CN109320254A - 一种碳化硅增强氮化铝陶瓷及其制备方法 - Google Patents
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Abstract
本发明公开了一种碳化硅增强氮化铝陶瓷,所述陶瓷的重量百分比组成为:氮化铝85%~93%,碳化硅5%~10%和硅2%~5%。还公开了其制备方法,包括:(1)将碳化硅和硅加入去离子水中,再添加粘结剂,球磨混合45~90min,获得碳化硅‑硅浆料;(2)采用喷雾造粒工艺对所述碳化硅‑硅浆料进行喷雾干燥,获得碳化硅‑硅造粉粒;(3)向碳化硅‑硅造粉粒中加入氮化铝造粉粒,过筛,混合均匀,在60~100MPa条件下进行压制,然后在80~90℃条件下烘干12~24h,获得氮化铝素坯;(4)将上述氮化铝素坯后放入烧结炉中,在1600~2300℃条件下进行烧结,并在100~1000℃条件下保温2~5小时,获得碳化硅增强氮化铝陶瓷。采用本发明方法制成的陶瓷具有较高硬度、断裂韧性和弯曲强度。
Description
技术领域
本发明涉及材料技术领域,特别是涉及一种碳化硅增强氮化铝陶瓷及其制备方法。
背景技术
机械密封行业所需的陶瓷,要求材料具有高强度、高韧性、低蠕变性、耐磨擦磨损、耐腐蚀性以及良好的抗氧化性。碳化硅陶瓷具有优异的机械性能,较低的热膨胀系数和高的热传导系数,使得碳化硅陶瓷呈现出优异的抗热震性能,而且还具有高热稳定性、良好的耐腐蚀、耐磨擦性能,因此能广泛的应用在机械密封环领域。
由于碳化硅化学键特性,其陶瓷烧结条件较为苛刻。常压烧结的出现使得碳化硅陶瓷工业化生产得到了广泛实现。常压烧结包括固相烧结和液相烧结,固相烧结需要较高的烧结温度(>2100℃),使得碳化硅晶粒尺寸较大,陶瓷断裂方式也多为穿晶断裂,导致断裂韧性较低。烧结助剂一般常用的有B-C、Al-B-C、Al2O3、Al2O3-Re2O3等,其中Re代表稀土元素的一种或几种;但是这些烧结助剂在高温时候和碳化硅发生反应或挥发比较严重,使得烧结体质量损失严重,不利于烧结致密。近年来人们发现,由于碳化硅和氮化铝材料在原子尺寸、分子量、密度和晶体结构上的相似,在1800~2100℃的温度范围内会形成固溶体;随着固溶体的形成,材料的烧结活性、显微结构、力学性能及抗氧化性均得到较大程度的改善和提高。但是因为氮化铝和水在机械搅拌的情况下会发生反应,目前采用氮化铝为烧结助剂制备碳化硅陶瓷的工艺大都采用乙醇为溶剂进行球磨混料,但是这种工艺生产出的陶瓷成本较高,喷雾造粒时容易发生爆炸。
为此,有必要针对上述问题,提出一种碳化硅增强氮化铝陶瓷及其制备方法,其能够解决现有技术中存在的问题。
发明内容
本发明的目的在于提供一种碳化硅增强氮化铝陶瓷及其制备方法,以克服现有技术中的不足。
为实现上述目的,本发明提供如下技术方案:
一种碳化硅增强氮化铝陶瓷,所述陶瓷的重量百分比组成为:氮化铝85%~93%,碳化硅5%~10%和硅2%~5%。
本发明还提供一种碳化硅增强氮化铝陶瓷的制备方法,包括以下步骤:
(1)将碳化硅和硅加入去离子水中,再添加粘结剂,球磨混合45~90min,获得碳化硅-硅浆料;
(2)采用喷雾造粒工艺对所述碳化硅-硅浆料进行喷雾干燥,获得碳化硅-硅造粉粒,其中,干燥温度为80~100℃;
(3)向上述碳化硅-硅造粉粒中加入氮化铝造粉粒,过筛,混合均匀,在60~100MPa条件下进行压制,然后在80~90℃条件下烘干12~24h,获得氮化铝素坯;
(4)将上述氮化铝素坯后放入烧结炉中,在1600~2300℃条件下进行烧结,并在100~1000℃条件下保温2~5小时,获得碳化硅增强氮化铝陶瓷。
优选的,步骤(3)中,所述氮化铝造粉粒的制备方法包括:1)将碳黑均匀分散于一定量的水中,然后将硝酸铝及添加剂溶解按比例分散于碳黑溶液中,混合均匀后,在100~600℃温度下加热,溶液发生反应后得到前驱物;2)将所述前驱物在1200~1600℃的流动氮气或氨气气氛中碳热还原60~600min,获得碳热还原反应产物;3)将所述碳热还原反应产物经在500~800℃的温度下氧化除碳30~600min,获得氮化铝造粉粒。
优选的,所述粘结剂选自聚乙烯醇、聚乙烯醇缩丁醛、甲基纤维素中的一种。
优选的,所述粘结剂的重量为碳化硅和硅总重的0.1~0.2%。
优选的,步骤1)中,所述添加剂为尿素、硝酸铵、硝酸。
与现有技术相比,本发明的优点在于:本发明中,通过加入碳化硅和硅,大大提高了本发明中氮化铝陶瓷的硬度、断裂韧性和弯曲强度。
具体实施方式
本发明通过下列实施例作进一步说明:根据下述实施例,可以更好地理解本发明。然而,本领域的技术人员容易理解,实施例所描述的具体的物料比、工艺条件及其结果仅用于说明本发明,而不应当也不会限制权利要求书中所详细描述的本发明。
本发明公开一种碳化硅增强氮化铝陶瓷,所述陶瓷的重量百分比组成为:氮化铝85%~93%,碳化硅5%~10%和硅2%~5%,优选的,氮化铝91.5%,碳化硅6%和硅2.5%。
本发明公开了上述碳化硅增强氮化铝陶瓷的制备方法,包括以下步骤:
(1)将碳化硅和硅加入去离子水中,再添加粘结剂,球磨混合45~90min,获得碳化硅-硅浆料;
(2)采用喷雾造粒工艺对所述碳化硅-硅浆料进行喷雾干燥,获得碳化硅-硅造粉粒,其中,干燥温度为80~100℃;
(3)向上述碳化硅-硅造粉粒中加入氮化铝造粉粒,过筛,混合均匀,在60~100MPa条件下进行压制,然后在80~90℃条件下烘干12~24h,获得氮化铝素坯;
(4)将上述氮化铝素坯后放入烧结炉中,在1600~2300℃条件下进行烧结,并在100~1000℃条件下保温2~5小时,获得碳化硅增强氮化铝陶瓷。
上述步骤(1)中,所述粘结剂选自聚乙烯醇、聚乙烯醇缩丁醛、甲基纤维素中的一种,且所述粘结剂的重量为碳化硅和硅总重的0.1~0.2%。
上述步骤(3)中,所述氮化铝造粉粒的制备方法包括:1)将碳黑均匀分散于一定量的水中,然后将硝酸铝及添加剂溶解按比例分散于碳黑溶液中,混合均匀后,在100~600℃温度下加热,溶液发生反应后得到前驱物;2)将所述前驱物在1200~1600℃的流动氮气或氨气气氛中碳热还原60~600min,获得碳热还原反应产物;3)将所述碳热还原反应产物经在500~800℃的温度下氧化除碳30~600min,获得氮化铝造粉粒。
其中,步骤1)中,所述添加剂为尿素、硝酸铵、硝酸。
实施例
碳化硅增强氮化铝陶瓷的制备方法,包括以下步骤:
(1)将碳化硅和硅按照6%和2.5%的比例混合,加入100份去离子水中,再添加0.15%聚乙烯醇,球磨混合60min,获得碳化硅-硅浆料;
(2)采用喷雾造粒工艺对所述碳化硅-硅浆料进行喷雾干燥,获得碳化硅-硅造粉粒,其中,干燥温度为80℃;
(3)向碳化硅-硅造粉粒中加入上述方法制备得到的氮化铝造粉粒,过筛,混合均匀,在80MPa条件下进行压制,然后在80℃条件下烘干24h,获得氮化铝素坯;
(4)将上述氮化铝素坯后放入烧结炉中,在1850℃条件下进行烧结,并在400℃条件下保温5小时,获得碳化硅增强氮化铝陶瓷。
本发明中,采用HV-5型维氏硬度计测试氮化铝陶瓷的维氏硬度为16.2GPa,采用Instrong3382万能电子实验机测试氮化铝陶瓷的弯曲强度和断裂韧性分别为480MPa和5.12MPa·m1/2,通过加入碳化硅和硅,大大提高了本发明中氮化铝陶瓷的硬度、断裂韧性和弯曲强度。
最后,还需要说明的是,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
Claims (6)
1.一种碳化硅增强氮化铝陶瓷,其特征在于,所述陶瓷的重量百分比组成为:氮化铝85%~93%,碳化硅5%~10%和硅2%~5%。
2.根据权利要求1所述的碳化硅增强氮化铝陶瓷的制备方法,其特征在于,包括以下步骤:
(1)将碳化硅和硅加入去离子水中,再添加粘结剂,球磨混合45~90min,获得碳化硅-硅浆料;
(2)采用喷雾造粒工艺对所述碳化硅-硅浆料进行喷雾干燥,获得碳化硅-硅造粉粒,其中,干燥温度为80~100℃;
(3)向上述碳化硅-硅造粉粒中加入氮化铝造粉粒,过筛,混合均匀,在60~100MPa条件下进行压制,然后在80~90℃条件下烘干12~24h,获得氮化铝素坯;
(4)将上述氮化铝素坯后放入烧结炉中,在1600~2300℃条件下进行烧结,并在100~1000℃条件下保温2~5小时,获得碳化硅增强氮化铝陶瓷。
3.根据权利要求2所述的碳化硅增强氮化铝陶瓷的制备方法,其特征在于,步骤(3)中,所述氮化铝造粉粒的制备方法包括:1)将碳黑均匀分散于一定量的水中,然后将硝酸铝及添加剂溶解按比例分散于碳黑溶液中,混合均匀后,在100~600℃温度下加热,溶液发生反应后得到前驱物;2)将所述前驱物在1200~1600℃的流动氮气或氨气气氛中碳热还原60~600min,获得碳热还原反应产物;3)将所述碳热还原反应产物经在500~800℃的温度下氧化除碳30~600min,获得氮化铝造粉粒。
4.根据权利要求2所述的碳化硅增强氮化铝陶瓷的制备方法,其特征在于,所述粘结剂选自聚乙烯醇、聚乙烯醇缩丁醛、甲基纤维素中的一种。
5.根据权利要求2所述的碳化硅增强氮化铝陶瓷的制备方法,其特征在于,所述粘结剂的重量为碳化硅和硅总重的0.1~0.2%。
6.根据权利要求3所述的碳化硅增强氮化铝陶瓷的制备方法,其特征在于,步骤1)中,所述添加剂为尿素、硝酸铵、硝酸。
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CN114315371A (zh) * | 2021-10-25 | 2022-04-12 | 郴州功田电子陶瓷技术有限公司 | 一种氮化铝陶瓷基板 |
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