真空抽滤结合反应熔渗法制备ZrB<sub>2</sub>-ZrC-SiC改性碳/碳复合材料的力学性能及烧蚀行为

ZHANG Jia-ping; SU Xiao-xuan; LI Xin-gang; WANG Run-ning; FU Qian-gang

doi:10.1016/S1872-5805(24)60841-3

真空抽滤结合反应熔渗法制备ZrB₂-ZrC-SiC改性碳/碳复合材料的力学性能及烧蚀行为

doi: 10.1016/S1872-5805(24)60841-3

西北工业大学陕西省纤维增强轻质复合材料重点实验室, 西安 710072

基金项目: 国家自然科学基金(52002321, 52272044); 基础科学中心燃气轮机项目(P2021-A-IV-003-001); 先进陶瓷纤维及复合材料科技基金(6142907220302); 河南省科技研究发展计划联合基金(Grant No. 225200810002); 国家科技重大专项(J2022-VI-0011-0042); 基础研究项目(JCKY2021607B035)

详细信息

通讯作者:
张佳平, 博士生导师. E-mail: zhangjiaping@nwpu.edu.cn

中图分类号: TB33
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出版历程
- 收稿日期: 2023-10-10
- 录用日期: 2024-01-08
- 修回日期: 2024-01-06
- 网络出版日期: 2024-01-15

Ablation behaviour and mechanical performance of ZrB₂-ZrC-SiC modified carbon/carbon composites prepared by vacuum filtration combined with reactive melt infiltration

Shaanxi Key Laboratory of Fiber Reinforced Light Composite Materials, Northwestern Polytechnical University, Xi’an 710072, China

Funds: This work was supported by the National Natural Science Foundation of China (52002321, 52272044), the Science Center for Gas Turbine Project (P2021-A-IV-003-001), the fund of Science and Technology on Advanced Ceramic Fibers and Composites Laboratory (6142907220302), the Joint Fund of Henan Province Science and Technology R&D Program (225200810002), National Science and Technology Major Project (J2022-VI-0011-0042) and National Basic Scientific Research (JCKY2021607B035)

More Information

Corresponding author: ZHANG Jia-ping, Ph.D, E-mail: zhangjiaping@nwpu.edu.cn;

摘要

摘要: 采用真空抽滤ZrB₂作为反应熔渗ZrSi₂的补充，成功地将ZrB₂-ZrC-SiC引入到C/C基体中，使引入的陶瓷相含量增加且分布均匀。与仅通过反应熔渗制备的C/C-ZrC-SiC相比，C/C-ZrB₂-ZrC-SiC复合材料的质量烧蚀率和线性烧蚀率分别降低了68.9%和29.7%。烧蚀性能提高的原因在于B₂O₃的挥发带走部分热量，同时能够形成更多均匀分布的ZrO₂，促进ZrO₂-SiO₂连续保护层的形成，从而有效地抵抗机械剥蚀，阻碍氧气的渗入。
- 碳/碳复合材料 /
- ZrB₂-ZrC-SiC /
- 真空抽滤 /
- 反应熔渗 /
- 烧蚀
Abstract: The development of advanced aircrafts relies on high performance thermal-structural materials and composites of carbon/carbon (C/C) with ultrahigh-temperature ceramics are ideal candidates. However, traditional routes of compositing are either inefficient and expensive or lead to non-uniform distribution of ceramics in the matrix. Here, vacuum filtration of ZrB₂ was successfully applied to introduce ZrB₂-ZrC-SiC into C/C as a supplement for reactive melt infiltration ZrSi₂, which contributed to the content increase and uniform distribution of the introduced ceramic phases. The mass and linear ablation rates of the composites were reduced by 68.9% and 29.7%, respectively, compared to those of C/C-ZrC-SiC composites prepared through reactive melt infiltration. The ablation performance was improved because of the volatilization of B₂O₃, taking a part of the heat away, and more uniformly distributed ZrO₂ that could promote the formation of ZrO₂-SiO₂ continuous protective layer. This efficiently resisted the mechanical denudation and hindered the oxygen infiltration.
- C/C composites /
- ZrB₂-ZrC-SiC /
- Vacuum filtration /
- Reactive melt infiltration /
- Ablation.

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Figure 1. Vacuum infiltration device and its partial enlarged view

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Figure 2. Schematic diagram of ablation test

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Figure 3. Visual appearances and phase compositions of the prepared composites: (a) CSZ, (b) CSZZ, (c) XRD patterns

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Figure 4. Cross-section morphologies of composites: (a) CSZ, (b) CSZZ

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Figure 5. Enlarged views of the cross-section morphologies of composites: (a, d) C/C-ZrB₂; (b, e) CSZ; (c, f) CSZZ

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Figure 6. Flexural properties of C/C, CSZ and CSZZ

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Figure 7. Visual appearances of the composites after ablation: (a) CSZ, (b) CSZZ

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Figure 8. Surface temperature versus time curves of CSZ and CSZZ during ablation

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Figure 9. XRD pattern of CSZ and CSZZ after ablation.

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Figure 10. Central region microstructure of the composites after ablation: (a, c, e) CSZ (c, e: the enlarged view of area Ⅰ, Ⅱ); (b, d, f) CSZZ (d, f: the enlarged view of area Ⅲ, Ⅳ)

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Figure 11. Transition region microstructure and EDS analysis of the composites after ablation: (a)(c)(e) CSZ, (c, e: the enlarged view of Area Ⅰ, Ⅱ); (b)(d)(f) CSZZ, (d, f: the enlarged view of Area Ⅲ, Ⅳ); (g) EDS of Spot 1, (h) EDS of Spot 2

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Figure 12. Cross-section micrograph at the central regions of CSZ and CSZZ after ablation: (a) CSZ; (b) CSZZ

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Figure 13. Schematic diagram of ablation mechanism for CSZ and CSZZ

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Table 1. Density, phase content and porosity of the composites

Sample	Density/(g/cm³)	Carbon content/%	SiC content/%	ZrC content/%	ZrB₂ content/%	Porosity/%
CSZ	2.66	35.2%	28.3%	36.5%	—	10.19%
CSZZ	3.06	29.4%	25.5%	32.9%	12.2%	11.68%

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Table 2. Ablation properties compared with other studies (Abbreviation in the table: chemical vapor infiltration (CVI)

Sample	Methods	Density/(g/cm³)	Porosity/%	Linear ablation rate/(μm/s)	Mass ablation rate/(mg/s)	Ref.
C/C-ZrC-ZrB₂-SiC	CVI+PIP	1.98	13.02	0.50±0.01	2.21±0.60	[37]
C/C-ZrC-ZrB₂-SiC	RMI+SI	−	−	−0.65	0.69	[38]
C/C-ZrC-SiC	RMI	2.98	23.45	−5.30±0.50	0.70	[39]
C/C-SiC-ZrC	RMI	2.66	10.19	−1.72	0.61	This work
C/C-SiC-ZrB₂-ZrC	Vacuum filtration+RMI	3.06	11.68	−1.21	0.19	This work

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