CN111223677B - 一种钾离子混合电容器的电极材料及其制备方法 - Google Patents
一种钾离子混合电容器的电极材料及其制备方法 Download PDFInfo
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Abstract
一种钾离子混合电容器的电极材料,包括碳包覆的FeS2。本发明的碳包覆的FeS2复合材料(C/FeS2/C)与金属氧化物、氢氧化物相比具有更高的电容和丰富的氧化还原反应活性位点。并且本发明的电极材料其毒性低,比电容大,是安全有效的钾离子混合电容器电极材料。
Description
技术领域
本发明涉及一种电极材料,尤其涉及一种钾离子混合电容器的电极材料及其制备方法。
背景技术
钾离子混合电容器拥有容量大、充放电速度快以及寿命长等优点,因此可以作为高效的小型储能元件。根据储能机理不同,钾离子混合电容器可以分为双电层电容器与赝电容电容器。赝电容器又称法拉第准电容器,因其高功率密度、高放电、长循环寿命和高安全性等性能受到广泛关注。与通过阴阳离子在电解液和电极表面进行交替沉积储存能量的双电层电容器不同,赝电容器是通过在电极表面进行的一系列快速氧化还原反应来存储和释放电量。当对赝电容器施加电压时,电极材料表面发生可逆的氧化还原反应,电容器单元产生电荷和感应电流,电荷存储到电极中提高电容器的充电电压;相应地,当其外接负载放电时,储存在电极中的电荷通过外接回路释放,形成电流,进入活性材料中的离子由于失去电场的作用回到电解液中。正因为工作原理的不同,同样的赝电容器电容量往往比双电层电容器高几十甚至上百倍。然而,目前赝电容器的发展应用却并不理想,这主要是因为绝大多数赝电容器的电极活性材料,如过渡金属氧化物等,属于半导体或绝缘体,限制了电子/离子的传输,使电极性能随电子/离子的传输距离增加而急剧下降,从而失去实用价值。
双电层电容器与赝电容电容器的电极材料前者主要为碳材料,后者主要为金属氧化物、氢氧化物等过渡金属化合物。然而氧化物与氢氧化物的导电性差因而限制了它在钾离子混合电容器中的应用。
发明内容
本发明要解决的技术问题是克服现有技术的不足,提供一种大的理论比电容、制备成本低等优点的钾离子混合电容器的电极材料及其制备方法。
为解决上述技术问题,本发明提出的技术方案为:一种钾离子混合电容器的电极材料,包括碳包覆的FeS2。
一种钾离子混合电容器的电极材料的制备方法,包括以下步骤,
1)棒状Fe-MOF的合成;
①将FeCl3与富马酸溶解于N,N-二甲基甲酰胺中,搅拌形成黄色透明的溶液;
②向步骤①的溶液中滴加氢氧化钠搅拌均匀;
③将步骤②的溶液转移到高压釜内,在80-120℃的温度下反应12-36小时;
④将步骤③的产物清洗干净后,真空干燥,得到棒状Fe-MOF;
2)有机物的包覆;
I将1份步骤1)制备的棒状Fe-MOF溶解于5-10份去离子水中,然后依次加入2-4份十六烷基三甲基溴化铵、0.2-1份间苯二酚、2-5份乙醇以及0.05-0.2份氨水溶液,室温下充分搅拌均匀,份数均匀重量份;
II在持续的搅拌条件下向步骤I的溶液中滴加4-6倍氨水体积的福尔马林溶液;在搅拌5-7小时后于室温下老化10小时以上得到有机物保护的Fe-MOF材料;
3)硫化;
将1重量份有机物包覆的Fe-MOF与10重量份的硫粉分别放置在两个容器中,在氩气气氛下以1-2℃ min-1的速率升到500℃以上,维持2-5h后自然冷却到室温,得到碳包覆的FeS2复合材料(C/FeS2/C)。
上述的钾离子混合电容器的电极材料的制备方法,优选的,所述步骤1)中FeCl3为FeCl3·6H2O。
上述的钾离子混合电容器的电极材料的制备方法,优选的,所述步骤1)中①为将0.54g FeCl3·6H2O与0.4g富马酸溶解于27mLN,N-二甲基甲酰胺中,搅拌20min形成黄色透明溶液。
上述的钾离子混合电容器的电极材料的制备方法,优选的,所述步骤1)中氢氧化钠的浓度为0.4mol L-1。
上述的钾离子混合电容器的电极材料的制备方法,优选的,所述步骤1)中高压釜的内壁设置有聚四氟乙烯内衬。
与现有技术相比,本发明的优点在于:本发明的碳包覆的FeS2复合材料(C/FeS2/C)与金属氧化物、氢氧化物相比具有更高的电容和丰富的氧化还原反应活性位点。并且本发明的电极材料其毒性低,比电容大,是安全有效的钾离子混合电容器电极材料。
附图说明
图1为实施例1中棒状Fe-MOF的SEM扫描图。
图2为实施例1中有机物保护的Fe-MOF材料的SEM扫描图。
图3为实施例1碳包覆的FeS2复合材料(C/FeS2/C)的SEM扫描图。
图4为实施例1中碳包覆的FeS2复合材料(C/FeS2/C)的充放电曲线图。
图5为实施例1中碳包覆的FeS2复合材料(C/FeS2/C)的循环曲线和库伦效率图。
具体实施方式
为了便于理解本发明,下文将结合较佳的实施例对本发明作更全面、细致地描述,但本发明的保护范围并不限于以下具体的实施例。
需要特别说明的是,当某一元件被描述为“固定于、固接于、连接于或连通于”另一元件上时,它可以是直接固定、固接、连接或连通在另一元件上,也可以是通过其他中间连接件间接固定、固接、连接或连通在另一元件上。
除非另有定义,下文中所使用的所有专业术语与本领域技术人员通常理解的含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的,并不是旨在限制本发明的保护范围。
实施例1
本实施例的钾离子混合电容器的电极材料的制备方法包括以下步骤:
1)棒状Fe-MOF的合成:棒状Fe-MOF参考文献上的方法合成8。首先,0.54g FeCl3·6H2O 与0.44g富马酸溶解于27mLN,N-二甲基甲酰胺中,搅拌20min形成黄色透明溶液。接着,将3mL 0.4mol L-1的氢氧化钠溶液缓慢加入到上述溶液中,搅拌10min后将溶液转移到容量为50mL的聚四氟乙烯内衬不锈钢高压釜中,在100℃下反应24h。反应完后将产物用乙醇清洗三次,60℃真空干燥12h。图1为棒状Fe-MOF的SEM扫描图。
2)有机物包覆:将0.1g上一步得到的Fe-MOF超声溶解于8mL去离子水中,然后依次加入0.285g十六烷基三甲基溴化铵、0.0435g间苯二酚、3.53mL乙醇以及12.5μL氨水溶液,室温下搅拌30min。最后,在持续搅拌的条件缓慢滴加62.5μL福尔马林溶液到上述溶液中,搅拌6h后于室温下老化12h得到有机物包覆的Fe-MOF材料。图2为有机物保护的Fe-MOF材料的SEM扫描图。
3)硫化:将0.1g有机物包覆的Fe-MOF与1g硫粉分别放置在两个瓷舟中,在氩气气氛下以2℃ min-1的速率升到500℃,维持3h后自然冷却到室温,得到碳包覆的FeS2复合材料(C/FeS2/C)。图3为碳包覆的FeS2复合材料(C/FeS2/C)的SEM扫描图。
为了测试本实施例得到的碳包覆的FeS2复合材料(C/FeS2/C)的性能,将不让你实施例的FeS2复合材料(C/FeS2/C)、乙炔黑和羧甲基纤维素钠研磨充分至细腻浆料。把浆料滴涂在预处理后的铜箔上,在真空干燥箱中60℃干燥充分,取出之后将活性物质用压片机在15Mpa 压力下压实,采用三电极测试体系,采用3M的KPF6@DME电解液,对复合材料进行充放电测试,图4为实施例1中碳包覆的FeS2复合材料(C/FeS2/C)的充放电曲线图。图5为实施例1中碳包覆的FeS2复合材料(C/FeS2/C)的循环曲线和库伦效率图。
由于高的自然丰度、低的氧化还原电位与溶剂化半径,钾离子电池被认为是具有极高应用价值的电化学储能系统。然而,钾离子电池功率密度低下,循环稳定性差,而钾离子混合电容器是一种能在不牺牲寿命的情况下提供高功率的新型能源设备,因而成为有望替代钾离子电池的理想设备。对于本实施例的碳包覆的FeS2复合材料(C/FeS2/C)的储能机理,在钾离子混合电容器能量存储和转换的过程中,KPF6的中K+在电极材料中进行嵌入和脱嵌,而电能和化学能进行相互转化。在充电期间,K+从正极脱嵌,并在外部电势的驱动下通过隔膜和电解质迁移到负极。同时,电子通过外部电路从正极向负极迁移,并被K+捕获,形成钾金属,来自外部电路的电能被转换为化学能并存储在负极材料中。在放电期间,存储在负极中的金属钾转化为K+,这些K+通过电解质和隔膜迁移到正极,并嵌入正极材料的晶格中。充放电过程的反应式如下:
放电过程:FeS2+xK++xe-→KxFeS2
KxFeS2+(4-x)K++(4-x)e-→Fe+2K2S
充电过程:KxFeS2→FeS2+xK++xe-
Fe+2K2S→KxFeS2+(4-x)K++(4-x)e- 。
Claims (5)
1.一种钾离子混合电容器的电极材料的制备方法,其特征在于:包括以下步骤,
1)棒状Fe-MOF的合成;
2)有机物的包覆;
将1份步骤1)制备的棒状Fe-MOF溶解于5-10份去离子水中,然后依次加入2-4份十六烷基三甲基溴化铵、0.2-1份间苯二酚、2-5份乙醇以及0.05-0.2份氨水溶液,室温下充分搅拌均匀,份数均匀重量份;
3)硫化;
将1重量份有机物包覆的Fe-MOF与10重量份的硫粉分别放置在两个容器中,在氩气气氛下以1-2 °C min−1的速率升到500 °C以上,维持2-5 h后自然冷却到室温,得到碳包覆的FeS2复合材料。
2.根据权利要求1所述的钾离子混合电容器的电极材料的制备方法,其特征在于:所述步骤1)中FeCl3为FeCl3·6H2O。
4.根据权利要求1所述的钾离子混合电容器的电极材料的制备方法,其特征在于:所述步骤1)中氢氧化钠的浓度为0.4 mol L-1。
5.根据权利要求1所述的钾离子混合电容器的电极材料的制备方法,其特征在于:所述步骤1)中高压釜的内壁设置有聚四氟乙烯内衬。
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