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石墨烯與聚苯胺復(fù)合海綿制備及性能研究

發(fā)布時(shí)間:2018-12-21 14:32
【摘要】:聚苯胺(PANI)是一種具有良好熱穩(wěn)定性、高比電容且易于合成的導(dǎo)電高分子材料,但純PANI合成后易團(tuán)聚且電化學(xué)循環(huán)穩(wěn)定性較差。作為目前科研前沿的材料,石墨烯(GN)是碳原子通過以六邊形晶格的形式非常緊密的堆積而形成的單層二維材料,在性能方面具有一些比較優(yōu)良的性能,如:優(yōu)異的機(jī)械性能、高比表面積、高導(dǎo)電率等。本文將二者結(jié)合,成功制備出海綿狀GN/PANI復(fù)合海綿,可廣泛應(yīng)用于可壓縮超級電容器及傳感器等。 本文采用Hummers法、改進(jìn)Hummers法分別制備出氧化石墨烯(GO),并通過XRD、AFM及稱重對其氧化程度、粒徑及產(chǎn)量進(jìn)行表征與分析。結(jié)果表明無論從氧化程度、粒徑大小及產(chǎn)量進(jìn)行對比,改進(jìn)法都占有優(yōu)勢,含雜質(zhì)較少,產(chǎn)量較大,故以改進(jìn)法所制備的GO為原材料進(jìn)行下一步實(shí)驗(yàn)。通過在GO分散液中原位聚合苯胺單體,制備分散均勻的GO/PANI復(fù)合材料,并經(jīng)冷凍干燥工藝形成GO/PANI復(fù)合海綿。然后將GO/PANI復(fù)合海綿置于水合肼氣氛中還原1h,即得GN/PANI復(fù)合海綿。 在對復(fù)合海綿進(jìn)行力學(xué)壓縮性能分析時(shí)發(fā)現(xiàn),當(dāng)應(yīng)變ε=40%時(shí),第10次壓縮循環(huán)與第1次相比,石墨烯海綿和RGP1:0.6的彈性變形都接近于100%,然而RGP1:3和RGP1:5的彈性變形分別為98.3%和94.5%。通過SEM表征發(fā)現(xiàn)制備的GO/PANI結(jié)構(gòu)和成分比較均勻,GO的分散性較好。對其進(jìn)行電化學(xué)性能分析,,同比例情況下,GN/PANI海綿比電容均高于GO/PANI海綿,在2mV/s掃速下,RGP1:5比電容為487F/g,而GOP1:5僅為152F/g,純PANI為397F/g,純GN為162F/g。而不同比例下,PANI的含量和材料的比電容成正比關(guān)系,PANI的負(fù)載有效地提高了石墨烯多孔結(jié)構(gòu)的電容特性,當(dāng)GN:PANI為1:5時(shí)(即RGP1:5),復(fù)合海綿比電容為487F/g,但此時(shí)復(fù)合海綿壓縮性能變?nèi),塑性變形明顯,而在2mV/s掃速下,RGP1:3比電容為448F/g,且其彈性變形范圍較大,故綜合力學(xué)壓縮性能和電化學(xué)性能,RGP1:3性能更為全面。
[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.
【學(xué)位授予單位】:哈爾濱理工大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TQ317;TB332

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