CN106316453B - 一种用于激光设备的氮化硅多孔陶瓷的制备方法 - Google Patents

一种用于激光设备的氮化硅多孔陶瓷的制备方法 Download PDF

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CN106316453B
CN106316453B CN201610710855.2A CN201610710855A CN106316453B CN 106316453 B CN106316453 B CN 106316453B CN 201610710855 A CN201610710855 A CN 201610710855A CN 106316453 B CN106316453 B CN 106316453B
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汪思保
林永兴
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Anhui Kechuang Zhongguang Technology Co ltd
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Abstract

本发明公开了一种用于激光设备的氮化硅多孔陶瓷的制备方法，属于特种陶瓷材料技术领域，包括以下步骤，按重量份计，取35～85％氮化硅粉、3～15％碳酸铵、3～15％聚丙烯酸胺、4～10％SiO2、1～5％Al2O3、1～5％MgO、2～10％B2O3和1～5％Li2O作为原料，将原料球磨2～6h，然后加入原料重量5～30倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体，在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷。本发明通过引入胺系造孔剂，有利于减少原料残留，减少坯体烧结过程中体积的收缩率，并形成畅通的孔道，减少裂纹的发生，降低废品率。

Description

一种用于激光设备的氮化硅多孔陶瓷的制备方法
技术领域
本发明涉及一种用于激光设备的氮化硅多孔陶瓷的制备方法，属于特种陶瓷材料技术领域和激光应用领域。
背景技术
激光设备功率大，发热量大，需要采用合适高强度导热的耐磨、抗氧化、耐腐蚀性能好等高性能材料。氮化硅陶瓷具有强度高、抗热震稳定性好、疲劳韧性高、室温抗弯强度高、耐磨、抗氧化、耐腐蚀性能好等高性能，已被广泛应用于各行各业。
多孔氮化硅是经高温烧制而成，体内具有相通或闭合气孔的陶瓷材料，高孔隙率的多孔氮化硅陶瓷通常可以用作高温下的过滤器、催化剂载体、雷达天线罩等。
采用现有方法制备氮化硅多孔陶瓷时，产品上经常产生裂纹，导致产品报废。
发明内容
针对上述现有技术存在的问题，本发明提供一种用于激光设备的氮化硅多孔陶瓷的制备方法，有效减少裂纹的发生，降低废品率。
为了实现上述目的，本发明采用的一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤，按重量份计，取35～85％氮化硅粉、3～15％碳酸铵、3～15％聚丙烯酸胺、4～10％SiO2、1～5％Al2O3、1～5％MgO、2～10％B2O3和1～5％Li2O作为原料，将原料球磨2～6h，然后加入原料重量5～30倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体，在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷。
作为改进，煅烧过程的温度按如下程序设定：
按0.1～3℃/min的升温速率，在100℃保温0.3～2h，300℃保温0.5～5h，600°保温1～3h，1200～1400℃保温2～8h。
作为进一步改进，冷却过程温度按如下程序设定：
按10℃/min的降温速率，在1100℃保温2.5h，在800℃保温1.5h，在500℃保温3h。
作为改进，冷却过程温度按如下程序设定：
按2～10℃/min的降温速率，在1100℃保温0.2～3h，在800℃保温0.5～2h，在500℃保温0.3～6h。
作为进一步改进，冷却过程温度按如下程序设定：
按8℃/min的降温速率，在1100℃保温3h，在800℃保温1.5h，在500℃保温3h。
作为进一步改进，按重量份计，原料包括65％氮化硅粉、5％碳酸铵、5％聚丙烯酸胺、10％SiO2、2.5％Al2O3、2.5％MgO、5％B2O3和5％Li2O。
与现有技术相比，本发明通过引入胺/铵系造孔剂(如碳酸铵、聚丙烯酸胺)，通过胺/铵类的高温分解挥发，一方面有利于减少原料残留，减轻杂质含量，同时能在坯体中形成畅通的孔道，有利于氮气等反应物的渗透，提高氮化反应速率；另一方面，通过胺/铵类物质低温分解形成的孔结构可以显著减少高温环境下坯体烧结过程中体积的收缩率，减少裂纹的发生，降低废品率，同时通过本专利提出的阶梯式烧结制度使部分孔壁单质硅会发生部分融化现象，通过氮化反应固化后可以增强孔壁强度，从而提高产品的强度。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明了，下面通过实施例，对本发明进行进一步详细说明。但是应该理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限制本发明的范围。除非另有定义，本文所使用的所有的技术术语和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同，本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。
实施例一
一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤：
1)按重量份计，取65％氮化硅粉、5％碳酸铵、5％聚丙烯酸胺、10％SiO2、2.5％Al2O3、2.5％MgO、5％B2O3和5％Li2O作为原料；
2)将原料球磨2h，然后加入原料重量5倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体；
3)在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷，其中，煅烧过程的温度按如下程序设定：按0.1℃/min的升温速率，在100℃保温0.3h，300℃保温0.5h，600°保温1h，1200℃保温2h；另外，冷却过程温度按如下程序设定：按2℃/min的降温速率，在1100℃保温0.2h，在800℃保温0.5h，在500℃保温0.3h。
实施例二
一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤：
1)按重量份计，取55％氮化硅粉、15％碳酸铵、5％聚丙烯酸胺、10％SiO2、2.5％Al2O3、1％MgO、9％B2O3和2.5％Li2O作为原料；
2)将原料球磨3h，然后加入原料重量10倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体；
3)在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷，其中，煅烧过程的温度按如下程序设定：按1.5℃/min的升温速率，在100℃保温1h，300℃保温2.5～5h，600°保温2h，1300℃保温5h；另外，冷却过程温度按如下程序设定：按6℃/min的降温速率，在1100℃保温1h，在800℃保温1h，在500℃保温2h。
实施例三
一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤：
1)按重量份计，取70％氮化硅粉、5％碳酸铵、5％聚丙烯酸胺、5％SiO2、2.5％Al2O3、2.5％MgO、8％B2O3和2％Li2O作为原料；
2)将原料球磨6h，然后加入原料重量30倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体；
3)在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷，其中，煅烧过程的温度按如下程序设定：按3℃/min的升温速率，在100℃保温2h，300℃保温5h，600°保温3h，400℃保温8h；另外，冷却过程温度按如下程序设定：按10℃/min的降温速率，在1100℃保温3h，在800℃保温2h，在500℃保温6h。
实施例四
一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤：
1)按重量份计，取35％氮化硅粉、15％碳酸铵、15％聚丙烯酸胺、10％SiO2、5％Al2O3、5％MgO、10％B2O3和5％Li2O作为原料；
2)将原料球磨4h，然后加入原料重量20倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体；
3)在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷，其中，煅烧过程的温度按如下程序设定：按3℃/min的升温速率，在100℃保温2h，300℃保温0.5h，600°保温3h，1200℃保温8h；另外，冷却过程温度按如下程序设定：按8℃/min的降温速率，在1100℃保温3h，在800℃保温1.5h，在500℃保温3h。
实施例五
一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤：
1)按重量份计，取45％氮化硅粉、15％碳酸铵、10％聚丙烯酸胺、10％SiO2、5％Al2O3、5％MgO、5％B2O3和5％Li2O作为原料；
2)将原料球磨2h，然后加入原料重量10倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体；
3)在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷，其中，煅烧过程的温度按如下程序设定：按0.1℃/min的升温速率，在100℃保温0.3h，300℃保温1.5h，600°保温1.5h，1200℃保温3h；另外，冷却过程温度按如下程序设定：按6℃/min的降温速率，在1100℃保温0.2h，在800℃保温0.5h，在500℃保温4.5h。
实施例六
一种用于激光设备的氮化硅多孔陶瓷的制备方法，包括以下步骤：
1)按重量份计，取50％氮化硅粉、10％碳酸铵、5％聚丙烯酸胺、10％SiO2、5％Al2O3、5％MgO、10％B2O3和5％Li2O作为原料；
2)将原料球磨3h，然后加入原料重量15倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体；
3)在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷，其中，煅烧过程的温度按如下程序设定：按2.3℃/min的升温速率，在100℃保温2h，300℃保温5h，600°保温1.3h，1250℃保温6h；另外，冷却过程温度按如下程序设定：按10℃/min的降温速率，在1100℃保温0.4h，在800℃保温1.52h，在500℃保温0.6h。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换或改进等，均应包含在本发明的保护范围之内。

Claims (4)

1.一种用于激光设备的氮化硅多孔陶瓷的制备方法，其特征在于，包括以下步骤，按重量计，取35~85%氮化硅粉、3~15 %碳酸铵、3~15 %聚丙烯酸胺、4~10 %SiO2、1~5 %Al2O3、1~5%MgO、2~10 %B2O3和1~5 %Li2O作为原料，将原料球磨2~6h，然后加入原料重量5~30倍的水，混合均匀，放入模具中压制成型，得氮化硅陶瓷坯体，在氮气气氛中煅烧，冷却得到氮化硅多孔陶瓷；
煅烧过程的温度按如下程序设定：
按0.1~3°C/min的升温速率，在100°C保温0.3~2h，300°C保温0.5~5 h，600°保温1~3 h，1200~1400°C保温2~8h；
冷却过程温度按如下程序设定：
按2~10°C/min的降温速率，在1100°C保温0.2~3h，在800°C保温0.5~2h，在500°C保温0.3~6h。
2.如权利要求1所述的一种用于激光设备的氮化硅多孔陶瓷的制备方法，其特征在于，冷却过程温度按如下程序设定：
按10°C/min的降温速率，在1100°C保温2.5h，在800°C保温1.5h，在500°C保温3h。
3.如权利要求1所述的一种用于激光设备的氮化硅多孔陶瓷的制备方法，其特征在于，冷却过程温度按如下程序设定：
按8°C/min的降温速率，在1100°C保温3h，在800°C保温1.5h，在500°C保温3h。
4.如权利要求1所述的一种用于激光设备的氮化硅多孔陶瓷的制备方法，其特征在于，按重量计，原料包括65%氮化硅粉、5%碳酸铵、5 %聚丙烯酸胺、10 %SiO2、2.5 %Al2O3、2.5 %MgO、5 %B2O3和5 %Li2O。
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