晶粒互锁结构与短切碳纤维增韧ZrB2-SiC复合材料的制备与力学性能

doi:10.15541/jim20180557

无机材料学报 ›› 2019, Vol. 34 ›› Issue (9): 918-924.DOI: 10.15541/jim20180557 CSTR: 32189.14.10.15541/jim20180557

所属专题：陶瓷基复合材料

晶粒互锁结构与短切碳纤维增韧ZrB₂-SiC复合材料的制备与力学性能

张兆甫¹,沙建军^1,²(),祖宇飞¹,代吉祥¹

1.大连理工大学辽宁省空天飞行器前沿技术重点实验室
2.航空航天学院, 工业装备结构分析国家重点实验室, 大连 116024

收稿日期:2018-11-28 修回日期:2019-01-22 出版日期:2019-09-20 网络出版日期:2019-05-22
作者简介:张兆甫(1990-), 男, 博士研究生. E-mail: zhangzhaofu@mail.dlut.edu.cn
基金资助:
国家自然科学基金(51805069);中国博士后科学基金(2016M600201);中国博士后科学基金(2018T110214);中国博士后科学基金(2016M601304);辽宁省自然科学基金(20170540154);航空科学基金(2016ZF63007)

ZrB₂-SiC Composites Toughened by Interlocking Microstructure and Chopped Carbon Fiber

ZHANG Zhao-Fu¹,SHA Jian-Jun^1,²(),ZU Yu-Fei¹,DAI Ji-Xiang¹

1.Key Lab of Advanced Technology for Aerospace Vehicles, Dalian University of Technology, Dalian 116024, China
2.State Key Lab. of Structural Analyses for Industrial Equipment, School of Aeronautics and Astronautics, Dalian University of Technology, Dalian 116024, China

Received:2018-11-28 Revised:2019-01-22 Published:2019-09-20 Online:2019-05-22
Supported by:
National Natural Science Foundation of China(51805069);China Postdoctoral Science Foundation(2016M600201);China Postdoctoral Science Foundation(2018T110214);China Postdoctoral Science Foundation(2016M601304);Natural Science Foundation of Liaoning Province, China(20170540154);Aviation Science Foundation of China(2016ZF63007)

摘要/Abstract

摘要：

ZrB₂-SiC基复合材料具有比单体ZrB₂更优异的抗氧化性能及力学性能, 但其相对较低的韧性限制了其实际工程应用, 采用微结构设计或引入增韧相是改善陶瓷材料韧性的两个有效途径。本研究采用反应热压烧结工艺, 分别制备了具有独特片状ZrB₂晶粒互锁结构的ZrB₂-SiC复合材料和以短切碳纤维(C_sf)为增韧相的C_sf/ZrB₂-SiC复合材料。对比研究发现, 晶粒互锁结构展现出优异的自强韧化效果, 使ZrB₂-SiC复合材料具有较高的弯曲强度及断裂韧性, 但材料表现出典型的脆性断裂特征; C_sf/ZrB₂-SiC复合材料弯曲强度下降, 但C_sf具有显著的增韧作用, 不仅使材料具有较高的断裂韧性, 而且临界裂纹尺寸及断裂功都得到显著提高, 从而表现出非灾难性破坏模式。

关键词: 超高温陶瓷, 晶粒互锁结构, 短切碳纤维, ZrB₂-SiC, 断裂性能

Abstract:

ZrB₂-SiC ceramics present better oxidation resistance and mechanical properties than monolithic ZrB₂ ceramics. However, the small damage tolerance and poor crack growth resistance, which result in the low fracture toughness, limit the engineering application of ZrB₂-SiC ceramics. Focusing on this issue, microstructure design and introduction of toughening phase are two effective approaches to improve the fracture toughness of ZrB₂-SiC ceramics. In this work, ZrB₂-SiC and C_f/ZrB₂-SiC composites were toughened respectively by interlocking microstructure and chopped carbon fibers via reactive hot pressing. For the ZrB₂-SiC composites, the interlocking microstructure formed by in-situ ZrB₂ platelets presented excellent self-enhancing effect. The ZrB₂-SiC composites had high bending strength and fracture toughness. However, the composite exhibited typical brittle fracture characteristics. Compared with ZrB₂-SiC composite, the flexural strength of C_f/ZrB₂-SiC composite decreased, but the fracture toughness was comparable with the ZrB₂-SiC composite. Furthermore, the critical crack size and the work of fracture of C_f/ZrB₂-SiC composites significantly improved, and the composite presented the non-catastrophic failure mode.

Key words: ultra-high temperature ceramic, interlocking microstructure, chopped carbon fiber, ZrB₂-SiC, fracture property

中图分类号:

TB332

张兆甫,沙建军,祖宇飞,代吉祥. 晶粒互锁结构与短切碳纤维增韧ZrB₂-SiC复合材料的制备与力学性能[J]. 无机材料学报, 2019, 34(9): 918-924.

ZHANG Zhao-Fu,SHA Jian-Jun,ZU Yu-Fei,DAI Ji-Xiang. ZrB₂-SiC Composites Toughened by Interlocking Microstructure and Chopped Carbon Fiber[J]. Journal of Inorganic Materials, 2019, 34(9): 918-924.

图/表 9

图1 ZrB2-SiC(ZS)及Csf/ZrB2-SiC(Csf/ZS)复合材料致密化曲线

Fig. 1 The densification curves of ZrB2-SiC(ZS) and Csf/ZrB2-SiC(Csf/ZS) composites

表1 ZS及Csf/ZS样品密度、相对密度及孔隙率

Table 1 Density, porosity and relative density of ZS and Csf/ZS composites

Sample	Theoretical density/ (g?cm^-3)	Bulk density/ (g?cm^-3)	Open porosity/ %	Closed porosity/ %	Relative density/ %
ZS	4.52	4.41	1.72	0.68	97.6
C_sf/ZS	3.97	3.79	3.27	1.13	95.6

图2 球磨后混合粉体及反应热压烧结样品的XRD图谱

Fig. 2 XRD patterns of ball-milled powder mixture and reactive hot pressed composites

图3 (a) ZS样品抛光表面背散射电子显微照片; (b) ZS样品断面二次电子显微照片; (c) 图3(a)中A点EDS分析结果

Fig. 3 (a) Backscattered electron micrograph taken from polished surface of ZS sample, (b) secondary electron micrograph taken from fracture surface of ZS sample, and (c) EDS analysis taken from the point A in (a)

图4 Csf/ZS复合材料电子显微照片

Fig. 4 SEM micrographs of Csf/ZS composites (a) Polished surface; (b) Interfacial domain

表2 ZS及Csf/ZS复合材料的力学性能

Table 2 Mechanical properties of ZS and Csf/ZS composites

Sample	Vickers hardness /GPa	Flexural strength, σ/MPa	Fracture toughness, K_IC/ (MPa?m^1/2)	K_IC/σ	Work of fracture/ (J?m^-2)
ZS	(17.1±0.7)	(655±21)	6.08±0.17	0.009	149.40
C_sf/ZS	(13.8±0.2)	(368±27)	(5.41±0.25)	0.015	264.06

图5 ZS与Csf/ZS复合材料的SENB测试载荷-位移曲线

Fig. 5 Load-displacement curves of ZS and Csf/ZS composites during SENB tests

图6 (a) ZS样品断面二次电子显微照片; (b) ZS样品表面裂纹扩展背散射电子显微照片

Fig. 6 (a) Secondary electron micrograph taken from fracture surface of ZS sample, and (b) backscattered electron micrograph of indentation crack propagation on polished surface of ZS sample

图7 Csf/ZS复合材料的SEM照片

Fig. 7 SEM micrographs of Csf/ZS composites (a) Fracture surface; (b) Matrix; (c, d) Crack propagation path

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晶粒互锁结构与短切碳纤维增韧ZrB₂-SiC复合材料的制备与力学性能

ZrB₂-SiC Composites Toughened by Interlocking Microstructure and Chopped Carbon Fiber

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