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碳纤维高温气相氧化对聚醚醚酮复合材料拉伸和层间剪切性能的影响

王成博 张代军 李军 陈祥宝

王成博, 张代军, 李军, 等. 碳纤维高温气相氧化对聚醚醚酮复合材料拉伸和层间剪切性能的影响[J]. 复合材料学报, 2024, 42(0): 1-13.
引用本文: 王成博, 张代军, 李军, 等. 碳纤维高温气相氧化对聚醚醚酮复合材料拉伸和层间剪切性能的影响[J]. 复合材料学报, 2024, 42(0): 1-13.
WANG Chengbo, ZHANG Daijun, LI Jun, et al. Effect of high-temperature gas-phase oxidation of carbon fiber on tensile and interlaminar shear properties of PEEK composites[J]. Acta Materiae Compositae Sinica.
Citation: WANG Chengbo, ZHANG Daijun, LI Jun, et al. Effect of high-temperature gas-phase oxidation of carbon fiber on tensile and interlaminar shear properties of PEEK composites[J]. Acta Materiae Compositae Sinica.

碳纤维高温气相氧化对聚醚醚酮复合材料拉伸和层间剪切性能的影响

基金项目: 国家重点研发计划(2022YFB3709402);工信部民机专项 (MJZ1-11N22);国家重点研发计划(2018YFA0703300)
详细信息
    通讯作者:

    张代军,博士,研究员,博士生导师,研究方向为树脂基复合材料 E-mail: 15810534483@139.com

    陈祥宝,博士,研究员,博士生导师,研究方向为树脂基复合材料 E-mail: xiangbao.chen@biam.ac.cn

  • 中图分类号: TB332

Effect of high-temperature gas-phase oxidation of carbon fiber on tensile and interlaminar shear properties of PEEK composites

Funds: National Key R&D Program of China (2022YFB3709402);Civil Aircraft Special Item of Ministry of Industry (MJZ1-11N22);National Key R&D Program of China (2018YFA0703300)
  • 摘要: 聚醚醚酮(PEEK)复合材料具有优异的抗冲击性能,在航空领域具有重要的应用价值。然而,聚醚醚酮复合材料成型温度高,成型过程中可能存在环氧上浆剂分解残留,导致界面强度降低、载荷传递变差等问题,影响其使用性能。系统地研究了碳纤维(CF)高温气相氧化对CF/PEEK复合材料拉伸和层间剪切性能的影响。首先采用不同氧化工艺处理碳纤维,采用XPS、IGC、复丝拉伸等方法表征了碳纤维表面活性、表面能以及拉伸性能。结果表明,合适的氧化条件有利于改善纤维表面活性和表面能,但同时会降低纤维拉伸强度。采用熔体法制备了CF/PEEK预浸料,研究了高温气相氧化对CF/PEEK复合材料拉伸和层间剪切性能的影响。结果表明,纤维高温氧化后CF/PEEK复合材料0°拉伸强度下降超过20%,表明高温氧化会导致纤维严重损伤;90°拉伸强度变化不超过10%,层间剪切强度变化小于5%,表明碳纤维高温氧化未能实现复合材料界面性能改善。上述结果表明,在预浸料制备工艺中增加碳纤维高温氧化工序,不利于改善复合材料性能。

     

  • 图  1  预浸料制备流程示意图

    Figure  1.  Schematic diagram of prepreg preparation process

    图  2  碳纤维XPS扫描全谱图

    Figure  2.  Wide-scan XPS spectra of CFs

    图  3  不同工艺条件处理的碳纤维XPS扫描C1s图谱

    Figure  3.  C1 s spectra of CFs under different conditions

    图  4  碳纤维复丝拉伸性能

    Figure  4.  Bundle tensile properties of CFs

    图  5  预浸料拉伸性能

    Figure  5.  Tensile properties of prepregs

    图  6  预浸料截面抛光形貌(a)纤维未处理(b)纤维高温处理

    Figure  6.  Sectional polished morphology of prepregs (a) CF untreated,(b) CF oxidized at high-temperature

    图  7  聚醚醚酮复合材料0°拉伸性能

    Figure  7.  0° tensile properties of PEEK composites

    图  8  聚醚醚酮复合材料0°拉伸断口宏观形貌(a)碳纤维未处理,(b)碳纤维高温处理

    Figure  8.  Fracture macro-morphology of 0° tensile samples of PEEK composites (a) CF untreated, (b) CF oxidized at high-temperature

    图  9  聚醚醚酮复合材料0°拉伸试样截面抛光形貌(a)碳纤维未处理,(b)碳纤维高温处理

    Figure  9.  Sectional polished morphology of 0° tensile specimens of PEEK composites (a) CF untreated, (b) CF oxidized at high-temperature

    图  10  试验件断口侧面形貌(a)碳纤维未处理,(b)碳纤维高温处理

    Figure  10.  Fracture side face morphology of specimens (a) CF untreated, (b) CF oxidized at high-temperature

    图  11  试验件断口端面形貌(a)碳纤维未处理,(b)碳纤维高温处理

    Figure  11.  Fracture end face morphology of specimens (a) CF untreated, (b) CF oxidized at high-temperature

    图  12  聚醚醚酮复合材料90°拉伸性能

    Figure  12.  90° tensile properties of PEEK composites

    图  13  聚醚醚酮复合材料90°拉伸断口形貌(a)碳纤维未处理,(b)碳纤维高温氧化处理

    Figure  13.  fracture morphology of 90° tensile specimens of PEEK composites (a) CF untreated, (b) CF oxidized at high-temperature

    图  14  碳纤维树脂界面剪切强度

    Figure  14.  Interface shear strength(IFSS) of CF/PEEK

    图  15  碳纤维树脂界面破坏形貌

    Figure  15.  Failure morphology of CF/PEEK

    图  16  聚醚醚酮复合材料层间剪切强度

    Figure  16.  Interlaminar shear strength(ILSS) of PEEK composites

    表  1  碳纤维(CF)表面处理方法

    Table  1.   Surface treatment method of carbon fiber (CF)

    Sample Method Temperature Time
    1# Untreated
    2# Oxidized 300℃ 60 s
    3# Oxidized 300℃ 120 s
    4# Oxidized 300℃ 600 s
    5# Oxidized 350℃ 60 s
    6# Acetone dissolved
    下载: 导出CSV

    表  2  碳纤维表面元素含量

    Table  2.   Surface element content of CFs

    Sample Conditions Element content /mol % O/C
    C O Si N
    1# Untreated 92.01 6.91 0.00 1.08 0.08
    2# 300℃,60 s 93.65 6.35 0.00 0.00 0.07
    3# 300℃,120 s 91.87 7.27 0.86 0.00 0.08
    4# 300℃,600 s 88.49 8.54 0.97 1.20 0.10
    5# 350℃,60 s 91.91 7.08 0.00 0.99 0.08
    6# Acetone dissolved 94.39 5.61 0.00 0.00 0.06
    下载: 导出CSV

    表  3  不同处理条件碳纤维表面官能团含量

    Table  3.   Content of CF surface functional groups under different conditions

    sample conditions functional group content(mol%)
    —C—C—
    or —C—H
    —C—OH
    or —C—OR
    —COOH
    or —COOR
    ratio of active functional
    groups (mol%)
    1# untreated 83.08 16.13 0.79 16.92
    2# 300℃,60 s 74.93 20.26 4.81 25.07
    3# 300℃,120 s 65.34 26.67 7.99 34.66
    4# 300℃,600 s 69.4 25.44 6.05 30.6
    5# 350℃,60 s 64.95 30.21 4.84 35.05
    6# acetone dissolved 82.37 9.84 7.80 17.64
    下载: 导出CSV

    表  4  不同处理条件下碳纤维表面能

    Table  4.   Surface energy of CFs under different conditions

    Sample Conditions γd/(mJ·m−2) γp/(mJ·m−2) γ/(mJ·m−2)
    1# Untreated 38.33 7.33 45.66
    2# 300℃,60 s 41.68 6.47 48.15
    3# 300℃,120 s 42.58 6.34 48.92
    4# 300℃,600 s 44.87 8.92 53.79
    5# 350℃,60 s 42.68 6.86 49.54
    6# Acetone dissolved 46.12 5.60 51.72
    Note: γd: dispersion component,γp: polar component,γ: total surface energy
    下载: 导出CSV
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  • 收稿日期:  2024-04-03
  • 修回日期:  2024-04-30
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