论文总字数：18983字

摘 要

本实验设计合成了石墨烯量子点，运用“自下而上”的一步水热法，以无水柠檬酸和丙烯酰胺为原料，通过水热合成制备出具有高量子产率的石墨烯量子点。在合成实验中，对影响量子产率的实验条件（水热时间、水热温度、柠檬酸和丙烯酰胺的摩尔配比）进行了探究优化，根据正交实验法，设计了三因素三水平的正交表，最终的到最佳制备方案：水热温度200 ℃、水热时间8 h、摩尔比1：10。运用一系列表征手段进行表征后，得到了所制备的石墨烯量子点的相关性质，并通过计算得出实验制得的石墨烯量子点拥有较高的量子产率（41.64%），在金属离子选择性实验中发现Fe³ 可以使石墨烯量子点发生荧光猝灭，这揭示了运用该量子点进行Fe³ 离子检测的可行性。在接下来对Fe³ 灵敏度测试的实验中，在0~400 μM的线性范围内通过数据拟合得到R²=0.998的拟合曲线：y=0.00148x 0.00699，检测限为58.03μM。

关键词：一步水热法 荧光猝灭 石墨烯量子点 荧光探针 铁离子

Preparation and application of doped graphene quantum dots

Abstract

This experiment was designed to synthesize graphene quantum dots. Using a "bottom-up" method named one-step hydrothermal method. Anhydrous citric acid and acrylamide were used as raw materials to prepare graphene quantum dots with high quantum yield. In this experiment the experimental conditions (hydrothermal time, hydrothermal temperature, molar ratio of critic acid and acrylamide) affecting the quantum yield were investigated and optimized. According to the orthogonal experiment method, orthogonal table with three factors and three levels were designed. The final and best preparation plan was hydrothermal temperature 200 ℃,hydrothermal time 8 h, molar ratio 1:10.After using a series of methods to characterize, the relevant properties of the prepared graphene quantum dots were obtained .It is noted that this GQDs has a really high quantum yield (41.64%).In the selectivity experiment of metal ions ,it was found that Fe³ can quench the fluorescence of graphene quantum dots, which reveals the feasibility of using this quantum dots for Fe³ detection. In the next Fe³ sensitivity experiment, the R² of fitting curve obtained by data fitting in the linear range of 0~400μM was 0.998. Fitted curve was y=0.00148x 0.00699, LOD was 58.03 μM.

Key words: Hydrothermal method; Fluorescence quenching; Graphene quantum dots; Fluorescent probe; Iron ion

目录

摘要 I

Abstract II

第一章 文献综述 1

1.1引言 1

1.2石墨烯量子点的结构 2

1.3石墨烯量子点的性质 3

1.4石墨烯量子点的制备方法 3

1.4.1脉冲激光法 4

1.4.2电化学剥离法 5

1.4.3液相剥离法 5

1.4.4水热法 5

1.4.5微波水热法 6

1.5石墨烯量子点的应用 6

1.5.1超级电容器 6

1.5.2离子检测器 6

1.5.3生物传感器 7

1.5.4生物成像 7

1.6本实验的研究方法 8

第二章 实验部分 9

2.1 实验材料与仪器 9

2.1.1仪器与试剂 9

2.2 实验内容 10

2.2.1石墨烯量子点的合成 10

2.2.2石墨烯量子点的表征 10

2.2.3荧光量子产率的测定 10

2.2.4对铁离子的检测条件 11

2.2.4.1离子强度对石墨烯量子点荧光强度的影响 11

2.2.4.2 pH对石墨烯量子点荧光强度的影响 11

2.2.4.3 对铁离子的检测 11

第三章 实验结果与讨论 12

3.1结果与讨论 12

3.1.1石墨烯量子点合成条件的选择 12

3.1.2 石墨烯量子点的表征 13

3.1.2.2 石墨烯量子点的FTIR表征 13

3.1.2.3 石墨烯量子点的紫外和荧光谱图分析 13

3.1.3离子强度对石墨烯量子点荧光强度的影响 15

3.1.4pH对石墨烯量子点荧光强度的影响 16

3.2石墨烯量子点对铁离子的检测 17

3.2.1石墨烯量子点对Fe³ 选择性的检测 17

3.2.2石墨烯量子点对Fe³ 的灵敏性检测 18

第四章 结论与展望 21

4.1结论 21

4.2展望 21

参考文献 22

致 谢 25

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