CN108538646B - 一种纳米花状聚吡咯氧化锰复合材料的制备方法及应用 - Google Patents
一种纳米花状聚吡咯氧化锰复合材料的制备方法及应用 Download PDFInfo
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 66
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- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 5
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Abstract
本发明属于纳米材料制备技术领域,特别涉及纳米花状聚吡咯‑氧化锰复合材料的制备方法。利用氧化锰(MnO2)与导电聚合物电化学共沉积,制备了具有大电位窗范围(‑0.3~0.9V vs.SCE)的纳米花状聚吡咯‑氧化锰复合材料,该材料可用作超级电容器电极材料,并有效扩大了氧化锰(0~0.9V vs.SCE)和聚吡咯(‑0.3~0.5V vs.SCE)的储能电位范围;本发明所采用的电化学共沉积方法制备方便快速、对环境友好,并且具有实验反应条件易于控制,产品无需后处理等特点。
Description
技术领域
本发明属于纳米材料制备技术领域,特别涉及纳米花状聚吡咯-氧化锰复合材料的制备方法及应用。
背景技术
利用氧化锰(MnO2)与导电聚合物电化学共沉积,制备了具有大电位窗范围的纳米花状聚吡咯-氧化锰复合材料,该材料可用作超级电容器电极材料,对新型储能材料的发展有着重要的意义。聚吡咯(PPy)是一种典型的导电聚合物,其研究可追溯到1916年,人们合成出了PPy粉末;上世纪初Angeli等已通过氧化吡咯首次制得了聚吡咯;1968年Dallolio等在硫酸水溶液中采用电化学的方法制备出导电PPy膜;1979年Diaz和Kanazawa等人首次在有机溶剂乙腈中以电化学方法,通过阳极氧化反应,在铂电极表面可以得到了一种柔性的、性能较稳定的优质导电PPy薄膜,其电导率高达100S·cm-1,从此PPy受到学界的广泛关注。此后人们便开始对其合成结构性能及应用等进行研究目前已初步显示出它的理论价值和实际应用前景。
PPy是由吡咯单体聚合而成的一种新型导电聚合物;由于吡咯单体的α和β位具有相近的聚合能力,聚合过程中极易交联成颗粒状的PPy。研究证明,PPy的骨架结构是吡咯单体环的(2,5)偶联;在整个PPy分子骨架结构中相邻吡咯环的排列方向不同,因此PPy分子中由两个吡咯环构成一个重复单元,PPy中的N是sp2杂化,N上孤对电子参与形成π共轭体系,难以质子化,碱性很弱,因此Py的α位为活性位点;本征态PPy导电性很差,并且难溶于有机溶液,难于加工,这些因素制约了它的应用,通常制备的PPy以菜花状结构存在。
目前普遍用表面活性剂或者掺杂离子的办法以制备大比表面积的PPy,进而提高PPy的导电能力和存储电荷的能力。采用“掺杂”的方法,即采用化学或电化学方法使导电聚合物发生氧化还原反应,从而具有导电能力;其原理是利用“掺杂”来改变其能带填充状况或减小能带分裂造成的能级差;即将电子从导电聚合物顶部移出或者向底部注入电子,使导电聚合物离子化。在合成过程中加入各种掺杂剂以及与纳米粒子进行掺杂或复合,不仅可有效地提高PPy的电导率,而且还可改善其热稳定性、机械延展性以及光电性能,因而成为国内外研究的热点。
聚吡咯与氧化锰电化学共沉积,则可利用氧化锰的纳米花状结构进一步引导吡咯聚合时电极表面的结构,进而制备出纳米花状聚吡咯-氧化锰复合材料。
发明内容
常情况下PPy均以不规则颗粒形式存在,这不利于其与电解液充分接触,不利于发挥其电荷存储能力。前人尝试了利用软硬模板法的办法来改变聚吡咯的形貌结构,从而提高其导电性。
本发明的目的之一在于利用MnO2纳米花活性种子控制PPy的聚合,提供一种制备纳米花状聚吡咯-氧化锰复合材料的方法;
本发明的目的之二在于提供一种合成的一维结构的PPy,增大了PPy的导电率;
本发明的目的之三在于提供一种简单方便快捷的制备纳米花状聚吡咯-氧化锰复合材料的方法,该制备工艺简单、成本低,对环境无污染、符合绿色化学的要求;
为达到上述目的,本发明提供了一种简单的制备纳米花状聚吡咯-氧化锰复合材料的方法。该方法包括如下步骤:
包括如下步骤:取乙酸锰、乙酸铵和吡咯,在恒电位条件下反应,在碳材料上电化学共沉积氧化锰和聚吡咯,制备纳米花状聚吡咯-氧化锰复合材料,然后用去离子水冲洗,烘干。
取0.03M乙酸锰、0.05M乙酸铵和0.2mL吡咯,在恒电位0.9Vvs.SCE条件下反应45分钟,在碳材料上电化学共沉积氧化锰和聚吡咯,制备纳米花状聚吡咯-氧化锰复合材料;然后用去离子水冲洗,烘干。
本发明的有益效果:
利用氧化锰(MnO2)与导电聚合物电化学共沉积,制备了具有大电位窗范围(-0.3~0.9V vs.SCE)的纳米花状聚吡咯-氧化锰复合材料,该材料可用作超级电容器电极材料,并有效扩大了氧化锰(0~0.9V vs.SCE)和聚吡咯(-0.3~0.5V vs.SCE)的储能电位范围。由此可见,氧化锰与聚吡咯的复合,扩展了储能电位窗,同时纳米花状结构的复合材料为电极活性材料与电解液有效接触且充分发挥储能性能奠定了基础,有效提高电极材料的存储电荷的能力,满足储能设备的发展需求。相关工作可为聚吡咯的形貌结构提供新的研究路线。
电化学共沉积方法制备方便快速、对环境友好,并且具有实验反应条件易于控制,产品无需后处理等特点。
附图说明
为了便于本领域技术人员理解,下面结合附图对本发明作进一步的说明。
图1为纳米花状聚吡咯-氧化锰复合材料的SEM图片;
图2为本发明纳米花状聚吡咯-氧化锰复合材料和聚吡咯的充放电曲线图;
图3为纳米花状聚吡咯-氧化锰复合材料和聚吡咯的交流阻抗图谱图。
具体实施方式
实施例1
取0.03M乙酸锰、0.05M乙酸铵和0.2mL吡咯,在恒电位0.9Vvs.SCE条件下反应45分钟,在碳材料上电化学共沉积氧化锰和聚吡咯,制备纳米花状聚吡咯-氧化锰复合材料;然后用去离子水冲洗,烘干。即聚吡咯与氧化锰电化学共沉积,则可利用氧化锰的纳米花状结构进一步引导吡咯聚合时电极表面的结构,进而制备出纳米花状聚吡咯-氧化锰复合材料,如图1。
在0.5M Na2SO4溶液中对纳米花状聚吡咯-氧化锰复合材料和聚吡咯在2mA/cm2进行恒电位充放电应用,如图2所示,纳米花状聚吡咯-氧化锰复合材料的放电时间较长,存储电荷能力远远优于聚吡咯。纳米花状的复合结构增加了材料的比表面积,进而增大了与电解液接触的空间。
实施例2
在0.5M Na2SO4溶液中对纳米花状聚吡咯-氧化锰复合材料和聚吡咯进行交流阻抗应用,如图3所示,在高频域中没有半圆形出现,表明电极和电解质界面的电荷转移电阻是可以忽略不计的。在低频领域,纳米花状聚吡咯-氧化锰复合材料显示陡峭的斜坡,这意味着它有小于聚吡咯的离子扩散电阻。
实施例3
将实施例1所制备的纳米花状聚吡咯-氧化锰复合材料和聚吡咯组装成对称型超级电容器,有纳米花状聚吡咯-氧化锰复合材料和聚吡咯组装的器件在小于1分钟在充电的情况下,可以给LED灯泡供电7分钟。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节,也不限制该发明仅为所述的具体实施方式。显然,根据本说明书的内容,可作很多的修改和变化。本说明书选取并具体描述这些实施例,是为了更好地解释本发明的原理和实际应用,从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (1)
1.一种纳米花状聚吡咯氧化锰复合材料的制备方法,其特征在于,包括如下步骤:取乙酸锰、乙酸铵和吡咯,在恒电位条件下反应,在碳材料上电化学共沉积氧化锰和聚吡咯,制备纳米花状聚吡咯-氧化锰复合材料,然后用去离子水冲洗,烘干;
具体包括如下步骤:取 0.03 M 乙酸锰、0.05 M 乙酸铵和0.2 mL吡咯,在相对饱和甘汞电极为恒电位0.9 V的条件下反应45分钟,在碳材料上电化学共沉积氧化锰和聚吡咯,制备纳米花状聚吡咯-氧化锰复合材料,然后用去离子水冲洗,烘干;
制备的纳米花状聚吡咯氧化锰复合材料,具有大电位窗,相对饱和甘汞电极为恒电位的范围是:-0.3 ~ 0.9 V;
该材料可用作超级电容器电极材料,和聚吡咯可组装成对称型超级电容器。
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