聚苯胺石墨烯复合材料的制备及其在锂电池中的应用

摘要

聚苯胺（PANI）是由苯胺单体进行氧化聚合而形成的导电高分子聚合物，由于其具有较好的氧化还原可逆性，较高的理论比容量（294 mAh/g）且成本低廉，环境友好，因此可以用作锂电池的正极材料。然而，纯聚苯胺分子共轭程度低，自身团聚严重，作为电极材料的比容量较低，循环可逆性较差。基于此，本文以不同功能化石墨烯（RGO）为模板，采用吸附双氧化剂法制备出PANI/RGO以及PANI/RGO/CNTs复合材料，从而来提高聚苯胺的电化学性能。

首先，以不同氧化程度的石墨烯为模板，制备出PANI/RGO复合材料。采用SEM、TEM、FT-IR和XRD等技术对材料的物相结构及微观形貌及物相结构进行了分析，结果表明复合材料形成了层状结构，具有较好的形态学和结晶度。CV和EIS测试表明，还原态复合材料具有更好的电化学性能。电池充放电测试可知，还原态复合材料的比容量更高，循环性能更好，而电池在不同电流密度下进行充放电测试，电池的放电比容量越高，容量衰减越严重。背心式连衣裙

其次，对石墨烯材料进行了不同的功能化处理（羧酸化、草酸化和苯磺酸化），并以此为模板，制备出功能化的PANI/RGO复合材料，同时将1%RGO和1%AC与聚苯胺复合得到PANI/RGO/AC复合材料。红外测试表明，不同功能化的石墨烯和聚苯胺复合材料都出现了对应特征官能团的吸收峰，而还原态聚苯

胺与氧化态相比，醌式吸收峰减弱，苯式吸收峰增强，说明材料被较好还原。SEM和XRD测试表明，还原态复合材料具有更好的结晶度和规整性。电池EIS 测试表明，苯磺酸化的材料具有最小的电荷迁移阻抗。CV测试表明还原态复合材料具有更大的峰电流密度和闭合面积。电池充放电测试表明，在0.1 C电流密度下，电池库伦效率接近100%，其中还原态苯磺酸化的材料放电比容量最高，达到202.7 mAh/g，50次充放循环后，容量衰减10.6%；PANI/RGO/AC的循环性能最好，0.1 C下，循环50次，衰减9.6%；0.2 C下，循环100次，衰减3.5%；

0.5 C下，循环300次，衰减24.8%；1 C下，循环500次，衰减27.6%。

最后，将RGO和CNTs同时与PANI复合，改变三者的质量分数，得到不同的PANI/RGO/CNTs复合材料。SEM测试表明RGO为2%，CNTs为5%时，复合材料的形貌特征较好。红外和XRD测试表明，RGO和CNTs用量不同，复合材料中特征峰的峰强度也不同。CV和EIS测试表明，随着RGO和CNTs 用量增加，复合材料的可逆性变差。在0.2 C电流密度下，电池进行充放电循环100次，其中RGO为2%，CNTs为5%时，复合材料的循环稳定性最好，而随

着RGO和CNTs用量的增加，循环稳定性逐渐变差。对所制备的材料进行了市场分析，与其它的锂电池正极材料相比，聚苯胺复合材料具有成本低廉，环境友好，放电稳定等优点，因此具有广阔的发展

空间。

关键词：聚苯胺；还原氧化石墨烯；复合材料；锂电池

Abstract

Polyaniline (PANI) is a conductive polymer formed by oxidation polymerization of aniline monomer, because of its good redox reversibility, higher theoretical specific capacity (294 mAh/g), low cos tand environmentally friendly, so it can be used as cathode material for lithium batteries. However, for pure polyaniline molecules, the degree of conjugation is low and self aggregation is serious. Therefore, pure polyaniline has lower specific capacity as cathode material for batteries, and its reversibility is poor. In this paper, PANI/RGO and PANI/RGO/CNTs composite materials were prepared by adsorption double oxidant method with different functional reduced graphene oxidized (RGO) as template, so as to improve the electrochemical performance of polyaniline.

2010年央视中秋晚会

朝阳办照Firstly, PANI/RGO composites were prepared by using graphene with different oxidation degree as template. Some physical characterization methods (SEM, TEM, FT-IR and XRD) were used to analy

ze the material, and the composite formed a layered structure with good morphology and crystallinity. The CV and EIS tests showed that the reduced state composite has better electrochemical properties. The charging and discharging tests for batteries showed that the reduced composite obtained the higher specific capacity and better cycling performance compared with the oxidized. It was confirmed that the higher discharge capacity the batteries get, the more serious attenuation the capacity became when charging and discharging tests under different current density.

Secondly, the graphene materials were functionalized with different groups (carboxylic acid, oxalic acid and benzene sulfonate), then were used as the template in the preparation of the functional PANI/RGO composites, and also the PANI/RGO/AC composite was prepared while 1% RGO and 1% AC (Active Carbon) were used. The FT-IR test showed that reduced graphene oxidized and polyaniline composites with different functions behaved the characteristic absorption bands of functional groups, and the for the reduction and oxidation state of polyaniline, that the quinoid absorption peak decreased and the benzene type absorption increased prove that the material is well reduced. The SEM and XRD tests showed that the reduced composites acquired better crystallinity and regularity. Electrochemical impedance spectroscopy (EIS) tests were carried out to s

how that benzene sulfonate materials exhibited minimal charge transfer resistance. The CV test showed that the reduced composites possessed greater peak current density and a broader closed area. The batteries’ charging and discharging tests showed that, under the current density of 0.1 C, the coulombic efficiency of batteries is close to 100%, among all of the

composites, the specific capacity of discharge for the benzene sulfonic acid of the reduced composite was highest, reached 202.7 mAh/g, and 50 charging and discharging cycles, the capacity has been reduced by 10.6%; and the cycle performance of the PANI/RGO/AC was best, for 0.1 C, 50 cycles, 9.6% attenuation;

0.2 C, 100 cycles, attenuation of 3.5%; 0.5 C, 300 cycles, attenuation of 24.8%; 1 C, 500 cycles, 27.6% attenuation.

Finally, RGO and CNTs were combined with PANI with changing the mass fraction of the three, and different PANI/RGO/CNTs composites were obtained. The SEM test showed that the composites had better morphology when RGO was 2% and CNTs was 5%. The FT-IR and XRD tests showed that the peak intensities of the characteristic peaks in the composites were different when the amount of

RGO and CNTs was different. CV and EIS tests showed that the reversibility of the composites becomed worse as the amount of RGO and CNTs increased. At 0.2 C current density, the battery was recharged for 100 cycles, it was clear that the cycle stability of the composite was the best when the RGO was 2% and CNTs was 5%. However, with the increase of the amount of RGO and CNTs, the stability of the composites became worse. The preparation of the composites in the market analysis, compared with other lithium battery cathode materials, polyaniline composite material had the advantages of low cost, environment friendly, stable discharging for work, so it had a broad prospect for development in the future.

Keywords: Polyaniline, Reduced Graphene Oxidized, Composites, Lithium batteries

摘要 .......................................................................................................................... I ABSTRACT ............................................................................................................... I II 第1章绪论 .. (1)

1.1课题背景及研究的目的和意义 (1)

1.2聚苯胺的发展概述 (2)

1.2.1 聚苯胺的结构 (2)

1.2.2 聚苯胺的掺杂 (3)

1.2.3 聚苯胺的二次掺杂 (5)

1.2.4 聚苯胺合成方法的研究 (6)

1.2.5 聚苯胺的应用 (7)

1.3聚苯胺复合材料 (10)

1.4锂-聚苯胺二次电池 (13)

1.4.1 锂-聚苯胺电池机制 (13)

1.4.2聚苯胺在锂电池中的应用 (14)

1.5本文研究的主要内容 (15)

第2章试验原料与测试方法 (16)

作为生物的社会2.1试验药品及仪器 (16)

2.1.1 试验药品 (16)

2.1.2 试验仪器 (17)

2.2正极片的制备和电池的组装 (17)

2.3材料表征及测试方法 (19)

2.3.1 场发射扫描电子显微镜 (19)

性空虚2.3.2 X射线衍射分析 (19)

2.3.3 傅里叶变换红外光谱分析 (20)

2.3.4 塔菲尔测试 (20)

中国投资环境

2.3.5 电化学交流阻抗测试 (20)

2.3.6 循环伏安测试 (20)

2.3.7 电池充放电测试 (21)

第3章氧化石墨烯的制备及与聚苯胺的复合 (22)

3.1引言 (22)

3.2氧化石墨烯的制备及还原 (22)

3.3聚苯胺/石墨烯复合材料的制备 (23)

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