CN107651964A - 一种AlN基复合陶瓷及其制备方法 - Google Patents

一种AlN基复合陶瓷及其制备方法 Download PDF

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CN107651964A
CN107651964A CN201711020757.7A CN201711020757A CN107651964A CN 107651964 A CN107651964 A CN 107651964A CN 201711020757 A CN201711020757 A CN 201711020757A CN 107651964 A CN107651964 A CN 107651964A
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aln
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伍尚华
刘聪
郭伟明
赵哲
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Guangdong University of Technology
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Abstract

本申请属于陶瓷技术领域，具体涉及一种AlN基复合陶瓷及其制备方法。本发明所提供的AlN基复合陶瓷包括：AlN和添加剂；所述添加剂为Re2O3和ZrO2；Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。本发明通过引入Re2O3促进AlN致密化，并引入ZrO2使其高温反应生成ZrN，进一步强化了本发明AlN基复合陶瓷的晶界。本发明还提供了上述AlN基复合陶瓷的制备方法，采用AlN作为基本原材料，以Re2O3作为烧结助剂，并适量添加纳米级ZrO2进行热压烧结。由本发明制备方法得到的AlN基复合陶瓷具有较好的热导率和断裂韧性，力学性能良好，可广泛应用于陶瓷、冶金、电子和化工等多种领域。

Description

一种AlN基复合陶瓷及其制备方法
技术领域
本发明属于陶瓷技术领域，具体涉及一种AlN基复合陶瓷及其制备方法。
背景技术
AlN陶瓷是以氮化铝为主晶相的陶瓷，具有高热导率、良好的电绝缘性能、较低的热膨胀系数、耐高温等优良的性能，是重要的基板封装材料和高温结构材料。但是AlN陶瓷的力学性能较差，尤其是断裂韧性，这增加了实际应用过程中的加工难度，从而限制了其广泛应用。
发明内容
为了解决现有AlN陶瓷断裂韧性较差的这一技术问题，本发明的目的在于提供一种力学性能较好的AlN基复合陶瓷。
本发明的具体技术方案如下：
一种AlN基复合陶瓷，其制备原料包括：AlN和添加剂；
所述添加剂为Re2O3和ZrO2；
Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
优选的，所述AlN、Re2O3和ZrO2的质量比优选为(80～98):(1～10):(0～15)，更优选为(83～94):(2～6):(4～10)。
本发明还提供了一种AlN基复合陶瓷的制备方法，包括：在惰性气体和真空条件下，将AlN、Re2O3和ZrO2进行热压烧结，得到所述AlN基复合陶瓷；
其中，所述AlN、Re2O3和ZrO2的质量比为(80～98):(1～10):(1～10)；
Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
优选的，所述热压烧结包括：
a)将AlN、Re2O3和ZrO2的混合粉体以第一升温速率升温至第一温度1000～1250℃，得到一次烧结体；
b)将所述一次烧结体以第二升温速率升温至第二温度1300～1600℃，得到二次烧结体；
c)将所述二次烧结体以第三升温速率升温至第三温度1600～2000℃；保温0.5～4h后，以降温速率降至1000～1400℃，最后随炉冷却，得到所述AlN复合陶瓷。
更优选的，所述第一升温速率、第二升温速率和第三升温速率优选为5～15℃/min，更优选为15℃/min、10℃/min或5℃/min；
所述降温速率优选为5～15℃/min，更优选为10℃/min。
优选的，所述惰性气体为氮气；所述真空条件的真空度为10Pa～0.1MPa。
优选的，所述热压烧结的载荷为15～40MPa。
优选的，在所述热压烧结之前还包括：将AlN、Re2O3和ZrO2球磨，得到AlN、Re2O3和ZrO2的混合粉体；
球磨介质为ZrO2球，ZrO2球的粒径优选为1～5mm。
更优选的，所述球磨的球料比优选为(1～5):1，更优选为3:1；球磨时间优选为4～48h，更优选为24h。
优选的，在所述球磨和所述热压烧结之间还包括：对所述混合粉体进行预压；
所述预压的载荷优选为5～10MPa，更优选为10MPa。
综上所述，本发明提供了一种AlN基复合陶瓷，其制备原材料包括：AlN和添加剂；所述添加剂为Re2O3和ZrO2；Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。本发明通过引入Re2O3促进AlN致密化，并引入ZrO2使其高温反应生成ZrN，进一步强化了本发明AlN基复合陶瓷的晶界。本发明还提供了上述AlN基复合陶瓷的制备方法，采用AlN作为基本原材料，以Re2O3作为烧结助剂，并适量添加纳米级ZrO2进行热压烧结。由本发明制备方法得到的AlN基复合陶瓷，主相为AlN，并由Al5Y3O12、ZrN相，强化了晶界。因此，本发明AlN基复合陶瓷具有较好的热导率和断裂韧性，力学性能良好，可广泛应用于陶瓷、冶金、电子和化工等多种领域。经过实验证明，采用本发明方法得到的AlN基复合陶瓷的相对密度高于95％，硬度为10～15GPa，抗弯强度为300～400MPa，断裂韧性为2～4MPa﹒m1/2。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
(1)以AlN粉末(粒径小于2μm，含氧量为0.53wt％)作为为原料，以Y2O3粉(纯度为99.9％)和ZrO2(四方晶，粒径为30nm)为添加剂，置于辊式球磨机中混合；按重量份数进行配料，91份AlN粉，4份Y2O3，5份ZrO2。
在球磨时，以乙醇为溶剂，以ZrO2球为球磨介质，球料比调节为3:1，球磨时间为24h，经混料、干燥后，得到混合均匀的AlN-Y2O3-ZrO2混合粉体。
(2)将AlN-Y2O3-ZrO2混合粉体放入石墨模具中，经预压(常温下以10MPa预压5min)后，在真空条件和惰性气体保护环境下进行热压烧结；首先以15℃/min的升温速率升温至第一温度1200℃，然后以10℃/min的升温速率继续将温度升至第二温度1600℃，接着再以5℃/min的升温速率将温度升至第三温度1800℃，接着以10℃/min的降温速率将温度降至1200℃，最后随炉冷却。
其中，热压烧结的载荷(热压烧结过程中模具压头施加的机械压力)为25MPa，最高温度下保温保压2h，整个烧结过程的气氛为N2，气压大小为0.1MPa。
经过检测，本实施的AlN基陶瓷的相对密度为100％，硬度为10.08GPa，抗弯强度为312.63MPa，断裂韧性为2.87MPa﹒m1/2。
实施例2
本实施例与实施例1的区别在于：在步骤(1)中，配料时：86份AlN粉，4份Y2O3，10份ZrO2。其余地方与实施例1基本相同，此处不再一一赘述。
经过检测，本实施的AlN基陶瓷的相对密度为99.5％，硬度为10.45GPa，抗弯强度为302.12MPa，断裂韧性为3.02MPa﹒m1/2。
实施例3
本实施例与实施例1的区别在于：在步骤(1)中，配料时：84份AlN粉，4份Y2O3，12份ZrO2。其余地方与实施例1基本相同，此处不再一一赘述。
经过检测，本实施的AlN基陶瓷的相对密度为99.6％，硬度为10.3GPa，抗弯强度为320MPa，断裂韧性为3.20MPa﹒m1/2。
实施例4
本实施例与实施例1的区别在于：在步骤(1)中，配料时：81份AlN粉，4份Y2O3，15份ZrO2。其余地方与实施例1基本相同，此处不再一一赘述。
经过检测，本实施的AlN基陶瓷的相对密度为99.0％，硬度为10.0GPa，抗弯强度为317MPa，断裂韧性为3.30MPa﹒m1/2。
实施例5
本实施例与实施例1的区别在于：在步骤(1)中，配料时：96份AlN粉，4份Y2O3。其余地方与实施例1基本相同，此处不再一一赘述。
经过检测，本实施的AlN基陶瓷的相对密度为100％，硬度为10.2GPa，抗弯强度为333MPa，断裂韧性为2.4MPa﹒m1/2。

Claims (10)

1.一种AlN基复合陶瓷，其特征在于，其制备原料包括：AlN和添加剂；
所述添加剂为Re2O3和ZrO2；
Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
2.根据权利要求1所述的AlN基复合陶瓷，其特征在于，所述AlN、Re2O3和ZrO2的质量比为(80～98):(1～10):(0～15)。
3.一种权利要求1或2所述的AlN基复合陶瓷的制备方法，其特征在于，包括：在惰性气体和真空条件下，将AlN、Re2O3和ZrO2进行热压烧结，得到所述AlN基复合陶瓷；
其中，所述AlN、Re2O3和ZrO2的质量比为(80～98):(1～10):(1～10)；
Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
4.根据权利要求3所述的制备方法，其特征在于，所述热压烧结包括：
a)将AlN、Re2O3和ZrO2的混合粉体以第一升温速率升温至第一温度1000～1250℃，得到一次烧结体；
b)将所述一次烧结体以第二升温速率升温至第二温度1300～1600℃，得到二次烧结体；
c)将所述二次烧结体以第三升温速率升温至第三温度1600～2000℃；保温0.5～4h后，以降温速率降至1000～1400℃，最后随炉冷却，得到所述AlN基复合陶瓷。
5.根据权利要求4所述的制备方法，其特征在于，所述第一升温速率、第二升温速率和第三升温速率为5～15℃/min；
所述降温速率为5～15℃/min。
6.根据权利要求3所述的制备方法，其特征在于，所述惰性气体为氮气；
所述真空条件的真空度为10Pa～0.1MPa。
7.根据权利要求3所述的制备方法，其特征在于，所述热压烧结的载荷为15～40MPa。
8.根据权利要求3所述的制备方法，其特征在于，在所述热压烧结之前还包括：将AlN、Re2O3和ZrO2球磨，得到AlN、Re2O3和ZrO2的混合粉体；
球磨介质为ZrO2球。
9.根据权利要求8所述的制备方法，其特征在于，所述球磨的球料比为(1～5):1；
球磨时间为4～48h。
10.根据权利要求8所述的制备方法，其特征在于，在所述球磨和所述热压烧结之间还包括：对所述混合粉体进行预压；
所述预压的载荷为5～10MPa。
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