无机材料学报 ›› 2022, Vol. 37 ›› Issue (12): 1275-1280.DOI: 10.15541/jim20220294 CSTR: 32189.14.10.15541/jim20220294
吴西士1,2(), 朱云洲2(
), 黄庆1, 黄政仁1,2(
)
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;作者简介:
吴西士(1991-), 男, 博士. E-mail: wuxishi@nimte.ac.cn
基金资助:
WU Xishi1,2(), ZHU Yunzhou2(
), HUANG Qing1, HUANG Zhengren1,2(
)
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;About author:
WU Xishi (1991-), male, PhD. E-mail: wuxishi@nimte.ac.cn
Supported by:
摘要:
连接技术是实现大尺寸以及复杂构型Cf/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Cf/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Cf/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Cf/SiC复合材料的制备和工程应用具有重要意义。
中图分类号:
吴西士, 朱云洲, 黄庆, 黄政仁. 树脂基多孔碳孔结构对Cf/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 Cf/SiC Composites[J]. Journal of Inorganic Materials, 2022, 37(12): 1275-1280.
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
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 |
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
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 |
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
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 |
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 |
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)
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