摘要
超级电容器作为一种介于传统电容器和电池之间的新型储能器件,已经成为了人们关注和研究的热点。导电聚苯胺(PANI)原料易得、合成简便、成本低廉,具有良好的化学稳定性、导电性和赝电容储能特性,被认为是一种极具发展潜力的超级电容器电极材料。特别是具有一维纳米结构的聚苯胺纤维,还具有高比表面积、高长径比和高孔隙率等特点,因而在电极材料领域具有重要的研究价值。
本文在文献调研基础上,通过选取简便易行的方法合成聚苯胺纳米纤维,系统研究和优化了工艺技术条件,实现了聚苯胺的形貌可控合成；研究了不同形貌聚苯胺电极在硫酸水溶液中的电化学电容性能；对聚苯胺纳米纤维进行了结构修饰,研究了不同结构修饰技术对聚苯胺电极电容特性的影响；采用金属离子对聚苯胺进行掺杂,考察了不同金属离子掺杂聚苯胺电极的电容特性；在此基础上,制备了聚苯胺纳米纤维/活性炭复合材料,研究了复合材料在水系及有机系超级电容器中的电容性能,主要研究结果如下：
(1)采用化学滴加法、快速混合法以及界面聚合法,通过精确调控合成工艺,可以制备出尺寸均一、形貌规整的聚苯胺纳米纤维,纤维直径在50～100nm之间、长度为500nm至几微米不等；其中化学滴加法和快速混合法具有操作简便、生产效率高、成本低廉等优势,有望实现产业化。
(2)在硫酸水溶液中,聚苯胺纳米纤维具有比聚苯胺颗粒更高的比容量,0.1A·g-1电流密度下,聚苯胺纳米长纤维的比容量达404F·g-1,聚苯胺纳米短纤维的比容量更高达436F·g-1,而聚苯胺颗粒的比容量仅为392F·g-1。与聚苯胺颗粒相比,聚苯胺纳米长纤维具有更好的功率性能和循环性能,电流密度从0.1A·g-1增加到0.5A·g-1,比容量仅下降了9.7%,1000次循环后容量衰减了17.5%。
(3)通过大分子有机酸掺杂、共聚和取代的方法实现了聚苯胺的结构修饰。十二烷基苯磺酸(DBSA)和樟脑磺酸(CSA)掺杂聚苯胺具有与盐酸掺杂聚苯胺相当的比容量,但循环性能较差。苯胺与间甲基苯胺共聚所得共聚物PAMD具有与盐酸掺杂聚苯胺相当的导电性和比容量,并且具有更好的循环性能(0.1A·g-1电流密度下比容量为381F·g-1,1000次循环后容量仅衰减15.8%),证实在聚苯胺分子链上引入甲基可以有效改善聚苯胺的循环稳定性。卤代烷与本征态聚苯胺取代反应后得到卤代烷掺杂聚苯胺,其中溴代烷掺杂聚苯胺具有较好的电容特性(0.1A·g-1电流密度下比容量为408F·g-1,1000次循环后容量衰减了20.1%),是一种新型的超级电容器电极材料。
(4)采用LiCl、ZnCl2、MnCl2和FeCl3掺杂本征态聚苯胺,制备了金属盐掺杂聚苯胺纳米纤维材料PLi、PZn、PMn和PFe。发现LiCl、ZnCl2和MnCl2掺杂属赝质子化掺杂,而FeCl3掺杂既存在赝质子化掺杂反应,又发生氧化还原反应。在硫酸水溶液中,PZn具有最好的电容特性(0.1A·g-1电流密度下比容量为340F·g-1,1000次循环后容量衰减25.6%),而PFe不具备电容特性。在LiPF6有机电解液中,金属盐掺杂聚苯胺可获得远高于盐酸掺杂聚苯胺(PH)的比容量(PLi、PZn、PMn的比容量为123F·g-1、147F·g-1和105F·g-1,PH的比容量仅为47F·g-1),同时还能有效改善聚苯胺材料的循环稳定性和电性能,但存在电压降较大、有效储能电位区间窄等问题。
(5)通过聚合过程中原位掺杂,制备了不同金属离子与H+共掺杂聚苯胺纳米纤维材料PHLi、PHZn和PHMn。在硫酸水溶液中,与盐酸掺杂聚苯胺纳米纤维(PH)相比,各种共掺杂聚苯胺材料均具有更高的比容量和更好的循环性能(其中PHZn在0.1A·g-1电流密度下比容量为419F·g-1,比PH(404F·g-1)高15F·g-1,1000次循环后容量仅衰减了11.8%)。(6)通过聚合过程中原位复合,制备了盐酸掺杂聚苯胺纳米纤维/活性炭复合材料,当活性炭添加量为苯胺质量的30%时,复合电极具有最小的电荷转移内阻,并且表现出较好的功率性能和循环性能。硫酸水溶液中,盐酸掺杂聚苯胺纳米纤维/活性炭复合电极(PANI/C30)在0.1A·g-1电流密度下比容量为414F·g-1,1000次循环后容量衰减了14.3%；改性聚苯胺纳米纤维/活性炭复合电极(PANI/C-1)在0.1A·g-1电流密度下比容量达427F·g-1,1000次循环后容量衰减10.3%。在LiPF6有机电解液中,改性聚苯胺纳米纤维/活性炭复合电极(PANI/C-2)的比容量达128F·g-1,放电电压降和循环性能也有所改善。
As a kind of new energy storage device combining advantages of the high specific power of dielectric capacitors and the high specific energy of rechargeable batteries, supercapacitor has drawn great attention of academic and industrial circles. Conductive polyaniline (PANI) has been regarded as one of the most potential supercapacitor electrode materials, due to its desirable chemical stability, good conductivity and high faradic pseudo capacitance, as well as the advantages of low cost, facile synthesis and good environmental stability. Especially one-dimensional nano-structure PANI material with high specific surface area, high long-diameter ratio, high porosity and excellent electrical properties, has great research value in electrode field.
In this paper, PANI nanofiber material was prepared by selecting convenient and easy polymerization methods on the base of review of plentiful literatures. The polymerization conditions were investigated and optimized systematically, thus the PANI appearance can be controlled; the electrochemical capacitance behaviors of PANI with different appearances were studied in H2SO4aqueous solution; several structure modification techniques were studied and the capacitance behaviors of modified PANI were investigated; The capacitive behaviors of PANI doped with different metal salts were studied, then the proper metal type and doping method were confirmed; Finally, on the base of above research, modified and metal doped PANI and activated carbon composites were prepared by in-situ polymerization, meanwhile their capacitance behaviors were investigated in aqueous or organic solution. The main research results and conclusions are as follows:
(1) Chemical adding, rapid mixing and interfacial polymerization were used to prepare PANI nanofiber. Through strictly control and optimizing polymerization conditions, polyaniline nanofiber with uniform size and good morphology can be prepared. The fiber's average diameter is about50～100nm and length ranges from500nm to several micrometers. Chemical adding and rapid mixing polymerization are promising in industrialization because the advantages of easy operation, low cost and high product efficiency.
(2) In H2SO4aqueous solution, polyaniline nanofiber exhibits higher specific capacitance (at the current density of0.1A·g-1, long and short polyaniline nanofiber shows the specific capacitance of404F·g-1and436F·g-1respectively, and granular polyaniline shows the specific capacitance of392F·g-1). Compared with granular polyaniline, long polyaniline nanofiber exhibits better power characteristic and cycle performance (electrode capacitance reduces by9.7%when current density increased from0.1A·g-1to0.5A·g-1and degradation of capacitance is about17.5%after1000cycles).
(3) The structure of polyaniline were modified by doping with macromolecule organic acid, copolymerization and substitution methods. The polyaniline doped by dodecyl benzenesulfonic acid (DBSA) and Camphorsulfonic acid (CSA) show similar specific capacitance but cycle properties are deteriorated compared with that doped by HC1(PH). Aniline-m-toluidine copolymer (PAMD) exhibits the similar conductivity and capacitance behaviors as PH, and performances better in cycle stability (at the current density of0.1A·g-1, the specific capacitance of PAMD is381F·g-1, and degradation of capacitance is about15.8%after1000cycles), which demonstrates that introducing methyl group to polyaniline molecule can improve the cycle stability to some extent. A new N-alkylation of polyaniline materials were prepared by treating the emeraldine base polyaniline directly with various alkyl halides and the acquired polyaniline doped with1-Bromobutane (C4H9Br) exhibits good capacitance behaviors (at the current density of0.1A·g-1the specific capacitance is408F·g-1and degradation of capacitance is about20.1%after1000cycles), which proves it can be used as electrode material for supercapacitor.
(4) Metal salts doped polyaniline nanofiber (PLi\PZn\PMn\PFe) were obtained by using different metal salts as dopant, and the results show that LiCl、ZnCl2、and MnCl2doping are pseudo-protonation but FeCl3doping is pseudo-protonation with redox reaction. In H2SO4aqueous solution, PZn exhibits the best capacitance behaviors (at the current density of0.1A·g-1, the specific capacitances of PZn is340F·g-1and degradation of capacitance is about25.6%after1000cycles), but PFe exhibits no capacitance nearly. In LiPF6organic electrolyte, metal salts doped polyaniline show much higher specific capacitances than PH (the specific capacitances of PLi、PZn and PMn are123F·g-1、147F·g-1and105F·g-1, but the value of PH is only47F·g-1), moreover it can greatly improve electrode cycle stability and electricity performance, but several problems such as excessive voltage drop and narrow energy storage potential range remain exist.
(5) Polyaniline nanofiber materials co-doped with various metal ions and H+(PHLi、PHZn and PHMn) were prepared though in-situ doping in polymerization. Compared with that doped with H+(PH), all the co-doped polyaniline electrodes exhibit higher specific capacitance and better cycle stability (at the current density of0.1A·g-1, the specific capacitance of PHZn is419F·g-1and the degradation of capacitance is about11.8%after1000cycles).
(6) HC1doping polyaniline nanofiber and activated carbon composites were prepared by in situ polymerization. When activated carbon adding quantum is30%of the mass of aniline, the composited electrode shows the lowest charge transfer resistance as well as good power capability and cycle stability in H2SO4soultion (The specific capacitance is414F·g-1at current density of0.1A·g-1and degradation of capacitance is about14.3%after1000cycles). The modified polyaniline nano fiber/carbon composites for aqueous solution (PANI/C-1) can achieve the specific capacitance of427F·g-1and the degradation of capacitance is about10%after1000cycles. Another modified polyaniline nanofiber/carbon composites for organic solution (PANI/C-2) can achieve the specific capacitance of128F·g-1in LiPF6organic electrolyte, the electrode discharge voltage drop reduced greatly and the cycle performance was also improved.
引文
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