浆料浸渍辅助PIP工艺制备C/HfC-SiC复合材料的微观结构及性能研究

doi:10.15541/jim20230471

无机材料学报 ›› 2024, Vol. 39 ›› Issue (6): 726-732.DOI: 10.15541/jim20230471

浆料浸渍辅助PIP工艺制备C/HfC-SiC复合材料的微观结构及性能研究

粟毅¹(), 史扬帆¹, 贾成兰¹, 迟蓬涛², 高扬², 马青松¹, 陈思安¹()

1.国防科技大学新型陶瓷纤维及其复合材料重点实验室, 长沙 410073
2.中国运载火箭技术研究院空间物理重点实验室, 北京 100076

收稿日期:2023-10-13 修回日期:2023-12-05 出版日期:2024-06-20 网络出版日期:2024-03-05
通讯作者: 陈思安, 副研究员. E-mail: chensian07@nudt.edu.cn
作者简介:粟毅(2000-), 男, 硕士研究生. E-mail: suyi@nudt.edu.cn
基金资助:
国防科技重点实验室基金(6142907210301);国防基础科研项目(2023-JCJQ-ZD-042-00)

Microstructure and Properties of C/HfC-SiC Composites Prepared by Slurry Impregnation Assisted Precursor Infiltration Pyrolysis

SU Yi¹(), SHI Yangfan¹, JIA Chenglan¹, CHI Pengtao², GAO Yang², MA Qingsong¹, CHEN Sian¹()

1. Science and Technology on Advanced Ceramic Fibers ＆Composites Laboratory, National University of Defense Technology, Changsha 410073, China
2. Science and Technology on Space Physics Laboratory, China Academy of Launch Vehicle Technology, Beijing 100076, China

Received:2023-10-13 Revised:2023-12-05 Published:2024-06-20 Online:2024-03-05
Contact: CHEN Sian, associate professor. E-mail: chensian07@nudt.edu.cn
About author:SU Yi (2000-), male, Master candidate. E-mail: suyi@nudt.edu.cn
Supported by:
National Defense Science and Technology Key Laboratory Fund(6142907210301);National Key Basic Research Program(2023-JCJQ-ZD-042-00)

摘要/Abstract

摘要：

针对高速飞行器对于防热/承载一体化超高温陶瓷基复合材料的迫切需求, 以及现有反应型HfC先驱体存在的成本高、效率低和致密效果差等不足, 本研究将HfC亚微米粉体配制成稳定的陶瓷浆料, 利用浆料加压浸渍辅助先驱体浸渍裂解(PIP)工艺制备了HfC基体均匀分布的C/HfC-SiC复合材料, 探讨了HfC含量对于复合材料微观结构、力学与烧蚀性能的影响。结果表明, 当HfC实际体积分数为13.1%~20.3%时, 复合材料密度为2.20~2.58 g·cm^-3, 开孔率约为5%。通过单层碳布加压浸渍陶瓷浆料, HfC颗粒能够分散到纤维束内部, 且在复合材料中分布比较均匀。提高HfC含量会降低复合材料纤维含量, 其力学性能也呈现出降低趋势。当HfC体积分数为20.3%时, 复合材料的密度、拉伸强度和断裂韧性分别为2.58 g·cm^-3、147 MPa和9.3 MPa·m^1/2; 经氧乙炔焰烧蚀60 s后, 复合材料的线烧蚀率和质量烧蚀率分别为0.0062 mm/s和0.005 g/s, 烧蚀过程中形成的熔融相Hf_xSi_yO_z能覆盖在材料表面, 起到良好的保护作用。

关键词: C/HfC-SiC复合材料, 浆料浸渍, 力学性能, 抗烧蚀性能

Abstract:

In response to the urgent demand for ultra-high temperature ceramic matrix composites with integrated thermal protection and load-bearing capabilities for high-speed aircrafts, this study prepared stable ceramic slurry from submicron HfC ceramic powder, and utilized the slurry pressure impregnation-assisted precursor infiltration pyrolysis (PIP) process to fabricate C/HfC-SiC composites with uniformly distributed HfC matrix to overcome the shortcomings of the existing reaction-derived HfC precursor, such as high cost, low efficiency, and poor densification effect. The influence of HfC content on the microstructure, mechanical properties, and ablation resistance of composites was investigated. Results showed that the composites had density of 2.20-2.58 g·cm^-3 and open porosity of approximately 5% when the actual volume fraction of HfC was in range of 13.1%-20.3%. Utilizing a single layer of carbon cloth to impregnate the ceramic slurry with pressure, HfC particles were able to disperse into the interior of the fiber bundle and distributed relatively evenly in the composites. Increasing the HfC content resulted in reducted fiber content, and decreased mechanical properties of composites. Specifically, when HfC volume fraction was 20.3%, the composites exhibited density, tensile strength and fracture toughness of 2.58 g·cm^-3, 147 MPa and 9.3 MPa·m^1/2, respectively. Following 60 s of ablation under an oxygen acetylene flame, the composites demonstrated linear ablation rate of 0.0062 mm/s and mass ablation rate of 0.005 g/s. The molten phase Hf_xSi_yO_z formed during the ablation process could effectively cover the composites surface and provide protection.

Key words: C/HfC-SiC composite, slurry impregnation, mechanical property, ablation resistance

中图分类号:

TB332

粟毅, 史扬帆, 贾成兰, 迟蓬涛, 高扬, 马青松, 陈思安. 浆料浸渍辅助PIP工艺制备C/HfC-SiC复合材料的微观结构及性能研究[J]. 无机材料学报, 2024, 39(6): 726-732.

SU Yi, SHI Yangfan, JIA Chenglan, CHI Pengtao, GAO Yang, MA Qingsong, CHEN Sian. Microstructure and Properties of C/HfC-SiC Composites Prepared by Slurry Impregnation Assisted Precursor Infiltration Pyrolysis[J]. Journal of Inorganic Materials, 2024, 39(6): 726-732.

图/表 10

图1 浆料加压浸渍辅助PIP工艺制备C/HfC-SiC复合材料的示意图

Fig. 1 Schematic diagram of C/HfC-SiC composites prepared by slurry pressure impregnation-assisted PIP process

表1 C/HfC-SiC复合材料的密度、开孔率及组成

Table 1 Densities, open porosities and compositions of C/HfC-SiC composites

Sample	Density/ (g·cm^-3)	Open porosity/%	Fiber/% (in vol)	HfC/% (in vol)	SiC/% (in vol)
S-15	2.20	5.4	43.4	13.1	32.6
S-20	2.37	4.3	40.8	16.5	31.2
S-25	2.58	5.6	37.1	20.3	30.9

图2 C/HfC-SiC复合材料的微观形貌及对应EDS分析

Fig. 2 Microstructure and corresponding EDS analyses of C/HfC-SiC composites

图3 C/HfC-SiC复合材料的微观形貌

Fig. 3 Morphologies of C/HfC-SiC composites (a, b) S-15; (c, d) S-20; (e, f) S-25

表2 C/HfC-SiC复合材料的力学性能

Table 2 Mechanical properties of C/HfC-SiC composites

Sample	Bending strength/MPa	Bending modulus/GPa	Tensile strength/MPa	Tensile modulus/GPa	Fracture toughness/(MPa·m^1/2)
S-15	333±18	56.0±2.6	152±16	62.0±4.5	12.0±3.2
S-20	295±31	50.0±1.4	145±5	60.0±1.8	11.0±1.7
S-25	307±9	53.4±1.9	147±16	62.5±5.1	9.3±1.8

图4 C/HfC-SiC复合材料的断口微观形貌

Fig. 4 Fracture morphologies of C/HfC-SiC composites (a) S-15; (b) S-20; (c) S-25

图5 C/HfC-SiC复合材料烧蚀后的宏观形貌

Fig. 5 Macro morphologies of C/HfC-SiC composites after ablation (a) S-15; (b) S-20; (c) S-25

图6 C/HfC-SiC复合材料抗氧乙炔焰的烧蚀性能

Fig. 6 Ablation behavior of C/HfC-SiC composites under oxyacetylene torch flame

图7 C/HfC-SiC复合材料烧蚀后的表面XRD谱图

Fig. 7 XRD pattern of surface for C/HfC-SiC composites after ablation

图8 S-25烧蚀中心的微观形貌(a~c)及其EDS分析(d)

Fig. 8 SEM images of ablation centers (a-c) and their corresponding EDS analyses (d) of S-25

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浆料浸渍辅助PIP工艺制备C/HfC-SiC复合材料的微观结构及性能研究

Microstructure and Properties of C/HfC-SiC Composites Prepared by Slurry Impregnation Assisted Precursor Infiltration Pyrolysis

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