氮掺杂葡萄糖酸碳量子点的合成及其光学性能的研究
发布时间：2018-10-12 21:32
【摘要】：碳量子点(CQDs)因原料丰富,制备方法多样而备受研究者关注。其光学性能为荧光纳米材料的开发和应用提供了更广泛的前景。在水相中,阳离子与阴离子能够将CQDs产生的荧光进行猝灭和还原,可应用于传感。高荧光量子产率是CQDs广泛应用的前提,所以找到能够提高CQDs产量的方法非常重要,本文研究了碳量子点的不同制备方法、光学性能和应用,主要工作如下:第一部分:以葡萄糖酸为本实验所需碳源,使用一些常用的制备方法如微波法,热解法,水热法,制备了CQDs。在第一章节中研究了微波时间,热解温度和热解时间,水热时间和葡萄糖酸浓度对所制备碳量子点荧光强度的影响。比较了三种不同方法制得的碳量子点的粒径大小及光学特性,其中微波法和热解法制备出的碳量子点荧光发射依赖激发,水热法制备出的CQDs具有发射不依赖激发的光学性质,荧光量子产率最高,为6.01%。第二部分:以葡萄糖酸为碳源,乙二胺为氮源,通过水热法成功制备出了氮掺杂碳量子点N-CQDs。研究了乙二胺体积、pH值、氯化钠浓度对合成N-CQDs荧光强度的影响。制备的N-CQDs形状似球形,分散均匀,平均粒径为6.22 nm,有与石墨烯相似的清晰的晶格条纹,得到的荧光产率为24.66%,是未掺杂CQDs的近4倍。所制备的N-CQDs荧光发射不依赖激发,荧光激发峰在386 nm,荧光寿命为6.22 ns。第三部分:将高荧光量子产率的N-CQDs用于离子检测。通过荧光猝灭法测定汞离子,Hg~(2+)在0.1~5.0μM浓度范围内F/F0与Hg~(2+)的浓度呈线性关系,检出限为0.06μM(12.1μg/L)。接着,向N-CQDs-Hg~(2+)体系分别加入12种阴离子,根据荧光恢复现象确定了体系对碘阴离子的高选择性。探讨了pH值对测定的影响,找到了体系检测碘离子的最佳pH值,从而建立起测定碘离子浓度可行性方法。可检测0.2 50.0μM浓度范围内的I-,检出限为0.098μM(14.11μg/L),由于其线性范围跨度较宽,可用于检测药物中碘离子的含量,成功用于实际药品西地碘华素片中碘离子检测,获得令人满意的结果。
[Abstract]:Carbon quantum dots (CQDs) have attracted much attention due to their rich raw materials and various preparation methods. Its optical properties provide a broad prospect for the development and application of fluorescent nanomaterials. In aqueous phase, cations and anions can quench and reduce the fluorescence produced by CQDs, which can be used for sensing. High fluorescence quantum yield is a prerequisite for the wide application of CQDs, so it is very important to find a way to increase the yield of CQDs. In this paper, the different preparation methods, optical properties and applications of carbon quantum dots are studied. The main work is as follows: the first part: using gluconic acid as the carbon source of this experiment, using some common preparation methods such as microwave method, pyrolysis method, hydrothermal method, we prepared CQDs.. In the first chapter, the effects of microwave time, pyrolysis temperature, pyrolysis time, hydrothermal time and concentration of gluconic acid on the fluorescence intensity of the prepared carbon quantum dots were studied. The particle size and optical properties of the carbon quantum dots prepared by three different methods were compared. The fluorescence emission dependence of the carbon quantum dots prepared by microwave and pyrolysis was dependent on excitation, and the CQDs prepared by hydrothermal method had the optical properties of emission independent. The fluorescence quantum yield was the highest, 6.01%. The second part: N-doped carbon quantum dots N-CQDswere successfully prepared by hydrothermal method using gluconic acid as carbon source and ethylenediamine as nitrogen source. The effects of the volume of ethylenediamine, the pH value and the concentration of sodium chloride on the fluorescence intensity of synthetic N-CQDs were studied. The prepared N-CQDs is spherical in shape and uniform in dispersion. The average particle size of 6.22 nm, has clear lattice stripes similar to graphene. The fluorescence yield of the prepared N-CQDs is 24.66, which is nearly 4 times of that of undoped CQDs. The fluorescence emission of the prepared N-CQDs is independent of excitation, and the fluorescence excitation peak is 6.22 ns. at 386 nm,. Part three: N-CQDs with high fluorescence quantum yield is used for ion detection. The concentration of Hg~ (2) was linear to that of Hg~ (2) in the concentration range of 0.1 渭 M, and the detection limit was 0.06 渭 M (12.1 渭 g / L). Then, 12 kinds of anions were added to N-CQDs-Hg2 system, and the high selectivity of iodide anions was determined according to the fluorescence recovery phenomenon. The influence of pH value on the determination of iodide ion was discussed. The best pH value for the determination of iodine ion in the system was found, and the feasible method for the determination of iodine ion concentration was established. The detection limit is 0.098 渭 M (14.11 渭 g / L). Because of its wide linear range, it can be used for the determination of iodine ion in the drug. It has been successfully applied to the determination of iodine ion in the actual drug ciliodol tablets with satisfactory results.
【学位授予单位】：江西师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.3
本文编号：2267669
[Abstract]:Carbon quantum dots (CQDs) have attracted much attention due to their rich raw materials and various preparation methods. Its optical properties provide a broad prospect for the development and application of fluorescent nanomaterials. In aqueous phase, cations and anions can quench and reduce the fluorescence produced by CQDs, which can be used for sensing. High fluorescence quantum yield is a prerequisite for the wide application of CQDs, so it is very important to find a way to increase the yield of CQDs. In this paper, the different preparation methods, optical properties and applications of carbon quantum dots are studied. The main work is as follows: the first part: using gluconic acid as the carbon source of this experiment, using some common preparation methods such as microwave method, pyrolysis method, hydrothermal method, we prepared CQDs.. In the first chapter, the effects of microwave time, pyrolysis temperature, pyrolysis time, hydrothermal time and concentration of gluconic acid on the fluorescence intensity of the prepared carbon quantum dots were studied. The particle size and optical properties of the carbon quantum dots prepared by three different methods were compared. The fluorescence emission dependence of the carbon quantum dots prepared by microwave and pyrolysis was dependent on excitation, and the CQDs prepared by hydrothermal method had the optical properties of emission independent. The fluorescence quantum yield was the highest, 6.01%. The second part: N-doped carbon quantum dots N-CQDswere successfully prepared by hydrothermal method using gluconic acid as carbon source and ethylenediamine as nitrogen source. The effects of the volume of ethylenediamine, the pH value and the concentration of sodium chloride on the fluorescence intensity of synthetic N-CQDs were studied. The prepared N-CQDs is spherical in shape and uniform in dispersion. The average particle size of 6.22 nm, has clear lattice stripes similar to graphene. The fluorescence yield of the prepared N-CQDs is 24.66, which is nearly 4 times of that of undoped CQDs. The fluorescence emission of the prepared N-CQDs is independent of excitation, and the fluorescence excitation peak is 6.22 ns. at 386 nm,. Part three: N-CQDs with high fluorescence quantum yield is used for ion detection. The concentration of Hg~ (2) was linear to that of Hg~ (2) in the concentration range of 0.1 渭 M, and the detection limit was 0.06 渭 M (12.1 渭 g / L). Then, 12 kinds of anions were added to N-CQDs-Hg2 system, and the high selectivity of iodide anions was determined according to the fluorescence recovery phenomenon. The influence of pH value on the determination of iodide ion was discussed. The best pH value for the determination of iodine ion in the system was found, and the feasible method for the determination of iodine ion concentration was established. The detection limit is 0.098 渭 M (14.11 渭 g / L). Because of its wide linear range, it can be used for the determination of iodine ion in the drug. It has been successfully applied to the determination of iodine ion in the actual drug ciliodol tablets with satisfactory results.
【学位授予单位】：江西师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.3
【引证文献】
相关期刊论文 前1条
1 张敬然;宫子璇;张晓凡;刘广涵;;碳量子点的合成与表征[J];现代盐化工;2018年01期
，本文编号：2267669
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