CN108503357A - 氧化锆陶瓷及其制备方法 - Google Patents

氧化锆陶瓷及其制备方法 Download PDF

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CN108503357A
CN108503357A CN201810699765.7A CN201810699765A CN108503357A CN 108503357 A CN108503357 A CN 108503357A CN 201810699765 A CN201810699765 A CN 201810699765A CN 108503357 A CN108503357 A CN 108503357A
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yttrium
zirconia ceramics
nickel oxide
nano zircite
sintering
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CN108503357B (zh
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章波
郭元
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ANHUI JUSHENG ACCESSORIES OF PETROLEUM DRILLING Co.,Ltd.
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Wuhu Corey Yuen New Mstar Technology Ltd
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Abstract

本发明提出了一种氧化锆陶瓷及其制备方法，以钇稳定的纳米氧化锆为基体，添加微米氧化镍作为增强相，以纳米三氧化二铁、二氧化硅和氮化硼作为烧结助剂，经热压烧结而成。该陶瓷工模具具有更好的综合力学性能，不仅具有很高的硬度、耐磨性，还具有很好的韧性。

Description

氧化锆陶瓷及其制备方法
技术领域
本发明属于陶瓷工模具材料技术领域，具体涉及一种氧化锆陶瓷及其制备方法。
背景技术
氧化锆陶瓷具有优异的力学性能，在实验与理论的研究中早已成为热点主题，而且，已经在陶瓷、机械、化工、电子、能源等工业领域中作为结构陶瓷、耐磨耐腐蚀陶瓷、高温电解质材料等得到广泛应用。其中，氧化钇稳定的四方多晶氧化锆材料，是氧化锆增韧陶瓷中的一种。它的烧结温度低，在室温时内部含有高含量的四方氧化锆相，起到相变增韧作用，表现出极佳的力学性能。如果在氧化锆基体中加入磁性颗粒分散相，将会在兼顾其优异力学性能的同时，增加其功能方面的性质，扩宽其应用领域，实现结构—功能一体化。
从已有的研究可以看出，陶瓷材料还是存在成本较高，韧性不够、脆性大、硬度参差不齐、散热性差、自润滑性不好等问题，需要解决。
发明内容
为了克服现有技术不足之处，本发明提出一种氧化锆陶瓷，该陶瓷工模具具有更好的综合力学性能，不仅具有很高的硬度、耐磨性，还具有很好的韧性。
本发明的技术方案是这样实现的：
一种氧化锆陶瓷，以钇稳定的纳米氧化锆为基体，添加微米氧化镍作为增强相，以纳米三氧化二铁、二氧化硅和氮化硼作为烧结助剂，经热压烧结而成，原料组分重量百分比为：微米氧化镍7～15％、二氧化硅1～3％、氮化硼0.6～1.2％、纳米三氧化二铁2～5％，其余为钇稳定的纳米氧化锆；其中，所述烧结助剂需要经过预处理。
作为优选本发明一些实施例中，烧结助剂预处理方法为：先将纳米三氧化二铁与二氧化硅放入羟基纤维素的水溶液中进行搅拌分散，再将加入氮化硼进行搅拌分散，过滤，滤饼洗涤后进行真空干燥，再进行研磨即可。
作为优选本发明一些实施例中，羟基纤维素的水溶液中羟基纤维素的质量浓度为2～6％。
作为优选本发明一些实施例中，所述钇稳定的纳米氧化锆含4～6mol％钇。
本发明的另一个目的是提供一种氧化锆陶瓷的制备方法，包括以下步骤：
(1)按比例称取钇稳定的纳米氧化锆，以聚乙二醇为分散剂，以钇稳定的纳米氧化锆质量为基数计，分散剂的添加量为0.2～1.0wt％，以适量无水乙醇为分散介质，配成钇稳定的氧化锆悬浮液，搅拌并超声分散，调节悬浮液的pH值为3～4；
(2)按比例称取氧化镍进行球磨，然后在电热真空干燥箱中110～120℃温度下连续干燥，完全干燥后在惰性气体气流中过筛，加无水乙醇配成氧化镍悬浮液，充分搅拌与超声分散；
(3)将步骤1)的钇稳定的纳米氧化锆悬浮液、步骤2)氧化镍悬浮液与烧结助剂混合均匀，然后加入有机粘剂溶剂，充分混合研磨，然后热压法烧结，在热压炉中将研磨混合物压模烧结成型。
作为优选本发明一些实施例中，步骤(3)热压法烧结工艺参数为：保温温度1150～1250℃，热压压力18～28MPa，保温时间40～80min，升温速率15～25℃/min。
作为优选本发明一些实施例中，所述有机粘剂溶剂为PVB和异丙醇按照重量比为1:2的比例混合而成。
本发明的有益效果：
本发明采用经过预处理的纳米三氧化二铁、二氧化硅和氮化硼的烧结助剂替代传统的氧化镁、氧化硅作为烧结助剂，发现纳米三氧化二铁促进烧结，提高了陶瓷的硬度和耐磨性能。将纳米三氧化二铁、二氧化硅和氮化硼经过羟基纤维素浸泡处理之后，三者与其他组分形成独有的强韧化机制与氧化锆相变增韧、裂纹偏转、裂纹分支、裂纹桥联等多种增韧补强机理协同作用，共同改善材料的力学性能，能够明显提高陶瓷材料的韧性，迅速降低材料气孔率和提高材料密度，从而较大程度降低四方多晶氧化锆(TZP)材料的烧结温度。
具体实施方式
实施例1
一种氧化锆陶瓷，以钇稳定的纳米氧化锆为基体，添加微米氧化镍作为增强相，以纳米三氧化二铁、二氧化硅和氮化硼作为烧结助剂，经热压烧结而成，原料组分重量百分比为：微米氧化镍10％、二氧化硅2％、氮化硼0.8％、纳米三氧化二铁3％，其余为钇稳定的纳米氧化锆，纳米氧化锆含5mol％钇；烧结助剂预处理方法为：先将纳米三氧化二铁与二氧化硅放入质量浓度为4％的羟基纤维素的水溶液中进行搅拌分散，再将加入氮化硼进行搅拌分散，过滤，滤饼洗涤后进行真空干燥，再进行研磨即可。
氧化锆陶瓷的制备方法，包括以下步骤：
(1)按比例称取钇稳定的纳米氧化锆，以聚乙二醇为分散剂，以钇稳定的纳米氧化锆质量为基数计，分散剂的添加量为0.7wt％，以适量无水乙醇为分散介质，配成钇稳定的氧化锆悬浮液，搅拌并超声分散，调节悬浮液的pH值为3；
(2)按比例称取氧化镍进行球磨，然后在电热真空干燥箱中110℃温度下连续干燥，完全干燥后在惰性气体气流中过筛，加无水乙醇配成氧化镍悬浮液，充分搅拌与超声分散；
(3)将步骤1)的钇稳定的纳米氧化锆悬浮液、步骤2)氧化镍悬浮液与烧结助剂混合均匀，然后加入有机粘剂溶剂(有机粘剂溶剂为PVB和异丙醇按照重量比为1:2的比例混合而成)，充分混合研磨，然后热压法烧结，在热压炉中将研磨混合物压模烧结成型。热压法烧结工艺参数为：保温温度1140℃，热压压力25MPa，保温时间60min，升温速率18℃/min，1000℃时施加120min保温。
将制得的陶瓷材料试样进行切割加工，测得其力学性能参数为：抗弯强度1172MPa、断裂韧性13.02MPa·m1/2、维氏硬度18.13GPa。
实施例2
一种氧化锆陶瓷，以钇稳定的纳米氧化锆为基体，添加微米氧化镍作为增强相，以纳米三氧化二铁、二氧化硅和氮化硼作为烧结助剂，经热压烧结而成，原料组分重量百分比为：微米氧化镍7％、二氧化硅3％、氮化硼0.6％、纳米三氧化二铁5％，其余为钇稳定的纳米氧化锆，纳米氧化锆含4mol％钇；烧结助剂预处理方法为：先将纳米三氧化二铁与二氧化硅放入质量浓度为2％的羟基纤维素的水溶液中进行搅拌分散，再将加入氮化硼进行搅拌分散，过滤，滤饼洗涤后进行真空干燥，再进行研磨即可。
氧化锆陶瓷的制备方法，包括以下步骤：
(1)按比例称取钇稳定的纳米氧化锆，以聚乙二醇为分散剂，以钇稳定的纳米氧化锆质量为基数计，分散剂的添加量为0.2wt％，以适量无水乙醇为分散介质，配成钇稳定的氧化锆悬浮液，搅拌并超声分散，调节悬浮液的pH值为4；
(2)按比例称取氧化镍进行球磨，然后在电热真空干燥箱中120℃温度下连续干燥，完全干燥后在惰性气体气流中过筛，加无水乙醇配成氧化镍悬浮液，充分搅拌与超声分散；
(3)将步骤1)的钇稳定的纳米氧化锆悬浮液、步骤2)氧化镍悬浮液与烧结助剂混合均匀，然后加入有机粘剂溶剂(有机粘剂溶剂为PVB和异丙醇按照重量比为1:2的比例混合而成)，充分混合研磨，然后热压法烧结，在热压炉中将研磨混合物压模烧结成型。热压法烧结工艺参数为：保温温度1150℃，热压压力18MPa，保温时间80min，升温速率15℃/min，1000℃时施加100保温。
将制得的陶瓷材料试样进行切割加工，测得其力学性能参数为：抗弯强度1071MPa、断裂韧性12.24MPa·m1/2、维氏硬度17.11GPa。
实施例3
一种氧化锆陶瓷，以钇稳定的纳米氧化锆为基体，添加微米氧化镍作为增强相，以纳米三氧化二铁、二氧化硅和氮化硼作为烧结助剂，经热压烧结而成，原料组分重量百分比为：微米氧化镍15％、二氧化硅1％、氮化硼1.2％、纳米三氧化二铁2％，其余为钇稳定的纳米氧化锆，纳米氧化锆含6mol％钇；其中，烧结助剂预处理方法为：先将纳米三氧化二铁与二氧化硅放入质量浓度为6％的羟基纤维素的水溶液中进行搅拌分散，再将加入氮化硼进行搅拌分散，过滤，滤饼洗涤后进行真空干燥，再进行研磨即可。
氧化锆陶瓷的制备方法，包括以下步骤：
(1)按比例称取钇稳定的纳米氧化锆，以聚乙二醇为分散剂，以钇稳定的纳米氧化锆质量为基数计，分散剂的添加量为1.0wt％，以适量无水乙醇为分散介质，配成钇稳定的氧化锆悬浮液，搅拌并超声分散，调节悬浮液的pH值为4；
(2)按比例称取氧化镍进行球磨，然后在电热真空干燥箱中120℃温度下连续干燥，完全干燥后在惰性气体气流中过筛，加无水乙醇配成氧化镍悬浮液，充分搅拌与超声分散；
(3)将步骤1)的钇稳定的纳米氧化锆悬浮液、步骤2)氧化镍悬浮液与烧结助剂混合均匀，然后加入有机粘剂溶剂(有机粘剂溶剂为PVB和异丙醇按照重量比为1:2的比例混合而成)，充分混合研磨，然后热压法烧结，在热压炉中将研磨混合物压模烧结成型。热压法烧结工艺参数为：保温温度1250℃，热压压力28MPa，保温时间40min，升温速率25℃/min，1000℃时施加150min保温。
将制得的陶瓷材料试样进行切割加工，测得其力学性能参数为：抗弯强度1123MPa、断裂韧性11.78MPa·m1/2、维氏硬度16.85GPa。
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、改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种氧化锆陶瓷，其特征在于，以钇稳定的纳米氧化锆为基体，添加微米氧化镍作为增强相，以纳米三氧化二铁、二氧化硅和氮化硼作为烧结助剂，经热压烧结而成，原料组分重量百分比为：微米氧化镍7～15％、二氧化硅1～3％、氮化硼0.6～1.2％、纳米三氧化二铁2～5％，其余为钇稳定的纳米氧化锆；其中，所述烧结助剂需要经过预处理。
2.根据权利要求1所述的氧化锆陶瓷，其特征在于，烧结助剂预处理方法为：先将纳米三氧化二铁与二氧化硅放入羟基纤维素的水溶液中进行搅拌分散，再将加入氮化硼进行搅拌分散，过滤，滤饼洗涤后进行真空干燥，再进行研磨即可。
3.根据权利要求2所述的氧化锆陶瓷，其特征在于，羟基纤维素的水溶液中羟基纤维素的质量浓度为2～6％。
4.根据权利要求1所述的氧化锆陶瓷，其特征在于，所述钇稳定的纳米氧化锆含4～6mol％钇。
5.如权利要求1至4任意一项所述的氧化锆陶瓷的制备方法，其特征在于，包括以下步骤：
(1)按比例称取钇稳定的纳米氧化锆，以聚乙二醇为分散剂，以钇稳定的纳米氧化锆质量为基数计，分散剂的添加量为0.2～1.0wt％，以适量无水乙醇为分散介质，配成钇稳定的氧化锆悬浮液，搅拌并超声分散，调节悬浮液的pH值为3～4；
(2)按比例称取氧化镍进行球磨，然后在电热真空干燥箱中110～120℃温度下连续干燥，完全干燥后在惰性气体气流中过筛，加无水乙醇配成氧化镍悬浮液，充分搅拌与超声分散；
(3)将步骤1)的钇稳定的纳米氧化锆悬浮液、步骤2)氧化镍悬浮液与烧结助剂混合均匀，然后加入有机粘剂溶剂，充分混合研磨，然后热压法烧结，在热压炉中将研磨混合物压模烧结成型。
6.根据权利要求5所述的氧化锆陶瓷的制备方法，其特征在于，步骤(3)热压法烧结工艺参数为：保温温度1150～1250℃，热压压力18～28MPa，保温时间40～80min，升温速率15～25℃/min。
7.根据权利要求5所述的氧化锆陶瓷的制备方法，所述有机粘剂溶剂为PVB和异丙醇按照重量比为1:2的比例混合而成。
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