本文選題：石墨烯　切入點：硫化銅　出處：《中國礦業(yè)大學(xué)》2017年碩士論文

【摘要】：石墨烯因其獨特的物理化學(xué)性能在儲能材料領(lǐng)域具有廣闊的應(yīng)用前景,近年來石墨烯基超級電容器復(fù)合材料已經(jīng)成為儲能材料研究領(lǐng)域的研究熱點。本文采用氧化-熱還原法將石墨先氧化成氧化石墨,在空氣中對氧化石墨進行快速加熱,使其片層發(fā)生剝離和還原,制得石墨烯粉末,并通過X射線衍射(XRD),紅外光譜(FT-IR),拉曼光譜(Raman),X射線光電子能譜(XPS),透射電鏡(TEM)等表征手段討論快速熱還原對樣品還原程度的影響。在此基礎(chǔ)之上,采用一步水熱法分別制備了硫化銅-石墨烯復(fù)合材料和多相鎳硫化物-石墨烯復(fù)合材料,并表征了復(fù)合材料的結(jié)構(gòu)和成分,討論了復(fù)合材料作為超級電容器電極活性材料的電化學(xué)電容性能。主要研究內(nèi)容和結(jié)論如下:1.采用熱板作為熱源,在空氣中將氧化石墨粉直接噴向熱板進行還原,使得樣品的制備十分迅速。樣品的結(jié)構(gòu)和成分分析表明,隨著溫度的升高,氧化石墨的結(jié)構(gòu)逐漸向石墨烯的結(jié)構(gòu)進行轉(zhuǎn)變。在快速熱還原過程中,氧化石墨的片層堆疊結(jié)構(gòu)發(fā)生剝離和還原,形成石墨烯的微晶結(jié)構(gòu)。比表面積和孔徑分析表明,這種還原產(chǎn)物具有高達737 m2?g-1的比表面積和0.70 cm3?g-1?nm-1的孔體積。這種制備方法對于實現(xiàn)石墨烯大規(guī)模工業(yè)化生產(chǎn)具有重要的借鑒意義。2.在快速熱還原制備石墨烯的基礎(chǔ)上,采用一步水熱法在石墨烯基底上生長出花球狀硫化銅微球,改善了以有機溶劑作為反應(yīng)溶劑的方法,是一種環(huán)境友好的制備工藝。電化學(xué)電容性能測試表明,在1 A?g-1時比容量最高可達1222.5F?g-1,并且在5 A?g-1時連續(xù)循環(huán)3000次后,電容保持率達到92.11%。3.利用水熱法制備了多相鎳硫化物-石墨烯復(fù)合材料,在石墨烯表面負載的鎳硫化物微球為多種鎳硫化物(NiS,NiS2和Ni3S4)的混合相。探討了反應(yīng)溫度和時間對產(chǎn)物的結(jié)構(gòu)與成分的影響,并將這種復(fù)合材料應(yīng)用于超級電容器電極活性材料。電化學(xué)電容性能測試表明,在1 A?g-1時比容量可達1602.2 F?g-1,并具有良好的倍率特性與循環(huán)穩(wěn)定性(循環(huán)3000次后的電容量保持率為90.81%)。
[Abstract]:Graphene has a wide application prospect in the field of energy storage materials because of its unique physical and chemical properties. In recent years, graphene based supercapacitor composites have become a research hotspot in the field of energy storage materials.In this paper, graphite was oxidized to graphite oxide by oxidation-thermal reduction method. Graphite oxide was heated rapidly in air, and its lamellar layer was stripped and reduced to produce graphene powder.The effects of rapid thermal reduction on the reduction degree of the samples were discussed by means of X-ray diffraction (XRD), FTIR (FT-IRT), Raman spectroscopy (Ram), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM).On this basis, copper sulphide graphene composites and polyphase nickel sulfide-graphene composites were prepared by one-step hydrothermal method, and the structure and composition of the composites were characterized.The electrochemical capacitance performance of composite material as electrode active material of supercapacitor was discussed.The main contents and conclusions are as follows: 1.Using hot plate as heat source, the oxidized graphite powder was sprayed directly into the hot plate in air, which made the preparation of the sample very rapid.The structure and composition analysis of the samples showed that the structure of graphite oxide gradually changed to that of graphene with the increase of temperature.In the process of rapid thermal reduction, the lamellar stacked structure of graphite oxide is stripped and reduced to form the microcrystalline structure of graphene.The specific surface area and pore size analysis showed that the reduction product had a specific surface area of 737 m2?g-1 and a pore volume of 0.70 cm3?g-1?nm-1.This preparation method has important reference significance for realizing the large-scale industrial production of graphene.On the basis of rapid thermal reduction to prepare graphene, copper sulfide microspheres were grown on graphene substrate by one step hydrothermal method, which improved the method of using organic solvent as reaction solvent and was an environmentally friendly preparation process.The electrochemical capacitance performance test shows that the maximum specific capacity can reach 1222.5 FU g-1 at 1 A?g-1, and the capacitance retention rate reaches 92.11.1 after 3000 continuous cycles at 5 A?g-1.Multiphase nickel sulfide-graphene composites were prepared by hydrothermal method. The nickel sulfide microspheres supported on the surface of graphene were mixed with various nickel sulfides, NiS _ 2 and Ni _ 3S _ 4).The effects of reaction temperature and time on the structure and composition of the product were discussed, and the composite was applied to the electrode active material of supercapacitor.The electrochemical capacitance performance test shows that the specific capacity can reach 1602.2 FG-1 at 1 A?g-1, and has good rate characteristics and cycle stability (the capacitance retention rate of 3000 cycles is 90.81%).
【學(xué)位授予單位】：中國礦業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TM53;TQ127.11;TB332

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