CN106206034A - 一种用于线状光电能量器件的多功能电极及其制备方法 - Google Patents
一种用于线状光电能量器件的多功能电极及其制备方法 Download PDFInfo
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Abstract
本发明属于线状光电能量器件的技术领域,尤其涉及一种用于线状光电能量器件的多功能电极及其制备方法;解决的技术问题为:提供一种性能较高、制备简单、可以应用在各式各样的线状能量器件中的多功能电极及其制备方法;采用的技术方案为:一种用于线状光电能量器件的多功能电极,包括:碳纤维,所述碳纤维的外表面具有TiO2涂层,所述TiO2涂层上具有MoS2纳米薄膜;本发明适用于电极制造领域。
Description
技术领域
本发明属于线状光电能量器件的技术领域,尤其涉及一种用于线状光电能量器件的多功能电极及其制备方法。
背景技术
随着化石能源的日益枯竭,发展各种可再生能源已成为人类最紧迫的任务。它关系到了我们人类能否继续发展乃至继续生存,其重要性是不言而喻的。在此背景下,研究者们提出了各种各样的能量器件,比如可以将太阳能转换为电能的太阳能电池、可以将电能存储起来以便我们随时使用的锂离子电池和超级电容器、以及无污染的的氢氧燃料电池等。到目前为止,这些能源器件主要是以平面结构存在,比如:第三代太阳能电池主要是以FTO导电玻璃为基底,锂离子电池和超级电容器主要是以不锈钢的外壳包装等。我们知道,这样的结构使得它们在我们的实际生活应用中很有限,不能够满足我们生活中的很多要求,比如:柔性,方便携带等。因此,近来研究者们提出了柔性线状能量器件的概念,比如:柔性线状染料敏化太阳能电池、柔性线状超级电容器、柔性线状锂离子电池等(Xue Y.etal.,Sci.Adv.2015,1,1400198.)。这些柔性线状能量器件的提出,很好地解决了传统平面结构的不足,然而却带来了新的问题,其中最主要的问题便是柔性线状能量器件的性能比传统平面结构的能量器件性能低。我们知道,与能量器件性能息息相关的主要是能量器件的电极材料,因此,制备更加适合柔性能量器件的电极材料、以获得与传统平面结构的能量器件可以相比拟的性能,是我们研究柔性线状能量器件最主要的任务。
由于有着高导电性,高强度,质量轻等特点,线状碳材料(包括碳纳米管纤维、石墨纤维、碳纤维等)被视为很有前途的一种能量器件电极材料。然而,到目前为止,由于这些线状碳材料自身在电化学活性方面的缺点,使得它们在实际的应用中受到了很大的阻碍。比如,Zou和他的合作者们曾经用碳纤维作为对电极材料而制备出线状染料敏化太阳能电池,然而,该电池的光电转换效率仅仅只有1%左右。随后,他们用CoNi2S4活性材料来修饰该碳纤维,虽然效率上升到了7%左右,然而相对于目前平面结构的染料敏化太阳能电池的效率而言,该效率还有待继续提高(Chen L,et al.,Nano Energy,2015,11,697-703.)。再比如,在柔性线状超级电容器里,Lee和他的合作者们利用全碳的电极材料,制备了全固态的柔性线状超级电容器。然而,当扫速从2mV/s上升到200mV/s的时候,该电容器的电容只剩下了46%,也就是说该电容器的比容量相对于传统平面的超级电容器而言非常的低(Le V.T.,et al.,ACS Nano,2013,7,5940.)。因此,寻找更加合适的活性材料生长在碳纤维电极上,以获得高性能的柔性线状能量器件是现在我们急需解决的问题。
再者,我们前面提到柔性线状能量器件包括有能量转换器件(比如柔性线状染料敏化太阳能电池)和能量存储器件(比如柔性纤维超级电容器和柔性纤维锂离子电池)。如果我们将这两种器件合为一个自行充电能量器件,这将会大大减少其制备的成本,而且可以将能量转换器件得到的电能暂时的存储起来,以便我们需要的时候再使用。这样的概念,到目前为止在传统的平面结构能量器件中已经有一些工作的报道,在这些报道中,它们将太阳能电池和超级电容器或锂离子电池连接起来,组成自行充电能量器件(Cohn A.P.etal.,Nano Lett.2015,15,2727.)。然而,正如我们上面提到的,由于这些自行充电能量器件是由传统平面结构的能量器件组成的,因此,它们仍然具有传统平面能量器件所具有的缺乏柔性、便携的缺点。所以,如果我们能够将柔性线状能量器件组装在一起,组成柔性线状自充电能量器件,将会大大提高其在我们实际生活中的应用。当然,到目前为止,已经有少数几项工作报道了关于这方面的研究(Fu Y.P.et al.,Energy Environ.Sci.2013,6,805.)。然而,同样的,由于电极材料的限制,其性能相对于传统平面结构的性能还是比较低,因此,探索并且寻找一种具有多功能的柔性线状电极材料,使其可以同时在柔性线状能量转换和能量存储器件中使用,是我们制备柔性线状自行供电能量器件的首要任务。
综上,对于目前的柔性线状能量器件而言,其相对较低的性能还存在着很大的提升空间,而提高其性能最主要的便是电极材料的制备。因此,制备高性能的电极材料是目前我们制备高性能线状能量器件最主要的任务。同时,对于不同的线状能量器件,其对电极材料对性能方面有着不同的要求,而制备出一种可以具有各种线状能量器件所需要的性能的多功能电极材料,以便使其应用在各种线状能量器件,以及线状自充电能量器件中也将是我们制备线状器件目前面临的一个问题。
发明内容
本发明克服现有技术存在的不足,所要解决的技术问题为:提供一种性能较高、制备简单、可以应用在各式各样的线状能量器件中的多功能电极及其制备方法。
为了解决上述技术问题,本发明采用的技术方案为:一种用于线状光电能量器件的多功能电极,包括:碳纤维,所述碳纤维的外表面具有TiO2涂层,所述TiO2涂层上具有MoS2纳米薄膜。
相应地,一种用于线状光电能量器件的多功能电极的制备方法,包括以下步骤:
a)配制TiCl4水溶液;
b)将碳纤维浸泡于TiCl4水溶液中,以使碳纤维的外表面上生长一层TiO2涂层;
c)将碳纤维从TiCl4水溶液中取出,清洗干净;
d)配制生长MoS2的前驱体溶液;
e)将外表面已具有TiO2涂层的碳纤维置于聚四氟乙烯内衬中,同时将配制好的生长MoS2的前驱体溶液倒入内衬中,将反应釜放入马弗炉中进行反应,以使碳纤维外表面的TiO2涂层上生长一层MoS2纳米薄膜;
f)将反应完的碳纤维取出,清洗干净。
可选地,所述步骤d)中的前驱体溶液包括:0.03~0.09g的Na2MoO4、0.08~0.16g的C2H5NS,以及20~40mL的超纯水。
可选地,所述步骤b)中,将碳纤维浸泡于TiCl4水溶液中后,将其置于60~80℃的环境下,并保持1~2个小时。
可选地,所述步骤e)中,外表面已具有TiO2涂层的碳纤维置于聚四氟乙烯内衬中,同时将配制好的生长MoS2的前驱体溶液倒入内衬中,将反应釜放入马弗炉中在180~240℃的条件下进行反应20~40个小时。
可选地,所述步骤b)中,将碳纤维浸泡于TiCl4水溶液之前,先用丙酮、乙醇和水依次将碳纤维进行清洗。
可选地,所述步骤a)中,TiCl4水溶液的浓度范围为0.2~0.6mmol/L,并且配制好TiCl4水溶液后,将TiCl4水溶液搅拌0.5~1个小时。
可选地,所述步骤c)中,将碳纤维从TiCl4水溶液中取出后,用乙醇和水清洗干净。
可选地,所述步骤f)中,将反应完的碳纤维取出后,用乙醇和水清洗干净。
可选地,所述步骤e)中,聚四氟乙烯内衬的容积范围为50~80mL。
本发明与现有技术相比具有以下有益效果:
本发明中的多功能电极是在碳纤维的外表面先生长了一层TiO2涂层,再在TiO2涂层上生长一层MoS2纳米薄膜,首先,由于碳纤维的疏水性较强,直接将MoS2纳米薄膜制作在碳纤维上会使得做出来的电极性能较差,如果在生长MoS2纳米薄膜之前先在碳纤维的外表面生长一层TiO2涂层,由于TiO2具有亲水性,它能够改进碳纤维的疏水表面,进而能够很好地负载MoS2纳米薄膜,其次,TiO2是一个很好的电子捕获体,MoS2的电子在光电或者电化学的反应过程中会转移到TiO2上,因而制作出来的电极其性能较高;本发明中多功能电极的制备方法简单,而且成本非常低,为其在实际生活中的应用创造了有利的条件,该多功能电极还可以应用在各式各样的线状能量器件中,比如线状染料敏化太阳能电池、线状超级电容器、线状锂离子电池和线状电解水制氢等,解决了目前把所有能量器件结合在一起的困难,而且,该多功能电极可以同时应用在线状染料敏化太阳能电池和线状超级电容器中,解决了太阳能电池产生的电量必须即时即用的不足,满足了人们随时使用其产生的电能的需求。
附图说明
下面结合附图对本发明做进一步详细的说明;
图1为本发明实施例提供的在碳纤维上生长出MoS2纳米薄膜的SEM图;
图2为本发明实施例提供的单根生长有MoS2纳米薄膜的碳纤维的SEM图以及对应的元素Mapping图;
图3为本发明实施例提供的在碳纤维上生长出MoS2纳米薄膜的TEM图;
图4为本发明实施例提供的生长有MoS2纳米薄膜的碳纤维的XPS图谱;
图5为将本发明中的多功能电极应用在柔性线状染料敏化太阳能电池中时该太阳能电池的光电性能表征图;
图6为将本发明中的多功能电极应用在柔性线状超级电容器中时该超级电容器的电化学性能表征图;
图7为将本发明中的多功能电极应用在柔性线状锂离子电池中时该锂离子电池的电化学性能表征图;
图8为将本发明中的多功能电极作为工作电极电解水制氢的电化学性能表征图;
图9为将本发明中的多功能电极作为柔性线状染料敏化太阳能电池和柔性线状超级电容器的公共电极而制备出来的柔性线状自行供电能量纤维的示意图及性能表征图;
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,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,所描述的实施例是本发明的一部分实施例,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作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。
一种用于线状光电能量器件的多功能电极,可包括:碳纤维,所述碳纤维的外表面具有TiO2涂层,所述TiO2涂层上具有MoS2纳米薄膜。
对应地,一种用于线状光电能量器件的多功能电极的制备方法,可包括以下步骤:
a)配制TiCl4水溶液;
b)将碳纤维浸泡于TiCl4水溶液中,以使碳纤维的外表面上生长一层TiO2涂层;
c)将碳纤维从TiCl4水溶液中取出,清洗干净;
d)配制生长MoS2的前驱体溶液;
e)将外表面已具有TiO2涂层的碳纤维置于聚四氟乙烯内衬中,同时将配制好的生长MoS2的前驱体溶液倒入内衬中,将反应釜放入马弗炉中进行反应,以使碳纤维外表面的TiO2涂层上生长一层MoS2纳米薄膜;
f)将反应完的碳纤维取出,清洗干净。
具体地,所述步骤d)中的前驱体溶液可包括:0.03~0.09g的Na2MoO4、0.08~0.16g的C2H5NS,以及20~40mL的超纯水。
更具体地,前驱体溶液可包括:0.06g的Na2MoO4、0.12g的C2H5NS,以及30mL的超纯水,该前驱体溶液可制备出来的超薄、多孔的MoS2纳米薄膜,使的整个多功能电极具有较好的性能。
具体地,所述步骤b)中,将碳纤维浸泡于TiCl4水溶液中后,将其置于60~80℃的环境下,并保持1~2个小时。
更具体地,将碳纤维浸泡于TiCl4水溶液中后,将其置于70℃的环境下,并保持1个小时。
具体地,所述步骤e)中,将外表面已具有TiO2涂层的碳纤维置于聚四氟乙烯内衬中,同时将配制好的生长MoS2的前驱体溶液倒入内衬中,将反应釜放入马弗炉中在180~240℃的条件下进行反应20~40个小时。
更具体地,将反应釜放入马弗炉中在200℃的条件进行反应30个小时。
具体地,所述步骤b)中,将碳纤维浸泡于TiCl4水溶液之前,先用丙酮、乙醇和水依次将碳纤维进行清洗。
具体地,所述步骤a)中,TiCl4水溶液的浓度范围为0.2~0.6mmol/L,并且配制好TiCl4水溶液后,将TiCl4水溶液搅拌0.5~1个小时。
更具体地,TiCl4水溶液的浓度范围为0.4mmol/L,并且配制好TiCl4水溶液后,将TiCl4水溶液搅拌半个小时,该TiCl4水溶液制备出来的TiO2涂层较薄,约为几个纳米厚。
具体地,所述步骤c)中,将碳纤维从TiCl4水溶液中取出后,用乙醇和水清洗干净。
具体地,所述步骤f)中,将反应完的碳纤维取出后,用乙醇和水清洗干净。
具体地,所述步骤e)中,聚四氟乙烯内衬的容积范围为50~80mL。
更具体地,聚四氟乙烯内衬的容积范围为50mL。
图1为本发明实施例提供的在碳纤维上生长出MoS2纳米薄膜的SEM图,其中图1a为整体形貌SEM图,图1b、图1c分别为不同放大倍数下的表面形貌细节SEM图,图2为本发明实施例提供的单根生长有MoS2纳米薄膜的碳纤维的SEM图以及对应的元素Mapping图,图3为本发明实施例提供的在碳纤维上生长出MoS2纳米薄膜的TEM图。
图4为本发明实施例提供的生长有MoS2纳米薄膜的碳纤维的XPS图谱,如图4所示,对长有MoS2纳米薄膜的碳纤维利用X射线光电子能谱(XPS)进行了元素表征,结果显示,该材料中含有元素碳、钛、氧、钼和硫。
将长有MoS2纳米薄膜的碳纤维作为柔性线状染料敏化太阳能电池的对电极,制备出了柔性线状染料敏化太阳能电池,紧接着,对该柔性线状染料敏化太阳能电池的性能进行了测试,如图5所示,图5为将本发明中的多功能电极应用在柔性线状染料敏化太阳能电池中时该太阳能电池的光电性能表征图。图5a给出了柔性线状染料敏化太阳能电池的原理图。图5b给出了阳极氧化制备出的二氧化钛纳米管阵列图。图5c给出了该柔性线状染料敏化太阳能电池有着很好的柔性特性,可以按需要折叠成各种各样的形状。图5d给出了一根长度为17cm的柔性线状染料敏化太阳能电池,其长度可以根据实际的需求去制造,可长可短。图5e给出了长有MoS2纳米薄膜的碳纤维在电解液中的循环伏安扫描(CV)图像,其中,CF@TiO2@MOS2表示长有MoS2纳米薄膜的碳纤维。为了对比性能,测试了其他材料的CV图像,比如长有TiO2纳米颗粒的碳纤维(CF@TiO2)、没有做任何处理的碳纤维(CF)、以及铂丝(Pt)。图中显示,CF@TiO2@MOS2对电解液的性能最好。图5f给出了CV图中左边一对峰值随着扫描速度的变化,同样显示CF@TiO2@MOS2对电解液的性能比铂的性能还要好。图5g给出了柔性线状染料敏化太阳能电池的电流-电压图,图中显示基于CF@TiO2@MOS2为对电极的柔性线状染料敏化太阳能电池的性能最优,其光电转换效率达到了9.5%。图5h给出了这些柔性线状染料敏化太阳能电池阻抗谱,从中可以看出基于CF@TiO2@MOS2为对电极的柔性线状染料敏化太阳能电池的内阻最小。图5i给出了基于CF@TiO2@MOS2为对电极的柔性线状染料敏化太阳能电池在不同弯曲角度下的光电转换性能,图中显示该柔性线状电池有着很好的柔性。图5j给出了基于CF@TiO2@MOS2为对电极的柔性线状染料敏化太阳能电池在不同弯曲次数下的光电转换性能。该图进一步说明了基于CF@TiO2@MOS2为对电极的柔性线状染料敏化太阳能电池有着很好的柔性特性。
将长有MoS2纳米薄膜的碳纤维作为柔性线状超级电容器的两个电极,制备出了柔性线状超级电容器。紧接着,对该柔性线状超级电容器的性能进行了测试,如图6所示,图6为将本发明中的多功能电极应用在柔性线状超级电容器中时该超级电容器的电化学性能表征图。图6a给出了柔性线状超级电容器的原理图。图6b给出了柔性线状超级电容器在扫速为100mV/s的情况下的CV图,从图中我们可以得到,基于CF@TiO2@MOS2电极的柔性线状超级电容器具有最好的性能。图6c和图6d分别给出了基于CF@TiO2@MOS2电极的柔性线状超级电容器在不同扫速下的CV图像和不同充电电流下的充电-放电图像。图6e给出了基于CF@TiO2@MOS2电极的柔性线状超级电容器在不同充电电流下的电容值。以上三个图说明了基于CF@TiO2@MOS2电极的柔性线状超级电容器的性能很好。图6f给出了基于CF@TiO2@MOS2电极的柔性线状超级电容器在充放电3000圈的性能,说明该超级电容器有着很好的稳定性。图6g-i给出了三个基于CF@TiO2@MOS2电极的柔性线状超级电容器的串联原理图以及测试的CV图和充电-放电曲线,从图中我们可以看出串联后的超级电容器的电压窗口从0.8V上升到了2.4V。
将长有MoS2纳米薄膜的碳纤维作为柔性线状锂离子电池的正极,制备出了柔性线状锂离子电池。紧接着,我们对该柔性线状锂离子电池的性能进行了测试,如图7所示,图7为将本发明中的多功能电极应用在柔性线状锂离子电池中时该锂离子电池的电化学性能表征图。图7a给出了柔性线状锂离子电池的原理图。图7b显示刚制备好的柔性线状锂离子电池的初始电压有3.271V。图7c表明了制备好的柔性线状锂离子电池可以点亮一个额定电压在2.0V左右的LED灯泡。图7d给出了柔性线状锂离子电池在3.0mA/m的充电电流下的充电-放电曲线。从图中我们可以看出,相对于第二圈而言,该柔性线状锂离子电池仍然保持着有80%左右的性能。
将长有MoS2纳米薄膜的碳纤维作为工作电极,利用电化学工作站等仪器,研究了其电解水的能力,如图8所示,图8为将本发明中的多功能电极作为工作电极电解水制氢的电化学性能表征图。图8a和b给出了CF@TiO2@MOS2工作电极和其它两个工作电极的电解水的极化曲线和阻抗图,从图中可知CF@TiO2@MOS2工作电极具有最好的电解水的能力。图8c给出了这三个电极的TAFEL曲线,从中可以看到CF@TiO2@MOS2工作电极的TAFEL斜率最小。图8d给出了CF@TiO2@MOS2工作电极在重复扫CV曲线500次后的极化曲线图,从图中得知CF@TiO2@MOS2工作电极在酸性溶液中具有很好的稳定性。
最后,将CF@TiO2@MOS2电极作为线状染料敏化太阳能电池和线状超级电容器的公共电极,而制备出了线状自行供电能量纤维,并且对它的光充电性能做了系统的研究,图9为将本发明中的多功能电极作为柔性线状染料敏化太阳能电池和柔性线状超级电容器的公共电极而制备出来的柔性线状自行供电能量纤维的示意图及性能表征图。图9a给出了该线状自行供电能量纤维的示意图。图9b给出了该线状自行供电能量纤维在3种不同的测试模式下的测试曲线,这三种测试模式分别是:只是电充线状超级电容器、只是光充线状超级电容器以及将电充和光充结合起来给线状超级电容器充电。从三种曲线中我们可以看出,由线状染料敏化太阳能电池给线状超级电容器充电比传统的电充线状超级电容器所需的时间非常的短。图9c给出了该线状自行供电能量纤维总体的转换效率,我们可以看出在光充电2秒的时候该效率达到了最大。
本发明中多功能电极的制备方法简单,而且成本非常低,为其在实际生活中的应用创造了有利的条件,该多功能电极还可以应用在各式各样的线状能量器件中,比如线状染料敏化太阳能电池、线状超级电容器、线状锂离子电池和线状电解水制氢等,解决了目前把所有能量器件结合在一起的困难,而且,该多功能电极可以同时应用在线状染料敏化太阳能电池和线状超级电容器中,解决了太阳能电池产生的电量必须即时即用的不足,满足了人们随时使用其产生的电能的需求。
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种用于线状光电能量器件的多功能电极,其特征在于:包括:碳纤维,所述碳纤维的外表面具有TiO2涂层,所述TiO2涂层上具有MoS2纳米薄膜。
2.一种如权利要求1所述的用于线状光电能量器件的多功能电极的制备方法,其特征在于:包括以下步骤:
a)配制TiCl4水溶液;
b)将碳纤维浸泡于TiCl4水溶液中,以使碳纤维的外表面上生长一层TiO2涂层;
c)将碳纤维从TiCl4水溶液中取出,清洗干净;
d)配制生长MoS2的前驱体溶液;
e)将外表面已具有TiO2涂层的碳纤维置于聚四氟乙烯内衬中,同时将配制好的生长MoS2的前驱体溶液倒入内衬中,将反应釜放入马弗炉中进行反应,以使碳纤维外表面的TiO2涂层上生长一层MoS2纳米薄膜;
f)将反应完的碳纤维取出,清洗干净。
3.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤d)中的前驱体溶液包括:0.03~0.09g的Na2MoO4、0.08~0.16g的C2H5NS,以及20~40mL的超纯水。
4.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤b)中,将碳纤维浸泡于TiCl4水溶液中后,将其置于60~80℃的环境下,并保持1~2个小时。
5.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤e)中,外表面已具有TiO2涂层的碳纤维置于聚四氟乙烯内衬中,同时将配制好的生长MoS2的前驱体溶液倒入内衬中,将反应釜放入马弗炉中在180~240℃的条件下进行反应20~40个小时。
6.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤b)中,将碳纤维浸泡于TiCl4水溶液之前,先用丙酮、乙醇和水依次将碳纤维进行清洗。
7.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤a)中,TiCl4水溶液的浓度范围为0.2~0.6mmol/L,并且配制好TiCl4水溶液后,将TiCl4水溶液搅拌0.5~1个小时。
8.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤c)中,将碳纤维从TiCl4水溶液中取出后,用乙醇和水清洗干净。
9.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤f)中,将反应完的碳纤维取出后,用乙醇和水清洗干净。
10.根据权利要求2所述的一种用于线状光电能量器件的多功能电极的制备方法,其特征在于:所述步骤e)中,聚四氟乙烯内衬的容积范围为50~80mL。
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