CN110797210B - 一种聚3,4-乙撑二氧噻吩柔性电极材料的制备方法 - Google Patents
一种聚3,4-乙撑二氧噻吩柔性电极材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种聚3,4‑乙撑二氧噻吩柔性电极材料的制备方法,属于超级电容器电极材料制备技术领域。其是先将预处理棉线浸入到3,4‑乙撑二氧噻吩中,再浸入到过硫酸铵的盐酸溶液中,使其经化学氧化制备成所述聚3,4‑乙撑二氧噻吩柔性电极材料。本发明制得的聚3,4‑乙撑二氧噻吩柔性电极材料不仅具有高的比电容和好的循环稳定性,而且原料成本低廉,制备工艺简便,适合大规模工业化生产,具有较高的经济价值和社会效益。
Description
技术领域
本发明属于超级电容器电极材料制备技术领域,具体涉及一种聚3,4-乙撑二氧噻吩柔性电极材料的制备方法。
背景技术
柔性线状超级电容器由于其具有充放电速度快、功率密度高、循环寿命长、重量轻和灵活性好等优点,被认为是可穿戴设备实现广泛应用的必要元器件。棉线具有成本低、比表面积大、溶液易渗透等优势,已经成为柔性电极材料理想的柔性基底。聚3,4-乙撑二氧噻吩具有较窄的能隙、较高的电导率、较好的成膜性和优良的环境稳定性,是一种重要的超级电容器电极材料。Chayanika Das(Chayanika Das, Kothandam Krishnamoorthy;Flexible microsupercapacitors using silk and cotton substrates, ACS AppliedMaterials & Interfaces, 2016, 8(43): 29504-29510)先采用化学方法在棉线上沉积一层金属金,然后利用电化学方法在金的表面聚合聚3,4-乙撑二氧噻吩,结果显示,当充放电电流密度为1 A/g时,产物具有最高的比电容,其值为250 F/g。但是,这种方法的原料价格较高,生产工艺复杂,且不易实现大规模工业化生产。
发明内容
本发明针对现有聚3,4-乙撑二氧噻吩负载棉线柔性电极材料的原料价格较高、生产工艺复杂以及不易实现大规模工业化生产等问题,提供了一种新的聚3,4-乙撑二氧噻吩柔性电极材料的制备方法。其制得的聚3,4-乙撑二氧噻吩柔性电极材料不仅具有高的比电容和好的循环稳定性,而且其原料成本低廉,制备工艺简便,适合大规模工业化生产,具有较高的经济价值和社会效益。
为实现上述目的,本发明采用如下技术方案:
一种聚3,4-乙撑二氧噻吩柔性电极材料的制备方法,其是先将预处理棉线浸入3,4-乙撑二氧噻吩中,再将吸附有3,4-乙撑二氧噻吩的棉线浸入到过硫酸铵的盐酸溶液中,使其在超声作用进行化学氧化。其具体包括以下步骤:
(1)将棉线置于去离子水中,室温下超声30 min后取出,沥干棉线上的水分后,再置于无水乙醇中,在室温下继续超声30 min,取出,60 ℃真空干燥24 h制得所述预处理棉线;
(2)将1~2 g直径为0.2~0.4 mm的预处理棉线置于20 mL 3,4-乙撑二氧噻吩中,室温下超声5~10 min后取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(3)将步骤(2)制得的吸附有3,4-乙撑二氧噻吩的棉线置于过硫酸铵的盐酸溶液中,在室温下超声1~4 h;反应结束后,用甲醇和去离子水交替洗涤2~4次,再于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线,即所述聚3,4-乙撑二氧噻吩柔性电极材料。
所述过硫酸铵的盐酸溶液中,过硫酸铵的浓度为1 mol/L,盐酸的浓度为1 mol/L,溶剂为去离子水。
本发明的显著优点在于:
(1)棉线具有体积小、价格低、来源广和质量轻等特点,采用棉线作为载体材料制备的柔性超级电容器具有良好的可弯曲折叠性,在便携式可佩戴电子设备中具有巨大应用潜力。
(2)在棉线上聚合的聚3,4-乙撑二氧噻吩呈疏松多孔结构,改变了本征态聚3,4-乙撑二氧噻吩堆积致密的缺点,增加了电极材料与电解液的界面面积,能够促进电荷的传导和离子的迁移。
(3)本发明制备的聚3,4-乙撑二氧噻吩柔性电极材料具有较高的比电容和良好的循环稳定性,在充放电电流密度分别为0.2 A/g、0.5 A/g、1 A/g和2 A/g时,比电容分别为255 F/g、226 F/g、208 F/g和197 F/g,循环2000次后,比电容的保持率为92 %,而且原料成本低廉,制备工艺简便,适合大规模工业化生产,具有较高的经济价值和社会效益。
附图说明
图1为实施例1制备的聚3,4-乙撑二氧噻吩负载棉线的红外吸收光谱图;
图2为预处理棉线(A)与实施例1制备的聚3,4-乙撑二氧噻吩负载棉线(B)的扫描电镜图。
图3为市售棉线(A)与对比例1制备的聚3,4-乙撑二氧噻吩负载棉线(B)的扫描电镜图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
所用预处理棉线是将市售棉线置于去离子水中,室温下超声30 min后取出,沥干棉线上的水分后,再置于无水乙醇中,在室温下继续超声30 min,取出,于60 ℃真空干燥24h制得。
实施例1
(1)将1.5 g直径为0.3 mm的预处理棉线置于20 mL 3,4-乙撑二氧噻吩中,在室温下超声8 min,取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于含1 mol/L过硫酸铵的浓度为1 mol/L的盐酸水溶液中,在室温下超声3 h;反应结束后,用甲醇和去离子水交替洗涤3次,于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线,即所述聚3,4-乙撑二氧噻吩柔性电极材料。
图1为本实施例制备的聚3,4-乙撑二氧噻吩负载棉线的红外吸收光谱图。从图中可以看出,2918 cm-1和2837 cm-1处的吸收峰对应3,4-乙撑二氧噻吩的亚甲基C-H伸缩振动吸收峰,1639 cm-1和1371 cm-1处的吸收峰分别对应噻吩环上C=C和C-C的伸缩振动吸收峰,667 cm-1和613 cm-1处的吸收峰对应噻吩环上C-S-C的弯曲振动吸收峰,这说明聚3,4-乙撑二氧噻吩成功负载在棉线上。
图2为所用预处理棉线(A)与本实施例制备的聚3,4-乙撑二氧噻吩负载棉线(B)的扫描电镜图。从图中可以看出,经去离子水和无水乙醇处理后棉线表面比较粗糙,有利于聚3,4-乙撑二氧噻吩在棉线表面的均匀负载,且负载后的棉线呈疏松多孔的结构,该结构能够增加电极材料与电解液的界面面积,促进电荷的传导和离子的迁移。
实施例2
(1)将1 g直径为0.2 mm的预处理棉线置于20 mL 3,4-乙撑二氧噻吩中,在室温下超声5 min,取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于含1 mol/L过硫酸铵的浓度为1 mol/L的盐酸水溶液中,在室温下超声1 h;反应结束后,用甲醇和去离子水交替洗涤2次,于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线,即所述聚3,4-乙撑二氧噻吩柔性电极材料。
实施例3
(1)将2 g直径为0.4 mm的预处理棉线置于20 mL 3,4-乙撑二氧噻吩中,在室温下超声10 min,取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于含1 mol/L过硫酸铵的浓度为1 mol/L的盐酸水溶液中,在室温下超声4 h;反应结束后,用甲醇和去离子水交替洗涤4次,于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线,即所述聚3,4-乙撑二氧噻吩柔性电极材料。
对比例1
(1)将1.5 g直径为0.3 mm的市售棉线置于20 mL 3,4-乙撑二氧噻吩中,在室温下超声8 min,取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于含1 mol/L过硫酸铵的浓度为1 mol/L的盐酸水溶液中,在室温下超声3 h;反应结束后,用甲醇和去离子水交替洗涤3次,于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线。
图3为市售棉线(A)与本对比例制备的聚3,4-乙撑二氧噻吩负载棉线(B)的扫描电镜图。从图中可以看出,市售棉线的表面比较光滑致密,这使聚3,4-乙撑二氧噻吩在棉线上的负载量偏少,且分布不均匀,这不利于提高聚3,4-乙撑二氧噻吩负载棉线的电化学性能。
对比例2
(1)将1 g直径为0.2 mm的市售棉线置于20 mL 3,4-乙撑二氧噻吩中,在室温下超声5 min,取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于含1 mol/L过硫酸铵的浓度为1 mol/L的盐酸水溶液中,在室温下超声1 h;反应结束后,用甲醇和去离子水交替洗涤2次,于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线。
对比例3
(1)将2 g直径为0.4 mm的市售棉线置于20 mL 3,4-乙撑二氧噻吩中,在室温下超声10 min,取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于含1 mol/L过硫酸铵的浓度为1 mol/L的盐酸水溶液中,在室温下超声4 h;反应结束后,用甲醇和去离子水交替洗涤4次,于60 ℃真空干燥24 h,制得聚3,4-乙撑二氧噻吩负载棉线。
性能测试
将0.2 g羧基化纤维素纳米纤维、0.5 g石墨烯和0.1 g十二烷基硫酸钠加入到10g去离子水中,室温超声1 h,制得石墨浆料。在尺寸为3 cm×2 cm的石墨纸上均匀涂覆2 g石墨浆料后,将实施例或对比例制得的聚3,4-乙撑二氧噻吩负载棉线均匀摆放在石墨纸上。将石墨纸三等分对折(1 cm×2 cm),以牢固包裹棉线,于60 ℃下真空干燥24 h,制得工作电极;然后以铂丝作为对电极,以饱和甘汞电极作为参比电极,以1 mol/L硫酸水溶液作为电解液组装电容器,利用恒流充放电方法测试比电容,利用循环伏安法测试电化学循环稳定性,其中,电压范围为-0.2 V~0.8 V,充放电电流密度分别为0.2 A/g、0.5 A/g、1 A/g和2 A/g,扫描速率为100 mV/s,测试结果如表1所示。
表1 性能测试结果
从性能测试结果可以看出,实施例所制得的聚3,4-乙撑二氧噻吩柔性电极材料均具有较高的比电容和良好的循环稳定性。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (3)
1.一种聚3,4-乙撑二氧噻吩柔性电极材料的制备方法,其特征在于:先将预处理棉线浸入3,4-乙撑二氧噻吩中,再将吸附有3,4-乙撑二氧噻吩的棉线浸入到过硫酸铵的盐酸溶液中,使其在超声作用下进行化学氧化;
所述预处理棉线是将棉线置于去离子水中,室温下超声30 min后取出,沥干棉线上的水分后,再置于无水乙醇中,在室温下继续超声30 min,取出,真空干燥制得。
2.根据权利要求1所述的聚3,4-乙撑二氧噻吩柔性电极材料的制备方法,其特征在于:具体包括以下步骤:
(1)将1~2 g直径为0.2~0.4 mm的预处理棉线置于20 mL 3,4-乙撑二氧噻吩中,室温下超声5~10 min后取出,制得吸附有3,4-乙撑二氧噻吩的棉线;
(2)将步骤(1)制得的吸附有3,4-乙撑二氧噻吩的棉线置于过硫酸铵的盐酸溶液中,在室温下超声1~4 h;反应结束后,用甲醇和去离子水交替洗涤2~4次,再于60 ℃真空干燥24h,制得所述聚3,4-乙撑二氧噻吩柔性电极材料。
3. 根据权利要求1所述的聚3,4-乙撑二氧噻吩柔性电极材料的制备方法,其特征在于:所述过硫酸铵的盐酸溶液中,过硫酸铵的浓度为1 mol/L,盐酸的浓度为1 mol/L,溶剂为去离子水。
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