CN111416097B - 一种柔性电极的制备方法及其应用 - Google Patents
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Abstract
本发明公开了一种柔性电极的制备方法,具体按照以下步骤实施:步骤1、制备单分散的碳纳米管氯磺酸溶液;步骤2、向碳纳米管氯磺酸溶液中加入活性材料并搅拌均匀得电极浆料;步骤3、将极浆料均匀地涂覆在衬底上,经固化、清洗、干燥后得到柔性电极。本发明还公开了该方法制备的柔性电极及其应用。本发明的有益效果在于:(1)碳纳米管和活性材料在浆料中分散均匀,且碳纳米管能够实现单分散,提高柔性电极的机械性能和电化学性能;(2)柔性电极中不包含导电添加剂、聚合物粘结剂等惰性组成,可有效提高柔性电极的能量密度;活性材料的选取具有一定的普适性;(3)制备方法简单易行,且该技术适合于工业化生产。
Description
技术领域
本发明属于电极制备技术领域,具体涉及一种柔性电极的制备方法,还涉及该方法制备的柔性电极的应用。
背景技术
近年来,可穿戴电子设备已经成为人们日常生活中的重要组成部分。传统的电池具有笨重、刚性等缺点,很难满足这些设备的需求。因此,急需开发轻便、柔性电源(电池、超级电容器等)与之匹配作为动力来源。作为电源的关键部件之一,柔性电极的开发至关重要。
柔性电极主要由“刚性”的活性材料和“柔性”的基底材料组成。其中,活性材料提供容量,基底材料提供机械支撑和导电网络。柔性电极应同时兼顾良好的电化学性能和机械性能。碳纳米管具有优异的热稳定性、化学稳定性、良好的导电性和机械性能,被认为是制造柔性电极的最佳候选基底材料之一。在柔性电极中,碳纳米管和活性材料的分散均匀性会直接影响其力学性能和电化学性能。受限于碳纳米管独特的一维管状结构,很难获得均匀分散的、高浓度(粘度合适)的碳纳米管/活性材料复合浆料。因此,目前制备柔性电极的主要方法为真空抽滤法、静电纺丝法等,很难采用工业上常见的刮涂法或者对辊法来制备以碳纳米管为基底的、且兼顾电化学性能和机械性能的柔性电极。
发明内容
本发明的目的是提供一种柔性电极的制备方法,解决了现有技术制备的以碳纳米管为基底的柔性电极不能兼顾电化学性能和机械性的问题。
本发明所采用的技术方案是,一种柔性电极的制备方法,具体按照以下步骤实施:
步骤1、将碳纳米管分散于氯磺酸溶液中,得单分散的碳纳米管氯磺酸溶液;
步骤2、向碳纳米管氯磺酸溶液中加入活性材料并搅拌均匀,得电极浆料;
步骤3、采用刮涂法或对辊法将极浆料均匀地涂覆在衬底上,经固化、清洗、干燥后得到柔性电极。
本发明的特点还在于:
步骤1中,碳纳米管的质量分数为0.01~10wt.%;
步骤2中,活性材料与碳纳米管的质量比例为1:20~20:1。
步骤2中,活性材料为不与氯磺酸反应的单质、化合物以及复合材料。
步骤2中,活性材料包括但不限于Si@C、S@C、P@C中一种。
本发明的另一目的是提供上述方法制备的柔性电极。
本发明的第三个目的是提供柔性电极的应用。
柔性电极在电源中应用。
本发明的特点还在于:
柔性电极在锂离子电池中应用。
柔性电极在钠离子电池中应用。
柔性电极在钾离子电池中应用。
本发明的有益效果是:(1)碳纳米管和活性材料在浆料中分散均匀,且碳纳米管能够实现单分散,碳纳米管和活性材料的均匀分散能提高柔性电极的机械性能和电化学性能;(2)柔性电极中不包含导电添加剂、聚合物粘结剂等惰性组成,可有效提高柔性电极的能量密度;(3)活性材料的选取具有一定的普适性,不与氯磺酸反应的单质、化合物以及复合材料均可作为活性材料;(4)制备方法简单易行,且该技术适合于工业化生产。
附图说明
图1是本发明一种柔性电极的制备方法及其应用的制备流程图;
图2是本发明一种柔性电极的制备方法及其应用中柔性电极的扫描电镜图;
图3是本发明一种柔性电极的制备方法及其应用中柔性电极的光学电镜图;
图4是本发明一种柔性电极的制备方法及其应用中柔性电极的机械性能图;
图5是本发明一种柔性电极的制备方法及其应用中柔性电极应用于锂离子电池的储锂性能图;
图6是本发明一种柔性电极的制备方法及其应用中柔性电极应用于锂硫电池的储锂性能图;
图7是本发明一种柔性电极的制备方法及其应用中柔性电极应用于钠离子电池的储钠性能图;
图8是本发明一种柔性电极的制备方法及其应用中柔性电极应用于钾离子电池的储钾性能图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明一种柔性电极的制备方法,如图1所示,具体按照以下步骤实施:
步骤1、将碳纳米管分散于氯磺酸溶液中,得单分散的碳纳米管氯磺酸溶液;
步骤2、向碳纳米管氯磺酸溶液中加入活性材料并搅拌均匀,得电极浆料,活性材料为不与氯磺酸反应的单质、化合物以及复合材料,包括但不限于Si@C、S@C、P@C中一种。
步骤3、采用刮涂法或对辊法将极浆料均匀地涂覆在衬底上,经固化、清洗、干燥后得到柔性电极;
优选的,活性材料与碳纳米管的质量比例为1:20~20:1;
优选的,碳纳米管的质量分数为0.01~10wt.%;
其中,衬底可以为聚四氟乙烯薄板或其他柔性物质。
实施例1
步骤1、将15mg碳纳米管放置于1.8mL氯磺酸中,得到单分散的碳纳米管氯磺酸溶液;
步骤2、将15mg的活性材料Si@C(碳包覆硅纳米颗粒,硅质量分数为90%)加入到上述溶液中,搅拌均匀后得到电极浆料;
步骤3、将电极浆料采用刮涂法均匀地涂覆在衬底聚四氟乙烯薄板的表面,接着将聚四氟乙烯薄板放入乙醚溶液中固化半个小时后,将脱落的薄膜在去离子水中清洗至中性,烘干后得到柔性电极,其扫描电镜照片见图2,光学照片见图3。
测试该柔性电极的力学性能,其拉伸强度为4.00MPa,应变延长率为15.77%,如图4所示,完全满足柔性电极对机械性能的要求。
将柔性电极用作负极组装锂离子电池,其中锂片为对电极和参比电极,进行储锂性能测试,在0.1Ag-1的电流密度下循环50圈后,其可逆放电容量保持在1237mAhg-1,容量保持率高达88.7%,如图5所示。
实施例2
步骤1、将15mg碳纳米管放置于1.8mL氯磺酸中,得到单分散的碳纳米管氯磺酸溶液;
步骤2、将15mg的活性材料S@C(碳包覆硫单质,硫质量分数为85%)粉末加入到上述溶液中,搅拌均匀后得到电极浆料;
步骤3、将电极浆料采用刮涂法均匀地涂覆在衬底聚四氟乙烯薄板的表面,接着将聚四氟乙烯薄板放入乙醚溶液中固化半个小时后,将脱落的薄膜在去离子水中清洗至中性,烘干后得到柔性电极。
将柔性电极用作正极材料组装锂硫电池,其中锂片为对电极和参比电极,进行储锂性能测试,在1.0A g-1的电流密度下循环300圈后,其可逆放电容量保持在430mA h g-1,容量保持率高达89.4%,如图6所示。
实施3
步骤1、将15mg碳纳米管放置于1.8mL氯磺酸中,得到单分散的碳纳米管氯磺酸溶液;
步骤2、将15mg的活性材料P@C(碳包覆红磷,其中磷质量分数为70%)加入到上述溶液中,搅拌均匀后得到电极浆料;
步骤3、将电极浆料采用刮涂法均匀地涂覆在衬底聚四氟乙烯薄板的表面,接着将聚四氟乙烯薄板放入乙醚溶液中固化半个小时后,将脱落的薄膜在去离子水中清洗至中性,烘干后得到柔性电极。
将柔性电极用作负极组装钠离子电池,其中钠片为对电极和参比电极,进行储钠性能测试,在1.0A g-1的电流密度下循环100圈后,其可逆放电容量保持在953mA h g-1,容量保持率高达81.9%,如图7所示。
将柔性电极用作负极组装钾离子电池,其中钾片为对电极和参比电极,进行储钾性能测试,在1.0A g-1的电流密度下循环100圈后,其可逆放电容量保持在445mA h g-1,容量保持率高达78.3%,如图8所示。
Claims (4)
1.一种柔性电极的制备方法,其特征在于,具体按照以下步骤实施:
步骤1、将碳纳米管分散于氯磺酸溶液中,得单分散的碳纳米管氯磺酸溶液;
步骤2、向碳纳米管氯磺酸溶液中加入活性材料并搅拌均匀,得电极浆料;
步骤3、采用刮涂法将电极浆料均匀地涂覆在衬底上,经乙醚溶液固化后、清洗、干燥得到柔性电极;
所述步骤1中,碳纳米管的质量分数为0.01~10 wt. %;
所述步骤2中,活性材料与碳纳米管的质量比例为1:20~20:1,活性材料为不与氯磺酸反应的单质、化合物以及复合材料。
2.根据权利要求1所述的一种柔性电极的制备方法,其特征在于,所述步骤2中,活性材料为Si@C、S@C、P@C中一种。
3.根据权利要求1或2中任一项所述制备方法制备的柔性电极。
4.根据权利要求3所述的柔性电极在电源中应用,具体地包括在锂离子电池、钠离子电池、钾离子电池中应用。
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