高性能热塑性树脂基复合材料的诱导结晶行为研究

余坤; 姚佳楠; 张代军; 刘刚; 刘浩; 陈春海

高性能热塑性树脂基复合材料的诱导结晶行为研究

余坤¹,
姚佳楠¹,
张代军^{2, 3},
刘刚^{1, 4, ,},
刘浩^1, ,,
陈春海¹

1.
东华大学　材料科学与工程学院, 纤维材料改性国家重点实验室, 先进低维材料中心, 上海 201620
2.
中国航发北京航空材料研究院, 北京 100095
3.
先进复合材料重点实验室, 北京 100095
4.
北京化工大学, 先进技术与装备研究院, 北京 100029

基金项目: 上海市“科技创新行动计划”商用飞机复合材料标准体系研究项目(22DZ2206400)

详细信息

通讯作者:
刘刚，博士，研究员，博士生导师，研究方向为纤维增强树脂基复合材料　E-mail: liugang@dhu.edu.cn

刘浩，博士，研究员，博士生导师，研究方向为聚合物结晶　E-mail: liuh@dhu.edu.cn

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2024-06-20
- 修回日期: 2024-08-04
- 录用日期: 2024-08-28
- 网络出版日期: 2024-09-09

Research on the induced crystallization behavior of high-performance thermoplastics resin-based composites

YU Kun¹,
YAO Jianan¹,
ZHANG Daijun^{2, 3},
LIU Gang^{1, 4
, ,},
LIU Hao^{1
, ,},
Chen Chunhai¹

1.
State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, Center for Advanced Low-dimension Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China
2.
AECC Beijing Institute of Aeronautical Materials, Beijing 100095, China
3.
National Key Laboratory of Advanced Composites, Beijing 100095, China
4.
Institute of Advanced Technology and Equipment, Beijing University of Chemical Technology, Beijing 100029, China

Funds: Action Plan for Science, Technology and Innovation” Commercial Aircraft Composites Standard System Research Project of Shanghai (22DZ2206400)

摘要

摘要: 在热塑性树脂基复合材料中，优化界面性能对于提升复合材料的整体性能表现具有非常重要的作用。当碳纤维(CF)作为增强体与半结晶型的高性能热塑性树脂基体，如聚醚醚酮(PEEK)、聚芳醚酮(PAEK)或聚苯硫醚(PPS)等复合时，纤维与树脂界面上发生的诱导结晶现象，会对复合材料的界面性能产生显著影响。本文以高性能热塑性树脂基复合材料研究中诱导结晶问题为切入点，综述了该领域的研究进展。文章涵盖了从诱导结晶样品的制备方法到其最终性能变化的全过程，并分析了诱导结晶的类型及其影响因素，同时描述了高性能热塑性树脂中几种典型的横晶(TC)形态。此外，本文还着重探讨了TC结构对高性能热塑性树脂基复合材料界面性能的具体影响，并提出了当前该领域仍然存在的问题和面临的挑战。
- 诱导结晶 /
- 横晶 /
- 碳纤维 /
- 高性能热塑性树脂 /
- 界面性能
Abstract: In thermoplastic resin-based composites, optimizing interfacial properties is crucial for enhancing the overall characteristics of the composites. When carbon fibers (CFs) are employed as the reinforcement, combined with semi-crystalline high-performance thermoplastic resins such as polyetheretherketone (PEEK), polyaryletherketone (PAEK), or polyphenylene sulfide (PPS) as the matrix, the induced crystallization phenomenon at the fiber/resin interface significantly impacts the interfacial properties of the composite. Taking the issue of induced crystallization in the study of high-performance thermoplastic resin-based composites as the starting point, this article comprehensively reviews the research progress in this area. The article covers the entire process from the preparation methods of induced crystallization samples to their final performance changes, analyzes the classification and influencing factors of induced crystallization, and describes several typical transcrystallinity (TC) morphologies in high-performance thermoplastic resins. Additionally, this article focuses on discussing the specific impact of TC on the interfacial properties of high-performance thermoplastic resin-based composites, and proposes the existing problems and challenges in this field.
- Induced crystallization /
- Transcrystallinity /
- Carbon fiber /
- High-Performance thermoplastics /
- Interfacial properties

HTML全文

图 1 (a) 偏光样品制备模型，(b) 等温结晶，(c) 非等温结晶的温度控制程序示意图

Figure 1. (a) Schematic diagram of PLM sample preparation model.(b) Temperature control procedure for isothermal crystallization and (c) non-isothermal crystallization.

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图 2 溶液法制备复合材料薄膜示意图

Figure 2. Schematic diagram of solution method-based preparation of composite films

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图 3 三种诱导结晶示意图^[41]

Figure 3. Schematic diagram of three induced crystallization methods^[41]

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图 4 碳纤维增强聚醚醚酮(CF/PEEK)复合材料的TC结构^[14]

Figure 4. TC structure of carbon fiber reinforced polyetheretherketone (CF/PEEK) composites^[14]

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图 5 (a) PEEK中的标准模量AS4纤维的诱导结晶行为。(b) PEEK中高模量HMS纤维的诱导结晶行为^[43]

Figure 5. (a) Induced crystallization behavior of standard modulus AS4 fibers in PEEK. (b) Induced crystallization behavior of high modulus HMS fibers in PEEK^[43]

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图 6 两种碳纤维诱导PEEK结晶的示意图：(a) 纯CF，(b) PI上浆CF^[14]

Figure 6. Schematic diagrams of two carbon fiber-induced PEEK crystallization processes: (a) pure CF, (b) CF with PI sizing^[14]

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图 7 (a) 未施加应力。(b) 施加5 mm/min的剪切应力^[13]

Figure 7. (a) Without applied stress. (b) With applied shear stress of 5 mm/min^[13]

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图 8 在110，112.5，115℃下CF对聚乳酸的诱导结晶形貌^[22]

Figure 8. Induced crystallization morphology of poly (lactic acid) by carbon fiber at 110, 112.5 and 115℃^[22]

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图 9 CF/PEEK的偏光图片：样品保持在390℃持续(a) 0.5 h; (b) 2 h; (c) 3 h; (d) 4 h后以0.5℃/min冷却至270℃，然后淬火至室温^[47]

Figure 9. PLM images of CF/PEEK: the sample was maintained at 390℃ for (a) 0.5 h; (b) 2 h; (c) 3 h; (d) 4 h, and then cooled to 270℃ at a rate of 0.5℃/min followed by quenching to room temperature^[47]

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图 10 在不同温度下预热处理后的诱导结晶形态：(a) 未处理，(b) CF-280℃，(c) CF-340℃，(d) CF-370℃^[69]

Figure 10. Induced crystallization morphologies after pre-heat treatment at different temperatures: (a) untreated, (b) CF-280℃, (c) CF-340℃,(d) CF-370℃^[69]

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图 11 聚醚酮酮(PEKK)的对位和间位结构^[73]

Figure 11. Para- and meta-structures of polyetherketoneketone (PEKK)^[73]

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图 12 经过(a) 220℃, (b) 260℃, (c) 300℃等温保温后低温断裂的CF/PEKK样品的SEM^[74]

Figure 12. SEM images of CF/PEKK samples after low-temperature fracture after isothermal holding at (a) 220℃, (b) 260℃, (b) 300℃^[74]

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图 13 CF/PPS的偏光图片，(a) 未处理，(b) 7天后的水热老化^[81]

Figure 13. Polarizing images of CF/PPS, (a) untreated, (b) hydrothermal aging after 7 days^[81]

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图 14 四种测试方法示意图^{[86, 87, 89, 90]}

Figure 14. Schematic diagrams of four testing methods^{[86, 87, 89, 90]}

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图 15 (a) 使用结晶PEEK对CF进行上浆的示意图，(b) 微粘结试验示意图，(c) CF和PEEK基体之间的界面示意图^[92]

Figure 15. (a) The schematic of sizing CF with crystalline PEEK. (b) The schematic of microbond test. (c) The schematic of the interface between CF and PEEK matrix^[92]

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图 16 三种树脂的结晶模型以及界面剪切强度^[94]

Figure 16. Crystallization modeling and interfacial shear strength of three resins^[94]

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表 1 CF/聚合物界面处的剪切强度(MPa)^[91]

Table 1. Shear strength at the carbon fiber/polymer interface (MPa)^[91]

Resin type	Fast-cooling	Slow-cooling	Annealing
Polycarbonate (PC)	52	75	-
Polyphenylene sulfide (PPS)	36	61	71
Polyetheretherketone (PEEK)	74	97	112

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表 2 PEEK复合材料的90°拉伸性能^[47]

Table 2. Transverse tensile properties of PEEK composites^[47]

Composites type	Crystallinity	Modulus	Strength	Strain failure
	%	GPa	MPa	%
LS	36	3.9	111	4.8
LF	42	4.3	106	4.4
SF	42	3.9	63	1.9
SS	45	4.0	60	1.7
Note: The first letter L stands for long melt holding time -Long, S stands for short melt holding time -Short. The second letter S stands for slow cooling rate - Slow and F stands for fast cooling rate - Fast.

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高性能热塑性树脂基复合材料的诱导结晶行为研究

通讯作者:
刘刚，博士，研究员，博士生导师，研究方向为纤维增强树脂基复合材料　E-mail: liugang@dhu.edu.cn

刘浩，博士，研究员，博士生导师，研究方向为聚合物结晶　E-mail: liuh@dhu.edu.cn

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Research on the induced crystallization behavior of high-performance thermoplastics resin-based composites

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高性能热塑性树脂基复合材料的诱导结晶行为研究

通讯作者: 刘刚，博士，研究员，博士生导师，研究方向为纤维增强树脂基复合材料 E-mail: liugang@dhu.edu.cn 刘浩，博士，研究员，博士生导师，研究方向为聚合物结晶 E-mail: liuh@dhu.edu.cn

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Research on the induced crystallization behavior of high-performance thermoplastics resin-based composites

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通讯作者:
刘刚，博士，研究员，博士生导师，研究方向为纤维增强树脂基复合材料　E-mail: liugang@dhu.edu.cn

刘浩，博士，研究员，博士生导师，研究方向为聚合物结晶　E-mail: liuh@dhu.edu.cn