CN106365641A - 一种一次合成氮化硅和氮化铝的方法 - Google Patents
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Abstract
本发明公开了一种一次合成氮化硅和氮化铝的方法,属于特种陶瓷材料技术领域,包括以下步骤:1)将聚乙烯醇、氮化硅颗粒和二氧化硅粉混合搅拌后,通过浇筑,干燥形成聚乙烯醇‑氮化硅圆筒初样;2)将聚乙烯醇‑氮化硅圆筒初样置于戊烷蒸气中交联反应3~25h,得聚乙烯醇‑氮化硅圆筒;3)取两个不同直径的聚乙烯醇‑氮化硅圆筒,同轴放置,在两筒间的夹层压入合成氮化硅的起始粉料,内层圆筒中压入合成氮化铝的起始粉料;4)将聚乙烯醇‑氮化硅套筒烧结,降温,将氮化硅和氮化铝的边界切割分离,分别获得氮化硅和氮化铝。本发明方法通过采用合理的结构高效利用反应热,使体系的合成效率得到大幅提高,不仅能降低能耗,且使反应更加充分。
Description
技术领域
本发明涉及一种一次合成氮化硅和氮化铝的方法,属于特种陶瓷材料技术领域。
背景技术
氮化硅的合成方法有硅粉直接氮化法,等离子体化学气相沉积,胺解法等。目前规模化生产主要采用硅粉直接氮化法。采用该法存在的关键问题是硅粉的导热性差,生产过程中硅粉氮化后结块阻碍内部单质硅的反应,这些问题导致硅粉原料内部与外部温差大,使反应过程不稳定,同时结块导致部分硅粉不能完全氮化影响产品的纯度,导致工业上硅粉直接氮化反应时间长,能耗大,纯度难以控制。
氮化铝的合成方法有铝粉氮化法,氧化铝碳化氮化法等。其中铝粉氮化反应过程放出大量热量,造成铝粉烧结阻碍内部单质铝的氮化,与硅粉直接氮化合成氮化硅类似,需要延长时间提高氮化率,从而提高产品的纯度。在铝粉氮化合成氮化铝中反应热量不能得到有效利用,瞬间的高热造成系统温升过快使铝粉融化结块。
发明内容
为了克服氮化硅和氮化铝合成过程存在的共性问题而产生了本发明,通过采用合理的结构高效利用反应热,使体系的合成效率得到大幅提高,不仅能降低能耗,且使反应更加充分。
为了实现上述目的,本发明采用的一种一次合成氮化硅和氮化铝的方法,包括以下步骤:
1)将聚乙烯醇、氮化硅颗粒和二氧化硅粉混合搅拌后,通过浇筑,干燥形成壁厚为0.5~8mm、直径为30~300mm的聚乙烯醇-氮化硅圆筒初样;
2)将聚乙烯醇-氮化硅圆筒初样置于戊烷蒸气中交联反应3~25h,得交联聚乙烯醇-氮化硅圆筒;
3)取经步骤2)所得两个不同直径的交联聚乙烯醇-氮化硅圆筒,同轴放置,在两筒间的夹层压入合成氮化硅的起始粉料,内层圆筒中压入合成氮化铝的起始粉料;
4)将步骤3)中填装完料的聚乙烯醇-氮化硅套筒置于压力为0.2~5MPa的氮气气氛中,按照10~50℃/min速率升温,至烧结温度为1100~1380℃,烧结时间0.5~6h,降温,将氮化硅和氮化铝的边界进行切割分离,分别获得氮化硅和氮化铝。
作为改进,所述步骤3)中合成氮化硅的起始粉料包括氮化硅粉25~45wt%、Si粉35~75wt%、碳粉5~15wt%。
作为改进,所述步骤3)中合成氮化铝的起始粉料包括氮化铝粉15~40wt%、铝粉10~55wt%、氧化铝10~35wt%、碳粉5~25wt%。
作为改进,所述步骤1)中氮化硅颗粒直径为0.5~3mm。
作为改进,所述步骤1)中二氧化硅粉的直径小于0.1mm。
作为改进,所述步骤1)中氮化硅颗粒与二氧化硅粉的重量比为5~50:1,氮化硅颗粒与二氧化硅粉的总重量与聚乙烯醇的重量比为0.2~20:1。
作为改进,所述步骤1)中干燥温度为50~90℃。
与现有技术相比,本发明的方法通过氮化铝的反应热迅速提升体系的反应温度,有利于氮化硅的氮化反应的快速进行;同时由于氮化铝的导热特性有利于将热量迅速传递到氮化硅反应原料的内部,本发明为配合反应热量快速有效传递过程设计了多孔导热通道,即通过聚乙烯醇-氮化硅圆筒在加热过程中有机物的分解逃逸形成氮化硅多孔壁,同时高温下的SiO2形成玻璃相后与周围的氮化硅浸润,氮化后使氮化硅颗粒稳定有助于保持孔结构的稳定,使氮化硅的氮化时间比一般硅粉时间缩短40~70%以上,生产效率大为提高;另外,该多孔壁还为氮化铝与氮化硅提供了隔离屏障,方便产品分离。
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
一种一次合成氮化硅和氮化铝的方法,包括以下步骤:
1)将聚乙烯醇、氮化硅颗粒和二氧化硅粉混合搅拌后,通过浇筑,在50℃下干燥形成壁厚为0.5mm,直径分别为30mm、80mm的两个聚乙烯醇-氮化硅圆筒初样,其中,采用的氮化硅颗粒直径为0.5~3mm,采用的二氧化硅粉的直径小于0.1mm,另外,氮化硅颗粒与二氧化硅粉的重量比为5:1,氮化硅颗粒与二氧化硅粉的总重量与聚乙烯醇的重量比为0.2:1;
2)将两个聚乙烯醇-氮化硅圆筒初样置于戊烷蒸气中交联反应3h,得交联聚乙烯醇-氮化硅圆筒;
3)取经步骤2)所得两个不同直径的交联聚乙烯醇-氮化硅圆筒,同轴放置,在两筒间的夹层压入合成氮化硅的起始粉料,包括氮化硅粉25wt%、Si粉60wt%、碳粉15wt%,在内层圆筒中压入合成氮化铝的起始粉料,该合成氮化铝的起始粉料包括氮化铝粉15wt%、铝粉35wt%、氧化铝30wt%、碳粉20wt%;
4)将步骤3)中填装完料的聚乙烯醇-氮化硅套筒置于压力为0.2MPa的氮气气氛中,按照10℃/min速率升温,至烧结温度为1100℃,烧结时间6h,降温,将氮化硅和氮化铝的边界进行切割分离,分别获得氮化硅和氮化铝。
实施例二
一种一次合成氮化硅和氮化铝的方法,包括以下步骤:
1)将聚乙烯醇、氮化硅颗粒和二氧化硅粉混合搅拌后,通过浇筑,在90℃下干燥形成壁厚为8mm,直径分别为100mm、300mm的两个聚乙烯醇-氮化硅圆筒初样,其中,采用的氮化硅颗粒直径为0.5~3mm,采用的二氧化硅粉的直径小于0.1mm,另外,氮化硅颗粒与二氧化硅粉的重量比为50:1,氮化硅颗粒与二氧化硅粉的总重量与聚乙烯醇的重量比为20:1;
2)将两个聚乙烯醇-氮化硅圆筒初样置于戊烷蒸气中交联反应25h,得交联聚乙烯醇-氮化硅圆筒;
3)取经步骤2)所得两个不同直径的交联聚乙烯醇-氮化硅圆筒,同轴放置,在两筒间的夹层压入合成氮化硅的起始粉料,包括氮化硅粉45wt%、Si粉45wt%、碳粉10wt%,在内层圆筒中压入合成氮化铝的起始粉料,该合成氮化铝的起始粉料包括氮化铝粉35wt%、铝粉20wt%、氧化铝20wt%、碳粉25wt%;
4)将步骤3)中填装完料的聚乙烯醇-氮化硅套筒置于压力为5MPa的氮气气氛中,按照50℃/min速率升温,至烧结温度为1380℃,烧结时间0.5h,降温,将氮化硅和氮化铝的边界进行切割分离,分别获得氮化硅和氮化铝。
实施例三
一种一次合成氮化硅和氮化铝的方法,包括以下步骤:
1)将聚乙烯醇、氮化硅颗粒和二氧化硅粉混合搅拌后,通过浇筑,在60℃下干燥形成壁厚为4.5mm,直径分别为100mm、200mm的两个聚乙烯醇-氮化硅圆筒初样,其中,采用的氮化硅颗粒直径为0.5~3mm,采用的二氧化硅粉的直径小于0.1mm,另外,氮化硅颗粒与二氧化硅粉的重量比为20:1,氮化硅颗粒与二氧化硅粉的总重量与聚乙烯醇的重量比为10:1;
2)将两个聚乙烯醇-氮化硅圆筒初样分别置于戊烷蒸气中交联反应15h,得交联聚乙烯醇-氮化硅圆筒;
3)取经步骤2)所得两个不同直径的交联聚乙烯醇-氮化硅圆筒,同轴放置,在两筒间的夹层压入合成氮化硅的起始粉料,包括氮化硅粉25wt%、Si粉70wt%、碳粉5wt%,在内层圆筒中压入合成氮化铝的起始粉料,该合成氮化铝的起始粉料包括氮化铝粉40wt%、铝粉10wt%、氧化铝35wt%、碳粉15wt%;
4)将步骤3)中填装完料的聚乙烯醇-氮化硅套筒置于压力为3MPa的氮气气氛中,按照30℃/min速率升温,至烧结温度为1280℃,烧结时间3h,降温,将氮化硅和氮化铝的边界进行切割分离,分别获得氮化硅和氮化铝。
实施例四
浇筑成直径分别为150mm、300mm的两个聚乙烯醇-氮化硅圆筒初样,其余参数条件与实施例三相同。
实施例五
合成氮化硅的起始粉料包括氮化硅粉45wt%、Si粉46wt%、碳粉9wt%,其余参数条件与实施例一相同。
实施例六
通过浇筑,干燥形成一个壁厚为0.8mm、直径为50mm,另一个壁厚为4mm、直径为200mm的两个聚乙烯醇-氮化硅圆筒初样,其余参数条件与实施例二相同。
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 (7)
1.一种一次合成氮化硅和氮化铝的方法,其特征在于,包括以下步骤:
1)将聚乙烯醇、氮化硅颗粒和二氧化硅粉混合搅拌后,通过浇筑,干燥形成壁厚为0.5~8mm、直径为30~300mm的聚乙烯醇-氮化硅圆筒初样;
2)将聚乙烯醇-氮化硅圆筒初样置于戊烷蒸气中交联反应3~25h,得交联聚乙烯醇-氮化硅圆筒;
3)取经步骤2)所得两个不同直径的交联聚乙烯醇-氮化硅圆筒,同轴放置,在两筒间的夹层压入合成氮化硅的起始粉料,内层圆筒中压入合成氮化铝的起始粉料;
4)将步骤3)中填装完料的聚乙烯醇-氮化硅套筒置于压力为0.2~5MPa的氮气气氛中,按照10~50℃/min速率升温,至烧结温度为1100~1380℃,烧结时间0.5~6h,降温,将氮化硅和氮化铝的边界进行切割分离,分别获得氮化硅和氮化铝。
2.如权利要求1所述的一次合成氮化硅和氮化铝的方法,其特征在于,所述步骤3)中合成氮化硅的起始粉料包括氮化硅粉25~45wt%、Si粉35~75wt%、碳粉5~15wt%。
3.如权利要求1或2所述的一次合成氮化硅和氮化铝的方法,其特征在于,所述步骤3)中合成氮化铝的起始粉料包括氮化铝粉15~40wt%、铝粉10~55wt%、氧化铝10~35wt%、碳粉5~25wt%。
4.如权利要求1所述的一次合成氮化硅和氮化铝的方法,其特征在于,所述步骤1)中氮化硅颗粒直径为0.5~3mm。
5.如权利要求1或4所述的一次合成氮化硅和氮化铝的方法,其特征在于,所述步骤1)中二氧化硅粉的直径小于0.1mm。
6.如权利要求1所述的一次合成氮化硅和氮化铝的方法,其特征在于,所述步骤1)中氮化硅颗粒与二氧化硅粉的重量比为5~50:1,氮化硅颗粒与二氧化硅粉的总重量与聚乙烯醇的重量比为0.2~20:1。
7.如权利要求1所述的一次合成氮化硅和氮化铝的方法,其特征在于,所述步骤1)中干燥温度为50~90℃。
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JPS52145418A (en) * | 1976-05-29 | 1977-12-03 | Toshiba Ceramics Co | Refractories for fused metals |
CN1317460A (zh) * | 2001-06-01 | 2001-10-17 | 中国科学院上海硅酸盐研究所 | 一种提高氮化硅基陶瓷性能/价格比的方法 |
CN1456495A (zh) * | 2003-06-04 | 2003-11-19 | 北京科技大学 | 一种燃烧合成制备铝的氮化物和氮氧化物的方法 |
CN101708989A (zh) * | 2009-12-14 | 2010-05-19 | 哈尔滨工业大学 | 燃烧合成法制备氮化铝/氮化硼复合陶瓷的方法 |
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JPS52145418A (en) * | 1976-05-29 | 1977-12-03 | Toshiba Ceramics Co | Refractories for fused metals |
CN1317460A (zh) * | 2001-06-01 | 2001-10-17 | 中国科学院上海硅酸盐研究所 | 一种提高氮化硅基陶瓷性能/价格比的方法 |
CN1456495A (zh) * | 2003-06-04 | 2003-11-19 | 北京科技大学 | 一种燃烧合成制备铝的氮化物和氮氧化物的方法 |
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