CN106981376A - 超级电容器电极制备方法 - Google Patents
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
本发明提供了一种超级电容器电极制备方法,包括合成氧化铁、以合成的α‑FeOOH和α‑Fe2O3纳米材料为电极活性物,选择导电剂和粘结剂,得到悬浮液、将悬浮液涂在预先洗净的泡沫镍电极上、除去溶剂和水分,并压实,使粉料与泡沫镍电极接触紧密,形成超级电容器电极。本发明提供的超级电容器电极制备方法,制备出的超级电容器电极具有较高的结晶度,具有出色的结晶性和晶体结构排列的规整性,通过实验证明,具有很好的导电性。
Description
技术领域
本发明涉及一种超级电容器电极制备方法,属于纳米材料制备领域。
背景技术
氧化铁纳米材料由于其优良的性能被广泛应用于催化剂、能量储存与转化设备、磁性材料、水污染处理、气敏材料、颜料等方面。而超级电容器具有功率密度高、充放电速度快、循环稳定性好、寿命长等优点,作为一种新型的储能装置日益受到大家的关注。本文是在氧化铁纳米材料研究现状的基础上,主要尝试采用液相沉淀法等合成手段,可控制备合成了多种氧化铁纳米材料,如一维纳米结构、中空结构、多面体结构,利用X-射线衍射(XRD)、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)、比表面测试仪(BET)等现代分析测试技术表征了材料的微观形貌和结构,分别以制得的氧化铁纳米材料作为超级电容器和锂离子电池电极材料,组装成测试器件,使用循环伏安、交流阻抗、恒电流充放电测试方法研究了材料的电化学性能,得到了良好的测试结果。
作为一种新型储能装置,超级电容器具有输出功率高、充电时间短、工作温度范围宽、使用寿命长、安全且无污染等优点,有望成为本世纪新型的绿色电源。目前常用的用于超级电容器电极材料的包括碳材料、金属氧化物材料、导电聚合物材料等,但这些材料由于固有的一些问题,导致制备出的电极材料比容量相对较低,这势必对电容器的整体性能有很大的影响
发明内容
鉴于上述现有技术的不足之处,本发明的目的在于提供一种超级电容器电极制备方法。
本发明的目的是为了克服传统制备方法制备的材料的不足,提供了一种超级电容器电极制备方法。为了达到上述目的,本发明采取了以下技术方案:
本发明提供了一种超级电容器电极制备方法,包括以下步骤:
步骤一、合成氧化铁,分别将Fe(NO3)3·9H2O 和KOH 溶解在去离子水中;搅拌后,将混合溶液转移在干燥箱中反应;把所得沉淀离心出来,反复洗涤;将沉淀真空干燥,得到黄绿色的产物为α-FeOOH;将产物升温然后自然冷却,最后得到红色产物为α-Fe2O3;
步骤二、分别以合成的α-FeOOH和α-Fe2O3纳米材料为电极活性物,选择导电剂和粘结剂,按比例加入乙醇溶剂后超声分散得到均一的悬浮液;
步骤三、将步骤二得到的悬浮液涂在预先洗净的泡沫镍电极上,放入真空干燥箱中,一定时间后取出;
步骤四、除去溶剂和水分,并压实,使粉料与泡沫镍电极接触紧密,形成超级电容器电极。
优选的,上述步骤一具体包括:
步骤1.1、分别将Fe(NO3)3·9H2O 和KOH 溶解在去离子水中;
步骤1.2、将KOH溶液滴加入搅拌中的Fe(NO3)3·9H2O溶液中;
步骤1.3、加去离子水到混合溶液中,搅拌后,将混合溶液转移到反应釜内;
步骤1.4、盛有溶液的反应釜在干燥箱中反应;
步骤1.5、反应结束后待反应釜自然冷却到室温,把所得沉淀离心出来,用无水乙醇和蒸馏水反复洗涤,以除去未反应完的试剂;
步骤1.6、将洗好的沉淀真空干燥,得到黄绿色的产物为α-FeOOH;
步骤1.7、将产物然后放入马弗炉,升温至350°C保持,然后自然冷却到室温,最后得到干燥松散的红色产物为α-Fe2O3。
优选的,上述步骤1.1中分别将0.01mol Fe(NO3)3·9H2O和0.04mol KOH 溶解在10ml去离子水中。
优选的,上述步骤1.3中加20ml 去离子水到混合溶液中,搅拌10分钟后,将混合溶液转移到50ml的反应釜内。
优选的,上述步骤1.4中在盛有溶液的反应釜在100°C的干燥箱中反应6小时。
优选的,上述步骤二中导电剂为导电炭黑,粘结剂为聚四氟乙烯,按照质量比为75:15:10配比电极活性物、导电剂和粘结剂。
优选的,上述步骤三具体为用微量进样器将50μl的悬浮液涂在预先洗净的泡沫镍电极上,放入80°C的真空干燥箱中,10 h后取出。
优选的,上述步骤四具体为除去溶剂和水分,并于10 MPa的压力下压实,使粉料与泡沫镍电极接触紧密。
本发明提供的超级电容器电极制备方法,制备出的超级电容器电极具有较高的结晶度,具有出色的结晶性和晶体结构排列的规整性,通过实验证明,具有很好的导电性。
附图说明
图1为本发明制备的α-FeOOH纳米棒的X射线衍射(XRD)图谱示意图。
具体实施方式
本发明提供一种超级电容器电极制备方法,为使本发明的目的、技术方案及效果更加清楚、明确,以下参照附图并举实施例对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
本实施例提供的超级电容器电极制备方法,具体包括以下步骤:
水热合成氧化铁,首先分别将0.01mol Fe(NO3)3·9H2O和0.04mol KOH 溶解在10ml去离子水中。然后将KOH 溶液滴加入搅拌中的Fe(NO3)3·9H2O溶液中。加20ml 去离子水到混合溶液中,搅拌10分钟后,将混合溶液转移到50ml的反应釜内。盛有溶液的反应釜在100°C的干燥箱中反应6小时。反应结束后待反应釜自然冷却到室温,把所得沉淀离心出来,用无水乙醇和蒸馏水反复洗涤,以除去未反应完的试剂。将洗好的沉淀在60°C下真空干燥8h,得到黄绿色的产物为α-FeOOH。将产物然后放入马弗炉,升温至350°C保持3小时,然后自然冷却到室温,最后得到干燥松散的红色产物为α-Fe2O3。
分别以合成的α-FeOOH和α-Fe2O3纳米材料为电极活性物,导电炭黑为导电剂,聚四氟乙烯(PTFE)为粘结剂,按比例(质量比为75:15:10)加入乙醇溶剂后超声分散得到均一的悬浮液。用微量进样器将50μl的悬浮液涂在预先洗净的泡沫镍电极上,放入80°C的真空干燥箱中,10 h后取出。除去溶剂和水分,并于10 MPa的压力下压实,使粉料与泡沫镍电极接触紧密。后在1mol/L的KOH溶液中浸泡活化10小时,测试。本实施例的三电极体系中,以饱和甘汞电极为参比电极、泡沫镍电极为对电极、带活性材料的泡沫镍电极为工作电极,在1mol·L-1的KOH电解液中进行测试。
用X射线衍射(XRD)对通过水热方法合成的α-FeOOH纳米棒材料的晶体结构进行了表征和分析,如图1为产物的XRD图谱。从图中可以看到,大部分的衍射峰都可以很好的与标准谱图JCPDS 00-029-0713 报道的数据相对应,表明所得到的产物是正交晶系α-FeOOH。在(110)面有最强的衍射峰,表明材料在(110)方向有最大的衍射取向。其衍射峰已在谱图中标出,各个峰值所对应的晶面如图中所示。
运用扫描电镜(SEM)对所制备的α-FeOOH纳米材料进行了形貌和微结构的分析,可以得到样品尺寸和外形相对均一,有轻微团聚现象,外形均为纳米线状,所制备的粉体是由纳米棒组成,其尺寸长轴约为320-680nm,短轴约为20-80nm。加入PVP后,产物分散更好,但形貌不再是均一的纳米棒,出现些许片状结构,尺寸没有变化太多。
样品的透射电镜图进一步证实了其微观结构。在低倍数下,证实了通过水热方法合成的α-FeOOH确实是有纳米棒组成的,从较大的放大倍数下可以得到,纳米棒内部为实心。通过测量两列晶格纹的晶面间距分别为0.249nm和0.247nm,分别对应着(111)和(101)面,结果再一次证明了XRD的分析结果。
本发明提供的超级电容器电极制备方法,制备出的超级电容器电极具有较高的结晶度,具有出色的结晶性和晶体结构排列的规整性,通过实验证明,具有很好的导电性。
可以理解的是,对本领域普通技术人员来说,可以根据本发明的技术方案及其发明构思加以等同替换或改变,而所有这些改变或替换都应属于本发明所附的权利要求的保护范围。
Claims (8)
1.一种超级电容器电极制备方法,其特征在于:所述制备方法包括以下步骤:
步骤一、合成氧化铁,分别将Fe(NO3)3·9H2O 和KOH 溶解在去离子水中;搅拌后,将混合溶液转移在干燥箱中反应;把所得沉淀离心出来,反复洗涤;将沉淀真空干燥,得到黄绿色的产物为α-FeOOH;将产物升温然后自然冷却,最后得到红色产物为α-Fe2O3;
步骤二、分别以合成的α-FeOOH和α-Fe2O3纳米材料为电极活性物,选择导电剂和粘结剂,按比例加入乙醇溶剂后超声分散得到均一的悬浮液;
步骤三、将步骤二得到的悬浮液涂在预先洗净的泡沫镍电极上,放入真空干燥箱中,一定时间后取出;
步骤四、除去溶剂和水分,并压实,使粉料与泡沫镍电极接触紧密,形成超级电容器电极。
2.如权利要求1所述的超级电容器电极制备方法,其特征在于:所述步骤一具体包括:
步骤1.1、分别将Fe(NO3)3·9H2O 和KOH 溶解在去离子水中;
步骤1.2、将KOH溶液滴加入搅拌中的Fe(NO3)3·9H2O溶液中;
步骤1.3、加去离子水到混合溶液中,搅拌后,将混合溶液转移到反应釜内;
步骤1.4、盛有溶液的反应釜在干燥箱中反应;
步骤1.5、反应结束后待反应釜自然冷却到室温,把所得沉淀离心出来,用无水乙醇和蒸馏水反复洗涤,以除去未反应完的试剂;
步骤1.6、将洗好的沉淀真空干燥,得到黄绿色的产物为α-FeOOH;
步骤1.7、将产物然后放入马弗炉,升温至350°C保持,然后自然冷却到室温,最后得到干燥松散的红色产物为α-Fe2O3。
3.如权利要求2所述的超级电容器电极制备方法,其特征在于:所述步骤1.1中分别将0.01mol Fe(NO3)3·9H2O和0.04mol KOH 溶解在10ml去离子水中。
4.如权利要求2所述的超级电容器电极制备方法,其特征在于:所述步骤1.3中加20ml去离子水到混合溶液中,搅拌10分钟后,将混合溶液转移到50ml的反应釜内。
5.如权利要求2所述的超级电容器电极制备方法,其特征在于:所述步骤1.4中在盛有溶液的反应釜在100°C的干燥箱中反应6小时。
6.如权利要求1所述的超级电容器电极制备方法,其特征在于:所述步骤二中导电剂为导电炭黑,粘结剂为聚四氟乙烯,按照质量比为75:15:10配比电极活性物、导电剂和粘结剂。
7.如权利要求1所述的超级电容器电极制备方法,其特征在于:所述步骤三具体为用微量进样器将50μl的悬浮液涂在预先洗净的泡沫镍电极上,放入80°C的真空干燥箱中,10 h后取出。
8.如权利要求1所述的超级电容器电极制备方法,其特征在于:所述步骤四具体为除去溶剂和水分,并于10 MPa的压力下压实,使粉料与泡沫镍电极接触紧密。
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