CN111531918A - 一种纳米颗粒增强三维机织复合材料的制备方法 - Google Patents

一种纳米颗粒增强三维机织复合材料的制备方法 Download PDF

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CN111531918A
CN111531918A CN202010308451.7A CN202010308451A CN111531918A CN 111531918 A CN111531918 A CN 111531918A CN 202010308451 A CN202010308451 A CN 202010308451A CN 111531918 A CN111531918 A CN 111531918A
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黄涛
黎行豪
龚耀华
陈延东
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Northwestern Polytechnical University
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Abstract

本发明涉及一种纳米颗粒增强三维机织复合材料的制备方法，制备包括：采用碳纤维三向正交织物作为预制体，环氧树脂作为基体，纳米颗粒作为填料。将纳米颗粒均匀分散在环氧聚合物中，然后采用真空辅助树脂转移模塑(VARTM)成型工艺制备而成。本发明的方法制备简单，且制备成的复合材料具有优异的力学性能，能够适用于工业化生产。

Description

一种纳米颗粒增强三维机织复合材料的制备方法
技术领域
本发明属于树脂基碳纤维增强复合材料领域，涉及一种纳米颗粒增强三维机织复合材料的制备方法。
背景技术
环氧树脂具有耐高低温、低成本、化学稳定性好、易加工成型等优点，已被广泛应用于航天航空、粘接材料、半导体封装材料、纤维增强材料、层合板等领域。然而，环氧树脂也具有很高的脆性，这一缺点限制了环氧树脂在需要抗冲击性和高断裂强度的产品中的应用。
三维机织复合材料增强体为碳纤维，与二维碳纤维增强复合材料相比，它们具有优越的层间性能、弯曲性能和抗冲击性性能。然而，环氧树脂作为三维机织复合材料的一种基体材料，由于本身较脆，在一些重要领域的应用上受限制。解决这一问题的一种方法是通过在聚合物基体中加入刚性填料而不显著降低其韧性来改变环氧树脂的性能，进而可以改善三维机织复合材料的力学性能。
发明内容
要解决的技术问题
为了避免现有技术的不足之处，本发明提出一种纳米颗粒增强三维机织复合材料的制备方法，制备的复合材料力学性能优异，制备工艺简单。
技术方案
一种纳米颗粒增强三维机织复合材料的制备方法，其特征在于步骤如下：
步骤1：将质量分数为3％的TiO2纳米颗粒粉末加入球磨罐中，用行星式球磨机研磨；
步骤2：将环氧树脂双酚F环氧二缩水甘油醚加热到70～90度，加入研磨好的TiO2纳米颗粒粉末，在室温下进行搅拌后在超声波处理器中进行超声处理；所述搅拌时搅拌机的转速逐渐从0增加至3500r/min，然后保持180min，最后逐渐降为零；所述超声处理采用脉冲方式处理：超声搅拌1～2分钟，停顿5秒钟；所述超声波频率为55Hz；
步骤3：待冷却至室温后加入固化剂二乙基甲苯二胺DETDA，加入的固化剂与环氧树脂的重量配比为100︰27；采用机械搅拌机在室温下继续搅拌；
步骤4：在真空环境箱中进行脱泡处理，脱泡时长为150min；
步骤5：采用真空辅助树脂转移模塑VARTM成型工艺制备纳米颗粒增强三维机织复合材料；采用模具为钢化玻璃板，以碳纤维三向正交织物为碳纤维预制体，成型工艺的温度120℃～135℃，压力-0.1Mpa，时间8h～9h。
所述碳纤维三向正交织物的纱线规格为T300-3K。
所述环氧树脂双酚F环氧二缩水甘油醚的粘度为2000-5000Mpa.s。
所述固化剂二乙基甲苯二胺DETDA的粒径为15～25nm。
所述固化剂二乙基甲苯二胺DETDA的分子量为178.3。
有益效果
本发明提出的一种纳米颗粒增强三维机织复合材料的制备方法，制备包括：采用碳纤维三向正交织物作为预制体，环氧树脂作为基体，纳米颗粒作为填料。将纳米颗粒均匀分散在环氧聚合物中，然后采用真空辅助树脂转移模塑(VARTM)成型工艺制备而成。本发明的方法制备简单，且制备成的复合材料具有优异的力学性能，能够适用于工业化生产。
附图说明
图1为本发明在环氧树脂中加入纳米颗粒的制备流程图
图2为本发明VARTM成型工艺的制备流程图
图3为本发明制备的纳米颗粒增强三维机织复合材料结构图
具体实施方式
现结合实施例、附图对本发明作进一步描述：
实施例1
首先将质量分数为3％的TiO2纳米颗粒粉末加入球磨罐中，用行星式球磨机研磨后取出备好(球磨机转速为450r/min，持续60min)。同时将环氧树脂加热到80度以减小环氧树脂的粘度(利于纳米颗粒的分散)。再将研磨过的TiO2纳米颗粒粉末加入环氧树脂中，利用机械搅拌机在室温下进行搅拌(搅拌机的转速逐渐从0增加至3500r/min，然后保持180min，最后逐渐降为零)，然后在超声波处理器中搅拌60min(超声波处理器是采用脉冲方式处理，即超声搅拌1～2分钟，停顿5秒钟，超声波频率为55Hz)，待冷却至室温后加入固化剂二乙基甲苯二胺DETDA的粒径为25nm，加入的固化剂和环氧树脂的重量配比为100：27，最后用机械搅拌机在室温下继续搅拌60min(搅拌机转速为1000r/min)。机械搅拌过程中会产生大量气泡，需要进行脱泡处理，脱泡过程在真空环境箱中进行，脱泡时长为150min。脱泡完成后暂时放置一边。
纳米颗粒增强三维机织复合材料的制备采用真空辅助树脂转移膜塑(VARTM)工艺。VARTM工艺通常采用单面模具，表面平整并且无缺陷，本发明使用的模具为钢化玻璃板。主要制备流程如下：首先，用小刀片清理模具表面残留物，并用酒精清洗模具表面，清洗完后在模具四周边缘粘贴密封胶带，随后在模具表面抹上脱模剂，依次铺上脱模布、碳纤维预制体、脱模布、导流网(如图2所示)，然后在注入口和抽气口两端铺设真空管和缠绕管，最后封上真空袋。
所述碳纤维预制体采用碳纤维三向正交织物，纱线规格为T300-3K
封装好模具以后，需要检测真空袋内的密封状态。打开抽气口处阀门，抽真空并稳定一段时间后，关上阀门，放置2个小时，观察是否有明显漏气现象。同时把前面配置好的环氧树脂混合液加热到70度，降低树脂的粘度，以保证树脂在预制体中充分流动和浸润。树脂的注入过程持续50min，树脂注入完成后，把模具放到加热片上加热固化，固化条件为135℃+8h。最后冷却至室温，得到最终的二氧化钛纳米颗粒增强三维正交机织复合材料。
实施例2：工艺过程与材料选取与实施例一致，区别在于：
加入固化剂二乙基甲苯二胺DETDA的粒径为20nm；
成型工艺的温度130℃，压力-0.1Mpa，时间7h。
实施例3：工艺过程与材料选取与实施例一致，区别在于：
加入固化剂二乙基甲苯二胺DETDA的粒径为15nm；
成型工艺的温度120℃，压力-0.1Mpa，时间9h。

Claims (5)

1.一种纳米颗粒增强三维机织复合材料的制备方法，其特征在于步骤如下：
步骤1：将质量分数为3％的TiO2纳米颗粒粉末加入球磨罐中，用行星式球磨机研磨；
步骤2：将环氧树脂双酚F环氧二缩水甘油醚加热到70～90度，加入研磨好的TiO2纳米颗粒粉末，在室温下进行搅拌后在超声波处理器中进行超声处理；所述搅拌时搅拌机的转速逐渐从0增加至3500r/min，然后保持180min，最后逐渐降为零；所述超声处理采用脉冲方式处理：超声搅拌1～2分钟，停顿5秒钟；所述超声波频率为55Hz；
步骤3：待冷却至室温后加入固化剂二乙基甲苯二胺DETDA，加入的固化剂与环氧树脂的重量配比为100︰27；采用机械搅拌机在室温下继续搅拌；
步骤4：在真空环境箱中进行脱泡处理，脱泡时长为150min；
步骤5：采用真空辅助树脂转移模塑VARTM成型工艺制备纳米颗粒增强三维机织复合材料；采用模具为钢化玻璃板，以碳纤维三向正交织物为碳纤维预制体，成型工艺的温度120℃～135℃，压力-0.1Mpa，时间8h～9h。
2.根据权利要求2所述的一种纳米颗粒增强三维机织复合材料的制备方法，其特征在于：所述碳纤维三向正交织物的纱线规格为T300-3K。
3.根据权利要求1所述的一种纳米颗粒增强三维机织复合材料的制备方法，其特征在于：所述环氧树脂双酚F环氧二缩水甘油醚的粘度为2000-5000Mpa.s。
4.根据权利要求1所述的一种纳米颗粒增强三维机织复合材料的制备方法，其特征在于：所述固化剂二乙基甲苯二胺DETDA的粒径为15～25nm。
5.根据权利要求1或5所述的一种纳米颗粒增强三维机织复合材料的制备方法，其特征在于：所述固化剂二乙基甲苯二胺DETDA的分子量为178.3。
CN202010308451.7A 2020-04-18 2020-04-18 一种纳米颗粒增强三维机织复合材料的制备方法 Pending CN111531918A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4094929A1 (de) * 2021-05-14 2022-11-30 Otto Fuchs - Kommanditgesellschaft - Verfahren zum herstellen eines faserverstärkten kunststoffproduktes sowie anlage dafür

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106832780A (zh) * 2017-02-17 2017-06-13 海安县恒业制丝有限公司 介孔TiO2/CF碳纤维环氧树脂基复合材料
CN108871971A (zh) * 2018-07-05 2018-11-23 内蒙古工业大学 树脂基三维正交机织复合材料弯曲疲劳应力水平设置方法
CN109054289A (zh) * 2018-06-01 2018-12-21 内蒙古工业大学 一种用于风机叶片的三维机织复合材料及其纤维/树脂界面改性方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106832780A (zh) * 2017-02-17 2017-06-13 海安县恒业制丝有限公司 介孔TiO2/CF碳纤维环氧树脂基复合材料
CN109054289A (zh) * 2018-06-01 2018-12-21 内蒙古工业大学 一种用于风机叶片的三维机织复合材料及其纤维/树脂界面改性方法
CN108871971A (zh) * 2018-07-05 2018-11-23 内蒙古工业大学 树脂基三维正交机织复合材料弯曲疲劳应力水平设置方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4094929A1 (de) * 2021-05-14 2022-11-30 Otto Fuchs - Kommanditgesellschaft - Verfahren zum herstellen eines faserverstärkten kunststoffproduktes sowie anlage dafür

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Application publication date: 20200814