CN102888673B - 一种纳米碳纤维的制备方法 - Google Patents
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Abstract
本发明的目的在于提供一种纳米碳纤维的制备方法，其特征在于：以碳酸根离子为碳源，在熔融盐中，通过恒电流或恒电位直接还原碳酸根离子获得纳米碳纤维。该方法具有操作工艺简单、效率高和成本低等特点。
Description
技术领域
本发明涉及纳米碳纤维制备技术，特别提供了一种在不锈钢等金属基体表面直接制备纳米碳纤维的新方法，使得纳米碳纤维的制备更加简单、易行。
背景技术
自1991年日本NEC公司的饭岛(S.Iijima)博士发现纳米碳管以来，纳米碳管和纳米碳纤维受到广泛关注。纳米碳管是由碳原子形成的石墨烯片层卷成的无缝、中空的管体。一般可分为单壁纳米碳管（single-walled carbon nanotube）和多壁纳米碳管（Multi-walled carbon nanotube）。由于纳米碳管的直径很小、长径比大，故可视为准一维纳米材料。理论预测和实验研究发现纳米碳管具有奇特的电学性能，超高的力学性能和纳米尺度形成的细微结构。此外，纳米碳管还具有很好的吸附特性，如高效储存氢气。这些特异性能预示着纳米碳管在众多领域具有广阔的应用前景，如纳米尺度器件，制造纳米材料的模板，电子材料和器件，复合材料的增强剂，贮能、贮气材料和催化剂材料等。全球最大的计算机制造商IBM公司宣布他们已用纳米碳管研制出一种性能优于目前最好的硅半导体芯片的晶体管，该晶体管是制造更小巧、速度更快的计算机的关键。纳米碳纤维在结构、性能和应用等方面与纳米碳管相似，但其直径明显大于纳米碳管。
自发现纳米碳管以来，已形成了多种制备纳米碳管、纳米碳纤维的方法。根据碳源来源的不同大致可分为碳蒸发法，含碳气体及烃类或有机金属化合物的催化热解，固相热解法，电化学法，含碳无机物转化法，环芳构化形成简状齐聚物，扩散火焰法和低压烃火焰法等。
发展简单、安全、低成本的纳米碳管、纳米碳纤维的制备方法对于其工业化应用具有积极意义。
发明内容
本发明的目的在于提供一种纳米碳纤维的制备方法，该方法具有操作工艺简单、效率高和成本低等特点。
本发明具体提供了一种纳米碳纤维的制备方法，其特征在于：采用熔盐电化学方法在金属表面直接沉积纳米碳纤维。
本发明提供的纳米碳纤维制备方法, 其特征在于：以碳酸根离子为碳源，在熔融盐中，通过恒电流或恒电位直接还原碳酸根离子获得纳米碳纤维。
本发明提供的纳米碳纤维制备方法, 其特征在于：制备纳米碳纤维所需的熔盐体系必须为含碳酸盐的纯碳酸盐或碳酸盐与氯化物盐的混合盐。其中碳酸盐最好为碳酸钠、碳酸钾、碳酸锂中的一种或多种，氯化物盐最好为氯化锂、氯化钠、氯化钾、氯化钙中的一种或多种。混合盐体系可以是二元或多元的，但混合盐中必须含有至少一种碳酸盐，且各种盐的配比必须保证混合盐的熔点低于电沉积温度。
本发明提供的纳米碳纤维制备方法, 其特征在于：纳米碳纤维沉积温度为650-800℃。为避免在合成过程中发生氧化等副反应，需要在氩气等保护气氛中进行。
本发明提供的纳米碳纤维制备方法, 其特征在于：该方法制备纳米碳纤维所需盐的组份及组份含量必须使混合盐的熔点低于电沉积温度。
本发明提供的纳米碳纤维制备方法，其特征在于：恒电流沉积纳米碳纤维的电流密度为35~50mA/cm2。 恒电位沉积纳米碳纤维的电压为1.8~3V。
本发明提供的纳米碳纤维制备方法, 其特征在于：制备纳米碳纤维可以采用二电极体系，也可以采用三电极体系。阴极可以是不锈钢、镍、铁等金属(沉积纳米碳纤维)，阳极可以是石墨，也可以是铂、金等其它金属。
本发明提供的纳米碳纤维制备方法，其特征在于：纳米碳纤维可以是直的，也可以是螺旋状的，其直径和形态通过沉积电流和电压进行调节。
附图说明
图1 电沉积纳米碳纤维实验装置结构图，其中1热电偶；2氩气出气口; 3阴极；4阳极；5氩气进气口；6水冷套；7耐热钢反应室；8高温电阻炉；9氧化铝坩埚；10熔融盐；
图2 在750℃熔融(0.62Li,0.38K)2CO3（摩尔比）中，恒电流电流密度为38mA/cm2条件下获得的纳米碳纤维的形貌图。
具体实施方式
实施例1
采用双电极体系(实验装置如图1所示)，即以石墨为阳极，304不锈钢为阴极。纳米碳纤维制备在由碳酸锂和碳酸钾组成的混合熔盐中进行，其中碳酸锂：碳酸钾=62：38（摩尔比）。沉积温度为750℃，沉积电流密度为38mA/cm2，沉积时间为2小时。最终在不锈钢表面获得了大量纳米碳纤维。图2是在共晶碳酸锂-碳酸钾熔盐中获得的纳米碳纤维形貌图。其中碳纤维可以是直的，也可以是螺旋结构的。
实施例2
采用双电极体系，即以石墨为阳极，304不锈钢为阴极。纳米碳纤维制备在碳酸锂-碳酸钾混合熔盐中进行，其中碳酸锂：碳酸钾=62：38（摩尔比）。沉积温度为650℃，沉积电流密度为45mA/cm2，沉积时间为2小时。最终在不锈钢表面获得了大量纳米碳纤维。
实施例3
采用双电极体系，即以石墨为阳极，304不锈钢为阴极。纳米碳纤维制备在碳酸锂-碳酸钾-氯化钾混合熔盐（碳酸锂：碳酸钾：氯化钾=37：23：40（摩尔比））中进行。沉积温度为800℃，沉积电流密度为35mA/cm2，沉积时间为2小时。最终在不锈钢表面获得了大量纳米碳纤维。
实施例4
采用双电极体系，即以石墨为阳极，镍为阴极。纳米碳纤维制备在碳酸锂和碳酸钾的混合熔盐（碳酸锂：碳酸钾=43：57（摩尔比））中进行。沉积温度为750℃，沉积电流密度为35mA/cm2。最终在镍表面获得了大量纳米碳纤维。
实施例5
采用双电极体系，即以石墨为辅助电极，铁为工作电极。纳米碳纤维制备在碳酸锂和碳酸钾的混合熔盐（碳酸锂：碳酸钾=62：38（摩尔比））中进行。沉积温度为700℃，沉积电流密度为38mA/cm2。最终在铁表面获得了大量纳米碳纤维。
实施例6
采用双电极体系，即以石墨为阳极，304不锈钢阴极。纳米碳纤维制备在碳酸锂和碳酸钾的混合熔盐（碳酸锂：碳酸钾=70：30（摩尔比））中进行。沉积温度为750℃，沉积电流密度为42mA/cm2，沉积时间为1.5小时，最终在不锈钢表面获得了大量纳米碳纤维。
实施例7
采用三电极体系，即以石墨为辅助电极，304不锈钢为工作电极，金电极为参比电极。纳米碳纤维制备在碳酸锂和碳酸钾的混合熔盐（碳酸锂：碳酸钾=62：38（摩尔比））中进行。沉积温度为750℃，沉积电压为1.8V，沉积时间为两小时，最终在不锈钢表面获得了纳米碳纤维。
实施例8
采用三电极体系，即以石墨为辅助电极，镍为工作电极，金电极为参比电极。纳米碳纤维制备在碳酸锂和碳酸钾的混合熔盐（碳酸锂：碳酸钾=43：57（摩尔比））中进行。沉积温度为700℃，沉积电压为2.3V，沉积时间为30分钟，最终在镍表面获得了纳米碳管纤维。
实施例9
采用双电极体系，即以铂为阳极，304不锈钢为阴极。纳米碳纤维制备在碳酸锂和碳酸钾的混合熔盐（碳酸锂：碳酸钾=43：57（摩尔比））中进行。沉积温度为700℃，沉积电流密度为50mA/cm2。最终在不锈钢表面获得了大量纳米碳纤维。
Claims (5)
1.一种纳米碳纤维的制备方法，其特征在于：采用熔盐电化学方法在金属表面直接沉积纳米碳纤维；
其中，纳米碳纤维沉积温度为650-800℃；恒电流沉积纳米碳纤维的电流密度为35～50mA/cm2，恒电位沉积纳米碳纤维的电压为1.8～3V；以碳酸根离子为碳源，在熔融盐中，通过恒电流或恒电位直接还原碳酸根离子获得纳米碳纤维；
纳米碳纤维沉积在金属上，所述金属为不锈钢或铁。
2.按照权利要求1所述纳米碳纤维的制备方法，其特征在于：用于电沉积的熔盐体系既可以是纯碳酸盐，也可以是碳酸盐与氯化物盐的混合物。
3.按照权利要求2所述纳米碳纤维的制备方法，其特征在于：所述碳酸盐为碳酸钠、碳酸钾、碳酸锂中的一种或多种，氯化物盐为氯化锂、氯化钠、氯化钾、氯化钙中的一种或多种。
4.按照权利要求2所述纳米碳纤维的制备方法，其特征在于：混合盐体系可以是二元或多元的，但混合盐中必须含有至少一种碳酸盐，且各种盐的配比必须保证混合盐的熔点低于电沉积温度。
5.按照权利要求1所述纳米碳纤维的制备方法，其特征在于：纳米碳纤维可以是直的，也可以是螺旋状的，其直径和形态通过沉积电流和电压进行调节。
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| KR20080006814A (ko) * | 2006-07-13 | 2008-01-17 | 충남대학교산학협력단 | 전기도금에 의한 탄소나노튜브 전계방출소자의 제조 방법및 그로부터 제조된 탄소나노튜브 전계방출소자 |
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| Electrochemical formation of carbon nano-powders with various porosities in molten alkali carbonates;Kawamura H,et al;《Electrochimica Acta》;20091231;第54卷(第19期);第4566-4573页 * |
| Ingram M,et al.The electrolytic deposition of carbon from fused carbonate.《Electrochimica Acta》.1966,第11卷第1629-1639页. * |
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| The electrolytic deposition of carbon from fused carbonate;Ingram M,et al;《Electrochimica Acta》;19661231;第11卷;第1629-1639页 * |
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