树脂基多孔碳孔结构对Cf/SiC复合材料连接性能的影响

doi:10.15541/jim20220294

无机材料学报 ›› 2022, Vol. 37 ›› Issue (12): 1275-1280.DOI: 10.15541/jim20220294 CSTR: 32189.14.10.15541/jim20220294

树脂基多孔碳孔结构对C_f/SiC复合材料连接性能的影响

吴西士¹^,²(), 朱云洲²(), 黄庆¹, 黄政仁¹^,²()

1.中国科学院宁波材料技术与工程研究所, 宁波 315201
2.中国科学院上海硅酸盐研究所, 上海 201899

收稿日期:2022-05-25 修回日期:2022-06-30 出版日期:2022-12-20 网络出版日期:2022-08-04
通讯作者: 朱云洲, 副研究员. E-mail: yunzhouzhu@mail.sic.ac.cn;
黄政仁, 研究员. E-mail: zhrhuang@nimte.ac.cn
作者简介:吴西士(1991-), 男, 博士. E-mail: wuxishi@nimte.ac.cn
基金资助:
国家重点研发计划(2021YFB3701500);国家自然科学基金青年项目(52002379);浙江省博士后科研项目择优资助

Effect of Pore Structure of Organic Resin-based Porous Carbon on Joining Properties of C_f/SiC Composites

WU Xishi¹^,²(), ZHU Yunzhou²(), HUANG Qing¹, HUANG Zhengren¹^,²()

1. Ningbo Institute of Materials Technology & Engineering, Chinese Academy of Sciences, Ningbo 315201, China
2. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China

Received:2022-05-25 Revised:2022-06-30 Published:2022-12-20 Online:2022-08-04
Contact: ZHU Yunzhou, associate professor. E-mail: yunzhouzhu@mail.sic.ac.cn;
HUANG Zhengren, professor. E-mail: zhrhuang@nimte.ac.cn
About author:WU Xishi (1991-), male, PhD. E-mail: wuxishi@nimte.ac.cn
Supported by:
National Key R&D Program of China(2021YFB3701500);National Natural Science Foundation of China(52002379);Postdoctoral Science Preferential Funding of Zhejiang Province, China

摘要/Abstract

摘要：

连接技术是实现大尺寸以及复杂构型C_f/SiC复合材料制备及工程化应用的关键技术。本工作使用酚醛树脂作为碳源, 通过反应连接法实现了C_f/SiC复合材料的稳定连接, 研究了多孔碳坯的体积密度和孔径对接头连接性能和微观结构的影响, 讨论了惰性填料含量对接头连接性能和显微组织的影响。研究表明: 树脂基多孔碳素坯的体积密度和孔径分别选定在0.71~0.90 g·cm^-3和200~600 nm比较合适, 随着多孔碳素坯孔径增加, 游离硅尺寸逐渐增大; 当孔径为190 nm时, 连接件强度最大为(125±12) MPa。添加SiC惰性填料可以明显减小多孔碳素坯的体积收缩, 当SiC惰性填料质量分数为50%时, 连接件强度最高达到(216±44) MPa, 基本与基体材料强度相当。总体而言, 本研究为实现C_f/SiC复合材料稳定连接提供了理论指导, 对实现复杂形状或大型C_f/SiC复合材料的制备和工程应用具有重要意义。

关键词: 多孔碳, 反应连接, C_f/SiC复合材料, 力学性能, 微观结构

Abstract:

Joining technology has become an important part of the preparation and engineering application of large or complex-shaped C_f/SiC composites. In this study, the stable joining of C_f/SiC composites was achieved via the Si-C reaction joining method by using the phenolic resin as the carbon precursor. Effects of the bulk density and pore size of porous carbon blanks on the joining properties and microstructure of the joints were investigated. Effect of the content of inert fillers on the joining properties and microstructure of joint were discussed. Bulk density and pore size of the resin-based porous carbon blank are suitable to be set in the range of 0.71-0.90 g·cm^-3 and 200-600 nm, respectively. The size of free silicon increases gradually with the increase of the pore size. The flexural strength of the joined specimens can reach (125±12) MPa at pore size of 190 nm. Addition of SiC inert filler is obviously beneficial to reduce the volume shrinkage of the porous carbon blank. Flexural strength of the joined specimens reached the highest value, i.e., (216±44) MPa at the inert filler content of 50%. Overall, this study provides theoretical guidance for the stable joining of C_f/SiC composites, which has significance for realizing the preparation and engineering application of complex-shaped or large C_f/SiC composites.

Key words: porous carbon, reaction bonded joining, C_f/SiC composites, microstructure property, mechanical

中图分类号:

TQ174/TB332

吴西士, 朱云洲, 黄庆, 黄政仁. 树脂基多孔碳孔结构对C_f/SiC复合材料连接性能的影响[J]. 无机材料学报, 2022, 37(12): 1275-1280.

WU Xishi, ZHU Yunzhou, HUANG Qing, HUANG Zhengren. Effect of Pore Structure of Organic Resin-based Porous Carbon on Joining Properties of C_f/SiC Composites[J]. Journal of Inorganic Materials, 2022, 37(12): 1275-1280.

图/表 11

图1 不同体积密度碳素坯((a)0.51, (b)0.70, (c)0.90)接头微观结构, (d)连接样品力学性能

Fig. 1 Microstructures of joints with different volumn densities ((a) 0.51, (b) 0.70, (b) 0.90) and (d) flexural strengths of the joined specimens

表1 树脂溶液组成及裂解后多孔碳素坯性能参数

Table 1 Composition of resin solution and properties of porous carbons after pyrolysis

Sample	PF/%	EG/%	Pore former^*	Residual carbon^**/%	Average pore size/nm	Bulk density/(g·cm^-3)
1	50	50	FeCl₂ (1%)	23+1.1	190±15	0.73±0.01
2	50	50	H₃BO₃(1.5%)	24.3±0.9	642±15	0.74±0.01
3	50	50	FeCl₂ (1%) + H₃BO₃(1.5%)	24.1±1.7	1226±48	0.74±0.03
4	50	50	H₃BO₃(2.5%)	25.8±2.1	1552±38	0.79±0.03
5	50	50	H₃BO₃(3.5%)	26.7±1.5	2363±54	0.79±0.03

图2 HF-HNO3腐蚀前后不同孔径碳素坯制备反应烧结碳化硅陶瓷表面微观形貌

Fig. 2 Morphologies of the polished surfaces before and after HF-HNO3 corrosion of RBSC fabricated from preforms with different pore sizes (a, f) 190 nm; (b, g) 642 nm; (c, h) 1226 nm; (d, i) 1552 nm; (e, j) 2363 nm

图3 不同孔径多孔碳素坯反应烧结样品的XRD图谱

Fig. 3 XRD patterns of the RBSC fabricated from preforms with different pore sizes

表2 不同孔径的多孔碳素坯反应烧结样品性能

Table 2 Properties of the RBSC fabricated from preforms with different pore sizes

Pore size/nm	Open porosity/%	Density/ (g·cm^-3)	Flexural strength/MPa	Residual Si/(%, in volume)
190	0.97	2.93	296±28	16
642	1.26	2.91	268±46	14
1226	1.87	2.88	248±22	16
1552	3.51	2.81	238±44	12
2363	18.76	2.10	115±32	13

图4 HF-HNO3腐蚀后不同孔径多孔碳素坯连接样品表面形貌

Fig. 4 Surface microstructures after HF-HNO3 corrosion of joining samples with different pore sizes (a) 14 nm; (b) 190 nm; (c) 316 nm; (d) 642 nm; (e) 1226 nm

表3 不同孔径连接样品力学性能

Table 3 Properties of joining samples with different pore sizes

Pore size/nm	Flexural strength/MPa	Strength retention/%
14	90±28	61
190	125±12	85
316	77±10	52
642	107±15	73
1226	65±22	44

表4 树脂基浆料组成

Table 4 Composition of resin-based slurry

Sample	PF/ %	EG/ %	Dispersant^*/%	Pore former^** (FeCl₂)/%	α-SiC powder/%
1	40	40	4	1	20
2	35	35	4	1	30
3	30	30	4	1	40
4	25	25	4	1	50
5	22.5	22.5	4	1	55

图5 (a)惰性填料添加后作用示意图和(b)多孔碳素坯的体积收缩和孔隙率变化曲线

Fig. 5 (a) Schematic of the action of inert filler and (b) volume shrinkage and porosity change curves of porous carbon blanks

图6 不同含量((a) 30%; (b) 40%; (c) 50%; (d) 55%, 质量分数)惰性填料连接件表面微观结构及(e)图(d)的局部放大图

Fig. 6 Microstructures of the joint with different contents of inert filler ((a) 30%; (b) 40%; (c) 50%; (d) 55%, in mass) and (e) partial enlargement of (d)

图7 不同含量惰性填料连接件的力学性能

Fig. 7 Flexural strength of the joined samples with different contents of inert filler

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树脂基多孔碳孔结构对C_f/SiC复合材料连接性能的影响

Effect of Pore Structure of Organic Resin-based Porous Carbon on Joining Properties of C_f/SiC Composites

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树脂基多孔碳孔结构对Cf/SiC复合材料连接性能的影响

Effect of Pore Structure of Organic Resin-based Porous Carbon on Joining Properties of Cf/SiC Composites

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树脂基多孔碳孔结构对C_f/SiC复合材料连接性能的影响

Effect of Pore Structure of Organic Resin-based Porous Carbon on Joining Properties of C_f/SiC Composites