CN109243835A - 一种聚3,4-乙烯二氧噻吩纳米网状薄膜pedot-pd及其制备方法与应用 - Google Patents
一种聚3,4-乙烯二氧噻吩纳米网状薄膜pedot-pd及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种聚3,4‑乙烯二氧噻吩纳米网状薄膜PEDOT‑PD及制备方法。所述的聚3,4‑乙烯二氧噻吩纳米薄膜(PEDOT‑PD)呈网状结构。所述的制备方法为:在三电极电解池体系中,以3,4‑乙烯二氧噻吩为单体,以四乙基六氟磷酸铵为支持电解质,以二氯甲烷为电解溶剂,混合均匀得到电解液,以氧化铟锡导电玻璃电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,在室温下采用恒电位法,在1.3~1.7V电压条件下进行电化学聚合反应,得到沉积在工作电极上的聚合物薄膜,经淋洗、烘干得到聚3,4‑乙烯二氧噻吩纳米网状薄膜PEDOT‑PD。将制备所得的聚合物薄膜应用于超级电容器电极材料,比容量达到80~90F/g。
Description
技术领域
本发明涉及一种聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)及其制备方法,此方法合成的聚合物纳米网状薄膜可应用于超级电容器中。
背景技术
导电聚合物由于其结构的多样化以及可控性、质量轻、易加工等特点,在生物医药方面、电致变色材料、太阳能电池以及超级电容器等领域呈现出广泛的应用前景。
超级电容器作为一种新型电化学储能器件,凭借其较长的循环使用寿命、环境友好及安全性能高等优点,受到广泛的研究和关注。超级电容器的电极材料可分为三类:多孔碳材料、金属氧化物以及导电聚合物,导电聚合物作为超级电容器的研究对象起步相对比较晚,由于该类材料具有制备方便、成本低、比容高等优点,近年来成为超级电容器电极材料研究的热门。聚3,4-乙烯二氧噻吩(PEDOT)具有很好的导电性,稳定性好,并且具有很好的成膜性,是应用于超级电容器电极的导电聚合物优选材料。
发明内容
本发明的目的之一在于提供一种聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)及其制备方法与应用。
本发明为解决技术问题采用如下技术方案:
本发明所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)具体按照如下步骤进行制备:
在三电极电解池体系中,以3,4-乙烯二氧噻吩(EDOT)为单体,以四乙基六氟磷酸铵(TEAPF6)为支持电解质,以二氯甲烷为电解溶剂,混合均匀得到电解液,以氧化铟锡导电玻璃(ITO)电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,在室温下采用恒电位法,在1.3~1.7V电压条件下进行电化学聚合反应,当聚合电量达到0.05~0.2C时,聚合结束,在-1~-0.7V负电位下脱掺杂50~100s,得到沉积在工作电极上的聚合物薄膜,经淋洗、烘干得到聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD);所述的电解液中,所述的3,4-乙烯二氧噻吩单体的初始终浓度为1~10mmol/L;所述的支持电解质四乙基六氟磷酸铵(TEAPF6)的初始终浓度为0.01~0.1mol/L。
进一步,本发明中所述的3,4-乙烯二氧噻吩单体的初始终浓度优选为5mmol/L;所述的支持电解质四乙基六氟磷酸铵(TEAPF6)的初始终浓度优选为0.1mol/L;所述的二氯甲烷溶剂规格为分析纯。
进一步,所述的工作电极依次经过0.3%氢氧化钠溶液、乙醇、丙酮、甲苯、乙醇、丙酮分别超声清洗15~20min,用氮气吹干所述的工作电极表面剩余溶剂后置于60℃真空干燥箱干燥1~2h,备用。
进一步,优选所述的恒电位聚合法为:在上述电解液环境中,在1.4V电压条件下聚合,当聚合电量达到0.05~0.2C时聚合结束,并且在-0.8V负电位下脱掺杂50~100s,经淋洗后得到聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)。
再进一步,所述的淋洗、烘干过程具体操作为:用二氯甲烷淋洗沉积在工作电极上的聚合物薄膜,然后将所述的聚合物薄膜置于60~80℃真空干燥箱中干燥10~12h后得到成品聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)。
本发明所制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)通过扫描电镜表征了其清晰的网状结构的形貌以及通过红外光谱表征了聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的结构,证实了所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的形成。
本发明的目的之二在于所制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)在制备超级电容器电极中的应用。
进一步,所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的性能测试方法为:配制0.1moL/L的高氯酸锂/乙腈溶液,以所制得的沉积在ITO工作电极上的聚合物聚3,4-乙烯二氧噻吩纳米网状薄膜为超级电容器的工作电极,以铂片为辅助电极,以银/氯化银电极为参比电极,组成三电极体系,在一定电压范围内通过循环伏安法测试电极在不同扫速下的电容量;通过恒电流充放电测试电极在不同电流密度下的电容量。
进一步,所述的一定电压范围为-0.2~0.8V;所述的不同扫速分别选取为300mv/s、200mv/s、100mv/s、50mv/s、20mv/s、10mv/s。
进一步,所述的不同电流密度分别选取为1A/g、2A/g、5A/g、10A/g。
与现有技术相比,本发明的有益效果在于:
(1)本发明所制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)比容量达到80~90F/g,相比于文献中报道的PEDOT薄膜比容量为60F/g有了很大的提高。
(2)本发明通过改变聚合物微观结构能提高聚合物性能,具有很大的参考价值。
(3)本发明成本低,操作简单,且制备过程无污染,符合绿色化学,保护环境的生态理念。
附图说明
图1是本发明制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)在60000倍率下的扫描电镜图。
图2是本发明制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)在10000倍率下的扫描电镜图。
图3是本发明制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)在100000倍率下的扫描电镜图。
图4是本发明制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的红外光谱图。
图5是本发明制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的循环伏安图。
图6是本发明制备的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的恒电流充放电图。
具体实施方式
实施例1
在三电极电解池体系中,配制EDOT(0.07109g,0.5mmol),TEAPF6(2.7522g,0.01mol),二氯甲烷(100mL)的电解液,以氧化铟锡导电玻璃(2.76958g)电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,以饱和的氯化钾水溶液为第一液接,以所述的电解液为第二液接。在室温下采用恒电位1.4V进行电化学聚合,聚合电量0.05C,然后在负电位-0.8V下脱掺杂60s,得到沉积在工作电极上的聚合物薄膜,用二氯甲烷淋洗去除聚合物薄膜表面残留的电解液并在60℃真空干燥箱中干燥12h后得到聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD),称取所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)质量为2.76970g。该沉积有聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的ITO工作电极即用作超级电容器电极。
(2)超级电容器性能测试:将步骤(1)中的沉积有聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)ITO导电玻璃作为工作电极,配制0.1moL/L的高氯酸锂/乙腈溶液100mL作为电解液,以铂片(规格30*25*0.1mm)为辅助电极,以银/氯化银电极为参比电极,组成三电极体系。在-0.2~0.8V电压范围内通过循环伏安法测试电极的电容量,扫速从大到小为300mv/s、200mv/s、100mv/s、50mv/s、20mv/s、10mv/s,扫描圈数为10圈;通过恒电流充放电测试电极在不同电流密度下的电容量,电流密度由大到小为1A/g、2A/g、5A/g、10A/g;所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)作为超级电容器电极材料的比容量为85F/g。
实施例2
其与实施1不同之处在于,步骤(1)中,在三电极电解池体系中,配制EDOT(0.07109g,0.5mmol),TEAPF6(2.7522g,0.01mol),二氯甲烷(100mL)的电解液,以氧化铟锡导电玻璃(2.77145g)电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,以饱和的氯化钾水溶液为第一液接,以所述的电解液为第二液接。在室温下采用恒电位1.4V进行电化学聚合,聚合电量0.10C,然后在负电位-0.8V下脱掺杂70s,得到沉积在工作电极上的聚合物薄膜,用二氯甲烷淋洗去除聚合物薄膜表面残留的电解液并在60℃真空干燥箱中干燥12h后得到聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD),称取该聚合物薄膜质量为2.77159g。该沉积有聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的ITO工作电极即用作超级电容器电极。所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)作为超级电容器电极材料的比容量为83F/g。
实施例3
其与实施1不同之处在于,步骤(1)中,在三电极电解池体系中,配制EDOT(0.07109g,0.5mmol),TEAPF6(2.7522g,0.01mol),二氯甲烷(100mL)的电解液,以氧化铟锡导电玻璃(2.77292g)电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,以饱和的氯化钾水溶液为第一液接,以所述的电解液为第二液接。在室温下采用恒电位1.4V进行电化学聚合,聚合电量0.15C,然后在负电位-0.8V下脱掺杂80s,得到沉积在工作电极上的聚合物薄膜,用二氯甲烷淋洗去除聚合物薄膜表面残留的电解液并在60℃真空干燥箱中干燥12h后得到聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD),称取所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)质量为2.77303g。该沉积有聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的ITO工作电极即用作超级电容器电极。所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)作为超级电容器电极材料的比容量为86F/g。
实施例4
其与实施1不同之处在于,步骤(1)中,在三电极电解池体系中,配制EDOT(0.07109g,0.5mmol),TEAPF6(2.7522g,0.01mol),二氯甲烷(100mL)的电解液,以氧化铟锡导电玻璃(2.77863g)电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,以饱和的氯化钾水溶液为第一液接,以所述的电解液为第二液接。在室温下采用恒电位1.4V进行电化学聚合,聚合电量0.20C,然后再负电位-0.8V下脱掺杂90s,得到沉积在工作电极上的聚合物薄膜,用二氯甲烷淋洗去除聚合物薄膜表面残留的电解液并在60℃真空干燥箱中干燥12h后得到聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD),称取聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)质量为2.77878g。该沉积有聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)的ITO工作电极即用作超级电容器电极。所述的聚3,4-乙烯二氧噻吩纳米网状薄膜(PEDOT-PD)作为超级电容器电极材料的比容量为87F/g。
Claims (10)
1.一种聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD。
2.如权利要求1所述的聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD,其特征在于:所述的聚3,4-乙烯二氧噻吩纳米网状薄膜具体按如下方法进行制备:
在三电极电解池体系中,以3,4-乙烯二氧噻吩为单体,以四乙基六氟磷酸铵为支持电解质,以二氯甲烷为电解溶剂,混合均匀得到电解液,以氧化铟锡导电玻璃电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,在室温下采用恒电位法电化学聚合得到聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD。
3.如权利要求2所述的聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD的制备方法,其特征在于:所述的方法具体按照如下步骤进行制备:
在三电极电解池体系中,以3,4-乙烯二氧噻吩为单体,以四乙基六氟磷酸铵为支持电解质,以二氯甲烷为电解溶剂,混合均匀得到电解液,以氧化铟锡导电玻璃电极为工作电极,以铂电极为辅助电极,以银/氯化银电极为参比电极,在室温下采用恒电位法,在1.3~1.7V电压条件下进行电化学聚合反应,当聚合电量达到0.05~0.2C时,聚合结束,在-1~-0.7V负电位下脱掺杂50~100s,得到沉积在工作电极上的聚合物薄膜,经淋洗、烘干得到聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD;所述的电解液中,所述的3,4-乙烯二氧噻吩单体的初始终浓度为1~10mmol/L;所述的支持电解质四乙基六氟磷酸铵的初始终浓度为0.01~0.1mol/L。
4.如权利要求3所述的方法,其特征在于:所述的3,4-乙烯二氧噻吩单体的初始终浓度为5mmol/L。
5.如权利要求3所述的方法,其特征在于:所述的支持电解质四乙基六氟磷酸铵的初始终浓度为0.1mol/L。
6.如权利要求3所述的方法,其特征在于:所述的工作电极在使用前先依次经过质量分数为0.3%氢氧化钠溶液、乙醇、丙酮、甲苯、乙醇、丙酮分别超声清洗15~20min,然后用氮气吹干所述的工作电极表面剩余溶剂后置于60℃真空干燥箱干燥1~2h。
7.如权利要求3所述的方法,其特征在于:所述的恒电位聚合法为:所述的聚合电压为1.4V。
8.如权利要求3所述的方法,其特征在于:所述的脱掺杂负电位为-0.8V。
9.如权利要求3所述的方法,其特征在于:所述的淋洗、烘干过程具体操作为:用二氯甲烷淋洗沉积在工作电极上的聚合物薄膜,然后将所述的聚合物薄膜置于60~80℃真空干燥箱中干燥10~12h,得到成品聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD。
10.一种如权利要求1所述的聚3,4-乙烯二氧噻吩纳米网状薄膜PEDOT-PD在制备超级电容器电极中的应用。
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