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宇航级T800碳纤维复合材料界面调控

李天舒 王绍凯 武清 顾轶卓 李庆辉 李敏

李天舒,王绍凯,武清,等. 宇航级T800碳纤维复合材料界面调控[J]. 北京航空航天大学学报,2023,49(8):2011-2020 doi: 10.13700/j.bh.1001-5965.2021.0619
引用本文: 李天舒,王绍凯,武清,等. 宇航级T800碳纤维复合材料界面调控[J]. 北京航空航天大学学报,2023,49(8):2011-2020 doi: 10.13700/j.bh.1001-5965.2021.0619
LI T S,WANG S K,WU Q,et al. Interface adjustment of aerospace-grade T800 carbon fiber composite material[J]. Journal of Beijing University of Aeronautics and Astronautics,2023,49(8):2011-2020 (in Chinese) doi: 10.13700/j.bh.1001-5965.2021.0619
Citation: LI T S,WANG S K,WU Q,et al. Interface adjustment of aerospace-grade T800 carbon fiber composite material[J]. Journal of Beijing University of Aeronautics and Astronautics,2023,49(8):2011-2020 (in Chinese) doi: 10.13700/j.bh.1001-5965.2021.0619

宇航级T800碳纤维复合材料界面调控

doi: 10.13700/j.bh.1001-5965.2021.0619
详细信息
    通讯作者:

    E-mail:leemy@buaa.edu.cn

  • 中图分类号: TB332

Interface adjustment of aerospace-grade T800 carbon fiber composite material

More Information
  • 摘要:

    上浆剂对高性能碳纤维(CF)表面的修饰作用及对其复合材料界面性能的调制作用至关重要。以湿法制备的宇航级T800碳纤维为研究对象,分析上浆前后纤维表面微结构、化学组成和化学反应特性的变化规律,并对其复合材料的宏微观界面性能进行表征评价。采用X射线光电子能谱(XPS)、差式扫描量热法(DSC)、傅里叶变换红外光谱(FTIR)等表征方法,分析上浆剂的反应性及其与环氧树脂(EP)、双马来酰亚胺树脂(BMI)的化学反应行为。结果表明:在树脂固化温度条件下上浆剂与纤维表面基团发生化学反应,使得纤维上浆剂提取量及纤维表面活性碳元素含量降低,并且上浆剂与EP、BMI工艺具有良好的化学反应性。经过高温处理后CF表面的上浆剂失活,CF/EP的界面剪切强度发生一定变化,CF/BMI的界面剪切强度下降13%。综上可见:具有化学活性的环氧类上浆剂可明显改善CF表面特性,进而对复合材料的界面性能产生影响,其中上浆剂与树脂体系的反应性对界面亦有影响。

     

  • 图 1  F4纤维上浆前后的表面形貌

    Figure 1.  Surface morphologies and roughness of F4 fiber before and after sizing

    图 2  F1~F4纤维上浆前后的表面粗糙度

    Figure 2.  Surface roughness of F1~F4 fibers before and after sizing

    图 3  F1~F4纤维表面上浆剂的红外光谱图

    Figure 3.  FTIR of F1-F4 fibers surface sizing agents

    图 4  F4纤维在不同热处理工艺制度下提取上浆剂的含量

    Figure 4.  Content of sizing agent extracted from F4 fibers that treated by different heat processes

    图 5  F4纤维在不同工艺制度热处理后纤维表面粗糙度

    Figure 5.  Surface roughness of F4 fibers that treated by different heat processes

    图 6  不同工艺处理后的F4纤维提取上浆剂的红外光谱

    Figure 6.  IR of sizing agents extracted from F4 fibers that treated by different processes

    图 7  不同纤维/树脂界面剪切强度对比

    Figure 7.  Comparison of interface shear strength of different fibers/resins

    图 8  树脂、F4上浆剂及其混合物的DSC曲线

    Figure 8.  DSC curves of resins, F4sizing agents and their mixtures

    图 9  EP和BMI固化前后的红外光谱

    Figure 9.  FTIR of EP and BMI resins before and after curing

    图 10  树脂与上浆剂混合物的原位红外光谱

    Figure 10.  In-situ FTIR of resin and sizing agent mixture

    图 11  不同树脂与热处理前后F4纤维的界面剪切强度

    Figure 11.  IFSS of different resins and F4 fibers before and after heat treatment

    表  1  不同T800级CF上浆前后的表面元素

    Table  1.   Surface element content of different T800 grade CF before and after sizing

    纤维类型C/%O/%N/%Si/%S/%Na/%O/C
    F174.1216.832.26.010.8400.23
    F1-US78.7216.242.432.62000.21
    F274.3519.41.734.52000.26
    F2-US79.7414.052.993.22000.18
    F376.3216.392.983.390.730.20.21
    F3-US78.1617.122.282.44000.22
    F476.116.992.283.710.9100.22
    F4-US77.5816.852.363.21000.22
    下载: 导出CSV

    表  2  不同CF XPS的C1s分峰拟合结果

    Table  2.   XPS C1s peak fitting results of different CF %

    纤维类型参比基团含量−C−C−;
    −C−H−含量
    −C−OH−C−O−;
    −C−NH2含量
    C−O−C=O;
    环氧基团含量
    −C=O−
    C=N含量
    −O−C=OHO−
    C=O含量
    活性碳元素含量
    (Peak1,
    能量284.8 eV)
    (Peak2,
    能量285.0 eV)
    (Peak3,
    能量286.1 eV)
    (Peak4,
    能量286.6 eV)
    (Peak5,
    能量287.7 eV)
    (Peak6,
    能量289.4 eV)
    F138.5426.0510.9216.356.451.6935.41
    F1- US70.2211.650.006.027.154.9618.13
    F236.6712.5920.5917.493.319.3550.74
    F2- US37.0918.0224.050.0011.359.4944.89
    F344.2013.9216.3612.296.406.8541.90
    F3- US59.8120.801.533.756.797.3119.38
    F424.6113.7327.9722.034.906.7761.67
    F4- US73.217.382.844.436.665.4919.42
    下载: 导出CSV

    表  3  不同工艺制度处理后F4纤维表面元素

    Table  3.   Surface element content of F4 fiber after different heat treatment processes

    纤维类型C/%O/%N/%Si/%S/%O/C
    F476.116.992.283.710.910.22
    F4+EP工艺82.0315.932.04000.19
    F4+BMI 工艺89.9810.020000.11
    下载: 导出CSV

    表  4  不同工艺处理后F4纤维XPS的C1s分峰拟合结果

    Table  4.   XPS C1s peak fitting results of F4 fiber after different heat treatment processes %

    纤维类型参比基团含量−C−C−;
    −C−H−含量
    −C−OH−C−O−;
    −C−NH2含量
    C−O−C=O;
    环氧基团含量
    −C=O−
    C=N含量
    −O−C=OHO−
    C=O含量
    活性碳元素含量
    (Peak1,
    能量284.8 eV)
    (Peak2,
    能量285.0 eV)
    (Peak3,
    能量286.1 eV)
    (Peak4,
    能量286.6 eV)
    (Peak5,
    能量287.7 eV)
    (Peak6,
    能量289.4 eV)
    F424.6113.7327.9722.034.906.7761.67
    F4+EP工艺45.0526.6620.527.760028.28
    F4+BMI工艺37.2448.2911.383.090014.47
    下载: 导出CSV

    表  5  不同树脂/上浆剂的DSC峰值温度与放热

    Table  5.   DSC peak temperature and heat of different resins/sizing agents

    树脂/上浆剂第1峰值
    温度/℃
    第2峰值
    温度/℃
    第3峰值
    温度/℃
    放热/(J·g−1)
    EP 229.2 264.7 421.5
    F4282.7246.8
    EP和F4224.2282.7360.4
    BMI156.3258.1176.6482.8
    F4282.7246.8
    BMI和F4126.6277.7316.1
    下载: 导出CSV
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  • 收稿日期:  2021-10-21
  • 录用日期:  2022-01-02
  • 网络出版日期:  2022-01-29
  • 整期出版日期:  2023-08-31

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