放电等离子烧结制备ZrB<sub>2</sub>-SiC超高温陶瓷的力学性能及氧化行为

何慧娟; 闫晓杰; 树学峰; 肖革胜; 郝鑫; 李志刚

doi:10.11858/gywlxb.20200623

放电等离子烧结制备ZrB₂-SiC超高温陶瓷的力学性能及氧化行为

doi: 10.11858/gywlxb.20200623

太原理工大学机械与运载工程学院应用力学研究所，山西太原　030024

基金项目: 国家自然科学基金（11772217，11802198）

详细信息

作者简介:
何慧娟（1995－），女，硕士研究生，主要从事弹塑性力学研究. E-mail：1945106146@qq.com

通讯作者:
李志刚（1975－），男，副教授，主要从事弹塑性力学研究. E-mail：254970134@qq.com

中图分类号: O347.3
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出版历程
- 收稿日期: 2020-10-09
- 修回日期: 2020-11-06

Mechanical Properties and Oxidation Behavior of ZrB₂-SiC Ultra-High Temperature Ceramics Prepared by Spark Plasma Sintering

Institute of Applied Mechanics, College of Mechanical and Vehicle Engineering, Taiyuan University of Technology, Taiyuan 030024, Shanxi, China

摘要

摘要: 在服役环境中，超高声速飞行器表面与空气剧烈摩擦导致温度极高。超高温陶瓷相较于一般陶瓷而言具有高熔点和良好的抗氧化烧蚀性能，是目前极具前景的热防护材料之一。采用放电等离子两步烧结工艺将ZrB₂纳米粉末和SiC粉末在1 700 ℃下制备超高温陶瓷材料ZrB₂-20%SiC，通过纳米压痕微观实验、三点弯实验研究其力学性能及其在高温环境下的氧化行为，着重分析1 000、1 200、1 400和1 600 ℃ 4种不同氧化温度下ZrB₂-20%SiC超高温陶瓷的氧化表面、氧化截面和氧化层厚度。结果表明：ZrB₂-20%SiC超高温陶瓷的硬度为18 GPa，弹性模量为541 GPa，断裂韧性为5.7 MPa·m^1/2；当氧化温度为1600 ℃时，超高温陶瓷内部的SiC由被动氧化转变为主动氧化，并且随着氧化温度升高，超高温陶瓷氧化层厚度与氧化温度呈正相关。
- ZrB₂-SiC /
- 超高温陶瓷 /
- 放电等离子烧结 /
- 力学性能 /
- 氧化行为
Abstract: In the application environment, the surface of the ultra-high-speed aircraft is violently rubbed with the air to make the temperature extremely high. Compared with ordinary ceramics, ultra-high temperature ceramics possess a higher melting point with good oxidation and ablation resistance performance. Therefore, it is particularly interested to be used as thermal protection materials. In this paper, ZrB₂-20%SiC ultra-high temperature ceramic materials are prepared by using the spark plasma two-step sintering process of ZrB₂ nanopowder and SiC powder at 1700 ℃. The mechanical properties of ZrB₂-20%SiC are studied through nanoindentation experiment and three-point bending experiment. The oxidation behavior of ZrB₂-20%SiC ultra-high temperature ceramics at four different oxidation temperatures of 1000, 1200, 1400 and 1600 ℃ is analyzed in this paper. The results show that the hardness of the ZrB2-20%SiC ultra-high temperature is 18 GPa, and the elastic modulus is 541 GPa with the fracture toughness of 5.7 MPa·m^1/2. When the oxidation temperature is 1600 ℃, the SiC inside the ultra-high temperature ceramic would transform from passive oxidation to active oxidation. As the oxidation temperature increases, the thickness of the ultra-high temperature ceramic oxide layer and the oxidation temperature demonstrate a positive correlation trend.
- ZrB₂-SiC /
- ultra-high temperature ceramics /
- spark plasma sintering /
- mechanical properties /
- oxidationbehavior

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图 1 放电等离子烧结曲线

Figure 1. Curves of spark plasma sintering

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图 2 未抛光烧结试件

Figure 2. Unpolished sintered sample

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图 3 三点弯单边切口试验 (a)及试件断口形貌(b)

Figure 3. Schematic diagram of three-point bending single-side notch test (a) and fracture morphology of the specimen (b)

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图 4 GSX-1600高温氧化炉

Figure 4. GSX-1600 high temperature oxidation furnace

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图 5 ZrB₂-SiC的纳米压入实验：（a）载荷-位移曲线，（b）弹性模量-位移曲线，（c）硬度-位移曲线

Figure 5. ZrB₂-SiC nanoindentation experiment：(a) load-displacement curves，(b) elastic modulus-displacement curves， (c) hardness-displacement curves

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图 6 ZrB₂-20%SiC超高温陶瓷抛光表面

Figure 6. Polished surface of ZrB₂-20%SiC ultra-high temperature ceramic

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图 7 ZrB₂-20%SiC超高温陶瓷断裂截面

Figure 7. Fracture section of ZrB₂-20%SiC ultra-high temperature ceramic

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图 8 不同氧化温度( 1 000 ～ 1 600 ℃)下ZrB₂-20%SiC超高温陶瓷的氧化表面

Figure 8. Oxidized surface of ZrB₂-20%SiC ultra-high temperature ceramic at different oxidation temperatures (1 000–1 600 ℃)

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图 9 在不同氧化温度下（1200、1400 和 1600 ℃）ZrB₂-20%SiC的超高温陶瓷的氧化截面

Figure 9. Oxidation cross-sections of ZrB₂-20%SiC ultra-high temperature ceramicsat different oxidation temperatures (1200, 1400 and 1600 ℃)

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图 10 ZrB₂-SiC超高温陶瓷在不同氧化温度下（1000～1600 ℃）的氧化层厚度

Figure 10. Oxide layer thickness of ZrB₂-SiC ultra-high temperature ceramic at different temperatures (1000–1600 ℃)

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表 1 ZrB₂基陶瓷材料的粒径尺寸、相对密度及力学性能

Table 1. Particle size, relative density and mechanical properties of ZrB₂-based ceramic materials

Material	ZrB₂ particle size/μm	SiC particle size/μm	Relative density/%	Elastic modulus/MPa	Hardness/ GPa	Fracture toughness/ (MPa·m^1/2)	Preparation method
ZrB₂-20%SiC^[22]	3.0	1.50	94.4		13.4	4.8	Hot press sintering
ZrB₂-20%SiC^[23]	3.9	2.00	97.5	446		5.5	Hot press sintering
ZrB₂-20%SiC^[24]	1.2	1.00	99.8	520	20.7	4.6	Hot press sintering
ZrB₂-20%SiC	0.4	0.05	98.1	541	18.0	5.7	Spark plasma sintering

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