SiC<sub>f</sub>/TC25G复合材料界面热稳定性研究

孙武; 张育铭; 杨丽娜; 杨青; 刘迪; 王玉敏

doi:10.7513/j.issn.1004-7638.2024.05.010

SiC_f/TC25G复合材料界面热稳定性研究

doi: 10.7513/j.issn.1004-7638.2024.05.010

孙武^{1, 2,},
张育铭²,
杨丽娜^2, ,,
杨青²,
刘迪¹,
王玉敏²

1.
沈阳化工大学材料科学与工程学院，辽宁沈阳 110142
2.
中国科学院金属研究所师昌绪先进材料创新中心，辽宁沈阳 110016

基金项目: 国家部委计划重点研究项目（No.TMC-00-02）。

详细信息

作者简介:
孙武，1999年生，男，硕士研究生，主要从事纤维增强钛基复合材料研究，E-mail：sunwu1102@163.com

通讯作者:
杨丽娜，1983年生，女，辽宁辽阳人，博士，副研究员，主要从事纤维增强钛基复合材料研究，E-mail：lnyang@imr.ac.cn

中图分类号: TF823,TB333
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出版历程
- 收稿日期: 2024-04-16
- 网络出版日期: 2024-10-30
- 刊出日期: 2024-10-30

Study on interfacial thermal stability of SiC_f/TC25G composites

Sun Wu^{1, 2
,},
Zhang Yuming²,
Yang Lina^{2
, ,},
Yang Qing²,
Liu Di¹,
Wang Yumin²

1.
School of Materials Science and Engineering, Shenyang University of Chemical Technology, Shenyang 110142, Liaoning,China
2.
Shi-changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, Liaoning,China

摘要

摘要: TMCs在高温服役长时使用过程中，基体与纤维会发生严重的界面反应，导致复合材料力学性能下降。以磁控溅射先驱丝法+热等静压工艺制备的SiC_f/TC25G复合材料作为研究对象，结合TC25G钛合金服役温度，系统设计了不同热暴露条件下复合材料界面热稳定性试验，分析了热等静压态和热暴露态SiC_f/TC25G复合材料界面形貌和界面产物。结合SEM、TEM、EPMA、XRD、EBSD等技术分析表明，热等静压态的SiC_f/TC25G复合材料界面反应层主要产物为TiC，反应层靠近基体侧和基体中存在硅化物的析出。随着热暴露温度和保温时间增加，界面反应层厚度增加。根据界面反应层增量，总结出SiC_f/TC25G复合材料界面长大规律，利用Arrhenius公式计算获得SiC_f/TC25G复合材料界面反应层长大激活能为50.53 kJ/mol，反应层长大指数因子为1.23×10⁻⁷ m/s^1/2。
- 钛基复合材料 /
- TC25 G /
- SiC纤维 /
- 热稳定性 /
- 界面反应
Abstract: The prolonged exposure of TMCs to high temperatures results in severe interfacial reactions between the matrix and the fiber, leading to a degradation in the mechanical properties of the composites. In this study, SiC_f/TC25G composites were prepared using a magnetron sputtering precursor wire method followed by hot isostatic pressing process. The interface reaction and thermal stability of the composites were investigated. Specifically designed interfacial thermal stability experiments under different thermal exposure conditions were conducted based on the service temperature of TC25G titanium alloy. The resulting interfacial morphology and products of the composites under hot isostatic pressure and hot exposure were analyzed using various techniques including SEM, TEM, EPMA, XRD, and EBSD techniques. The primary product of the interface reaction layer in SiC_f/TC25G composites under hot isostatic pressure is validated as TiC, and the silicides in the reaction layer near the matrix side and the matrix precipitate in the form of (Ti, Zr)₆Si₃. As thermal exposure temperature and holding time increased, both the thickness of the interface reaction layer increases while that of the C coating decreases. Based on these observations, a growth law for SiC_f/TC25G composite was summarized. The activation energy for the growth of the interfacial reaction layer in SiC_f/TC25G composites is 50.53 kJ /mol, and the exponential factor for the reaction layer growth is 1.23×10⁻⁷ m/s^1/2.
- titanium matrix composites /
- TC25 G /
- SiC fiber /
- thermal stability /
- interfacial reaction

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图 1 SiC_f/TC25G复合材料试样棒毛坯制备流程

Figure 1. Schematic of SiC_f/TC25G composites sample blank preparation (HIP—hot isostatic pressing)

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图 2 热等静压态SiC_f/TC25G复合材料的SEM形貌

(a) 横截面；(b) 界面

Figure 2. SEM images of HIPed SiC_f/TC25G composites

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图 3 热等静压态SiC_f/TC25G复合材料界面区域的XRD谱

Figure 3. XRD spectra of the interface region of HIPed SiC_f/TC25G composites

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图 4 热等静压态SiC_f/TC25G复合材料界面的背散射电子像和EPMA元素面分布

(a)EBSD; (b)Si; (c)W; (d)C; (e)Ti ; (f)Al; (g)Sn; (h)M; (i)Zr

Figure 4. Backscattered electron image and EPMA maps of elements in the interface region of HIPed SiC_f/TC25G composites

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图 5 热等静压态SiC_f/TC25G复合材料界面的TEM像及EDS元素面扫图

(a)TEM; (b)Si; (c)W; (d)C; (e)Ti; (f)Al; (g)Sn; (h)Mo; (i) Zr

Figure 5. TEM image and corresponding EDS maps of elements of the interface of HIPed SiC_f/TC25 G composites

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图 6 热等静压态SiC_f/TC25G复合材料界面的TEM及不同区域的SAED花样

（a）图5(a)局部区域放大；(b)~(f)图5(a)中I、II、III、IV和V位置衍射花样

Figure 6. Magnification of the rectangle region and SAED patterns regions

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图 7 热等静压态和不同热暴露温度保温300 h后SiC_f/TC25G复合材料界面反应层及基体形貌的SEM像

（a）热等静压成型态；（b）550 ℃；（c）700 ℃；（d）850 ℃

Figure 7. SEM images of interfacial reaction layer and matrix of HIPed SiC_f/TC25G composites after 300 h exposure to different temperatures

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图 8 热等静压态和不同热暴露温度保温300 h后SiC_f/TC25G复合材料局部基体的EBSD相分布

(a) 热等静压态； (b) 550 ℃； (c) 700 ℃；(d) 850 ℃

Figure 8. EBSD phase distribution images of matrix in HIPed SiCf/TC25G composites, and samples after 300 h thermal exposure to different temperatures

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图 9 SiC_f/TC25G复合材料不同热暴露条件下界面反应层和基体微观形貌的SEM像

(a)~(d)550 ℃; (e)~(h)700 ℃; (i)~(l)850 ℃ ; (a)(e)( i) 50 h; (b)(f)( j) 100 h; (c)(g)(k)200 h; (d)(h)(l)300 h

Figure 9. SEM images of interfacial reaction layer and matrix of SiC_f/TC25G composites after thermal exposure

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图 10 SiC_f/TC25G复合材料在不同热暴露温度下保温300 h后的XRD谱

Figure 10. XRD spectra of SiC_f/TC25G composites under different thermal exposure temperatures for 300 h

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图 11 SiC_f/TC25G复合材料850 ℃、300 h热暴露处理样品背散射电子像和EPMA元素面分布

(a)EBSD; (b)Si; (c)W; (d)C; (e)Ti; (f)Al; (g)Sn; (h)Mo, (i)Zr

Figure 11. Backscattered electron image and EPMA maps of elements in SiC_f/TC25G composites after thermal exposal at 850 ℃ for 300 h

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图 12 SiC_f/TC25G复合材料从热等静压到850 ℃热暴露保温300 h过程中界面物相分布和各元素扩散路径示意

（a）先驱丝态；（b）热等静压成型；（c）热暴露前期；（d）热暴露后期

Figure 12. Schematics showing the interface phase distributions and element diffusion paths of SiC_f/TC25G composites during HTP state to thermal exposure to 850 ℃ for 300 h

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图 13 SiC_f/TC25G复合材料界面反应动力学曲线

Figure 13. Interfacial reactive kinetic curves of SiC_f/TC25G composites

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图 14 SiC_f/TC25G复合材料界面反应层长大Arrhenius关系

Figure 14. Arrhenius diagram of the interfacial reaction layer growth of SiC_f/TC25G composites

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表 1 热等静压态和不同热暴露温度保温300 h后SiC_f/TC25G复合材料的晶粒平均面积尺寸

Table 1. The average grain area sizes of HIPed SiC_f/TC25G composites after 300 h thermal exposure to different temperatures

物相	热等静压态	平均面积/μm²
物相	热等静压态	550 ℃/300 h	700 ℃/300 h	850 ℃/300 h
α-Ti	0.52	0.65	1.07	2.21
β-Ti	0.11	0.14	0.22	0.80
TiC	0.15	0.22	0.21	0.36
(Ti,Zr)₆Si₃	0.05	0.09	0.07	0.16

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表 2 热等静压态和不同热暴露温度保温300 h后SiC_f/TC25G复合材料不同相在基体中的面积分数

Table 2. The area fraction of different phases in SiC_f/TC25G composites matrix

物相	热等静压态	面积分数/%
物相	热等静压态	550 ℃/300 h	700 ℃/300 h	850 ℃/300 h
α-Ti	83.2	81.0	80.4	64.2
β-Ti	15.7	15.7	12.3	23.7
TiC	0.9	2.8	6.9	11.0
(Ti,Zr)₆ Si₃	0.1	0.4	0.3	1.0

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表 3 SiC_f/TC25G复合材料在不同热暴露条件下界面反应层的厚度

Table 3. Thicknesses of interfacial reaction layer of SiC_f/TC25G composites under different thermal exposure conditions

温度/ ℃	反应层厚度/μm
温度/ ℃	50 h	100 h	200 h	300 h
550	0.93±0.28	0.94±0.24	0.95±0.32	0.97±0.27
700	0.95±0.26	0.97±0.27	0.98±0.25	0.98±0.23
850	1.17±0.32	1.31±0.29	1.52±0.32	1.71±0.47

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表 4 不同材料的指数因子(k₀)和界面反应层长大激活能(Q)

Table 4. Exponential factors (k₀) and interfacial reactive layer growth activation energy (Q) of different materials

牌号	k₀/(m·s^−1/2)	Q/(kJ·mol⁻¹)
SiC_f/TC17^[16]	4.64×10⁻³	138
SiC_f/Ti60^[24]	2.27×10⁻⁴	118
SiC_f/Ti65^[25]	2.37×10⁻⁵	93
SiC_f/Ti₂AlNb^[26]	2.80×10⁻⁴	24.27
SiC_f/TC25G	1.23×10⁻⁷	50.53

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