硅酸盐学报

注射辅助真空浸渍制备C_f/C-ZrB₂复合材料性能及其各向异性

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蒋宁 ¹^,² , 邹冀 ¹^,² , 刘晶晶 ³ , 王为民 ¹^,² , 傅正义 ¹^,²

硅酸盐学报 | 研究论文 2026,54(6): 2091-2101

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硅酸盐学报 |研究论文 2026 , 54 (6) : 2091 -2101

注射辅助真空浸渍制备C_f/C-ZrB₂复合材料性能及其各向异性

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蒋宁¹^,², 邹冀¹^,², 刘晶晶³, 王为民¹^,², 傅正义¹^,²

作者信息

^1．武汉理工大学，材料复合新技术国家重点实验室，武汉 430070

^2．武汉理工大学，襄阳示范区湖北隆中实验室，湖北襄阳 441000

^3．武汉理工大学材料科学与工程学院，武汉 430070

通讯作者:

邹冀（1983—），男，研究员。

作者简介:

蒋宁（2000—），男，硕士研究生。

Anisotropic Study of C_f/C-ZrB₂ Composites Prepared by Injection-Assisted Vacuum Impregnation

Ning JIANG¹^,², Ji ZOU¹^,², Jingjing LIU³, Weimin WANG¹^,², Zhengyi FU¹^,²

Affiliations

^1.National Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China

^2.Hubei Longzhong Laboratory, Wuhan University of Technology Xiangyang Demonstration Zone, Xiangyang 441000, Hubei, China

^3.School of Materials Science and Engineering, Wuhan University of Technology, Wuhan 430070, China

Corresponding Author:

{ZOU} Ji (1983-), male, Ph.D., Professor. E-mail: ji.zou@whut.edu.cn

JIANG Ning (2000-), male, Master candidate. E-mail: 1591126441@qq.com

出版时间: 2026-05-12 doi: 10.14062/j.issn.0454-5648.20250492

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摘要

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注射辅助真空浸渍（IVI）作为连续碳纤维增强ZrB₂基复合材料制备的新型工艺，具有短周期、低成本和低制备温度等优点，本工作对比分析了以针刺毡为预制体，经IVI工艺制备的C_f/C-ZrB₂复合材料及其经化学气相渗透（CVI）增碳处理后的显微结构，并在5个特征方向（0°、30°、45°、60°和90°）进行取样以研究材料压缩性能和导热性能的各向异性。结果表明：C_f/C-ZrB₂复合材料中存在分布不均匀的孔隙，主要集中在纤维束内及纤维层间区域。压缩性能测试显示材料具有明显各向异性，0°和90°试样表现出较高的杨氏模量[（2.52±0.99） GPa，（3.80±1.03） GPa]和抗压强度[（41.62±9.60） MPa，（41.50±5.18） MPa]；60°试样表现出最低的杨氏模量（0.41±0.08） GPa和抗压强度（8.47±1.44） MPa；所有试样断裂后均保持一定残余强度。在导热性能测试中，90°试样的热扩散系数（25 ℃，1.40 mm²/s）和热导率[25 ℃，1.57 W/（m·K）]最高，0°试样的热扩散系数（25 ℃，0.84 mm²/s）最低。在CVI增碳过程中，热解碳通过柱状生长形成球冠结构，并团聚融合为层状沉积层，实现部分孔隙填充。CVI处理显著提升了材料的压缩性能，90°试样的抗压强度高达（155.98±39.22） MPa，但45°、60°和90°试样出现脆性断裂模式。热解碳的填充在提升导热性能方面具有显著效果，同时降低了热导率的各向异性。

关键词

碳纤维增强碳-二硼化锆多相复合材料 / 针刺型碳纤维 / 注射辅助真空浸渍 / 显微结构 / 压缩性能 / 导热性能 / 各向异性

Abstract

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Introduction

ZrB₂ is considered as a crucial candidate material for thermal protection systems in hypersonic vehicles due to its excellent high melting point and ablation resistance. However, the brittleness and poor thermal shock resistance severely limit practical application. To enhance the performance, the introduction of continuous carbon fiber-reinforced ZrB₂ (i.e., C_f/C-ZrB₂) composites becomes a research hotspot. Needle-punched carbon fiber preforms exhibit a promising reinforcement potential due to their flexible structural design and low preparation cost. To address the drawback of long processing cycles in conventional preparation methods, this study employed injection-assisted vacuum impregnation (IVI) to fabricate C_f/C-ZrB₂ composites. The as-fabricated composites subsequently underwent carbon densification treatment via chemical vapor infiltration (CVI). The anisotropic characteristics of mechanical and thermal conductivity properties were investigated from multiple fiber orientation angles before and after the CVI treatment.

Methods

ZrB₂ powder, phenolic resin, and acetone were mixed to prepare a ceramic-resin slurry of 20% solid content. This slurry was injected into a needle-punched carbon fiber preform with the sizes of 20 mm×20 mm×20 mm. Subsequently, two rounds of vacuum impregnation, drying, and pyrolysis at 800 ℃ were performed to obtain the C_f/C-ZrB₂ composite. Carbon densification treatment was then conducted via chemical vapor infiltration (CVI) with CH₄ as a carbon source and Ar as a carrier gas at 1000 ℃ for 144 h, yielding the CVI-C_f/C-ZrB₂ composite material. The macroscopic microstructure and 3D morphology of the composites were characterized by a model VHX-700 white light ultra-deep microscope (Keyence Co., Japan). The detailed microstructural features were analyzed by a model SU8230 cold field emission scanning electron microscope (Hitachi Co., Japan). To analyze the anisotropy of the material properties, the samples were cut at angles of 0°, 30°, 45°, 60° and 90° relative to the plane XY of the carbon fiber felt. The compressive strength was measured for the cuboid shaped samples with dimensions of 10 mm (width)×10 mm (length)×15 mm (height) by a model 34TM-30 screw-driven test frame (Instron Co., USA). The thermal diffusivity was determined by a model LFA 467 laser flash instrument (Netzsch Co., Germany) in a temperature range from room temperature to 900 ℃ on the samples with 10 mm (width)×10 mm (length)×1 mm (height).

Results and discussion

The C_f/C-ZrB₂ composites prepared by IVI exhibit a non-uniform internal pore distribution, with a pore volume of (10⁴-10⁶ μm³), concentrated primarily in fiber net felt and interlaminar region. After the CVI treatment, approximately 17.16% of pores are filled with pyrolytic carbon, reducing pore volume and increasing material density from 1.8 g/cm³ to 2.1 g/cm³. The microstructural analysis reveals that pyrolytic carbon grows in spherical crown-shaped configurations, gradually forming continuous layered coatings that fill material pores. Regarding the compressive properties, the samples at 0° and 90° orientations exhibit higher Young's moduli ((2.52±0.99) GPa and (3.80±1.03) GPa, respectively) and compressive strengths ((41.62±9.60) MPa and (41.50±5.18) MPa). The samples at 60° demonstrate the lowest modulus ((0.41±0.08) GPa) and strength ((8.47±1.44) MPa). The intermediate-angle samples show a reduced performance due to shear stress concentration at inter-layer pores. For the CVI carbon densification, the mechanical properties significantly improve in all orientations. The samples at 90° achieve Young's modulus of (10.79±2.21) GPa and compressive strength of (155.98±39.22) MPa, while the samples at 0° reach (6.76±0.82) GPa and (130.09±13.19) MPa. Although the intermediate angles show a substantial improvement, they maintain relatively low values due to a incomplete densification of inter-layer pores. The results of thermal conductivity test indicate that prior to CVI, the samples at 90° display a thermal diffusivity of 1.40 mm²/s and a thermal conductivity of 1.57 W/(m·K) at 25 ℃, significantly exceeding those of the samples at 0° Post-CVI, pyrolytic carbon enhances thermal pathways. The conductivity of the samples at 90° increases to 3.48 W/(m·K) and 0° to 2.37 W/(m·K), with a reduced anisotropy ratio. The samples at 30°-60° orientations also show significantly an enhanced thermal diffusivity, with a heat transfer capability approaching that of the 90° direction.

Conclusions

The C_f/C-ZrB₂ composites fabricated via IVI exhibited a non-uniform pore distribution. After CVI, pores were refined and partially filled, increasing material density and structural densification. The compressive properties showed a significant anisotropy. The orientations at 0° and 90° demonstrated an optimal mechanical performance, while intermediate angles suffered a substantial degradation due to the shear stress dominance and pore concentration. The CVI treatment could enhance the properties across all the orientations, with a maximum improvement at 90°. The thermal conductivity also exhibited an anisotropy, revealing a superior heat transfer efficiency along fiber-dominant directions. For the CVI process, the thermal diffusivity and conductivity both increased, accompanied by a significant reduction in thermal anisotropy ratio, as pyrolytic carbon filling improved heat transfer pathways.

Key words

carbon fiber reinforced carbon-zirconium boride composite / needle-punched carbon fabric / injection assisted vacuum impregnation / microstructure / compressive properties / thermal conductivity / anisotropy

引用本文

蒋宁, 邹冀, 刘晶晶, 王为民, 傅正义. 注射辅助真空浸渍制备C_f/C-ZrB₂复合材料性能及其各向异性. 硅酸盐学报, 2026 , 54 (6) : 2091 -2101 . DOI: 10.14062/j.issn.0454-5648.20250492

Ning JIANG, Ji ZOU, Jingjing LIU, Weimin WANG, Zhengyi FU. Anisotropic Study of C_f/C-ZrB₂ Composites Prepared by Injection-Assisted Vacuum Impregnation[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (6) : 2091 -2101 . DOI: 10.14062/j.issn.0454-5648.20250492

基金

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国家自然科学基金(52332003)
湖北省自然科学基金（杰出青年学者(2022CFA042)

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2026年第54卷第6期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250492

接收时间：2025-06-21
首发时间：2026-10-22
出版时间：2026-05-12

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出版历史

收稿日期：2025-06-21
修回日期：2025-07-13

基金

国家自然科学基金(52332003)

湖北省自然科学基金（杰出青年学者(2022CFA042)

作者信息

^1．武汉理工大学，材料复合新技术国家重点实验室，武汉 430070

^2．武汉理工大学，襄阳示范区湖北隆中实验室，湖北襄阳 441000

^3．武汉理工大学材料科学与工程学院，武汉 430070

通讯作者:

邹冀（1983—），男，研究员。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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