CN107190367A - 氮硫共掺杂多孔碳纤维的制备方法 - Google Patents
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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Abstract
本发明公开了一种以棉花为碳源制备机械性能良好的超级电容器用氮硫共掺杂多孔碳纤维的制备方法。具体涉及一种以棉花为原料,通过碳化、氮硫的引入,结合化学活化法制备机械性能良好的超级电容器用多孔碳纤维的新方法。本发明包括具体步骤如下:首先将棉花高温碳化为纤维,将碳纤维与活化试剂、氮硫化合物按一定质量比混合,再向其中加入适量蒸馏水浸渍一定时间后烘干,而后在管式炉中活化处理一定时间,固体洗涤、干燥,得到超级电容器用氮硫共掺杂多孔碳纤维。
Description
技术领域
本发明涉及一种氮硫共掺杂多孔碳纤维的制备方法,具体涉及一种首先将棉花碳化制备碳纤维,再将其与氮、硫源、活化试剂混合,高温处理制备超级电容器用氮硫共掺杂多孔碳纤维的新方法。
背景技术
超级电容器由于具有充放电速率快、高能力密度和功率密度、优异的循环稳定性以及高稳定性而成为科研工作者们广泛关注的储能设备。根据能源储存机理不同超级电容器可分为双电层和赝电容两种电容器,电极材料是决定超级电容器性能的关键因素之一。多孔碳由于化学性质稳定、比表面积大、孔隙发达、孔径可调等众多优点而被广泛应用于超级电容器电极材料。目前,应用于超级电容器的多孔碳材料有很多种,如球形碳,颗粒状碳,纤维状碳等。其中,多孔碳纤维质量轻,拉伸强度和热稳定性优异,其表面分布着丰富的孔隙结构,可增大其与电解质的接触面积,缩短离子传输路径。提高储能效率,这些性质促进了多孔碳纤维被广泛研究。同时研究成果表明,杂原子(N、B、P、S、F、Ni、Co等)掺杂是行之有效的提升碳材料电化学性能的路径。例如,在电容器电极材料领域,氮硫元素的掺杂可以通过影响碳材料的电子接收或供给特性,影响双电层的形成。另外,氮元素的掺杂还可以增强碳材料的导电性,促进离子的快速迁移,引入赝电容,从而提高碳材料在超级电容器电极材料上的表现。因此制备氮硫共掺杂的多孔碳材料具有重要的研究价值。
专利CN105931855A公开了一种超级电容器用氮硫共掺杂碳-聚苯胺复合材料的合成方法。其涉及水溶液法合成聚(苯胺-唆吩)复合材料,高温热解法合成氮硫共掺杂碳材料,化学氧化法合成氮硫共掺杂碳-聚苯胺复合材料并用于超级电容器的研究,包括以下步骤:制备聚(苯胺一唆吩)复合材料、制备氮硫共掺杂碳材料、制备氮硫共掺杂碳-聚苯胺复合材料电极。本发明的有益效果是:复合材料拥有更好的导电性,更小的电极电阻,更好的电容性能,且表现出更好的循环稳定性。专利CN105776178A公开了一种利用煤直接液化重质有机分制备的氮硫共掺杂多孔炭及其制备方法和应用。该方法包括如下步骤:(1)将煤直接液化重质有机物研磨成粉末,经过经基化、梭酸化或磺化得到亲水性第一产物;(2)将第一产物与甲醛和硫脉的混合物反应得到含氮、硫的第二产物;(3)将第二产物与一定比例的镁源机械混合,而后放置于炭化炉中炭化,得到氧化镁与氮硫共掺杂多孔炭混合物;经酸洗去除氧化镁得到氮硫共掺杂多孔炭。本发明制备的氮硫共掺杂多孔炭具有优异的电化学性能,是一种高性能的超级电容器电极材料。专利CN105084358A公开了一种用于超级电容器的氮硫共掺杂活性炭的制备方法。氮硫共掺杂活性炭主要由下述组合物按其重量份数比配比,经炭化和活化工艺而制取;所述的组合物为:大发梧桐科植物果实经炭化后粉状1-2份;碱性活化剂1-4份;该制备方法包括如下步骤,(1)炭化:①浸泡:②水热处理:③离心滤水;④烘干;⑤研磨;(2)活化:①采用阶段式升温和保温:②缓慢降温;③盐酸溶液浸泡:④水洗;⑤烘干;烘干后即成为超级电容器用氮硫共掺杂活性炭。专利CN106492749A公开了一种氮、硫共掺杂微孔-介孔碳微球的制备方法。本发明涉及一种氮、硫共掺杂微孔-介孔碳微球的制备方法。将氨基酚、甲醛溶液、L-半肤氨酸、表面活性剂、硅溶胶、乙醇和水按一定质量比混合。将水和乙醇在20-35℃下混匀并将其余原料依次加入其中,反应24h后于100℃水热处理24h,在氮气气氛中,以2-10℃/min的升温速率从室温升到600-900℃炭化,用NaOH除去二氧化硅,得到氮、硫共掺杂介孔碳微球。
以上专利原料多为有机化合物,合成过程相对复杂,制备的氮硫共掺杂的碳材料并非纤维状,因此以可再生的生物质为原料制备氮硫共掺杂的多孔碳纤维具有重要的研究意义。棉花是一种天然的具有纤维结构的生物质资源,碳化后仍能保持纤维结构,同时具有良好的机械性能。因此,以棉花为原料,通过碳化、活化、氮硫共掺杂的方式制备具有高比表面积、良好机械性能的超级电容器电极材料具有一定研究价值。
本专利是以棉花为原料,将其碳化为纤维,再通过氮、硫的引入,结合化学活化制备机械性能良好的超级电容器用氮硫共掺杂多孔碳纤维。本路线原料来源广泛、合成方法简便,通过调节活化试剂和氮硫的加入量控制多孔碳纤维的孔隙发达程度和氮硫掺杂量,最终制备机械性能良好的超级电容器用氮硫共掺杂多孔碳纤维。
发明内容
本发明目的是提供一种以棉花为碳源制备机械性能良好的超级电容器用氮硫共掺杂多孔碳纤维的新方法。
本发明首先将棉花700~950℃碳化为纤维,将碳纤维与活化试剂、硫脲按质量比1∶2∶2~1∶7∶6(g/g/g)混合,向其中加入适量蒸馏水混合均匀,将混合物浸渍12h后在105℃烘箱中干燥5h,将混合物在700~1000℃管式炉中活化处理0.5~3h,固体洗涤、干燥,得到的氮硫共掺杂多孔碳纤维进行电化学性能测试。
本发明的特征在于:所述活化剂为碳酸氢钾和氢氧化钾的混合物或碳酸氢钾和氢氧化钠的混合物。
具体实施方式
实施例1:首先将棉花在管式炉中850℃下碳化1h,将得到的碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶2)、硫脲按质量比1∶5∶4(g/g/g)混合,向其中加入适量蒸馏水混合均匀,将混合物浸渍14h后在105℃烘箱中干燥5h,将混合物在800℃管式炉中活化处理1.5h,固体洗涤、干燥,得到的氮硫共掺杂多孔碳纤维进行电化学性能测试,以6mol/L的氢氧化钾为电解液,测得比容量为338F/g,循环5000次容量保持率为98%左右。
实施例2:改变碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶2)、硫脲的质量比1∶4∶5(g/g/g),其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为315F/g,循环5000次容量保持率为97%左右。
实施例3:改变碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶2)、硫脲的质量比1∶6∶3(g/g/g),其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为323F/g,循环5000次容量保持率为97%左右。
实施例4:改变混合物800℃管式炉中活化处理时间为2h,其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为309F/g,循环5000次容量保持率为97%左右。
实施例5:改变混合物800℃管式炉中活化处理时间为1h,其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为318F/g,循环5000次容量保持率为96%左右。
实施例6:改变混合物在管式炉中活化处理温度为900℃,活化时间为1h,其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为298F/g,循环5000次容量保持率为97%左右。
实施例7:改变碳纤维与活化试剂(KHCO3∶NaOH的质量比为1∶3)、硫脲的质量比1∶5∶4(g/g/g),将混合物在800℃管式炉中活化处理2h,其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为315F/g,循环5000次容量保持率为97%左右。
实施例8:改变碳纤维与活化试剂(KHCO3∶NaOH的质量比为1∶3)、硫脲的质量比1∶6∶3(g/g/g),将混合物在850℃管式炉中活化处理1.5h,其他条件同实施例1,得到的氮硫共掺杂多孔碳纤维的比电容为328F/g,循环5000次容量保持率为97%左右。
Claims (2)
1.一种超级电容器用氮硫共掺杂多孔碳纤维的制备方法,其具体步骤如下:首先将棉花700~950℃碳化为纤维,将碳纤维与活化试剂、硫脲按质量比1∶2∶2~1∶7∶6(g/g/g)混合,向其中加入适量蒸馏水混合均匀,将混合物浸渍12h后在105℃烘箱中干燥5h,将混合物在700~1000℃管式炉中活化处理0.5~3h,固体洗涤、干燥,得到的氮硫共掺杂多孔碳纤维进行电化学性能测试。
2.一种如权利要求1所述的氮硫共掺杂多孔碳纤维的制备方法,其特征在于:所述活化剂为碳酸氢钾和氢氧化钾的混合物或碳酸氢钾和氢氧化钠的混合物。
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