高温热处理对国产KD-SA型SiC纤维组成结构与力学性能的影响

doi:10.15541/jim20220548

无机材料学报 ›› 2023, Vol. 38 ›› Issue (5): 569-576.DOI: 10.15541/jim20220548 CSTR: 32189.14.10.15541/jim20220548

高温热处理对国产KD-SA型SiC纤维组成结构与力学性能的影响

吴爽(), 苟燕子(), 王永寿, 宋曲之, 张庆雨, 王应德()

国防科技大学空天科学学院, 新型陶瓷纤维与及其复合材料重点实验室, 长沙 410073

收稿日期:2022-09-19 修回日期:2022-11-10 出版日期:2022-11-16 网络出版日期:2022-11-16
通讯作者: 苟燕子, 副研究员. E-mail: y.gou2012@hotmail.com;
王应德, 教授. E-mail: wangyingde@nudt.edu.cn
作者简介:吴爽(1996-), 女, 博士研究生. E-mail: alanwu37@163.com
基金资助:
国家自然科学基金(51772327);湖南省自然科学基金面上项目(2022JJ30662);科工局稳定支持科研项目(WDZC20205500504);科工局稳定支持科研项目(WDZC20215250507)

Effect of Heat Treatment on Composition, Microstructure and Mechanical Property of Domestic KD-SA SiC Fibers

WU Shuang(), GOU Yanzi(), WANG Yongshou, SONG Quzhi, ZHANG Qingyu, WANG Yingde()

Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, College of Aerospace Science and Engineering, National University of Defense Technology, Changsha 410073, China

Received:2022-09-19 Revised:2022-11-10 Published:2022-11-16 Online:2022-11-16
Contact: GOU Yanzi, associate professor. E-mail: y.gou2012@hotmail.com;
WANG Yingde, professor. E-mail: wangyingde@nudt.edu.cn
About author:WU Shuang(1996-), female, PhD candidate. E-mail: alanwu37@163.com
Supported by:
National Natural Science Foundation of China(51772327);Natural Science Foundation of Hunan Province(2022JJ30662);Fund of Industry for National Defence(WDZC20205500504);Fund of Industry for National Defence(WDZC20215250507)

摘要/Abstract

摘要：

高结晶近化学计量比SA型SiC纤维以其优异的耐温性, 在新一代航空发动机和高超声速飞行器等领域得到广泛应用。对比国产第二代SiC纤维(F-II), 本工作研究了第三代SA型SiC纤维(F-III)高温热处理前后的微观结构演变和拉伸强度及断裂行为。结果表明, F-III纤维主要由β-SiC晶粒(~200 nm)和少量游离碳组成, F-II纤维则由β-SiC晶粒(~5 nm)、游离碳和SiC_xO_y无定形相组成。与F-II纤维相比, F-III纤维具有更大的晶粒尺寸与孔隙, 室温下的拉伸强度较低。但经1800 ℃热处理后, F-III纤维结构和强度基本保持不变, 而F-II纤维由于发生了SiC_xO_y相的分解和晶粒长大, 强度明显降低。SA型SiC纤维的耐高温性能优异, 可归因于纤维组成结构上的高结晶、大晶粒和低碳氧含量。

关键词: SiC纤维, 高温热处理, 微观结构, 拉伸强度

Abstract:

Polycrystalline near stoichiometric SA type SiC fibers have a prospective application in the fields of the new generation aero engine and hypersonic vehicles due to their excellent temperature resistance. In this work, microstructure evolution, tensile strength as well as fracture behavior of the second-generation domestic F-II SiC and the third-generation SA (F-III) SiC fibers before and after heat treatment were studied. The results showed that F-III fiber was mainly composed of β-SiC grains (~200 nm) and a small amount of free carbon, while F-II fiber was composed of β-SiC grains (~5 nm), free carbon and amorphous SiC_xO_y phase. Compared with the F-II fiber, the F-III fiber showed lower tensile strength at room temperature, owing to their larger grain size and pores. However, after heat treatment at 1800 ℃, the structure and strength of F-III fiber remained almost unchanged, while the strength of F-II fiber decreased sharply due to decomposition of SiC_xO_y phase and grain growth. The excellent high temperature resistance of SA type fiber could be attributed to high crystallinity, large grain size, low carbon and oxygen content in microstructure and composition.

Key words: SiC fibers, heat treatment, microstructure, tensile strength

中图分类号:

TQ174

吴爽, 苟燕子, 王永寿, 宋曲之, 张庆雨, 王应德. 高温热处理对国产KD-SA型SiC纤维组成结构与力学性能的影响[J]. 无机材料学报, 2023, 38(5): 569-576.

WU Shuang, GOU Yanzi, WANG Yongshou, SONG Quzhi, ZHANG Qingyu, WANG Yingde. Effect of Heat Treatment on Composition, Microstructure and Mechanical Property of Domestic KD-SA SiC Fibers[J]. Journal of Inorganic Materials, 2023, 38(5): 569-576.

图/表 10

表1 热处理前后SiC纤维的组成和基本性能

Table 1 Composition and general properties of SiC fibers before and after heat treatment

Parameter	F-II	F-II-1800 ℃	F-III	F-III-1800 ℃
C/Si	1.34	1.42	1.08	1.08
Al content/ (%, in mass)	/	/	<1.00	<1.00
O content/ (%, in mass)	0.98	0.53	0.07	0.05
Diameter/μm	12.0	11.9	9.9	9.9
Density/ (g·cm^-3)	2.72	2.66	3.08	3.09
Tensile strength/ GPa	2.7	0.9	1.8	1.8
Elastic modulus/GPa	260	207	372	366

图1 (a)F-II, (b)F-II-1800 ℃、(c)F-III 和(d)F-III-1800 ℃ 纤维的Si2p的XPS图谱

Fig. 1 Si2p XPS spectra of (a) F-II, (b) F-II-1800 ℃, (c)F-III, and (d)F-III-1800 ℃ fibers

图2 纤维的(a)XRD图谱和(b)Raman图谱

Fig. 2 (a) XRD patterns and (b) Raman spectra of SiC fibers

表2 纤维中自由碳的拉曼峰信息

Table 2 Raman characteristics of free carbon phase of the fibers

Sample	D Band		G Band		I_D/I_G	L_a/nm
Sample	Position/cm^-1	FWHM	Position/cm^-1	FWHM	I_D/I_G	L_a/nm
F-II	1356.3	112.5	1599.8	122.7	1.39	13.8
F-II-1800 ℃	1351.3	59.9	1586.8	63.2	1.09	17.6
F-III	1352.9	79.9	1590.1	89.0	1.12	17.2
F-III-1800 ℃	1354.3	64.9	1593.0	72.8	1.18	16.3

图3 (a~c)F-II, (d~h)F-II-1800 ℃, (i~l)F-III, and (m~p)F-III-1800 ℃纤维的SEM形貌照片

Fig. 3 SEM morphologies of (a-c) F-II, (d-h) F-II-1800 ℃, (i-l) F-III, and (m-p) F-III-1800 ℃ fibers

图4 (a~e) F-II、(f~j) F-II-1800 ℃和(k~o) F-III-1800 ℃纤维的TEM和HRTEM照片

Fig. 4 TEM and HRTEM images of (a-e) F-II fibers, (f-j)F-II-1800 ℃ fibers, and (k-o) F-III-1800 ℃ fibers

图5 F-II-1800 ℃纤维的(a~c)TEM照片及其(d~f)元素分析

Fig. 5 (a-c) TEM images and (d-f) elemental distributions of the F-II-1800 ℃ fibers

图6 (a)F-II-1800 ℃纤维皮芯结构示意图和(b)F-III纤维热稳定性的示意图

Fig. 6 Schematic diagram of (a) formation process of skin-core structure of F-II-1800 ℃and (b) thermal stability of F-III fibers

图7 (a)纤维的应力-应变曲线和(b)Weibull分布

Fig. 7 (a) Representative strain-stress curves and (b) Weibull plots of the fibers

图8 (a, b)F-II、(c)F-II-1800℃和(d)F-III纤维的断口形貌照片

Fig. 8 Fracture morphologies of (a, b) F-II, (c) F-II-1800℃, and (d) F-III fibers

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高温热处理对国产KD-SA型SiC纤维组成结构与力学性能的影响

Effect of Heat Treatment on Composition, Microstructure and Mechanical Property of Domestic KD-SA SiC Fibers

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