石墨烯与聚苯胺复合海绵制备及性能研究
发布时间：2018-12-21 14:32
【摘要】：聚苯胺（PANI）是一种具有良好热稳定性、高比电容且易于合成的导电高分子材料，但纯PANI合成后易团聚且电化学循环稳定性较差。作为目前科研前沿的材料，石墨烯（GN）是碳原子通过以六边形晶格的形式非常紧密的堆积而形成的单层二维材料，在性能方面具有一些比较优良的性能，如：优异的机械性能、高比表面积、高导电率等。本文将二者结合，成功制备出海绵状GN/PANI复合海绵，可广泛应用于可压缩超级电容器及传感器等。 本文采用Hummers法、改进Hummers法分别制备出氧化石墨烯（GO），并通过XRD、AFM及称重对其氧化程度、粒径及产量进行表征与分析。结果表明无论从氧化程度、粒径大小及产量进行对比，改进法都占有优势，含杂质较少，产量较大，故以改进法所制备的GO为原材料进行下一步实验。通过在GO分散液中原位聚合苯胺单体，制备分散均匀的GO/PANI复合材料，并经冷冻干燥工艺形成GO/PANI复合海绵。然后将GO/PANI复合海绵置于水合肼气氛中还原1h，即得GN/PANI复合海绵。 在对复合海绵进行力学压缩性能分析时发现，当应变ε=40%时，第10次压缩循环与第1次相比，石墨烯海绵和RGP1:0.6的弹性变形都接近于100%，然而RGP1:3和RGP1:5的弹性变形分别为98.3%和94.5%。通过SEM表征发现制备的GO/PANI结构和成分比较均匀，GO的分散性较好。对其进行电化学性能分析，，同比例情况下，GN/PANI海绵比电容均高于GO/PANI海绵，在2mV/s扫速下，RGP1:5比电容为487F/g，而GOP1:5仅为152F/g，纯PANI为397F/g，纯GN为162F/g。而不同比例下，PANI的含量和材料的比电容成正比关系，PANI的负载有效地提高了石墨烯多孔结构的电容特性，当GN:PANI为1:5时（即RGP1:5），复合海绵比电容为487F/g，但此时复合海绵压缩性能变弱，塑性变形明显，而在2mV/s扫速下，RGP1:3比电容为448F/g，且其弹性变形范围较大，故综合力学压缩性能和电化学性能，RGP1:3性能更为全面。
[Abstract]:Polyaniline (PANI) is a kind of conductive polymer material with good thermal stability, high specific capacitance and easy to synthesize, but the pure PANI is easy to agglomerate and the electrochemical cycle stability is poor. Graphene (GN) is a single layer two-dimensional material formed by stacking carbon atoms in the form of hexagonal lattice, and has some excellent properties. Such as: excellent mechanical properties, high specific surface area, high conductivity and so on. In this paper, the spongy GN/PANI composite sponge was successfully prepared, which can be widely used in compressible supercapacitors and sensors. In this paper, graphene oxide (GO), was prepared by Hummers method and modified Hummers method. The degree of oxidation, particle size and yield of (GO), were characterized and analyzed by XRD,AFM and weighing. The results show that the improved method is superior in comparison with oxidation degree, particle size and yield. Therefore, the GO prepared by the improved method is used as the raw material for the next experiment. The uniformly dispersed GO/PANI composites were prepared by in-situ polymerization of aniline monomer in GO dispersions and GO/PANI composite sponges were prepared by freeze-drying process. Then the GO/PANI composite sponge was reduced in hydrazine hydrate atmosphere for 1 h, and the GN/PANI composite sponge was obtained. When the mechanical compression properties of the composite sponge are analyzed, it is found that the elastic deformation of the graphene sponge and RGP1:0.6 is close to 100 when the strain 蔚 = 40, compared with the first compression cycle. However, the elastic deformation of RGP1:3 and RGP1:5 were 98.3% and 94.5%, respectively. The structure and composition of GO/PANI were found to be uniform by SEM, and the dispersion of GO was better. At the same ratio, the specific capacitance of GN/PANI sponge was higher than that of GO/PANI sponge. At 2mV/s scan speed, the specific capacitance of RGP1:5 was 487F / g, while that of GOP1:5 was 152F / g, and that of pure PANI was 397F / g. The pure GN is 162 F / g. At different ratios, the content of PANI is proportional to the specific capacitance of the material. The capacitance characteristics of graphene porous structure are effectively improved by the loading of PANI. When GN:PANI is 1:5 (i.e. RGP1:5), the specific capacitance of composite sponge is 487F / g, and the specific capacitance of the composite sponge is 487F / g, when GN:PANI is 1:5 (RGP1:5), the specific capacitance of composite sponge is 487F / g. However, the compressibility of the composite sponge becomes weaker and the plastic deformation is obvious. The specific capacitance of RGP1:3 is 448 F / g at 2mV/s scanning speed, and its elastic deformation range is large. Therefore, the mechanical compression and electrochemical properties of the composite sponge are synthesized. RGP1:3 performance is more comprehensive.
【学位授予单位】：哈尔滨理工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ317;TB332
本文编号：2389042
[Abstract]:Polyaniline (PANI) is a kind of conductive polymer material with good thermal stability, high specific capacitance and easy to synthesize, but the pure PANI is easy to agglomerate and the electrochemical cycle stability is poor. Graphene (GN) is a single layer two-dimensional material formed by stacking carbon atoms in the form of hexagonal lattice, and has some excellent properties. Such as: excellent mechanical properties, high specific surface area, high conductivity and so on. In this paper, the spongy GN/PANI composite sponge was successfully prepared, which can be widely used in compressible supercapacitors and sensors. In this paper, graphene oxide (GO), was prepared by Hummers method and modified Hummers method. The degree of oxidation, particle size and yield of (GO), were characterized and analyzed by XRD,AFM and weighing. The results show that the improved method is superior in comparison with oxidation degree, particle size and yield. Therefore, the GO prepared by the improved method is used as the raw material for the next experiment. The uniformly dispersed GO/PANI composites were prepared by in-situ polymerization of aniline monomer in GO dispersions and GO/PANI composite sponges were prepared by freeze-drying process. Then the GO/PANI composite sponge was reduced in hydrazine hydrate atmosphere for 1 h, and the GN/PANI composite sponge was obtained. When the mechanical compression properties of the composite sponge are analyzed, it is found that the elastic deformation of the graphene sponge and RGP1:0.6 is close to 100 when the strain 蔚 = 40, compared with the first compression cycle. However, the elastic deformation of RGP1:3 and RGP1:5 were 98.3% and 94.5%, respectively. The structure and composition of GO/PANI were found to be uniform by SEM, and the dispersion of GO was better. At the same ratio, the specific capacitance of GN/PANI sponge was higher than that of GO/PANI sponge. At 2mV/s scan speed, the specific capacitance of RGP1:5 was 487F / g, while that of GOP1:5 was 152F / g, and that of pure PANI was 397F / g. The pure GN is 162 F / g. At different ratios, the content of PANI is proportional to the specific capacitance of the material. The capacitance characteristics of graphene porous structure are effectively improved by the loading of PANI. When GN:PANI is 1:5 (i.e. RGP1:5), the specific capacitance of composite sponge is 487F / g, and the specific capacitance of the composite sponge is 487F / g, when GN:PANI is 1:5 (RGP1:5), the specific capacitance of composite sponge is 487F / g. However, the compressibility of the composite sponge becomes weaker and the plastic deformation is obvious. The specific capacitance of RGP1:3 is 448 F / g at 2mV/s scanning speed, and its elastic deformation range is large. Therefore, the mechanical compression and electrochemical properties of the composite sponge are synthesized. RGP1:3 performance is more comprehensive.
【学位授予单位】：哈尔滨理工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ317;TB332
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