CN106120296B - 一种碳纳米管纤维纯化方法 - Google Patents

一种碳纳米管纤维纯化方法 Download PDF

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CN106120296B
CN106120296B CN201610462342.4A CN201610462342A CN106120296B CN 106120296 B CN106120296 B CN 106120296B CN 201610462342 A CN201610462342 A CN 201610462342A CN 106120296 B CN106120296 B CN 106120296B
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上媛媛
李淑荟
花春飞
王颖
余秀秀
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Zhengzhou University
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Abstract

本发明提供一种有效的碳纳米管纤维纯化方法，能够去除纤维中的杂质、增加了纯化效率。本发明是按照下述步骤进行的：(1)将导电胶粘在衬底之上，碳纳米管纤维的两端粘在导电胶上，涂覆银胶，并使碳纳米管纤维架空；(2)待银胶晾干后测量碳纳米管纤维的电阻，通电0.5～1s；(3)取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后在80℃干燥3‑5h。本发明具有以下优点：1.极大的降低了酸处理的时间，增加了纯化效率。2.对于均匀的碳纳米管纤维的纯化极其有效，且方法简单容易操作，可行性强。3.适用于各种使用浮动催化法生长的碳纳米管纤维的纯化，尤其是针对被碳层包覆的金属催化颗粒的纯化。

Description

一种碳纳米管纤维纯化方法
技术领域
本发明涉及碳纳米管应用领域，具体涉及一种碳纳米管纤维纯化方法。
背景技术
碳纳米管具有优良的力学、电学、热学和光学性能，因而具有极广泛的应用领域，成为化学、物理、材料学界关注的重点潜力材料。目前碳纳米管的制备方法多种多样，制备工艺也逐渐趋于成熟。然而，商业化大批量生产的碳纳米管不可避免有无定型碳、催化颗粒以及碳纳米粒子等杂质的存在，会在某些方面提升碳纳米管的性能，也会在另一些方面导致性能恶化。因而，有效快捷的除去杂质对深入研究和应用碳纳米管的应用是至关重要的。
碳纳米管有单壁碳纳米管、双壁碳纳米管和多壁碳纳米管之分，它们的性质不同、制备方法不同、杂质含量和种类不同，纯化方法也需要根据具体情况设定。目前纯化碳纳米管的方法主要有物理法、化学法和综合法。每种方法均有其各自的优点，综合法的提出使碳纳米管的纯化效率进一步提升，但是仍有很大的发展空间。
发明内容
本发明的目的是针对上述现有技术的不足，提供一种有效的碳纳米管纤维纯化方法，能够去除纤维中的杂质、增加了纯化效率。
本发明的技术方案是这样实现的：一种碳纳米管纤维纯化方法，是按照下述步骤进行的：(1)将导电胶粘在衬底之上，碳纳米管纤维的两端粘在导电胶上，涂覆银胶，并使碳纳米管纤维架空；(2)待银胶晾干后测量碳纳米管纤维的电阻，根据电阻选择合适的电压值通电0.5～1s；(3)取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后在80℃干燥3-5h。
优选的，步骤(3)中酸溶液为盐酸、硝酸、王水或硫酸。
优选的，步骤(1)中碳纳米管纤维的长度在1-20cm。
优选的，步骤(1)中碳纳米管纤维的直径为30～300μm。
本发明与现有技术相比，具有以下优点及突出性效果：1.对碳纳米管纤维瞬间通电的方法使得碳纳米管内的无定形碳、碳纳米颗粒以及部分金属催化剂颗粒灼烧，以烟雾的形式放出，暴露出被包裹的金属颗粒，金属催化颗粒瞬间热氧化，极易与酸发生化学反应，极大的降低了酸处理的时间，增加了纯化效率。2.这种方法对于均匀的碳纳米管纤维的纯化极其有效，且方法简单容易操作，可行性强。3.适用于各种使用浮动催化法生长的碳纳米管纤维的纯化，尤其是针对被碳层包覆的金属催化颗粒的纯化。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是实施例1中碳纳米管纤维通电后的微观形貌特征。
图2是实施例1中碳纳米管纤维纯化后的扫描电子显微镜照片。
图3是纯化前后的碳纳米管纤维电导率的变化图示。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有付出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
一种碳纳米管纤维纯化方法，是按照下述步骤进行的：
(1)将导电胶粘在玻璃衬底之上，碳纳米管纤维的两端粘在导电胶上，涂覆银胶，并使碳纳米管纤维架空；
(2)待银胶晾干后测量碳纳米管纤维的电阻，根据电阻选择合适的电压值通电0.5～1s；所加载的电压为恒定的，可以是直流或者交流。
(3)取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后在80℃干燥3-5h。
优选的，步骤(3)中酸溶液为盐酸、硝酸、王水或硫酸。
优选的，步骤(1)中碳纳米管纤维的长度在1-20cm，步骤(1)中碳纳米管纤维的直径为30～300μm。
热氧化法是纯化碳纳米管的一种普遍的方法，与其他方法结合能够有效除去碳纳米管附着的杂相，本申请是一种瞬间热氧化结合酸处理的方法，这种方法能够以极高的效率除去碳纳米管中的缺陷及杂质。通电产生的焦耳热使碳纳米管表面附着的无定型碳、碳颗粒、以及铁催化颗粒瞬间氧化，一部分铁催化颗粒随着二氧化碳在烧灼过程中以烟雾形式放出，剩余氧化铁仍附着在碳纳米管间隙中，经过稀酸浸泡能够很快的发生化学反应进入溶液中。值得一提的是，对于单壁碳纳米管，由于其直径在1-2μm，催化颗粒一般附着于管外部，通电氧化的金属催化颗粒存在于碳纳米管束的间隙之间，通电方法并不破坏长径比较大的单壁碳纳米管。
本发明提供碳纳米管纤维纯化方法，采用加载瞬时电压的方法，属于热氧化法的范畴。本发明适合应用于宏观的碳纳米管纤维，其直径几十到几百微米之间，长度1-20cm；所加载的恒定电流或者电压可以为直流也可以为交流。满足上述要求的碳纳米管纤维可以根据现有的方法合成，如采用CCVD法(浮动催化剂化学气相沉积)生长，或者可以参照Ya-LiLi,Ian A.Kinloch,Alan H.Windle,J.Science.2004,304,276-279中公开的方法合成。单壁碳纳米管通过CCVD方法生长的时候，以均匀的速度直接从管式炉中拉出，多股透明薄膜桶状单壁碳纳米管纤维平行堆叠，之后用电动马达放丝制备出直径几十到几百微米不等的纤维。
本申请适合应用于宏观的碳纳米管纤维，在纤维轴向所加载恒定电压值与碳纳米管纤维的电阻有关联：同一长度的纤维，直径越大，电阻越小，所加载的电压越小；同一直径，不同长度的纤维，长度越大，电阻越大，所施加的电压越大。
以下结合实施例详细说明本发明，实施例1～4用于说明通过对碳纳米管加载电流和电压实现碳纳米管快速有效纯化的方法。
实施例1，本实施例中碳纳米管通电纯化的方法如下：截取长度2.5cm、直径54μm均匀的碳纳米管纤维，将其两端粘在导电胶上，涂覆银胶，并使纤维架空，用万用表测量纤维的电阻为32Ω，根据电阻选择合适的电压值40V通电，通电时长约0.5-1s，这样防止通电时间过长或者电压电流过大致使碳纳米管纤维烧断；取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后放在鼓风干燥箱中80℃干燥4h。
本实施例通电后的碳纳米管纤维扫描电子显微镜如图1所示，纯化后碳纳米管纤维的扫描电子显微镜照片如图2所示。图1中的白点显示的为杂质，从图2中可以明显看出，经过纯化后，几乎看不到杂质。
本实例中，碳纳米管纤维的长度可以在1～20cm之间变化，比如1、5、10、15或20cm等，碳纳米管纤维越长，其电阻越大，所施加的电压也相应增加。
实施例2，本实施例中碳纳米管通电纯化的方法如下：截取长度5cm，直径92μm均匀的碳纳米管纤维，将其两端粘在导电胶上，涂覆银胶，并使纤维架空，用万用表测量纤维的电阻为70Ω，根据电阻选择合适的电压值83V通电，通电时长约0.5-1s，防止通电时间过长或者电压电流过大致使碳纳米管纤维烧断；取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后放在鼓风干燥箱中80℃干燥3-5h。
本实施例中，碳纳米管纤维的直径可以为30～300μm，比如30或100或200或300μm，碳纳米管纤维直径越大，其电阻越小，相应施加的电压也减小。
实施例3，本实施例中碳纳米管通电纯化的方法如下：截取长度7cm，直径80μm均匀的碳纳米管纤维，将其两端粘在导电胶上，涂覆银胶，并使纤维架空，用万用表测量纤维的电阻为65Ω，根据电阻选择合适的电压值110V通电，通电时长约0.5-1s，防止通电时间过长或者电压电流过大致使碳纳米管纤维烧断；取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后放在鼓风干燥箱中80℃干燥3-5h。
实施例4，本实施例中碳纳米管通电纯化的方法如下：截取长度10cm，直径123μm均匀的碳纳米管纤维，将其两端粘在导电胶上，涂覆银胶，并使纤维架空，用万用表测量纤维的电阻为113Ω，根据电阻选择合适的电压值135V通电，通电时长约0.5-1s，防止通电时间过长或者电压电流过大致使碳纳米管纤维烧断；取下碳纳米管纤维放入酸中浸泡6h；用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后放在鼓风干燥箱中80℃干燥3-5h。
以下的实施例5-8用于说明本发明经过通电的碳纳米管纤维的酸的处理时间相当短，使用实施例1中的样品。
实施例5-8
将实施例1中，经过通电的长度为2.5cm的碳纳米管纤维取下，放入酸中浸泡数个小时，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后放在鼓风干燥箱中80℃干燥3-5h。如表1所示。
表1
名称 酸的种类 酸的浓度(Mol/L) 反应时间(h)
实施例5 盐酸 1 6
实施例6 盐酸 0.5 6
实施例7 王水 1 4
实施例8 硝酸 1 6
本申请通过加载恒定电压，使无定形碳和碳纳米颗粒炭化，并且使碳纳米管纤维内部的铁催化颗粒氧化形成氧化铁颗粒，这些颗粒均匀分布于碳纳米管束的间隙之中，之后将通电的碳纳米管纤维依次放入稀盐酸和双氧水中浸泡。本发明所提供的纯化碳纳米管纤维的方法缩短了酸等溶液处理的时间，有效提高了碳纳米管的纯化效率；纯化后的致密度有所提高，表面和内部都极为干净，并且纯化后的电导率提高大约4倍。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (2)

1.一种碳纳米管纤维纯化方法，其特征在于是按照下述步骤进行的：
（1）将导电胶粘在衬底之上，碳纳米管纤维的两端粘在导电胶上，涂覆银胶，并使碳纳米管纤维架空；
（2）待银胶晾干后测量碳纳米管纤维的电阻，根据电阻选择合适的电压值通电0.5~1s；
（3）取下碳纳米管纤维放入酸中浸泡6h，用去离子水清洗过后放入双氧水中浸泡6h；用去离子水浸泡24h，最后在80℃干燥3-5h；
步骤（1）中碳纳米管纤维的长度在1-20cm；
步骤（1）中碳纳米管纤维的直径为30~300μm；
所述碳纳米管纤维是采用CCVD法制得的直径均匀的碳纳米管纤维。
2.根据权利要求1 所述的碳纳米管纤维纯化方法，其特征在于步骤（3）中酸溶液为盐酸、硝酸、王水或硫酸。
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