CN111653433B - 聚苯胺/银纳米线棉纤维电容器电极材料及制备方法 - Google Patents
聚苯胺/银纳米线棉纤维电容器电极材料及制备方法 Download PDFInfo
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Abstract
本发明涉及一种聚苯胺/银纳米线棉纤维电容器电极材料及制备方法,其赋予棉纤维良好的导电性、高电容量、高循环性。本发明包括如下步骤:步骤一:以银纳米线、棉织物为原料,通过浸渍法并控制浸渍的次数,得到高导电的银纳米线/棉纤维;步骤二:采用质量百分比为1%‑5%的γ―(2,3‑环氧丙氧)丙基三甲氧基硅烷KH‑560对银纳米线/棉纤维进行改性,控制环氧基的接枝率,得到环氧基银纳米线/棉纤维;步骤三:以0.500‑3.500质量份的苯胺、22.5质量份的过硫酸铵、1.250‑8.750质量份的盐酸、环氧基银纳米线/棉纤维为原料,通过原位聚合法,得到聚苯胺/银纳米线棉纤维柔性电容器电极材料。
Description
技术领域:
本发明涉及一种纤维基电极材料及制备方法,尤其是涉及一种聚苯胺/银纳米线棉纤维电容器电极材料及制备方法。
背景技术:
纺织纤维具有足够的韧性和强度,廉价易得,应用广泛,是高性能电容器基板的理想选择。纤维基高性能电容器是一种构建在纺织或纤维表面的高性能电容器,不仅具有充放电快、轻便灵活的优点,还可用于制备柔性可穿戴储能装置,同时可以进一步拓展智能纺织品的应用范围。
纳米银具有优良的导电性,在电化学反应中常被用作透明电极。随着纳米尺度的减小,一维银纳米线(AgNWs)不仅具有独特的物理化学性质、规整的形貌、高纵横比和稳定的性能,而且具有良好的导电性、导热性、高柔韧性和高机械强度。将其应用于织物整理时,其互连的导电网络可以赋予织物优异的导电性和柔韧性。同时,银纳米线具有较高的形貌特征,可以作为模板来提高电化学性能,促进电子的有效转移。
聚苯胺(PANI)具有高导电性、高电容性、高稳定性、低成本、电荷转移掺杂和质子化可逆控制等优异性能。但PANI的结构在氧化还原反应中容易被破坏,其循环中性能低于起始时,循环稳定性受到限制。研究人员经常使用导电材料与聚苯胺复合,导电材料被用作稳定聚苯胺的载体,改善聚苯胺的分散性,提高其循环寿命。同时,通过与导电材料的协同配合,使电极具有较高的导电性。
目前还没有将聚苯胺与银纳米线棉纤维结合制备容器电极材料的先例。
发明内容:
本发明的目的在于提供一种聚苯胺/银纳米线棉纤维电容器电极材料及制备方法,其赋予棉纤维良好的导电性、高电容量、高循环性,同时又可以避免铬鞣剂的使用所造成的环境污染和铬资源的浪费问题。
为实现上述目的,本发明采用的技术方案为:
一种聚苯胺/银纳米线棉纤维电容器电极材料,其特征在于:采用以下原料制成:1长度单位×1长度单位的棉织物;0.5mol/L银纳米线溶液;质量百分比1%-5%的γ―(2,3-环氧丙氧)丙基三甲氧基硅烷KH-560;1质量份的NaCl;0.500-3.500质量份的苯胺;22.5质量份的过硫酸铵;1.250-8.750质量份的盐酸;去离子水。
一种聚苯胺/银纳米线棉纤维电容器电极材料的制备方法,其特征在于:由以下步骤实现:
步骤一:以银纳米线、棉织物为原料,通过浸渍法并控制浸渍的次数,得到高导电的银纳米线/棉纤维;
步骤二:采用质量百分比为1%-5%的γ―(2,3-环氧丙氧)丙基三甲氧基硅烷KH-560对银纳米线/棉纤维进行改性,控制环氧基的接枝率,得到环氧基银纳米线/棉纤维;
步骤三:以0.500-3.500质量份的苯胺、22.5质量份的过硫酸铵、1.250-8.750质量份的盐酸、环氧基银纳米线/棉纤维为原料,通过原位聚合法,得到聚苯胺/银纳米线棉纤维柔性电容器电极材料。
由以下具体步骤实现:
步骤一:将1cm×1cm大小的棉织物浸渍在0.5mol/L银纳米线溶液中,一次浸渍时长为1min,通过控制浸渍的次数并在80℃烘干后,得到不同银纳米线负载量的棉织物;
步骤二:将质量百分比1%、2%、3%、4%、5%的KH-560、NaCl 1g溶解于100g去离子水中,滴加0.1mol/L的NaOH溶液,调节其pH为10;在60℃下将银纳米线/棉纤维加入溶液中反应30min后,于80℃下烘干,得到环氧基银纳米线/棉纤维;
步骤三:将0.500-3.500克的苯胺、1.250-8.750克的盐酸、环氧基银纳米线/棉纤维加入到100mL的去离子水中反应30min;将22.5克的的过硫酸铵溶解于50mL的去离子水中后,于30min内缓慢滴加入苯胺-盐酸溶液中,在室温、30rpm的搅拌速度下,反应2h后,将棉织物用去离子水洗涤后在80℃下烘干,得到聚苯胺/银纳米线复合棉纤维柔性电容器电极材料。
与现有技术相比,本发明具有的优点和效果如下:
1、本发明制备的聚苯胺/银纳米线棉纤维电容器电极材料,利用聚苯胺和银纳米线在棉纤维上组装形成相互贯通的导电通路,从而构筑纤维基高性能电容器的电极材料,利用聚苯胺和银纳米线的协同作用实现柔性电极材料的高导电性;通过银纳米线/棉纤维上环氧基团与苯胺中的氨基发生开环反应,将聚苯胺高分子链固定在银纳米线/棉纤维上,防止其脱掺杂,改善其循环性能,从而获得一种集高导电、比容量、循环性能为一体的柔性电容器电极材料。
2、本发明在棉纤维表面附着聚苯胺与银纳米线,获得高导电性能、多次循环寿命的柔性电极材料。首先对棉纤维进行表面环氧化修饰,进而通过原位聚合法制得PANI/AgNWs/棉纤维,使PANI与银纳米线形成相互贯通的导电通路。银纳米线的一维结构能够在棉纤维之间相互交织,形成导电网络;同时,银纳米线上环氧基团与苯胺中的氨基发生开环反应,将PANI高分子链固定在环氧基AgNWs/棉纤维上,从而获得一种集高导电、比容量、循环性能的柔性电容器电极材料。
具体实施方式:
下面结合具体实施方式对本发明进行详细的说明。这些实施例是用于说明本发明而不限于本发明的范围。实施例中采用的实施条件可以根据具体实验环境做进一步调整,未注明的实施条件通常为常规实验中的条件。
本发明涉及一种聚苯胺/银纳米线棉纤维电容器电极材料及制备方法,
本发明聚苯胺/银纳米线棉纤维电容器电极材料采用以下原料制成:1长度单位×1长度单位的棉织物;0.5mol/L银纳米线溶液;质量百分比1%-5%的γ―(2,3-环氧丙氧)丙基三甲氧基硅烷KH-560;1质量份的NaCl;0.500-3.500质量份的苯胺;22.5质量份的过硫酸铵;1.250-8.750质量份的盐酸;去离子水。
本发明基于聚苯胺/银纳米线棉纤维电容器电极材料的制备方法,由以下步骤实现:
步骤一:以银纳米线、棉织物为原料,通过浸渍法并控制浸渍的次数,得到高导电的银纳米线/棉纤维。具体步骤为:
将1cm×1cm大小的棉织物浸渍在银纳米线(0.5mol/L)溶液中,通过控制浸渍的次数(一次浸渍时长为1min)并在80℃烘干后,得到了不同银纳米线负载量的棉织物。
步骤二:采用质量百分比为1%-5%的γ―(2,3-环氧丙氧)丙基三甲氧基硅烷KH-560对银纳米线/棉纤维进行改性,控制环氧基的接枝率,得到环氧基银纳米线/棉纤维。具体步骤为:
将质量百分比为1%、2%、3%、4%、5%的KH-560、NaCl(1g)溶解于100g去离子水中,滴加0.1mol/L的NaOH溶液,调节其pH为10;在60℃下将银纳米线/棉纤维加入溶液中反应30min后,于80℃下烘干,得到环氧基银纳米线/棉纤维;
步骤三:以0.500-3.500质量份的苯胺、22.5质量份的过硫酸铵、1.250-8.750质量份的盐酸、环氧基银纳米线/棉纤维为原料,通过原位聚合法,得到聚苯胺/银纳米线棉纤维柔性电容器电极材料。具体步骤为:
将0.500-3.500克的苯胺、1.250-8.750克的盐酸、环氧基银纳米线/棉纤维加入到100mL的去离子水中反应30min;将22.5克的的过硫酸铵溶解于50mL的去离子水中后,于30min内缓慢滴加入苯胺-盐酸溶液中,在室温、30rpm的搅拌速度下,反应2h后,将棉织物用去离子水洗涤后在80℃下烘干,得到聚苯胺/银纳米线复合棉纤维柔性电容器电极材料。
实施例1:
第一步:银纳米线/棉纤维的制备:
将1cm×1cm大小的棉织物浸渍在银纳米线(0.5mol/L)溶液中,浸渍1次并在80℃烘干后,得到了负载9.8mg银纳米线的棉织物;
第二步:环氧基银纳米线/棉纤维的制备:
将0.700g的KH-560、NaCl(1g)溶解于100g去离子水中,滴加0.1mol/L的NaOH溶液,调节其pH为10。在60℃下将银纳米线/棉纤维加入溶液中反应30min后,于80℃下烘干,得到环氧基银纳米线棉纤维;
第三步:聚苯胺/银纳米线复合棉纤维柔性电容器电极材料的制备:
将0.500g的苯胺、1.250g的盐酸、环氧基银纳米线/棉纤维加入到100mL的去离子水中反应30min;将22.5g的过硫酸铵溶解于50mL的去离子水中后,于30min内缓慢滴加入苯胺-盐酸溶液中,在室温、30rpm的搅拌速度下,反应2h后,将棉织物用去离子水洗涤后在80℃下烘干,得到聚苯胺/银纳米线复合棉纤维柔性电容器电极材料。
实施例2:
第一步:银纳米线/棉纤维的制备:
将1cm×1cm大小的棉织物浸渍在银纳米线(0.5mol/L)溶液中,浸渍3次并在80℃烘干后,得到了负载12mg银纳米线的棉织物;
第二步:环氧基银纳米线/棉纤维的制备:
将1.400g的KH-560、NaCl(1g)溶解于100g去离子水中,滴加0.1mol/L的NaOH溶液,调节其pH为10。在60℃下将银纳米线/棉纤维加入溶液中反应30min后,于80℃下烘干,得到环氧基银纳米线/棉纤维;
第三步:聚苯胺/银纳米线复合棉纤维柔性电容器电极材料的制备:
将2.100g的苯胺、5.250g的盐酸、环氧基银纳米线/棉纤维加入到100mL的去离子水中反应30min;将22.5g的过硫酸铵溶解于50mL的去离子水中后,于30min内缓慢滴加入苯胺-盐酸溶液中,在室温、30rpm的搅拌速度下,反应2h后,将棉织物用去离子水洗涤后在80℃下烘干,得到聚苯胺/银纳米线复合棉纤维柔性电容器电极材料。
实施例3:
第一步:银纳米线/棉纤维的制备:
将1cm×1cm大小的棉织物浸渍在银纳米线(0.5mol/L)溶液中,浸渍5次并在80℃烘干后,得到了负载21.5mg银纳米线的棉织物;
第二步:环氧基银纳米线/棉纤维的制备:
将2.100g的KH-560、NaCl(1g)溶解于100g去离子水中,滴加0.1mol/L的NaOH溶液,调节其pH为10。在60℃下将银纳米线/棉纤维加入溶液中反应30min后,于80℃下烘干,得到环氧基银纳米线/棉纤维;
第三步:聚苯胺/银纳米线复合棉纤维柔性电容器电极材料的制备:
将3.500g的苯胺、8.750g的盐酸、环氧基银纳米线/棉纤维加入到100mL的去离子水中反应30min;将22.5g的过硫酸铵溶解于50mL的去离子水中后,于30min内缓慢滴加入苯胺-盐酸溶液中,在室温、30rpm的搅拌速度下,反应2h后,将棉织物用去离子水洗涤后在80℃下烘干,得到聚苯胺/银纳米线复合棉纤维柔性电容器电极材料。
采用实施例1方法制得一种聚苯胺/银纳米线复合棉纤维柔性电容器电极材料,当银纳米线浸渍次数为5次,KH-560的添加量为3%,苯胺质量为300wt%时,得到的电极材料的比容量最高可达154F/g、循环5000次充放电后,电容可保持在原来的96%。而聚苯胺/棉纤维柔性电容器电极材料的比容量最高可达64F/g,且电极材料在充放电5000次后比容量可保持初始值的76%,因此可以表明聚苯胺/银纳米线复合棉纤维柔性电容器电极材料具有高点容量和良好的循环性能。
上述实施例仅例示性说明本发明的原理及其功效,对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (3)
1.一种聚苯胺/银纳米线棉纤维电容器电极材料,其特征在于:采用以下原料制成:1长度单位×1长度单位的棉织物;0.5mol/L银纳米线溶液;质量百分比1%-5%的γ―(2,3-环氧丙氧)丙基三甲氧基硅烷KH-560;1质量份的NaCl;0.500-3.500质量份的苯胺;22.5质量份的过硫酸铵;1.250-8.750质量份的盐酸;去离子水。
2.一种聚苯胺/银纳米线棉纤维电容器电极材料的制备方法,其特征在于:由以下步骤实现:
步骤一:以银纳米线、棉织物为原料,通过浸渍法并控制浸渍的次数,得到高导电的银纳米线/棉纤维;
步骤二:采用质量百分比为1%-5%的γ―(2,3-环氧丙氧)丙基三甲氧基硅烷KH-560对银纳米线/棉纤维进行改性,控制环氧基的接枝率,得到环氧基银纳米线/棉纤维;
步骤三:以0.500-3.500质量份的苯胺、22.5质量份的过硫酸铵、1.250-8.750质量份的盐酸、环氧基银纳米线/棉纤维为原料,通过原位聚合法,得到聚苯胺/银纳米线棉纤维柔性电容器电极材料。
3.根据权利要求2所述的聚苯胺/银纳米线棉纤维电容器电极材料的制备方法,其特征在于:
由以下步骤实现:
步骤一:将1cm×1cm大小的棉织物浸渍在0.5mol/L银纳米线溶液中,一次浸渍时长为1min,通过控制浸渍的次数并在80℃烘干后,得到不同银纳米线负载量的棉织物;
步骤二:将质量百分比1%、2%、3%、4%、5%的KH-560、NaCl 1g溶解于100g去离子水中,滴加0.1mol/L的NaOH溶液,调节其pH为10;在60℃下将银纳米线/棉纤维加入溶液中反应30min后,于80℃下烘干,得到环氧基银纳米线/棉纤维;
步骤三:将0.500-3.500克的苯胺、1.250-8.750克的盐酸、环氧基银纳米线/棉纤维加入到100mL的去离子水中反应30min;将22.5克的的过硫酸铵溶解于50mL的去离子水中后,于30min内缓慢滴加入苯胺-盐酸溶液中,在室温、30rpm的搅拌速度下,反应2h后,将棉织物用去离子水洗涤后在80℃下烘干,得到聚苯胺/银纳米线复合棉纤维柔性电容器电极材料。
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