CN105948783B - 一种Si2N2O-Si3N4-TiN多孔陶瓷的制备方法 - Google Patents

一种Si2N2O-Si3N4-TiN多孔陶瓷的制备方法 Download PDF

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CN105948783B
CN105948783B CN201610283697.7A CN201610283697A CN105948783B CN 105948783 B CN105948783 B CN 105948783B CN 201610283697 A CN201610283697 A CN 201610283697A CN 105948783 B CN105948783 B CN 105948783B
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郭伟明
吴利翔
陈珊璐
林华泰
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JILIN CHANGYU TETAO NEW MATERIAL TECHNOLOGY Co.,Ltd.
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Abstract

本发明公开了一种Si2N2O‑Si3N4‑TiN多孔陶瓷的制备方法，包括下列步骤：按比例加入Si、TiO2和Al2O3‑Re2O3，经混料、球磨、干燥后，得到Si‑TiO2‑Al2O3‑Re2O3混合粉体；进一步在氮气氛下，通过气氛烧结制备得到Si2N2O‑Si3N4‑TiN多孔陶瓷。本发明的多孔陶瓷的气孔率高达60%，孔径在20～150μm，可作为良好的吸音材料；硬度为100～800HV，断裂韧性为1～4MPam1/2，抗弯强度为50～400Mpa，具有良好的抗热震、抗氧化等性能；介电常数为3.5～7.0，可用于航空航天、机械工业等领域的热防护材料和透波材料，还可用于汽车尾气处理和化学工程的反应器以及过滤器等。

Description

一种Si2N2O-Si3N4-TiN多孔陶瓷的制备方法
技术领域
本发明具体涉及一种Si2N2O-Si3N4-TiN多孔陶瓷的制备方法。
背景技术
Si2N2O陶瓷具有抗氧化、抗热震、高温热力学稳定等优异性能，广泛应用于高温电绝缘材料、固态电解质、耐火材料和高温耐热组件等。尤其是在某些极端恶劣的环境下，在空气和水的净化方面，Si2N2O也有很好的应用前景。为了最大程度上发挥Si2N2O的净化效果，需要增大其气孔率或改善气孔表面积，但这会很大程度上降低其相应的力学性能，使其无法满足在高温、酸性环境等的影响下，还保持足够的力学性能(如强度、硬度、断裂韧性等)，然而结合Si3N4优良的力学性能，制备Si2N2O-Si3N4多孔陶瓷，可以在增加气孔率或改善气孔表面积的同时保留甚至提高其强度，可使其在恶劣环境中实现了最大程度上达到净化效果的同时又具备优良的力学性能。
申请号 201210315790.3的中国专利“一种Si3N4-Si2N2O多孔复相陶瓷的制备方法”，是利用 (NH4)2HPO4的分解，原位形成生坯中的孔隙，经烧结后得以保留，形成Si3N4-Si2N2O 复相陶瓷中的孔隙结构。此方法需要涉及到复杂的造孔剂的引入，工艺相对复杂，成本偏高。
发明内容
本发明的目的在于提供一种多孔陶瓷的制备方法。
本发明所采取的技术方案是：
一种多孔陶瓷的制备方法，包括下列步骤：
1)按比例加入Si、TiO2和Al2O3-Re2O3，经混料、球磨、干燥后，得到Si-TiO2-Al2O3-Re2O3混合粉体；其中Re为稀土元素；
2)将步骤1）得到的Si-TiO2-Al2O3-Re2O3混合粉体定型，在氮气氛下，通过气氛烧结制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
优选的，步骤1）中，所加入组分按照质量百分比计，包括20%～79%的Si、20%～60%的TiO2和1%～20%的Al2O3-Re2O3。
优选的，Al2O3-Re2O3中的Al2O3和Re2O3质量百分比为（1%～99%）：（99%～1%）。
优选的，步骤1），所加入组分按照质量百分比计，包括30%～60%的Si、20%～60%的TiO2和10%～20%的Al2O3-Re2O3，其中Al2O3-Re2O3中的Al2O3和Re2O3质量百分比为（55%～90%）：（10%～45%）。
优选的，稀土元素Re选自Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy,Ho, Er, Tm, Yb, Lu。
优选的，稀土元素Re为Y, Yb, Gd, Ce, Eu。
优选的，稀土元素Re为Eu。
优选的，Si粉纯度为95%～100%，粒径为<10μm；TiO2纯度为98～100%，粒径为<10μm；Al2O3粉纯度为95%～100%，Re2O3纯度为95%～100%。
优选的，步骤1）中球磨为湿磨，球料比为（1:1）～（4:1），球磨时间为4～48h。
优选的，步骤1）中球磨为湿磨，溶剂为无水乙醇或丙酮，球磨介质为Si3N4，球磨时间为6～12h。
优选的，球磨时溶剂的量加到球磨罐3/4的位置。
优选的，步骤2）中气氛烧结的条件为：以20℃/min的升温速度将温度升至1300～1450℃并保温0.5～12h。
优选的，步骤2）中气氛烧结的条件为：以20℃/min的升温速度将温度升至1350～1450℃并保温1-2h。
优选的，气氛烧结时为了防止石墨污染，使用氮化硼坩埚。
本发明的有益效果是：
在本发明中以Si粉为原料，通过引入TiO2，在加快氮化的同时又可以显著促进Si2N2O的生成，因此可以通过控制TiO2的含量来调控Si2N2O-Si3N4各相的组分含量，同时还通过引入TiN增强相进一步提高多孔陶瓷的强度；通过控制不同烧结温度和引入TiO2-Al2O3-Re2O3（Re=Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb,Lu)烧结助剂来调控Si2N2O-Si3N4-TiN的气孔率以及力学性能。
以TiO2作为Si粉氮化的催化剂以及促进Si2N2O生成的添加剂，不仅可以显著加快Si粉的氮化速率以及促进Si2N2O的合成，很大程度上简化了工艺流程，而且还引入了TiN增强相，进一步提高了多孔陶瓷的强度。
通过反应烧结，控制不同的烧结温度以及TiO2-Al2O3-Re2O3烧结助剂有效调控Si2N2O-Si3N4-TiN多孔陶瓷的气孔率和力学性能。
本发明制备得到的Si2N2O-Si3N4-TiN多孔陶瓷的气孔率高达60%，孔径在20～150μm，可作为良好的吸音材料；硬度为100～800HV，断裂韧性为1～4MPam1/2，抗弯强度为50～400Mpa，具有良好的抗热震、抗氧化等性能。
本发明制备得到的多孔陶瓷的孔径在20～150μm之间，可作为良好的吸音材料，通过多孔结构对声波引起的空气压力进行分散达到吸音目的。
本发明的多孔陶瓷介电常数为3.5～7.0，可用于航空航天、机械工业等领域的热防护材料和透波材料；稳定的结构和优良的力学性能可使其用于汽车尾气处理和化学工程的反应器以及过滤器等。
具体实施方式
以下结合实施例进一步说明本发明，但不限于此。
实施例中所使用的原料：Si粉纯度为95%～100%，粒径为<10μm；TiO2纯度为99.9%，粒径为<10μm；Al2O3粉纯度为99.9%，Re2O3纯度为99.9%。
所获得多孔陶瓷，对其进行各种参数的测定。其中，气孔率用阿基米德排水法测试，硬度用维氏硬度计测试，断裂韧性采用单边切口梁法测试，抗弯强度用四点抗弯强度测试。
实施例1
本发明以Si粉（粒径<10μm）为原料，以TiO2粉（粒径<10μm）为氮化催化剂以及促进Si2N2O生成的添加剂，以TiO2，Al2O3（纯度为99.9%）和Y2O3(纯度为99.9%)组成的TiO2-Al2O3-Y2O3为烧结助剂。
按照下述质量百分比，准确称取各组分原料：包括50%的Si粉、40%的TiO2粉、10%的Al2O3-Y2O3（其中Al2O3：Y2O3的质量百分比为55%：45%），以乙醇为溶剂，以Si3N4球为球磨介质，在行星式球磨机上混合8h，经混料、干燥后，得到混合均匀的Si-TiO2-Al2O3-Y2O3混合粉体。
将Si-TiO2-Al2O3-Y2O3混合粉体放入模具中压制成型后，得到的Si-TiO2-Al2O3-Y2O3坯体放入氮化硼坩埚，以20℃/min的升温速度将温度升到1400℃保温2h，整个烧结过程处于氮气氛围下，通过这种烧结方式获得Si2N2O-Si3N4-TiN多孔陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN多孔陶瓷，其气孔率为60%，材料的硬度为600HV，断裂韧性为3MPam1/2，抗弯强度为300Mpa。
实施例2
按照下述质量百分比，准确称取各组分原料：包括40%的Si粉、50%的TiO2粉、10%的Al2O3-Yb2O3粉（其中Al2O3：Yb2O3的质量百分比为60%：40%），按照实施例1方法制备Si3N4陶瓷，其中烧结工艺为升温至1375℃保温1h，制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN多孔陶瓷，其气孔率为50%，材料的硬度为700HV，断裂韧性为3.5MPam1/2，抗弯强度为350Mpa。
实施例3
按照下述质量百分比，准确称取各组分原料：包括60%的Si粉、20%的TiO2粉、20%的Al2O3-Gd2O3粉（其中Al2O3：Gd2O3的质量百分比为75%：25%），按照实施例1方法制备Si3N4陶瓷，其中烧结工艺为升温至1450℃保温2h，制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN多孔陶瓷，其气孔率为55%，材料的硬度为750HV，断裂韧性为3MPam1/2，抗弯强度为380Mpa。
实施例4
按照下述质量百分比，准确称取各组分原料：包括60%的Si粉、30%的TiO2粉、10%的Al2O3-Ce2O3粉（其中Al2O3：Ce2O3的质量百分比为55%：45%），按照实施例1方法制备Si3N4陶瓷，其中烧结工艺为升温至1350℃保温1h，制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN多孔陶瓷，其气孔率为60%，材料的硬度为770HV，断裂韧性为3.8MPam1/2，抗弯强度为400Mpa。
实施例5
按照下述质量百分比，准确称取各组分原料：包括30%的Si粉、60%的TiO2粉、10%Al2O3-Eu2O3粉（其中Al2O3：Eu2O3的质量百分比为90%：10%），按照实施例1方法制备Si3N4陶瓷，其中烧结工艺为升温至1375℃保温1h，制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN多孔陶瓷，其气孔率为55%，材料的硬度为750HV，断裂韧性为3.5MPam1/2，抗弯强度为350Mpa。
多孔陶瓷孔径和介电常数的测定
对制备得到的多孔陶瓷（实施例1-5）进行孔径和介电常数的测定。
实验结果：本发明制备得到的多孔陶瓷的孔径在20～150μm之间，可作为良好的吸音材料，通过多孔结构对声波引起的空气压力进行分散达到吸音目的。本发明的多孔陶瓷介电常数为3.5～7.0，可用于航空航天、机械工业等领域的热防护材料和透波材料。用于汽车尾气处理和化学工程反应器以及过滤器时，在催化载体上覆盖催化剂后反应液体通过多孔陶瓷孔道将大大提高转换效率和反应速率，同时由于Si2N2O具有优良的抗热震性和Si3N4具有耐化学腐蚀性，因此可在极其苛刻的条件下使用。
对比例1
按照下述质量百分比，准确称取各组分原料：包括50%的Si粉、40%的TiO2粉、10%的Al2O3-Y2O3（其中Al2O3：Y2O3的质量百分比为55%：45%），以乙醇为溶剂，以Si3N4球为球磨介质，在行星式球磨机上混合8h，经混料、干燥后，得到混合均匀的Si-TiO2-Al2O3-Y2O3混合粉体。
将Si-TiO2-Al2O3-Y2O3混合粉体放入模具中压制成型后，得到的Si-TiO2-Al2O3-Y2O3坯体放入氮化硼坩埚，以20℃/min的升温速度将温度升到1600℃保温2h，整个烧结过程处于氮气氛围下，获得Si2N2O-Si3N4-TiN陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN陶瓷因升温温度过高导致大量的熔硅，阻碍Si粉的氮化，使得得到的陶瓷含有大量未反应的Si粉，大幅度降低了其力学性能；加之无法控制多孔陶瓷的气孔率和孔径大小，陶瓷中残余Si粉的存在而使其无法抵抗外界环境的侵蚀，限制了其应用。
对比例2
按照Si粉质量分数为25%、TiO2粉质量分数为50%、Al2O3-Eu2O3粉质量分数为25%进行配料（其中Al2O3：Eu2O3的质量百分比为90%：10%），按照实施例1方法制备Si3N4陶瓷，其中烧结工艺为升温至1375℃保温1h，制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
本实施例制备得到的Si2N2O-Si3N4-TiN陶瓷因晶界相含量过多，在高温烧结阶段有大量液相产生，不利于多孔陶瓷孔隙的形成，过多的晶界相会降低其力学性能，尤其是高温性能。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (8)

1.一种多孔陶瓷的制备方法，其特征在于，包括下列步骤：
1) 按质量百分比加入20%～79%的Si、20%～60%的TiO2和1%～20%的Al2O3-Re2O3，经混料、球磨、干燥后，得到Si-TiO2-Al2O3-Re2O3混合粉体；其中Re为稀土元素；
2) 将步骤1）得到的Si-TiO2-Al2O3-Re2O3混合粉体定型，在氮气氛下，以20℃/min的升温速度将温度升至1300～1450℃并保温0.5～12h，制备得到Si2N2O-Si3N4-TiN多孔陶瓷。
2.根据权利要求1所述的制备方法，其特征在于：Al2O3-Re2O3中的Al2O3和Re2O3质量百分比为（1%～99%）：（99%～1%）。
3.根据权利要求1所述的制备方法，其特征在于：步骤1），所加入组分按照质量百分比计，包括30%～60%的Si、20%～60%的TiO2和10%～20%的Al2O3-Re2O3，其中Al2O3-Re2O3中的Al2O3和Re2O3质量百分比为（55%～90%）：（10%～45%）。
4.根据权利要求1所述的制备方法，其特征在于：稀土元素Re选自Sc, Y, La, Ce, Pr,Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb或Lu。
5.根据权利要求1所述的制备方法，其特征在于：稀土元素Re为Y, Yb, Gd, Ce或Eu。
6.根据权利要求1所述的制备方法，其特征在于：步骤1）中球磨为湿磨，球料比为（1:1）～（4:1），球磨时间为4～48h。
7.根据权利要求1所述的制备方法，其特征在于：步骤1）中球磨为湿磨，溶剂为无水乙醇或丙酮，球磨介质为Si3N4，球磨时间为6～12h。
8.根据权利要求1所述的制备方法，其特征在于：步骤2）中气氛烧结的条件为：以20℃/min的升温速度将温度升至1350～1450℃并保温1-2h。
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CN102807389A (zh) * 2012-08-31 2012-12-05 哈尔滨工业大学 一种Si3N4-Si2N2O多孔复相陶瓷的制备方法
CN104086183A (zh) * 2014-07-02 2014-10-08 西安交通大学 一种气孔率可控多孔Si3N4的制备方法
CN104909765A (zh) * 2015-06-01 2015-09-16 广东工业大学 一种低成本、快速制备高性能Si3N4陶瓷球的方法

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CN102807389A (zh) * 2012-08-31 2012-12-05 哈尔滨工业大学 一种Si3N4-Si2N2O多孔复相陶瓷的制备方法
CN104086183A (zh) * 2014-07-02 2014-10-08 西安交通大学 一种气孔率可控多孔Si3N4的制备方法
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