CN1296436C - 一种基于碳纳米管的复合材料的制备方法 - Google Patents

一种基于碳纳米管的复合材料的制备方法 Download PDF

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CN1296436C
CN1296436C CNB2004100276323A CN200410027632A CN1296436C CN 1296436 C CN1296436 C CN 1296436C CN B2004100276323 A CNB2004100276323 A CN B2004100276323A CN 200410027632 A CN200410027632 A CN 200410027632A CN 1296436 C CN1296436 C CN 1296436C
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黄华
刘长洪
范守善
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Abstract

一种基于碳纳米管的复合材料的制备方法，其包括以下步骤：制备一种预聚物溶液或预聚物单体溶液；将碳纳米管加入上述溶液，用超声波清洗一段时间；加入引发剂，使预聚物溶液或预聚物单体溶液发生反应而聚合；将聚合后的聚合物放到挤出设备中挤出；将挤出物进行拉伸，得到含有整齐排列碳纳米管的复合材料。

Description

一种基于碳纳米管的复合材料的制备方法
【技术领域】
本发明涉及一种基于碳纳米管的复合材料的制备方法。
【背景技术】
自1991年日本NEC公司的Iijima发现碳纳米管(Carbon Nanotube，CNT)以来(Iilima S.，Nature，1991，354，56-58)，立即引起科学界及产业界的极大重视，是近年来国际科学研究的热点。碳纳米管具有与金刚石相同的热导和独特的力学性能，如抗张强度达100Gpa，模量高达1TGPa，且耐强酸、强碱，600℃以下基本不氧化等，利用碳纳米管作为填充物与工程材料复合成为碳纳米管研究的一个重要方向。
特别地，碳纳米管与聚合物的复合可以实现材料的优势互补或加强。碳纳米管具有高的长径比和中空的结构，具有优异的力学性能，可作为一种超级纤维，对复合材料起到增强作用。同时由于碳纳米管特殊电性能，形成的复合材料可具有抗静电、微波吸收和电磁屏蔽等性能。然而，由于碳纳米管易于聚集和缠结，到目前为止实验结果与理论预测仍相距甚远。
2003年4月16日公开的一篇申请号为02113457.X的中国专利申请(申请人为四川大学，发明人为夏和生、王琪等)，提出一种利用超声波的分散、粉碎、活化、引发等多重作用，破坏碳纳米管本身的聚集和缠绕，通过原位本体聚合制备聚合物/碳纳米管复合材料的方法。然而，该方法虽然能够基本解决碳纳米管在聚合物基体中的分散问题，得到均匀分散碳纳米管的复合材料，但是碳纳米管在聚合物基体中仍然为无序排列，在应用中，该聚合物/碳纳米管复合材料的性能在一定程度上仍然受到影响，不能充分发挥碳纳米管的优良性能。
因此，提供一种能够同时解决复合材料中碳纳米管在聚合物中的分散和排列问题，制备一种性能优良的基于碳纳米管的复合材料的方法十分必要。
【发明内容】
为解决现有技术的技术问题，本发明的目的是提供一种基于碳纳米管的复合材料的制备方法。
为实现本发明的目的，本发明提供一种基于碳纳米管的复合材料的制备方法，其包括以下步骤：制备一预聚物溶液或预聚物单体溶液；将碳纳米管加入上述溶液，用超声波清洗一段时间；加入引发剂，使预聚物溶液或预聚物单体溶液发生反应而聚合；将聚合后的聚合物放到挤出设备中挤出；将挤出物进行拉伸，得到含有整齐排列碳纳米管的复合材料。
与现有技术相比较，本发明基于碳纳米管的复合材料的制备方法不仅能够得到均匀分散有碳纳米管的复合材料，通过力的作用，还能够使分散均匀的碳纳米管在一定的方向上整齐排列，并且力的作用能使碳纳米管得到更好的分散，从而能够同时解决复合材料中碳纳米管在聚合物中的分散和排列问题，充分发挥碳纳米管的优良性能，得到性能卓越的复合材料。
【附图说明】
图1是本发明实施例中基于碳纳米管的复合材料的制备方法的流程图。
图2是本发明实施例采用的挤压装置的示意图。
图3是本发明实施例制得的基于碳纳米管的复合材料的SEM照片。
【具体实施方式】
下面将结合附图及具体实施例对本发明进行详细说明。
如图1所示，本发明基于碳纳米管的复合材料的制备方法包括以下步骤：
步骤1，提供一种分散均匀的预聚物溶液或预聚物单体溶液，本发明预聚物材料包括聚氨酯或环氧树脂。本发明的实施例采用聚氨酯(两组分铁锚101胶：A组分和B组分)，首先，将聚氨酯A组分用乙酸乙酯溶解稀释，降低其粘度，然后用超声波清洗一段时间，得到分散均匀的聚氨酯溶液。
步骤2，将碳纳米管加入上述溶液，并且用超声波清洗一段时间。其中，碳纳米管的重量百分比含量为1～10％。超声波清洗的作用是使碳纳米管能够在聚氨酯溶液中初步分散。本发明碳纳米管包括多壁碳纳米管或者单壁碳纳米管，碳纳米管的制备方法可采用现有技术中的CVD法、电弧放电法、激光烧蚀法等，本实施例采用CVD法，所用的碳纳米管直径范围为1-10微米。
另外，由于碳纳米管易于聚集和缠结，可以进一步通过超声波破碎仪破碎一段时间，将聚集和缠结的碳纳米管分开，然后再通过超声波清洗一段时间，从而能够使碳纳米管分散比较均匀。
步骤3，加入引发剂，使预聚物溶液或预聚物单体溶液发生反应或发生交联而聚合，得到基于碳纳米管的复合材料。引发剂的选择根据预聚物材料的不同而不同，本发明实施例中的引发剂可以采用分散有聚氨酯B组分的乙醇溶液或单纯的去离子水。将聚氨酯B组分的乙醇溶液倒入聚氨酯A组分的预聚溶液中，加入量视两者浓度之比以及聚氨酯比例的要求，本实施例预聚溶液与引发剂之比例为5∶1，适当的超声清洗一段时间，收集溶液中的膏状物质，即得到复合材料的预加工物。本发明得到的碳纳米管复合材料为碳纳米管-聚氨酯复合材料，其为膏状或黑色物体。
步骤4，将聚合后的复合材料放到挤出设备中挤出，通过挤压力的作用，使碳纳米管往一个方向上排列。挤出设备请参阅图2，首先将聚合后的复合材料11放入挤出设备10中，通过施加外力F，使复合材料11通过筛网13挤出。其中，筛网13的网孔的孔径为30-500微米。挤出物中碳纳米管在同一方向上的排列得到改善。
步骤5，将挤出物进行拉伸，通过拉伸力进一步得到含有整齐排列的碳纳米管的复合材料。本发明最后得到的复合材料为直径30～50微米的复合材料纤维，其中，碳纳米管在复合材料中沿垂直于直径的方向整齐排列，请参阅图3。
在应用时，由于碳纳米管在复合材料中整齐排列且均匀分散，能够充分发挥碳纳米管的优良性能，本发明基于碳纳米管的复合材料可广泛应用于导电、导热、抗静电、电磁屏蔽等领域，具有广泛的应用前景。

Claims (10)

1.一种基于碳纳米管的复合材料的制备方法，其包括以下步骤：
制备一预聚物溶液或预聚物单体溶液；
将碳纳米管加入上述溶液，用超声波清洗一段时间；
加入引发剂，使预聚物溶液或预聚物单体溶液发生反应而聚合；
将聚合后的聚合物通过挤出设备中挤出；
将挤出物进行拉伸，得到含有整齐排列碳纳米管的复合材料。
2.如权利要求1所述的基于碳纳米管的复合材料的制备方法，其特征在于用超声波清洗进一步包括以下步骤：
首先，将碳纳米管加入预聚物溶液或预聚物单体溶液后用超声波清洗一段时间；
然后将清洗后的溶液用超声波破碎仪破碎一段时间；
最后，将破碎后的溶液再用超声波清洗一段时间。
3.如权利要求1所述的基于碳纳米管的复合材料的制备方法，其特征在于该预聚物溶液包括聚氨酯溶液或环氧树脂溶液。
4.如权利要求3所述的基于碳纳米管的复合材料的制备方法，其特征在于该聚氨酯溶液的形成方法包括：
首先，将聚氨酯用乙酸乙酯溶解稀释，降低其粘度；
然后用超声波清洗一段时间，得到分散均匀的聚氨酯溶液。
5.如权利要求1所述的基于碳纳米管的复合材料的制备方法，其特征在于该引发剂包括乙醇溶液或单纯的去离子水。
6.如权利要求1所述的基于碳纳米管的复合材料的制备方法，其特征在于挤出设备中筛网的网孔孔径为30～500微米。
7.如权利要求1所述的基于碳纳米管的复合材料的制备方法，其特征在于该含有整齐排列碳纳米管的复合材料直径为30～50微米。
8.如权利要求7所述的基于碳纳米管的复合材料的制备方法，其特征在于该复合材料中，碳纳米管在复合材料中沿垂直于复合材料直径的方向整齐排列。
9.如权利要求1所述的基于碳纳米管的复合材料的制备方法，其特征在于该碳纳米管包括多壁碳纳米管或单壁碳纳米管。
10.如权利要求9所述的基于碳纳米管的复合材料的制备方法，其特征在于该碳纳米管的直径范围为1～10微米。
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