本文選題：氣凝膠 + 石墨烯�。� 參考：《江南大學(xué)》2015年碩士論文

【摘要】：氣凝膠是具有超低密度、大孔隙率和高比表面積的高度多孔型固體材料。石墨烯氣凝膠不僅具有傳統(tǒng)氣凝膠材料的高比表面積、低密度等特點(diǎn),還表現(xiàn)出石墨烯特有的高導(dǎo)電等特性,在能量存儲(chǔ)與轉(zhuǎn)換、催化、環(huán)境清潔及傳感器等領(lǐng)域具有廣泛的應(yīng)用前景。本文研究了石墨烯復(fù)合氣凝膠的可控合成及性能。以Hummers方法制備得到的氧化石墨烯為原料,通過自發(fā)組裝、相轉(zhuǎn)移及有機(jī)-無機(jī)氮源共摻雜調(diào)控石墨烯復(fù)合水/氣凝膠的三維結(jié)構(gòu)及組成,并對(duì)這些復(fù)合氣凝膠材料的微觀結(jié)構(gòu)及性能進(jìn)行了深入研究。具體內(nèi)容包括:通過氧化石墨烯與吡咯單體之間的自發(fā)組裝,無需添加其他氧化劑和還原劑、室溫下成功制備出石墨烯-聚吡咯(r GO-PPy)復(fù)合水凝膠,并進(jìn)一步超臨界二氧化碳干燥得到r GO-PPy復(fù)合氣凝膠。利用FT-IR、Raman、XPS以及XRD等測(cè)試手段對(duì)凝膠形成的機(jī)理進(jìn)行了深入研究。結(jié)果表明該自發(fā)組裝是基于氧化石墨烯與吡咯單體之間的氧化還原反應(yīng)。SEM、TEM等微觀測(cè)試及氮?dú)馕摳綔y(cè)試表明r GO-PPy復(fù)合氣凝膠中的PPy以納米顆粒的形式粘附于石墨烯片層上,因而復(fù)合氣凝膠具有較高的比表面積。另外,PPy在r GO-PPy氣凝膠中也充當(dāng)著“交聯(lián)劑”,從而導(dǎo)致r GO-PPy復(fù)合氣凝膠具有良好的機(jī)械性能,儲(chǔ)能模量高達(dá)12 MPa。該石墨烯-聚吡咯氣凝膠用作超級(jí)電容器電極材料時(shí),表現(xiàn)出較高的比電容(0.5 A/g電流密度下比電容為304 F/g)。以氧化石墨烯作為表面活性劑,得到了一系列氧化石墨烯穩(wěn)定的低維納米材料水性分散液,再經(jīng)過還原、超臨界二氧化碳干燥等步驟獲得一系列石墨烯與低維納米材料的復(fù)合水凝膠/氣凝膠。其中,低維納米材料包括零維的聚吡咯納米顆粒、一維的銀納米線、一維的氧化鎢納米線以及二維的二硫化鉬納米片。通過UV-Vis、Micro-IR以及Zeta電位等測(cè)試手段證明了相轉(zhuǎn)移過程;利用SEM、TEM及氮?dú)馕摳綔y(cè)試研究了復(fù)合氣凝膠的微觀形貌及孔洞結(jié)構(gòu);最后,通過石墨烯-銀納米線復(fù)合氣凝膠的表面增強(qiáng)拉曼散射效應(yīng),實(shí)現(xiàn)了對(duì)羅丹明B探針分子的痕量檢測(cè),其檢測(cè)極限可低至1.0×10-8 mol/L,并具有良好的重復(fù)性。以乙醇胺為有機(jī)氮源、氨氣為無機(jī)氮源,采用有機(jī)-無機(jī)氮源共摻雜法制備出氮摻雜石墨烯氣凝膠(N-G-NH3),考察了獲得的N-G-NH3氣凝膠的物理化學(xué)性能,并與以乙醇胺-石墨烯氣凝膠在氮?dú)鈼l件下退火得到的N-G-N2氣凝膠的相關(guān)性能作為對(duì)比。SEM和氮?dú)馕摳綔y(cè)試結(jié)果表明,N-G-NH3氣凝膠具有更高的比表面積和孔體積等特點(diǎn);利用EDX、XPS等測(cè)試技術(shù)對(duì)氣凝膠中氮元素的含量及存在形式進(jìn)行了詳細(xì)的研究,結(jié)果表明該有機(jī)-無機(jī)氮源共摻雜法不僅顯著提升了總氮含量,而且可對(duì)氣凝膠中不同形式的氮進(jìn)行調(diào)控。導(dǎo)電性能測(cè)試表明,N-G-NH3氣凝膠具有良好的導(dǎo)電性(154.2S/m),高于N-G-N2導(dǎo)電率(143.1 S/m)。以N-G-NH3氣凝膠修飾電極,電化學(xué)檢測(cè)對(duì)苯二酚的檢測(cè)極限為5.61×10-6 mol/L(S/N=3),線性范圍在1.0×10-5 mol/L~8.5×10-4mol/L之間。
[Abstract]:Aerogel is with low density, highly porous solid materials with high porosity and high surface area. The graphene aerogel has not only the traditional aerogel materials with high surface area, low density and other characteristics, also exhibit high conductivity properties of graphene unique, catalysis in energy storage and conversion, and has application prospect wide field of clean environment and sensors. This paper studies the controllable synthesis and properties of graphene composite aerogels. The Hummers method for preparation of graphene oxide as raw material, through self assemble, phase transfer and organic - inorganic nitrogen doped graphene composite control water / aerogel three-dimensional structure and composition. And the composite aerogel material microstructure and properties were studied. The specific contents include: the spontaneous between graphene oxide and pyrrole monomer assembly, without addition of oxygen and other agents Reducing agent at room temperature successfully prepared graphene / polypyrrole (R GO-PPy) composite hydrogel, and further supercritical carbon dioxide drying R GO-PPy composite aerogel. By using FT-IR, Raman, XPS and the mechanism of XRD and other testing methods on the gel forming were studied. The results show that the spontaneous assembly is oxidation oxidation graphene and pyrrole monomer reaction based on.SEM, TEM and other microscopic test and nitrogen adsorption desorption test showed that R GO-PPy composite aerogels in PPy in the form of nano particles adhered to the graphene layers, and composite aerogels with high specific surface area. In addition, PPy in R GO-PPy aerogels also act as a crosslinking agent, which can lead to R GO-PPy composite aerogel has good mechanical properties, the storage modulus of up to 12 MPa. of the polypyrrole graphene aerogel as electrode material of super capacitor, the more High specific capacitance (0.5 A/g current density under the specific capacitance of 304 F/g). Using graphene oxide as surfactant, obtained a series of graphene oxide stable low dimensional nano material aqueous dispersion, and then after reduction step, supercritical carbon dioxide drying to obtain the composite hydrogel / graphene and a series of low dimensional nano material aerogel. The polypyrrole nano particles of low dimensional nano materials including zero dimensional, one-dimensional silver nanowires, one dimensional tungsten oxide nanowires and molybdenum disulfide two-dimensional. Through UV-Vis, Micro-IR and Zeta potential test means that the phase transfer process by using SEM, TEM and nitrogen; the morphology and structure of suction holes of the composite aerogel desorption test; finally, by surface enhanced Raman scattering of graphene silver nanowires composite aerogels, the trace examination on Luo Danming B probe Test, the detection limit can be as low as 1 x 10-8 mol/L, and has good repeatability. With ethanolamine as organic nitrogen source, ammonia as inorganic nitrogen, using organic inorganic nitrogen sources were prepared by doping nitrogen doped graphene aerogel (N-G-NH3), physical and chemical properties of N-G-NH3 aerogels obtained. The investigation, related properties and N-G-N2 aerogel with ethanolamine - graphene aerogel by annealing in nitrogen conditions as compared with.SEM and nitrogen adsorption desorption test results show that the N-G-NH3 aerogel has higher specific surface area and pore volume; the use of EDX, XPS and other testing techniques are discussed in detail study on the nitrogen content in the aerogel and form. The results show that the organic inorganic nitrogen co doping method not only significantly enhance the total nitrogen content, but also on the different forms of nitrogen in the aerogel regulation. Conductivity tests show that N-G-NH3 Aerogels had good conductivity (154.2S/m), higher than N-G-N2 conductivity (143.1 S/m). The detection limit of electrochemical detection of hydroquinone was 5.61 * 10-6 mol/L (S/N=3), and the linear range was 1 * 10-5 mol/L~8.5 * 10-4mol/L based on N-G-NH3 aerogel modified electrode.

【學(xué)位授予單位】：江南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB383.1;O613.71

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