CN106396680A - 一种柔性超薄碳纳米管纸的制备方法 - Google Patents

一种柔性超薄碳纳米管纸的制备方法 Download PDF

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CN106396680A
CN106396680A CN201610806868.XA CN201610806868A CN106396680A CN 106396680 A CN106396680 A CN 106396680A CN 201610806868 A CN201610806868 A CN 201610806868A CN 106396680 A CN106396680 A CN 106396680A
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孙晓刚
邱志文
庞志鹏
蔡满园
陈珑
刘珍红
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Nanchang University
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Abstract

一种柔性超薄碳纳米管纸的制备方法，首先将经乙醇或丙酮润湿后的碳纳米管中加入蒸馏水中，超声分散处理，再加入纸浆纤维，采用高速剪切乳化机充分混合、分散，用普通造纸工艺制得碳纳米管导电纸，对碳纳米管纸的进行改性处理，之后，再进行石墨化处理，最后将碳纳米管纸通过对辊机轧制。本发明的碳纳米管纸较之前导电性提高明显，经轧制使得其强度、柔韧性得到明显改善。产品可裁剪成需要的形状和大小，或者直接制造成特定的形状和大小的碳纳米管导电纸产品。

Description

一种柔性超薄碳纳米管纸的制备方法
技术领域
本发明属于化学和功能材料领域，涉及碳纳米管的预处理、分散、炭化、石墨化及轧制等技术。
背景技术
碳纳米管拥有优异的电传导、热传导性能，使碳纳米管在许多领域有广泛的应用空间，特别是优秀力学性能和机械性能，由于碳纳米管为纳米材料，其优异的物理化学性能难以在宏观上表现。所以在很多研究中，可以依托纸作为基体承载碳纳米管得到一种复合的具有良好性能的导电纸。
目前报道的碳纳米管导电纸的制备方法大体分为两种：第一种，通过制备碳纳米管导电墨涂覆在纸上，这种方法可以保留良好纸的形态、强度等物理性能，但这种导电纸是单面导电的，很难形成三维的导电网络；第二种，将通过重新造纸的方法将碳纳米管导电墨和纸纤维复合后重新复合成纸，这种方法可以利用纸的吸附性和易成形性，使碳纳米管充分分散、吸附于纸纤维表面，形成三维导电网络，但这种方法得到的碳纳米管纸失去了原有纸的强度和物理性能，限制了其应用的空间。
炭化、石墨化是热处理中的常用手段，应用于碳材料中可以使材料的含碳率提高，使得非晶碳最大程度的转化为晶态结构，提高材料的导电性和导热性。轧制处理可以使材料内部结构紧实，缺陷较少，一致性提高，进而提高材料的强度和柔韧性。
发明内容
本发明的目的是一种柔性超薄碳纳米管纸的制备方法，可以简单、快捷、高效的制备柔性超薄碳纳米管纸，并通过一系列工艺处理改性碳纳米管的性能，从而提高碳纳米管纸的使用性能。
本发明是通过以下技术方案实现的，具体步骤包括如下。
（1）将经乙醇或丙酮润湿后的碳纳米管中加入蒸馏水中，采用超声分散处理1-3h，使碳纳米管均匀分散在液体中。
（2）采用高速剪切乳化机将预分散的碳纳米管和纸浆纤维充分混合、分散，得到复合悬浊液。
（3）采用普通造纸的方法将复合悬浊液沉积制得碳纳米管导电纸，置于真空烘干箱，65℃干燥1-3h。
（4）碳纳米管纸的改性处理，将剥离后的碳纳米管纸置于真空炭化炉中，以10-15℃/min升温至600℃，保温20-120min，再以2-5℃/min升温至800℃-1400℃，保温时间为1-10h，结束后冷却至室温取出。
（5）将步骤（4）炭化处理后的碳纳米管纸再置于石墨化炉中，以5-20℃/min的升温速度升温至2300℃-3000℃，石墨化处理过程中用氩气、氮气等保持非氧化的惰性气体保护，保温2-36h，随炉冷却至室温取出。
（6）将石墨化处理后的碳纳米管纸通过对辊机轧制，对辊机辊压厚度为0.05-1mm，辊压后碳纳米管纸为的密度0.1~0.4g/cm3，厚度为0.1-1mm。
本发明的碳纳米管纸较之前导电性提高明显，经轧制使得其强度、柔韧性得到明显改善。本发明产品可裁剪成需要的形状和大小，或者直接制造成特定的形状和大小的碳纳米管导电纸产品。
附图说明
附图1 为发明的碳纳米管导电纸SEM图。
附图2 为本发明的碳纳米管导电纸照片。
具体实施方式
本发明将通过以下实施例作进一步说明。
本实施例选用晶须状碳纳米管（ZL201210067937.1、ZL201210304345.7）作为导电剂。
实施例1。
1、将1g碳纳米管加入500ml 蒸馏水中，加入适量的分散剂，经超声分散处理1小时使碳纳米管均匀分散在液体中。
2、将上述碳纳米管溶液和纸浆搅拌混合，通过高速剪切乳化机将碳纳米管和纸浆充分均匀分散。
3、将分散好的碳纳米管和纸浆溶液通过抄滤成纸，真空干燥即制备成碳纳米管导电纸。
4、将碳纳米管纸置于充有氩气保护的碳化炉中，以10/min升温至600℃，保温60min，再以3℃/min升温至1200℃，保温5h，结束后冷却至室温取出。
5、将碳化处理后的碳纳米管纸置于石墨化炉中，通入氩气作为保护气体，以15℃/min的升温速度升温至2800℃，保温时间为12h，石墨化结束后冷却取出。
6、将石墨化处理后的碳纳米管纸通过对辊机轧制处理，密度约为0.22g/cm3，厚度为0.1mm。
实施例2。
1、将1g碳纳米管加入500ml 无水乙醇中，加入适量的分散剂，经超声分散处理1小时使碳纳米管均匀分散在液体中。
2、将上述碳纳米管溶液和纸浆搅拌混合，再用高速剪切乳化机将碳纳米管和纸浆充分均匀分散。
3、将分散好的碳纳米管和纸浆溶液通过抄滤成纸，真空干燥即制备成碳纳米管导电纸。
4、将碳纳米管纸置于充有氩气保护的碳化炉中，以12/min升温至600℃，保温50min，再以4℃/min升温至1400℃，保温6h，结束后冷却至室温取出。
5、将碳化处理后的碳纳米管纸置于石墨化炉中，通入氩气作为保护气体，以15℃/min的升温速度升温至2900℃，保温时间为18h，石墨化结束后冷却取出。
6、将石墨化处理后的碳纳米管纸通过对辊机轧制处理，密度约为0.39g/cm3，厚度为0.05mm。

Claims (1)

1.一种柔性超薄碳纳米管纸的制备方法，其特征是包括如下步骤：
（1）将经乙醇或丙酮润湿后的碳纳米管中加入蒸馏水中，超声分散处理1-3h，使碳纳米管均匀分散在液体中；
（2）采用高速剪切乳化机将预分散的碳纳米管和纸浆纤维充分混合、分散，得到复合悬浊液；
（3）采用普通造纸的方法将复合悬浊液沉积制得碳纳米管导电纸，置于真空烘干箱，65℃干燥1-3h；
（4）将剥离后的碳纳米管纸置于真空炭化炉中，以10-15℃/min升温至600℃，保温20-120min，再以2-5℃/min升温至800℃-1400℃，保温时间为1-10h，结束后冷却至室温取出；
（5）将步骤（4）炭化处理后的碳纳米管纸再置于石墨化炉中，以5-20℃/min的升温速度升温至2300℃-3000℃，石墨化处理过程中用氩气、氮气等保持非氧化的惰性气体保护，保温2-36h，随炉冷却至室温取出；
（6）将石墨化处理后的碳纳米管纸通过对辊机轧制，对辊机辊压厚度为0.05-1mm，辊压后碳纳米管纸为的密度0.1~0.4g/cm3，厚度为0.1-1mm。
CN201610806868.XA 2016-09-07 2016-09-07 一种柔性超薄碳纳米管纸的制备方法 Pending CN106396680A (zh)

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CN107012720A (zh) * 2017-03-13 2017-08-04 南昌大学 一种生物兼容的导电无纺布制备方法
CN108385450A (zh) * 2018-01-23 2018-08-10 柔电（武汉）科技有限公司 一种碳纳米管纸及其制备方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106835847A (zh) * 2017-03-13 2017-06-13 南昌大学 一种生物兼容性碳纳米管/羟基磷灰石复合纸的制备方法
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CN108385450A (zh) * 2018-01-23 2018-08-10 柔电（武汉）科技有限公司 一种碳纳米管纸及其制备方法
CN109167093A (zh) * 2018-09-03 2019-01-08 江西克莱威纳米碳材料有限公司 一种羟基化晶须碳纳米管纸及其制备方法和一种锂硫电池
CN109256564A (zh) * 2018-09-10 2019-01-22 江西克莱威纳米碳材料有限公司 碳纳米管-石墨复合材料、锂硫电池正极材料和锂硫电池
CN109256564B (zh) * 2018-09-10 2021-07-09 江西克莱威纳米碳材料有限公司 碳纳米管-石墨复合材料、锂硫电池正极材料和锂硫电池

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