石墨烯粉體及石墨烯水分散液的制備研究
發(fā)布時間:2018-01-11 16:24
本文關(guān)鍵詞:石墨烯粉體及石墨烯水分散液的制備研究 出處:《深圳大學(xué)》2017年碩士論文 論文類型:學(xué)位論文
更多相關(guān)文章: LPAN 石墨烯粉體 石墨烯水分散液 熱還原
【摘要】:自從2004年單原子厚度二維平面結(jié)構(gòu)的石墨烯在實驗室被發(fā)現(xiàn)后,就吸引了人們的廣泛關(guān)注。石墨烯所表現(xiàn)出來的諸多優(yōu)異特性,及其在各領(lǐng)域的潛在應(yīng)用,也引起了世界范圍內(nèi)廣泛的研究熱潮。如何實現(xiàn)石墨烯高質(zhì)量、大規(guī)模的生產(chǎn),是目前亟需解決的一大難題。所以如何對石墨烯的制備技術(shù)進行創(chuàng)新,或者在原有的基礎(chǔ)上對制備技術(shù)進行改進,以提高石墨烯的產(chǎn)量和質(zhì)量也就勢在必行了。本論文的內(nèi)容主要包括以下幾個部分:(1)通過改進原有的制備方法,獲得了高產(chǎn)量、高質(zhì)量的石墨烯粉體。本文將原本在空氣氣氛條件下進行的LPAN預(yù)燒結(jié)過程改進為在氮氣氣氛保護下進行,防止了在預(yù)燒結(jié)過程中LPAN分子鏈上氧化反應(yīng)的發(fā)生,減少了燒結(jié)過程中碳量的損失,以及石墨烯平面結(jié)構(gòu)上缺陷的產(chǎn)生,提高了最終產(chǎn)物的質(zhì)量和產(chǎn)量。這無疑對石墨烯的工業(yè)化生產(chǎn)研究有著重要的意義。(2)設(shè)計了一種簡單、有效的球磨方法:機械分裂與化學(xué)修飾法相結(jié)合,使石墨烯粉體與KOH在球磨過程中發(fā)生反應(yīng),制備出了濃度可達0.5 mg/ml的高質(zhì)量的石墨烯水分散液。其機理就是通過球磨過程中的機械力,使石墨烯片層分裂,在其分裂的邊緣部位,斷裂的C-C鍵形成了活性碳物種(離子,自由基等),非常易于與羥基化合物發(fā)生反應(yīng),從而在石墨烯片層邊緣的位置引入羥基官能團,這種球磨方法既增加了石墨烯的分散性也沒有破壞石墨烯的基面。將所得樣品分散在不同的溶劑中后可以發(fā)現(xiàn),球磨方法制備的石墨烯水分散液在大多數(shù)的極性溶劑中均具有良好的分散效果。(3)對石墨烯水分散液進行熱還原處理,通過拉曼、紫外、紅外等表征手段,對還原前后的產(chǎn)物進行了分析,進一步驗證了本文所提出的的球磨反應(yīng)的機理。此外,本文利用所得到的石墨烯水分散液抽濾制膜,對其薄層電阻進行測試,結(jié)果發(fā)現(xiàn)石墨烯又可以恢復(fù)到其原有的導(dǎo)電性能。這說明通過球磨方法,不僅制備出了較高濃度的石墨烯水分散液,同時很好的保留了石墨烯的本征結(jié)構(gòu),并基本保全了其優(yōu)異的性能。這對石墨烯材料在實際領(lǐng)域中的應(yīng)用有著非常重大的意義。
[Abstract]:Since the discovery of graphene with monoatomic thickness and two-dimensional planar structure in the laboratory in 2004, it has attracted much attention. And its potential applications in various fields have also caused a worldwide wide range of research upsurge. How to achieve high quality graphene production on a large scale. Therefore, how to innovate the preparation technology of graphene, or improve the preparation technology on the basis of the original. It is imperative to improve the yield and quality of graphene. The main contents of this paper include the following parts: 1) by improving the original preparation method, the high yield has been obtained. High quality graphene powder. In this paper, the pre-sintering process of LPAN under the condition of air atmosphere was improved to be carried out under the protection of nitrogen atmosphere. The oxidation reaction on LPAN molecular chain during pre-sintering process was prevented, and the loss of carbon content and the formation of planar defects in graphene structure were reduced. The quality and yield of the final product are improved, which is undoubtedly of great significance to the study of the industrial production of graphene.) A simple and effective ball milling method is designed, which is the combination of mechanical splitting and chemical modification. A high quality graphene aqueous dispersion with concentration up to 0.5 mg/ml was prepared by the reaction between graphene powder and KOH in the process of ball milling. The mechanism is the mechanical force in the process of ball milling. At the edge of the cleavage, the C-C bond breaks into active carbon species (ions, free radicals, etc.), which is very easy to react with hydroxyl compounds. Therefore, hydroxyl functional groups were introduced into the edge of graphene lamellar. The ball milling method not only increased the dispersion of graphene, but also did not destroy the base surface of graphene. The samples were found to be dispersed in different solvents. The graphene aqueous dispersion prepared by ball milling has good dispersion effect in most polar solvents. The products before and after reduction were analyzed, and the mechanism of ball milling reaction was further verified. In addition, the thin layer resistance of the film was tested by using the obtained graphene aqueous dispersion to filter the film. The results show that graphene can recover to its original electrical conductivity, which indicates that through ball milling method, not only high concentration of graphene aqueous dispersion was prepared, but also the intrinsic structure of graphene was well preserved. It is of great significance to the application of graphene materials in the practical field.
【學(xué)位授予單位】:深圳大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:TQ127.11
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