混合，混合粉中莫来石的体积分数为40％，在滚筒式混料机上混料15个小时；
(2)将步骤(1)得到的混合粉末经模具冷压成坯体；
(3)将步骤(2)得到的胚体置于流动氩气的管式炉中，在1400℃条件下保温处理2小时，得到反应产物；管式炉的升温速率为5℃/min，降温速率为5℃/min，氩气流量为200ml/min；
(4)将步骤(3)得到的Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光；
(5)将步骤(4)中粗磨、细磨和抛光后的Ti3AlC2/莫来石复合陶瓷置于箱式电阻炉中进行高温热暴露氧化处理，处理温度在1200℃，时间为10h。
得到的Ti3AlC2/莫来石复合陶瓷表面喷涂BN涂层后，即可用作生产玻璃制品的托板。
实施例5
一种低玻璃润湿性Ti3AlC2/莫来石复合陶瓷的制备方法，包括以下步骤：
(1)将200～400目的Ti3AlC2粉和200～400目的莫来石粉进行混合，混合粉中莫来石的体积分数为50％，在滚筒式混料机上混料20个小时；
(2)将步骤(1)得到的混合粉末经模具冷压成坯体；
(3)将步骤(2)得到的胚体置于流动氩气的管式炉中，在1600℃条件下保温处理1小时，得到反应产物；管式炉的升温速率为5℃/min，降温速率为5℃/min，氩气流量为200ml/min；
(4)将步骤(3)得到的Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光；
(5)将步骤(4)中粗磨、细磨和抛光后的Ti3AlC2/莫来石复合陶瓷置于箱式电阻炉中进行高温热暴露氧化处理，处理温度在1500℃，时间为4h。
得到的Ti3AlC2/莫来石复合陶瓷表面喷涂BN涂层后，即可用作生产玻璃制品的托板。
将本发明实施例1-5制备的产品进行X射线衍射测试，测试结果如图1所示，从图1中可以看出实施例1、实施例2、实施例3和实施例4得到的产品为Ti3AlC2/莫来石复合陶瓷，实施例5中得到的产品Ti3AlC2与莫来石发生了反应；将本发明实施例1-5制备的产品进行致密性测试，测试结果如图2所示，实施例1-5制备得到的产品致密度均大于65.92％，最高可达88.83％；将本发明实施例1-5得到的产品进行导热性测试，测试结果如图3所示，从图3中可以看出，实施例1-5制备得到的产品导热率均大于16.43W/(m·K)，最高可达21.90W/(m·K)；如4-8为本发明实施例1-5所制备产品的扫描电镜图；如图4-8所示，随着莫来石体积分数增大，Ti3AlC2/莫来石复合陶瓷的导热率将会越高，耐热性增强；但是复合陶瓷内部孔洞明显增多，致密度明显下降，力学性能也降低，抗热震性也会有所下降，使用寿命缩短。
在作为生产玻璃制品托板之前，通常先对其表面进行粗磨、细磨和抛光，再进行高温热暴露氧化处理，使其表面生成一层厚厚的TiO2和Al2O3致密氧化膜，从而具有低的玻璃润湿性，同时抗氧化性能和热稳定性能也得到加强；将实施例中制备的复合陶瓷用于生产玻璃制品试验，从实施例1-5所得产品的结果进行分析，实施例1中制备的产品将玻璃和Ti3AlC2/莫来石复合陶瓷分开比较困难，将会损坏玻璃制品；实施例2中将玻璃和Ti3AlC2/莫来石复合陶瓷分开比较容易；实施例3中将玻璃和Ti3AlC2/莫来石复合陶瓷分开也比较容易；实施例4中将玻璃和Ti3AlC2/莫来石复合陶瓷分开比较容易，但是可以看到Ti3AlC2/莫来石复合陶瓷上粘结有少量玻璃；实施例5中将玻璃和Ti3AlC2/莫来石复合瓷分开很困难，可以看到Ti3AlC2/莫来石复合陶瓷上粘结有大块玻璃，将会损坏玻璃制品。
从上述试验结果来看实施例2和实施例3中制备的Ti3AlC2/莫来石复合陶瓷可以完全替代从日本进口的氧化铝-莫来石陶瓷托板，不仅能延长陶瓷托板的使用寿命，而且可以降低生产成本，可以在玻璃厂广泛应用。
本发明Ti3AlC2/莫来石复合陶瓷是一种新型耐热复合陶瓷材料，兼具Ti3AlC2和莫来石的优点，具有很好的制备烧结性能，较高的耐热性和耐热震性，以及较低的导热率，适合作为陶瓷托板应用于生产玻璃制品，可以在高温下重复使用，达到工业化生产玻璃制品的要求。
文中钛三铝碳二/莫来石复合陶瓷即表示Ti3AlC2/莫来石复合陶瓷。

Claims (7)

1.一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，包括以下步骤：
（1）将 Ti3AlC2 粉和莫来石粉混合均匀，形成的混合物中莫来石体积分数为1～90%；
（2）将步骤（1）中的混合物经模具冷压成坯体；
（3）将步骤（2）得到坯体置于流动氩气环境中，在800～1600℃条件下反应0.5～5 小时，冷却后既得所需 Ti3AlC2/莫来石复合陶瓷；
（4）将步骤（3）得到的Ti3AlC2/莫来石复合陶瓷表面进行粗磨、细磨和抛光；
（5）将步骤（4）中粗磨、细磨和抛光后的Ti3AlC2/莫来石复合陶瓷置于箱式电阻炉中进行高温热暴露处理，处理温度在800℃～1200℃，处理时间为10～20h；
所述步骤（3）升温速率为 1～10℃/min，降温速率为1～10℃/min，氩气流量为50～250ml/min。
2.根据权利要求1所述的一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，得到 Ti3AlC2/莫来石复合陶瓷后，将其进行高温热暴露氧化处理，处理温度在800℃、1000℃、1200℃。
3.根据权利要求1所述的一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，所述步骤（1）中 Ti3AlC2 粉的粒径为200～400 目，莫来石粉的粒径为200～400 目。
4.根据权利要求1所述的一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，所述混合通过在滚筒式混料机上进行混合，混料5～20小时。
5.根据权利要求1所述的一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，所述步骤（2）中压力为 3～12 吨。
6.根据权利要求2所述的一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，所述高温热暴露氧化过程中升温速率为1～10℃/min，降温速率为1～10℃/min。
7.根据权利要求2所述的一种低玻璃润湿性钛三铝碳二/莫来石复合陶瓷的制备方法，其特征在于，所述高温热暴露氧化处理时间为20小时、16小时、10小时。
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