中温蠕变条件下SiC<sub>f</sub>/SiC复合材料界面的微观结构及其力学性能演变规律

陈乐; 管皞阳; 朱思雨; 王佳璇; 唐睿; 何宗倍; 张程煜

中温蠕变条件下SiC_f/SiC复合材料界面的微观结构及其力学性能演变规律

1.
中国核动力研究设计院反应堆燃料及材料重点实验室, 成都 610213
2.
西北工业大学超高温结构复合材料重点实验室, 西安 710072
3.
航空工业济南特种结构研究所, 济南 250023

基金项目: 国家自然科学基金(U2241239)；国防科技基础加强计划(No. 2023-JCJQ-LB-071)

详细信息

通讯作者:
张程煜，博士，教授，博士生导师，研究方向为陶瓷基复合材料　E-mail: cyzhang@nwpu.edu.cn

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2024-06-25
- 修回日期: 2024-08-16
- 录用日期: 2024-09-20
- 网络出版日期: 2024-09-30

Evolution on the microstructure and mechanical properties of the interface of crept SiC_f/SiC at intermediate temperatures

1.
Science and Technology on Reactor Fuel and Materials Laboratory, Nuclear Power Institute of China, Chengdu 610213, China
2.
Key Laboratory of Ultra-high Temperature Structural Composites, Northwestern Polytechnical University, Xi’an 710072, China
3.
Research Institute for Special Structures of Aeronautical Composites AVIC, Jinan 250023, China

Funds: National Natural Science Foundation of China (U2241239); The Basic Strengthening Program of China (No. 2023-JCJQ-LB-071)

摘要

摘要: 连续碳化硅纤维增强碳化硅复合材料(SiC_f/SiC)在中温(500~1000 ℃)范围内会发生蠕变断裂时间显著缩短的脆化现象，其机制主要与界面的微观结构和力学性能有关。为此，本文开展了国产二代平纹编织SiC_f/SiC (2D-SiC_f/SiC) 复合材料在中温范围的蠕变脆化失效机制研究。利用TEM分析了中温下不同蠕变条件后2D-SiC_f/SiC的界面微观结构，进一步利用微纳力学测试技术表征界面力学性能。结果表明：纤维/界面侧在500 ℃下出现多孔隙的富碳层；800 ℃时，界面出现自发氧化，同时SiO₂填充了部分BN界面因氧化消耗后产生的空隙。当温度进一步升高至1000 ℃后，氧元素主要分布于纤维/基体一侧。2D-SiC_f/SiC的中温脆化机制与界面结合状态高度相关，蠕变断裂时间与界面结合的强弱呈现明显的反比关系，表明过强的界面结合不能发挥界面脱粘、纤维拔出等相关增韧机制，此时裂纹直接贯穿纤维，显著缩短其中温蠕变断裂时间。
- SiC_f/SiC /
- 中温脆化 /
- 纤维推入 /
- 界面强结合 /
- 蠕变 /
- 失效机制
Abstract: The creep rupture time of continuous silicon carbide fiber reinforced silicon carbide composite (SiC_f/SiC) is shortened at intermediate temperature (500~1000 ℃) inevitably, known as creep embrittlement. The mechanism primarily depends on the microstructure and the interfacial bonding state of the fiber/matrix interface. Therefore, present work investigated the creep embrittlement mechanisms of the domestic 2^nd-generation plain woven SiC_f/SiC (2D-SiC_f/SiC) under intermediate temperature. The interfacial microstructure evolution and mechanical properties was characterized by transmission electron microscopy (TEM) and micro-mechanical testing techniques respectively. The results indicate that a carbon-rich layer with pores appear on the fiber/interface side at 500℃. Spontaneous oxidation of the interface occurs at 800℃, while a thin SiO₂ layer fills the gap generated at the BN in- terface due to oxidation. When the temperature increases to 1000℃, oxygen elements are mainly distributed on the fiber/matrix side. The intermediate temperature embrittlement mechanism of 2D-SiC_f/SiC is closely associated with interface bonding state. The creep rupture time shows a clear inverse relationship with the interface bonding state, indicating that excessively strong interface bonding hinders related toughening mechanisms such as interface debonding and fiber pullout. Consequently, cracks directly penetrate the fiber, shortening the creep rupture time significantly.
- SiC_f/SiC /
- intermediate temperature embrittlement /
- push-in /
- strong interfacial bonding /
- creep /
- failure mechanism

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图 1 纤维推入试验典型载荷-位移曲线

Figure 1. Typical load-displacement curve in push-in test

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图 2 国产二代2D-SiC_f/SiC复合材料纤维 push-in测试的位置选择

Figure 2. SEM images of positions on the domestic 2^nd-2D-SiC_f/SiC for fiber push-in testing

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图 3 国产二代2D-SiC_f/SiC复合材料中纤维的微观结构演变：(a) 原始试样；(b) 500℃/120 MPa；(c) 800℃/120 MPa；(d) 1000℃/120 MPa

Figure 3. Microstructure evolution of fibers in the domestic 2^nd-2D-SiC_f/SiC：(a) As-received；(b) 500℃/120 MPa； c) 800℃/120 MPa；(d) 1000℃/120 MP

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图 4 国产二代2D-SiC_f/SiC复合材料蠕变前后界面区域的明场TEM像和元素分布(Si、N、O、C)：(a)原始试样；(b) 500℃/120 MPa;(c) 800℃/120 MPa；(d) 1000℃/120 MPa

Figure 4. Bright fields TEM images and element distribution of interfacial regions of the domestic 2^nd-2D-SiC_f/SiC before and after intermediate temperature creep (Si、N、O、C): (a) As-received; (b) 500℃/120 MPa; (c) 800℃/120 MPa; (d) 1000℃/120 MPa

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图 5 国产二代SiC_f/SiC界面区域的微观结构演变：(a) 原始试样；(b) 500℃/120 MPa；(c) 800℃/120 MPa；(d) 1000℃/120 MPa

Figure 5. Microstructure-evolution of interfacial region in domestic 2^nd-generation SiC_f/SiC: (a) As-received; (b) 500℃/120 MPa;(c) 800℃/120 MPa; (d) 1000℃/120 MPa

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图 6 不同条件下的国产二代2D-SiC_f/SiC复合材料的纤维推入试验载荷-位移曲线

Figure 6. Load-displacement curves obtained of the push-in tests of the domestic 2 nd-2D-SiC_f/SiC.

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图 7 国产二代2D-SiC_f/SiC复合材料的界面力学性能、蠕变断裂时间与温度的关系：(a) IFSS；(b) G_i

Figure 7. Mechnical properties of fiber/matrix interphase and creep rupture time of domestic 2 nd-2D-SiC_f/SiC at different temperatures: (a) IFSS; (b) G_i

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表 1 本文研究试样的相关信息

Table 1. Information about samples used in this study

Conditions	Rupture time/h	Creep Rate/s⁻¹	Creep Strain/%
500℃/120 MPa	490	7.1×10⁻¹⁰	0.37
800℃/120 MPa	22	5.4×10⁻⁹	0.19
1000℃/120 MPa	33	1.7×10⁻⁸	0.39

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表 2 基于纤维推入获得的国产二代2D-SiC_f/SiC复合材料的界面力学性能

Table 2. The interfacial mechanical properties of domestic 2^nd-2D-SiC_f/SiC generated from push-in test

Conditions	P_c/mN	S₀/(N·mm⁻¹)	IFSS/MPa	G_i/(J·m⁻²)
As-received	168±35	614±61	97±27	5.0±2.1
500℃/120 MPa	226±24	829±51	128±9	8.8±1.8
800℃/120 MPa	350±38	962±60	231±27	21.2±4.5
1000℃/120 MPa	300±52	848±73	180±44	15.8±5.3
Notes：P_c is the critical load before interface debonding; S₀ is the slope of the second stage; IFSS is the interfacial shear strength; G_i is the interphase debond energy.

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