不同SiC纤维高温退火后抗蠕变性能的定量研究

doi:10.15541/jim20250498

无机材料学报 ›› 2026, Vol. 41 ›› Issue (7): 1011-1020.DOI: 10.15541/jim20250498

• 研究快报 • 上一篇

不同SiC纤维高温退火后抗蠕变性能的定量研究

周雪¹(), 刘喆², 任岩², 余金山¹(), 杨天月¹, 赵钟倩¹, 王洪磊¹, 周新贵¹, 苟燕子¹()

¹ 国防科技大学空天科学学院, 新型陶瓷纤维及其复合材料重点实验室, 长沙 410073
² 中国核动力研究设计院核燃料元件及材料研究所, 成都 610213

收稿日期:2025-12-15 修回日期:2026-02-23 出版日期:2026-02-28 网络出版日期:2026-02-28
通讯作者: 苟燕子, 副研究员. E-mail: y.gou2012@hotmail.com;
余金山, 副研究员. E-mail: jjss_y@163.com
作者简介:周雪(2001-), 女, 硕士研究生. E-mail: zhouxue23@nudt.edu.cn

Quantitative Investigation of the Creep Resistance of Different SiC Fibers after Annealing at High Temperature

ZHOU Xue¹(), LIU Zhe², REN Yan², YU Jinshan¹(), YANG Tianyue¹, ZHAO Zhongqian¹, WANG Honglei¹, ZHOU Xingui¹, GOU Yanzi¹()

¹ Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, College of Aerospace Science and Engineering, National University of Defense Technology, Changsha 410073, China
² Nuclear Fuel and Materials Research Sub-Institute, Nuclear Power Institute of China, Chengdu 610213, China

Received:2025-12-15 Revised:2026-02-23 Published:2026-02-28 Online:2026-02-28
Contact: GOU Yanzi, associate professor. E-mail: y.gou2012@hotmail.com;
YU Jinshan, associate professor. E-mail: jjss_y@163.com
About author:ZHOU Xue (2001-), female, Master candidate. E-mail: zhouxue23@nudt.edu.cn
Supported by:
National Natural Science Foundation of China(52572119);National Natural Science Foundation of China(52272100);Fund of National Key Laboratory of Nuclear Reactor Technology of Nuclear Power Institute of China(KGSW-0324-0301-08);Ningbo Major Research and Development Plan Project(2024Z101);State Administration for Science, Technology and Industry for National Defense(WDZC20235250502)

摘要/Abstract

摘要：

SiC纤维具有优异的高温稳定性和力学性能, 是可重复使用飞行器中先进陶瓷基复合材料的关键增强体。不同类型SiC纤维的组成与微观结构差异显著, 这直接影响其高温抗蠕变性能。然而, 热处理影响蠕变性能的微观机制尚不明确。本研究对比了Shincolon-Ⅱ (F-1)、KD-S (F-2)和KD-SA (F-3)三种SiC纤维的蠕变行为, 发现F-3因近化学计量比的组成及高结晶度结构而呈现最优的抗蠕变性能, 而F-2较F-1的抗蠕变性能提升主要源于游离碳含量较低与结构有序度更高。氩气环境高温热处理能普遍改善纤维的抗蠕变性能: 经1900 ℃热处理1 h后, 在1500 ℃测试条件下, F-1和F-2的应力松弛参数(m)较原始纤维提升超过10倍, F-3则提升约5倍。但不同纤维的增强机制存在差异: F-1和F-2主要得益于晶粒长大和碳的石墨化; F-3则主要依赖铝化合物与石墨化碳对晶界的稳定作用, 以及热处理后的结构致密化。本研究可为提升SiC纤维抗蠕变性能及优化其综合力学性能提供理论基础。

关键词: SiC纤维, 抗蠕变性能, 热处理, 微观结构, 陶瓷基复合材料

Abstract:

SiC fibers exhibit exceptional high-temperature stability and mechanical properties, making them a crucial reinforcement in advanced ceramic matrix composites for reusable launch vehicles. The composition and microstructure of different types of SiC fibers vary significantly, which directly influence their high-temperature creep resistance. However, the underlying microstructural mechanisms by which heat treatment influences creep performance remain unclear. This work presents a comparative analysis of the creep behaviors of Shincolon-Ⅱ (F-1), KD-S (F-2) and KD-SA (F-3) SiC fibers. The results reveal that the superior creep resistance of F-3 is attributed to its near-stoichiometric composition and highly crystalline microstructure, while the better performance of F-2 compared to F-1 is mainly due to its lower content of free carbon and higher degree of structural ordering. High-temperature heat treatment in argon can generally improve their creep resistance. After heat treatment at 1900 ℃ for 1 h, the stress relaxation parameter (m) increases by more than 10 times for F-1 and F-2, and by approximately 5 times for F-3, compared to that of the as-received fibers tested at 1500 ℃. The mechanisms by which heat treatment enhances creep resistance differ for the different fibers. For F-1 and F-2, the dominant factors are grain growth and carbon graphitization, whereas for F-3, the improvement relies primarily on the stabilization of grain boundaries by Al compounds and graphitized carbon, along with structural densification. The findings of this work provide a theoretical foundation for improving the creep resistance of SiC fibers and optimizing their comprehensive mechanical performance.

Key words: SiC fiber, creep resistance, heat treatment, microstructure, ceramic matrix composite

中图分类号:

TQ343

周雪, 刘喆, 任岩, 余金山, 杨天月, 赵钟倩, 王洪磊, 周新贵, 苟燕子. 不同SiC纤维高温退火后抗蠕变性能的定量研究[J]. 无机材料学报, 2026, 41(7): 1011-1020.

ZHOU Xue, LIU Zhe, REN Yan, YU Jinshan, YANG Tianyue, ZHAO Zhongqian, WANG Honglei, ZHOU Xingui, GOU Yanzi. Quantitative Investigation of the Creep Resistance of Different SiC Fibers after Annealing at High Temperature[J]. Journal of Inorganic Materials, 2026, 41(7): 1011-1020.

图/表 10

Table 1 Relevant parameters of SiC fibers employed in this work

Fiber	Generation	C/Si ratio	Oxygen/ % (in mass)	Al/% (in mass)	Diameter/µm	Young's modulus/GPa	Tensile strength/GPa
F-1	Second	1.35	0.89	-	10.0	301	3.6
F-2	Third	1.08	0.91	-	9.9	367	3.6
F-3	Third	1.01	0.07	<1.00	9.8	373	1.7

Fig. 1 Tensile strength and tensile strength retention of SiC fibers after heat treatment at different temperatures for 1 h

Fig. 2 (a-c) Variation of stress relaxation parameter (m) with BSR testing temperature for (a) F-1, (b) F-2 and (c) F-3 fibers after being annealed at different temperatures for 1 h; (d-f) Comparison of m values of (d) as-received three SiC fibers, and the three SiC fibers after heat treatment at (e) 1600 and (f) 1900 ℃ for 1 h

Fig. 3 XRD patterns of SiC fibers after being annealed at different temperatures for 1 h

Fig. 4 (a-c) Raman spectra of (a) F-1, (b) F-2 and (c) F-3 fibers after being annealed at different temperatures; (d) ID/IG values

Fig. 5 SEM images of surfaces of (a-d) F-1, (e-h) F-2 and (i-l) F-3 fibers before and after heat treatment at 1900 ℃ for 1 h

Fig. 6 SEM images of cross-sections of (a-d) F-1, (e-h) F-2 and (i-l) F-3 fibers before and after heat treatment at 1900 ℃ for 1 h

Fig. 7 HRTEM images of (a, d) F-1, (b, e) F-2 and (c, f) F-3 fibers (a-c) before and (d-f) after heat treatment at 1900 ℃ for 1 h

Table S1 Growth rates of m values for heat-treated SiC fibers relative to as-received fibers after BSR test at different temperatures

Fiber	Heat treatment temperature/℃	Growth rate of m value after BSR test/%
Fiber	Heat treatment temperature/℃	1100 ℃	1200 ℃	1300 ℃	1400 ℃	1500 ℃
F-1	1200	2.2	2.2	11.7	8.9	17.1
	1400	5.8	16.9	68.5	62.5	68.6
	1600	12.4	30.0	131.8	467.9	1102.9
	1800	17.3	40.4	162.3	604.5	1508.6
	1900	17.7	41.3	164.2	614.3	1677.1
F-2	1200	1.2	1.2	2.9	14.4	191.1
	1400	5.1	5.0	6.4	25.2	400.0
	1600	9.6	9.7	12.2	45.6	707.1
	1800	15.9	15.5	21.1	66.7	971.4
	1900	16.7	16.3	21.9	68.8	1037.5
F-3	1200	0.1	0.6	1.7	7.6	74.2
	1400	1.8	1.5	4.3	22.2	145.4
	1600	4.1	3.6	7.7	35.5	198.8
	1800	6.9	5.9	11.7	54.0	309.8
	1900	8.8	8.7	16.5	67.3	438.0

Fig. S1 SAED patterns of (a, d) F-1, (b, e) F-2 and (c, f) F-3 fibers (a-c) before and (d-f) after heat treatment at 1900 ℃ for 1 h

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不同SiC纤维高温退火后抗蠕变性能的定量研究

Quantitative Investigation of the Creep Resistance of Different SiC Fibers after Annealing at High Temperature

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