反应熔渗C/C-SiC-ZrC复合材料的界面特征及其力学性能

丁家鑫; 陈招科; 王铎; 熊翔

反应熔渗C/C-SiC-ZrC复合材料的界面特征及其力学性能

中南大学　轻质高强结构材料重点实验室, 长沙 410083

基金项目: 总装重点实验室基金(No.6142907200301)；国家自然科学基金面上项目(No.52072410)

详细信息

通讯作者:
陈招科，研究员，博士，研究方向为耐烧蚀高熵陶瓷、多元超高温陶瓷及其改性复合材料　E-mail: chenzhaoke2008@csu.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: 2023-12-14
- 修回日期: 2024-01-23
- 录用日期: 2024-02-21
- 网络出版日期: 2024-03-21

Interface characteristics and mechanical properties of reactive melt infiltrated C/C-SiC-ZrC matrix composites

Science and Technology on High Strength Structural Materials Laboratory, Central South University,Changsha 410083, China

Funds: Fund of Key Laboratory of Final Assembly (No.6142907200301); General Program of National Natural Science Foundation of China (No.52072410).

摘要

摘要: C/C-ZrC-SiC复合材料作为一种极具前景的热防护材料，在航空航天领域均有广泛应用。但是反应熔渗法(Reactive melt infiltration，RMI)制备的C/C-ZrC-SiC复合材料却存在力学性能偏低的缺点，成为制约其发展应用的主要因素。为了改善 C/C- SiC-ZrC 基复合材料的纤维损伤和力学性能，通过化学气相沉积(Chemical vapor deposition, CVD)在碳纤维针刺坯体中引入了300 nm厚的热解碳(Pyrolysis carbon，PyC)界面、300 nm厚的PyC/SiC双层界面和100 nm、300 nm、800 nm厚的(PyC+SiC)共沉积界面，再采用RMI制备出C/C-SiC-ZrC复合材料。采用XRD、SEM、EPMA和TEM等分析手段研究了C/C-SiC-ZrC复合材料的物相、微观形貌、元素分布以及RMI后C/C-SiC-ZrC复合材料的界面损伤情况，并利用三点弯曲试验评估了RMI后试样的弯曲性能。结果表明：界面的引入不仅起到了对纤维的保护作用，同时也改善了纤维和基体间的结合状态，极大的避免了反应熔渗对碳纤维的侵蚀；PyC界面对纤维的保护作用有限，而PyC/SiC双层界面的保护作用最好；界面类型和界面厚度对复合材料力学性能产生重要影响，当界面厚度相同时，含(PyC+SiC)共沉积界面复合材料和含PyC/SiC双层界面复合材料的抗弯强度分别为162.80 MPa和208.58 MPa，均优于含PyC界面的复合材料；随(PyC+SiC)共沉积界面厚度的增大，复合材料的力学性能呈现先上升后下降的趋势。
- C/C-SiC-ZrC复合材料 /
- 界面 /
- 反应熔渗 /
- 界面损伤 /
- 弯曲强度
Abstract: C/C-ZrC-SiC matrix composites are widely used in aerospace field as a kind of promising thermal protection materials. But C/C-ZrC-SiC matrix composites prepared by reactive melt infiltration (RMI) have the disadvantage of low mechanical properties, which is the main factor restricting its development and application. In order to improve the fiber damage and mechanical properties of the C/C- SiC-ZrC matrix composites, 300 nm pyrolysis carbon(PyC) interface, 300 nm PyC/SiC double-layer interface, and 100 nm, 300 nm, and 800 nm (PyC+SiC) co-deposited interfaces were introduced into carbon fiber needled preform by chemical vapor deposition(CVD); and then the C/C-SiC-ZrC matrix composites were prepared by RMI. The phase composition, micro-morphology, element distribution and interface damage were investigated by XRD, SEM, EPMA and TEM, and the mechanical properties of the composites after RMI were evaluated by three-point bending tests. The results show that the introduction of the interfaces not only protect the fibers, but also improve the bonding state between the fibers and the matrix, which greatly avoids the erosion of the carbon fibers by RMI. The PyC interface provided limited protection to the fibers, while the PyC/SiC double-layer interface provided the best protection. The interface type and interface thickness have an important effect on the mechanical properties of the composites. When the interface thickness is the same, the flexural strength of the composites with (PyC+SiC) co-deposited interface and the composites with PyC/SiC double-layer interface are 162.80 MPa and 208.58 MPa, respectively, which are superior to those of the composites containing the PyC interface; the mechanical properties of the composites show a first increase in the thickness of the interface with the increase in the thickness of the interface with the increase in the thickness of the interface. With the increase of (PyC+SiC) co-deposited interface thickness, the mechanical properties of the composites show the trend of increasing and then decreasing.
- C/C-SiC-ZrC matrix composites /
- interface /
- reactive melt infiltration /
- interface damage /
- flexural strength

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图 1 含不同界面低密度C/C坯体微观形貌及X射线衍射

(a)(d)PyC界面;(b)(e) 300 nm共沉积界面;(c)(f)PyC/SiC双层界面;(g)100 nm共沉积界面;(i)800 nm共沉积界面; (h) C/C坯体X射线衍射

Figure 1. Microstructures and X-ray diffraction of low-density C/C preforms with different interfaces (a)(d) PyC interface; (b)(e) 300 nm codeposition interface; (c)(f) PyC/SiC double-layer interface; (g)100 nm codeposition interface; (i)800 nm codeposition interface; (h) C/C body X-ray diffraction

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图 2 含不同界面C/C-SiC-ZrC复合材料X射线衍射结果

Figure 2. X-ray diffraction results of C/C-SiC-ZrC composites with different interfaces

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图 3 含不同界面C/C-SiC-ZrC复合材料低倍数SEM图像

(a) 热解碳(PyC)界面; (b) 100 nm(PyC+SiC)共沉积界面; (c) 300 nm(PyC+SiC)共沉积界面; (d) 800 nm(PyC+SiC)共沉积界面;(e) PyC/SiC双层界面

Figure 3. Low magnification SEM images of C/C-SiC-ZrC composites with different interfaces

(a) Pyrolysis carbon (PyC) interface; (b) 100 nm(PyC+SiC) co-deposition interface; (c) 300 nm(PyC+SiC) co-deposition interface; (d) 800 nm(PyC+SiC) codeposition interface; (e) PyC/SiC double-layer interface

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图 4 含PyC/SiC双层界面的C/C-SiC-ZrC复合材料内部微观结构及EDS分析

(a) 低倍数SEM图像; (b) 高倍数SEM图像; (c) (d) (e) EDS元素分析

Figure 4. EDS analysis of internal microstructure and elemental composition of C/C-SiC-ZrC composites with PyC/SiC double-layer interface

(a) low-magnification SEM images; (b) high-magnification SEM images; (c) (d) (e) EDS elemental analysis

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图 5 含不同界面复合材料高倍数SEM图像

(a) (b) (c) PyC界面; (d) (e) (f) (PyC+SiC)共沉积界面; (g) (h) (i) PyC/SiC双层界面

Figure 5. High-magnification SEM images of composites with different interfaces

(a) (b) (c) PyC interface; (d) (e) (f) (PyC+SiC) codeposition interface; (g) (h) (i) PyC/SiC double-layer interface

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图 6 熔渗后不同界面处元素分布线扫图

(a) (d) PyC界面; (b) (e) (PyC+SiC)共沉积界面; (c) (f) PyC/SiC双层界面

Figure 6. Line scan of element distribution at different interfaces after infiltration

(a) (d) PyC interface; (b) (e) (PyC+SiC) codeposition interface; (c) (f) PyC/SiC double-layer interface

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图 7 不同界面纤维与陶瓷相分界面及残余界面TEM图像

(a)(d) PyC界面; (b) (e) (PyC+SiC)共沉积界面; (c) (f) PyC/SiC双层界面

Figure 7. TEM images of the interface and residual interface between fibers and ceramic phases at different interfaces

(a)(d) PyC interface; (b) (e) (PyC+SiC) codeposition interface; (c) (f) PyC/SiC double-layer interface

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图 8 不同界面处陶瓷相分布情况

(a) PyC界面; (b) (PyC+SiC)共沉积界面;(c) PyC/SiC双层界面

Figure 8. Distribution of ceramic phases at different interfaces

(a) PyC interface; (b) (PyC+SiC) codeposition interface; (c) PyC/SiC double-layer interface

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图 9 含不同界面复合材料弯曲载荷-弯曲位移曲线

Figure 9. Bending load-bending displacement curves of composites with different interfaces

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图 10 含不同界面复合材料抗弯强度测试断口形貌

(a) (d) PyC界面; (b) (e) (PyC+SiC)共沉积界面; (c) (f) PyC/SiC双层界面

Figure 10. Fracture morphology of flexural strength test of composites with different interface composites

(a) (d) PyC interface; (b) (e) (PyC+SiC) codeposition interface; (c) (f) PyC/SiC double-layer interface

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图 11 含不同厚度(PyC+SiC)共沉积界面复合材料的抗弯曲线

Figure 11. Bending resistance lines of (PyC+SiC) co-deposited interfaces composites with different thicknesses

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图 12 含100 nm、800 nm (PyC+SiC)共沉积界面复合材料的抗弯断口形貌(a) (b) 100 nm; (c) (d) 800 nm

Figure 12. Bending fracture of composites with 100 nm and 800 nm (PyC+SiC) co-deposited interfaces (a) (b) 100 nm; (c) (d) 800 nm

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表 1 含不同类型、不同厚度界面的低密度碳纤维坯体的性能特征

Table 1. Parameters of low-density carbon fiber preforms with different type and thickness of interfaces

Sample	Type of interface	Thickness of interface/nm			Density/(g·cm⁻³)	Porosity/%
P	PyC		300	1.29		28.6
PS100	(PyC+SiC) co-deposition		100	1.31		29.3
PS300			300	1.40		24.1
PS800			800	1.39		26.3
PC	PyC/SiC		300/300	1.31		28.4

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表 2 含不同厚度(PyC+SiC)共沉积界面复合材料抗弯性能

Table 2. Mechanical properties of co-deposited interface composites with different thicknesses

Sample	Type of interface	Thiceness of interface/nm	Flexural strength/MPa
PS100	(PyC+SiC) co-deposition	100	139.68
PS300		300	162.80
PS800		800	128.95

下载: 导出CSV

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