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機械球磨法制備碳量子點及其應(yīng)用

發(fā)布時間:2018-01-06 02:04

  本文關(guān)鍵詞:機械球磨法制備碳量子點及其應(yīng)用 出處:《鄭州大學(xué)》2017年碩士論文 論文類型:學(xué)位論文


  更多相關(guān)文章: 碳量子點 Fe~(3+)檢測 氮摻雜 生物成像


【摘要】:碳量子點是一種顆粒尺寸在1-10 nm之間的新型熒光碳納米材料,具有獨特的光學(xué)性質(zhì)、良好的生物相容性、低細胞毒性、優(yōu)異的化學(xué)穩(wěn)定性、易于功能化和低成本等特點,在分析檢測、生物成像、光催化、電子器件等領(lǐng)域應(yīng)用廣泛。但在實際應(yīng)用和商業(yè)化進程中,其高產(chǎn)制備一直是個難題。機械球磨法是生產(chǎn)納米材料的常用方法,球磨過程中產(chǎn)生的高能量促使材料發(fā)生非平衡態(tài)相變和顯微組織結(jié)構(gòu)變化,產(chǎn)生新界面和缺陷,使材料粒徑更小、比表面積更大,性質(zhì)更優(yōu)異,操作過程簡便、可批量生產(chǎn)。本文構(gòu)建了一種新的機械球磨法來制備熒光碳量子點,對其熒光性能、形貌結(jié)構(gòu)進行探索,并嘗試將其應(yīng)用于離子檢測和生物成像領(lǐng)域,主要包含以下研究工作:一、首次以纖維素為碳源,鎂粉為還原劑,在球磨環(huán)境中制得Mg摻雜的熒光碳量子點(Mg-CQDs),并探索了球磨時間和原料比例對Mg-CQDs熒光性能的影響。通過透射電子顯微鏡(TEM)對其形貌粒徑進行表征,該Mg-CQDs粒徑分布均勻,平均尺寸在4.7 nm左右,可見明顯的晶格條紋。X射線衍射(XRD)、傅里葉變換紅外光譜(FTIR)、X射線光電子能譜(XPS)、拉曼光譜等表征結(jié)果均顯示該Mg-CQDs是無定型晶體,含有C、H、O、Mg等元素,且表面富含羥基、羧基等官能團,使得該Mg-CQDs有極好的水溶性。通過紫外可見吸收光譜(UV-vis)、熒光光譜(PL)等表征手段發(fā)現(xiàn),該Mg-CQDs具有很好的吸收和發(fā)射性能。此外,還具有優(yōu)良的抗光漂白性和光穩(wěn)定性,在強酸強堿、高濃度鹽溶液中Mg-CQDs的熒光強度幾乎都不改變。并且該Mg-CQDs對Fe~(3+)有較好的響應(yīng),可以作為檢測Fe~(3+)的納米探針,檢出限為0.9μΜ/L。二、為得到性能更優(yōu)越的碳量子點(CQDs),我們在本文第一部分研究的基礎(chǔ)上,對所得碳量子點進行修飾。即:在球磨的過程中,引入氮源(尿素、對氨基苯甲酸、L-谷氨酰胺等含氮化合物)。所得碳量子點的熒光強度和量子產(chǎn)率均得到提升,其中,以加入L-谷氨酰胺后性能提升最佳。通過透射電子顯微鏡(TEM)對其形貌粒徑進行表征,表明該CQDs粒徑分布均勻,平均尺寸在4.8 nm左右,表面富含羥基、羧基等官能團,以及新引入的氨基官能團,有很好的水溶性,同時具備優(yōu)良的抗光漂白性和光穩(wěn)定性,在強酸強堿、高濃度鹽溶液以及高溫環(huán)境中,該氮摻雜的碳量子點(Mg,N-CQDs)熒光強度能保持基本穩(wěn)定。細胞毒性實驗表明該Mg,N-CQDs生物相容性良好,同時,以MCF-7細胞為對象,考察了其作為細胞成像試劑的成像效果,結(jié)果證明其能進入細胞質(zhì)中,充分點亮細胞。
[Abstract]:Carbon quantum dots (QDs) are novel fluorescent carbon nanomaterials with particle sizes ranging from 1 nm to 10 nm, with unique optical properties, good biocompatibility, low cytotoxicity and excellent chemical stability. Easy to functionalize and low cost, it is widely used in analytical detection, biological imaging, photocatalysis, electronic devices and other fields, but in the practical application and commercialization process. Mechanical ball milling is a common method to produce nanomaterials. The high energy produced in the process of ball milling makes the materials undergo non-equilibrium phase transition and microstructure changes. New interfaces and defects are produced, which make the materials smaller in particle size, larger in specific surface area, better in properties, simpler in operation and can be produced in bulk. In this paper, a new mechanical ball milling method is proposed to prepare fluorescent carbon quantum dots. The fluorescence properties, morphology and structure were explored and applied in the field of ion detection and biological imaging, including the following research work: firstly, cellulose was used as carbon source and magnesium powder as reducing agent for the first time. Mg doped carbon quantum dots (Mg-CQDs) were prepared in ball milling environment. The effects of milling time and the ratio of raw materials on the fluorescence properties of Mg-CQDs were investigated. The particle size of Mg-CQDs was characterized by transmission electron microscopy (TEM). The size distribution of Mg-CQDs was uniform. The average size is about 4.7 nm, obvious lattice stripes. X ray diffraction and Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) can be seen. The results of Raman spectra showed that the Mg-CQDs was amorphous, containing elements such as CnH, O, mg, and the surface was rich in functional groups such as hydroxyl groups and carboxyl groups. The Mg-CQDs was characterized by UV-Vis and fluorescence spectra. The Mg-CQDs has good absorption and emission properties. In addition, it also has excellent photobleaching resistance and photostability in strong acid and alkali. The fluorescence intensity of Mg-CQDs in high concentration salt solution is almost unchanged, and the Mg-CQDs has a good response to Fe~(3, and can be used as a nano-probe for detecting Fe~(3). The detection limit is 0.9 渭 渭 m 路L ~ (-2). In order to obtain better performance carbon quantum dots (CQDsN), we have done some research in the first part of this paper. The carbon quantum dots were modified, that is, nitrogen sources (urea, p-aminobenzoic acid) were introduced into the milling process. The fluorescence intensity and quantum yield of the carbon quantum dots obtained by L- glutamine and other nitrogen-containing compounds have been improved. The particle size of L- glutamine was characterized by transmission electron microscopy (TEM). It was found that the particle size of CQDs was uniform and the average size was about 4.8 nm. The surface is rich in hydroxyl, carboxyl and other functional groups, as well as the newly introduced amino functional groups, which have good water solubility, good photobleaching resistance and photostability, and strong alkali in strong acids. The fluorescence intensity of the nitrogen-doped carbon quantum dot MgN-CQDsremained stable in high concentration salt solution and in high temperature environment. N-CQDs had good biocompatibility. At the same time, the imaging effect of N-CQDs as a cell imaging reagent was investigated. The results showed that N-CQDs could enter the cytoplasm and fully light the cells.
【學(xué)位授予單位】:鄭州大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:TB383.1;O657.3

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