连续纤维增强陶瓷基复合材料微观力学研究进展

doi:10.15541/jim20170421

摘要/Abstract

摘要：

微观力学参数是构建连续纤维增强陶瓷基复合材料(CFRCMCs)组分、微观结构和宏观力学性能的桥梁, 但受限于CFRCMCs的脆性和微观力学参数测试水平, 微观力学研究工作进展缓慢。随着基于纳米压痕的微观力学测试技术和基于聚焦离子束微观测试样品制备技术的飞速发展, 近年来CFRCMCs的微观力学研究工作取得显著进步。本文结合国防科技大学刘海韬课题组的研究工作, 重点对CFRCMCs组分的原位模量、断裂韧性以及界面结合强度的测试方法和典型应用进行了讨论, 最后举例说明了基于微观力学参数的CFRCMCs宏观力学行为的预判方法。

关键词: 陶瓷基复合材料, 微观力学, 纳米压痕, 聚焦离子束, 综述

Abstract:

Localized mechanical properties of composite components (fiber, matrix, and interface) are critical parameters bridging the composition, microstructure and macro-mechanical performance of continuous fiber-reinforced ceramic matrix composites (CFRCMCs). However, they are difficult to be acquired and decoupled from bulk composites based on the traditional macro-mechanical testing techniques, due to their limited testing volumes and complex heterogeneous composite structures. The above questions has been solved recently by novel nano/micro mechanical testing and focused ion beam milling (FIB) techniques, which provide powerful tools to quantify the micro-mechanical properties of CFRCMCs. In this paper, recent progress in micro-mechanical properties of CFRCMCs was firstly reviewed, with special emphasis on the in-situ modulus and toughness of ceramic fibers and matrix, and the shear property of fiber/matrix interface. Following that, a criterion based on the He-Hutchinson cracking model was proposed to predict the macro mechanical performance of CFRCMCs by using those micro-mechanical parameters.

Key words: ceramic matrix composites, micro-mechanics, nanoindentation, focused ion beam, review

中图分类号:

TB323

刘海韬, 杨玲伟, 韩爽. 连续纤维增强陶瓷基复合材料微观力学研究进展[J]. 无机材料学报, 2018, 33(7): 711-720.

LIU Hai-Tao, YANG Ling-Wei, HAN Shuang. Research Progress on Micro-mechanical Property of Continuous Fiber-reinforced Ceramic Matrix Composites[J]. Journal of Inorganic Materials, 2018, 33(7): 711-720.

图/表 13

图1 (a)不同温度制备的ASf/SiO2复合材料AS纤维模量与压头压入深度关系; 600℃(b)和1200℃(c)制备的ASf/SiO2复合材料AS纤维纳米压痕测试后的SPM(Scanning Probe Microscopy)照片[10]

Fig. 1 (a) Young's modulus of the AS fiber in ASf/SiO2 composites prepared at different temperatures as a function of penetration depth; SPM images of the nanoindentation imprints of ASf/SiO2 composites fabricated at 600℃ (b) and 1200℃ (c)[10]

图2 不同温度制备的ASf/SiO2复合材料SiO2基体模量与压头压入深度关系[10]

Fig. 2 Young°s modulus of the SiO2 matrix in ASf/SiO2 composites prepared at different temperatures as a function of penetration depth[10]

图3 碳化物陶瓷涂层压痕裂纹SEM照片[32]

Fig. 3 Radial cracks originating at the edges of a Berkovick indentation for carbide coating[32]

图4 (a)单边切口微梁尺寸示意图; SiCf/SiC复合材料碳化硅基体单边切口微梁加载前(b)后(c)的SEM照片[11,18]

Fig. 4 (a) Schematic representation of the micro-cantilever bending geometry; SEM images of a micro-cantilever prepared from SiC matrix in SiCf/SiC composites before (a) and after (b) testing[11,18]

图5 韧性测试失效微柱的SEM照片[17]

Fig. 5 SEM image of an example of a pillar after splitting[17]

图6 (a), (b)SiC纤维与基体微柱; (c), (d)SiC纤维与基体微柱失效的SEM照片; (e)典型SiC纤维与基体微柱载荷-位移曲线; (f)不同温度制备的复合材料SiC纤维与基体韧性[28]

Fig. 6 Morphologies of the micropillars on individual SiC matrix and SiC fiber (a, b); Micropillar morphologies of SiC fiber and SiC matrix after pillar splitting tests(c, d); Representive force-displacement curves of SiC matrix and SiC fiber by the micropillar splitting tests (e); Evolution of localized fracture toughness of the SiC matrix and SiC fiber as a function of composite fabrication temperature(f)[28]

图7 典型的束丝复合材料载荷-位移曲线[39]

Fig. 7 Typical features of the load-deformation curve of mini- composites[39]

图8 (a)单纤维顶出实验实施过程示意图; (b)典型纤维顶出实验载荷-位移曲线; SiCf/SiC复合材料顶出纤维压头正面(c)和背面(d)SEM照片[43]

Fig. 8 (a) Schematic drawing of fiber push-out measurement; (b) Typical load-displacement push-out test curve; SEM images of the frontside surface (c) and backside surface (d) of SiCf/SiC minicomposite after fiber push-out test using a flat punch indenter[43]

图9 (a)纤维顶入测试示意图和(b)典型纤维顶入实验载荷-位移曲线[45]

Fig. 9 (a) Schematic drawing of fiber push-in measurement, (b) Typical load-displacement push-in test curve[45]

表1 国防科技大学刘海韬课题组CFRCMCs界面结合强度研究工作

Table 1 Interfacial bonding strength of typical CFRCMCs investigated in our research group

Composites	Interphase	τ/MPa	Flexural strength/MPa	Fracture mode	Ref.
PIP 3D C_f/SiC	None	105	23	Brittle	[19]
PIP 3D C_f/SiC	PyC	30	378	Toughened	[19]
PIP 3D Nextel440 AS_f/SiC	None	293	45	Brittle	[34]
PIP 3D Nextel440 AS_f/SiC	PyC	42	163	Toughened	[34]
Sol-Gel 3D SiC_f/Mullite	None	537	230	Brittle	[46]
Sol-Gel 3D SiC_f/Mullite	PyC	155	35	Toughened	[46]
PIP 3D SiC_f/SiC	None	450	90	Brittle	[28]
PIP 3D SiC_f/SiC	BN	50	200	Toughened	[28]
Sol-Gel 3D ALF AS_f/SiO₂(600℃)	None	50	105	Toughened	[10]
Sol-Gel 3D ALF AS_f/SiO₂(1200℃)	None	260	45	Brittle	[10]

图10 单纤维顶入实验后ASf/SiC (a)和ASf/C/SiC (b)复合材料压入纤维的SEM照片[34]

Fig. 10 SEM images of the pushed fiber in ASf/SiC (a) and ASf/C/SiC (b) composites[34]

表2 国防科技大学刘海韬课题组研究的SiCf/SiC和SiCf/BN/SiC复合材料微观力学参数[28]

Table 2 Micro-mechanical parameters of SiCf/SiC and SiCf/BN/SiC composites investigated in Liu’s group[28]

Composites	E_m/GPa	E_f/GPa	Γ_m/(J·m^-2)	Γ_f/(J·m^-2)	E_{BN interphase}/GPa	Γ_{BN interphase}/(J·m^-2)
SiC_f/SiC (800℃)	118	160	49	29	-	-
SiC_f/SiC (900℃)	170	160	15	29	-	-
SiC_f/SiC (1000℃)	256	160	5	29	-	-
SiC_f/BN/SiC	-	160	-	29	70	4

图11 基于H-H模型的SiCf/SiC和SiCf/BN/SiC复合材料宏观力学行为预判[28]

Fig. 11 Predictions on macro-mechanical behavior of SiCf/SiC and SiCf/BN/SiC composites based on H-H model[28]

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