氮摻雜葡萄糖酸碳量子點的合成及其光學性能的研究
發(fā)布時間：2018-10-12 21:32
【摘要】：碳量子點(CQDs)因原料豐富,制備方法多樣而備受研究者關(guān)注。其光學性能為熒光納米材料的開發(fā)和應(yīng)用提供了更廣泛的前景。在水相中,陽離子與陰離子能夠?qū)QDs產(chǎn)生的熒光進行猝滅和還原,可應(yīng)用于傳感。高熒光量子產(chǎn)率是CQDs廣泛應(yīng)用的前提,所以找到能夠提高CQDs產(chǎn)量的方法非常重要,本文研究了碳量子點的不同制備方法、光學性能和應(yīng)用,主要工作如下:第一部分:以葡萄糖酸為本實驗所需碳源,使用一些常用的制備方法如微波法,熱解法,水熱法,制備了CQDs。在第一章節(jié)中研究了微波時間,熱解溫度和熱解時間,水熱時間和葡萄糖酸濃度對所制備碳量子點熒光強度的影響。比較了三種不同方法制得的碳量子點的粒徑大小及光學特性,其中微波法和熱解法制備出的碳量子點熒光發(fā)射依賴激發(fā),水熱法制備出的CQDs具有發(fā)射不依賴激發(fā)的光學性質(zhì),熒光量子產(chǎn)率最高,為6.01%。第二部分:以葡萄糖酸為碳源,乙二胺為氮源,通過水熱法成功制備出了氮摻雜碳量子點N-CQDs。研究了乙二胺體積、pH值、氯化鈉濃度對合成N-CQDs熒光強度的影響。制備的N-CQDs形狀似球形,分散均勻,平均粒徑為6.22 nm,有與石墨烯相似的清晰的晶格條紋,得到的熒光產(chǎn)率為24.66%,是未摻雜CQDs的近4倍。所制備的N-CQDs熒光發(fā)射不依賴激發(fā),熒光激發(fā)峰在386 nm,熒光壽命為6.22 ns。第三部分:將高熒光量子產(chǎn)率的N-CQDs用于離子檢測。通過熒光猝滅法測定汞離子,Hg~(2+)在0.1~5.0μM濃度范圍內(nèi)F/F0與Hg~(2+)的濃度呈線性關(guān)系,檢出限為0.06μM(12.1μg/L)。接著,向N-CQDs-Hg~(2+)體系分別加入12種陰離子,根據(jù)熒光恢復(fù)現(xiàn)象確定了體系對碘陰離子的高選擇性。探討了pH值對測定的影響,找到了體系檢測碘離子的最佳pH值,從而建立起測定碘離子濃度可行性方法�？蓹z測0.2 50.0μM濃度范圍內(nèi)的I-,檢出限為0.098μM(14.11μg/L),由于其線性范圍跨度較寬,可用于檢測藥物中碘離子的含量,成功用于實際藥品西地碘華素片中碘離子檢測,獲得令人滿意的結(jié)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.
【學位授予單位】：江西師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.3
本文編號：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.
【學位授予單位】：江西師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.3
【引證文獻】
相關(guān)期刊論文 前1條
1 張敬然;宮子璇;張曉凡;劉廣涵;;碳量子點的合成與表征[J];現(xiàn)代鹽化工;2018年01期
，本文編號：2267669
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