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

参考文献 24

[1]	FAHRENHOLTZ W G, HILMAS G E, TALMY I G ,et al. Refractory diborides of zirconium and hafnium. Journal of the American Ceramic Society, 2007,90(5):1347-1364.
[2]	CHAMBERLAIN A L, FAHRENHOLTZ W G, HILMAS G E ,et al. High-strength zirconium diboride-based ceramics. Journal of the American Ceramic Society, 2004,87(6):1170-1172.
[3]	GUO S Q . Densification of ZrB₂-based composites and their mechanical and physical properties: a review. Journal of the European Ceramic Society, 2009,29(6):995-1011.
[4]	ZHENG H Y, MENG C X, HU D L ,et al. EBSD Analysis for orientation relationship of textured ZrB₂-SiC ultra-high temperature ceramics. Journal of Inorganic Materials, 2018,33(4):380-384.
[5]	ZHANG G J, NI D W, ZOU J ,et al. Inherent anisotropy in transition metal diborides and microstructure/property tailoring in ultra- high temperature ceramics-a review. Journal of the European Ceramic Society, 2017,38(2):371-389.
[6]	WU W W, WANG Z, ZHANG G J ,et al. ZrB₂-MoSi₂ composites toughened by elongated ZrB₂ grains via reactive hot pressing. Scripta Materialia, 2009,61(3):316-319.
[7]	SHAHEDI ASL M, FARAHBAKHSH I, NAYEBI B . Characteristics of multi-walled carbon nanotube toughened ZrB₂-SiC ceramic composite prepared by hot pressing. Ceramics International, 2016,42(1):1950-1958.
[8]	ZHU T, XU L, ZHANG X H ,et al. Densification, microstructure and mechanical properties of ZrB₂-SiC_w ceramic composites. Journal of the European Ceramic Society, 2009,29(13):2893-2901.
[9]	HU P, GUI K X, HONG W H ,et al. High-performance ZrB₂-SiC-C_f composite prepared by low-temperature hot pressing using nanosized ZrB₂ powder. Journal of the European Ceramic Society, 2017,37(6):2317-2324.
[10]	GUI K X, LIU F Y, WANG G ,et al. Inhibited degradation of carbon fibers in ZrB₂-SiC-C_sf ultra-high temperature ceramic composites. Journal of Synthetic Crystals, 2018,47(2):418-423.
[11]	HE P G, JIA D C, LI Y T ,et al. Preparation and mechanical performance of ductile C_sf/Al₂O₃-BN composites-Part 2: Effects of fiber contents and ablation properties. Ceramics International, 2016,42(9):11063-11069.
[12]	BAI Y L, HE X D, ZHU C C ,et al. Microstructures, electrical, thermal, and mechanical properties of bulk Ti₂AlC synthesized by self-propagating high-temperature combustion synthesis with pseudo hot isostatic pressing. Journal of the American Ceramic Society, 2012,95(1):358-364.
[13]	WANG M C, ZHANG Z G, SUN Z J ,et al. Effect of fiber type on mechanical properties of short carbon fiber reinforced B₄C composites. Ceramics International, 2009,35(4):1461-1466.
[14]	ZU Y F, SHA J J, LI J ,et al. Effect of multi-walled carbon nanotubes on microstructure and fracture properties of carbon fiber- reinforced ZrB₂-based ceramic composite. Ceramics International, 2017,43(10):7454-7460.
[15]	SHA J J, ZHANG Z F, DI S X ,et al. Microstructure and mechanical properties of ZrB₂-based ceramic composites with nano-sized SiC particles synthesized by in-situ reaction. Materials Science and Engineering A, 2017,693:145-150.
[16]	SILVESTRONI L, MERIGGI G, SCITI D . Oxidation behavior of ZrB₂ composites doped with various transition metal silicides. Corrosion Science, 2014,83:281-291.
[17]	LIU H L, LIU J X, LIU H T ,et al. Changed oxidation behavior of ZrB₂-SiC ceramics with the addition of ZrC. Ceramics International, 2015,41(6):8247-8251.
[18]	HU C F, ZOU J, HUANG Q ,et al. Synthesis of plate-Like ZrB₂ Grains. Journal of the American Ceramic Society, 2012,95(1):85-88.
[19]	ZOU J, ZHANG G J, KAN Y M . Formation of tough interlocking microstructure in ZrB₂-SiC-based ultrahigh-temperature ceramics by pressureless sintering. Journal of Materials Research, 2009,24(7):2428-2434.
[20]	XU L, HUANG C Z, LIU H L ,et al. In situ synthesis of ZrB₂ -ZrC_x ceramic tool materials toughened by elongated ZrB₂ grains. Materials & Design, 2013,49:226-233.
[21]	ZHANG S C, HILMAS G E, FAHRENHOLTZ W G . Mechanical properties of sintered ZrB₂-SiC ceramics. Journal of the European Ceramic Society, 2011,31(5):893-901.
[22]	YANG F Y, ZHANG X H, HAN J C ,et al. Analysis of the mechanical properties in short carbon fiber-toughened ZrB₂-SiC ultra- high temperature ceramic. Journal of Composite Materials, 2010,44(8):953-961.
[23]	VINCI A, ZOLI L, SCITI D ,et al. Understanding the mechanical properties of novel UHTCMCs through random forest and regression tree analysis. Materials & Design, 2018,145:97-107.
[24]	TAYLOR D, CORNETTI P, PUGNO N . The fracture mechanics of finite crack extension. Engineering Fracture Mechanics, 2005,72(7):1021-1038.

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

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 9

参考文献 24

相关文章 15

编辑推荐

Metrics

本文评价

[1]	周帆, 田志林, 李斌. 热防护系统用碳化物超高温陶瓷抗烧蚀涂层研究进展[J]. 无机材料学报, 2025, 40(1): 1-16.
[2]	谭敏, 陈小武, 杨金山, 张翔宇, 阚艳梅, 周海军, 薛玉冬, 董绍明. 流延成型结合反应熔渗制备ZrB₂-SiC陶瓷及其微观结构与氧化行为研究[J]. 无机材料学报, 2024, 39(8): 955-964.
[3]	张幸红, 王义铭, 程源, 董顺, 胡平. 超高温陶瓷复合材料研究进展[J]. 无机材料学报, 2024, 39(6): 571-590.
[4]	蔡飞燕, 倪德伟, 董绍明. 高熵碳化物超高温陶瓷的研究进展[J]. 无机材料学报, 2024, 39(6): 591-608.
[5]	张育育, 吴轶城, 孙佳, 付前刚. 聚合物转化SiHfCN陶瓷的制备及其吸波性能[J]. 无机材料学报, 2024, 39(6): 681-690.
[6]	郑海亚, 孟晨曦, 胡冬力, 顾辉, 刘海涛, 张国军. 织构化ZrB₂-SiC超高温陶瓷中取向关系的EBSD研究[J]. 无机材料学报, 2018, 33(4): 380-384.
[7]	胡冬力, 邢娟娟, 郑强, 顾辉, 倪德伟, 张国军. HfB₂-SiC-HfC陶瓷相组成与相成分定量分析的对比研究[J]. 无机材料学报, 2014, 29(10): 1105-1109.
[8]	郑强, 王贤浩, 邢娟娟, 顾辉, 张国军. ZrB₂-SiC-ZrC复相超高温陶瓷相组成的定量分析[J]. 无机材料学报, 2013, 28(4): 358-362.
[9]	周海军, 张翔宇, 高乐, 胡建宝, 吴斌, 董绍明. ZrB₂-SiC超高温陶瓷涂层的抗烧蚀性能研究[J]. 无机材料学报, 2013, 28(3): 256-260.
[10]	伏金刚, 朱冬梅, 周万城, 罗发. 定向分布碳纤维复合材料介电性能研究[J]. 无机材料学报, 2012, 27(11): 1223-1227.
[11]	赵大方,王海哲,李效东. 先驱体转化法制备SiC纤维的研究进展[J]. 无机材料学报, 2009, 24(6): 1097-1104.
[12]	王新刚,刘吉轩,阚艳梅,张国军,王佩玲. ZrB₂-SiC陶瓷的注浆成型与无压烧结[J]. 无机材料学报, 2009, 24(4): 831-835.
[13]	闫永杰,张辉,黄政仁,刘学建. 常压烧结ZrB₂-SiC复相材料的抗氧化行为研究[J]. 无机材料学报, 2009, 24(3): 631-635.
[14]	杨飞宇,张幸红,韩杰才,杜善义. ZrB₂-SiC和C_sf/ZrB₂-SiC超高温陶瓷基复合材料烧蚀机理的研究[J]. 无机材料学报, 2008, 23(4): 734-738.
[15]	邹俭鹏,阮建明,周忠诚,黄伯云,陈启元. 316L纤维尺寸和含量对HA-ZrO₂(CaO)/316L纤维复合生物材料性能的影响[J]. 无机材料学报, 2007, 22(5): 1001-1006.