稀土铕离子掺杂硫化镉纳米粒子的合成及应用
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摘要
纳米技术和生物技术的结合是目前最受人关注的研究领域，而纳米粒子则是连接这两个领域的一个重要桥梁。荧光半导体纳米粒子表现出优异的光学性质，可将其作为生物标记物，它的性能可在多个方面超越现在广泛使用的有机染料标记物，将给生物学和医学带来极大的突破，同时也将大大加速纳米技术的产业化进程。本论文工作主要从事掺杂型荧光纳米粒子的合成、光学性质和表面修饰技术的研究，为开发新型纳米粒子生物标记物提供必要的理论基础。
1.用乙二醇做为配体溶剂，溶剂热法制备了CdS: Eu纳米粒子。讨论在不同反应时间、反应温度和不同掺杂浓度对合成CdS: Eu纳米粒子光学性质的影响，并研究了纳米粒子的稳定性。通过对反应体系pH值的研究，我们发现溶液的酸碱性影响着生成CdS: Eu纳米粒子的荧光强度和荧光波长。我们将所制备的CdS:Eu纳米粒子中加入电荷补偿剂（Na~+），制备出了CdS: Eu, Na纳米粒子，其荧光强度明显增强。此外，我们还利用巯基乙酸（TGA）对纳米粒子的表面进行修饰，并研究了TGA用量对纳米粒子的荧光性质的影响。
2.我们将所制备的CdS: Eu纳米粒子为内核，在其表面包覆了ZnS壳层，得到发光强度高、稳定性好的CdS:Eu/ZnS核壳型纳米粒子。通过调节反应温度、反应时间和反应物配比等实验参数来调节CdS: Eu/ZnS核壳型纳米粒子的光学性质。此外，我们将CdS: Eu/ZnS核壳型纳米粒子做了体外溶血实验，结果表明，CdS: Eu/ZnS纳米粒子的生物相容性明显好于单一的CdS: Eu纳米粒子。
3.用乙二醇甲醚做为配体溶剂，利用胶体化学法低温下制备了CdS: Eu纳米粒子。讨论了不同前驱体的配比、不同反应时间和不同反应温度对CdS:Eu纳米粒子光学性质的影响。实验中分别加入了三种电荷补偿剂Li~+、Na~+和K~+离子，随着三种电荷补偿剂的加入，纳米粒子的荧光强度都有不同程度的增强，加入Li~+离子的荧光强度最大，而K~+最小，并讨论了电荷补偿剂的作用机理。
4.用L-半胱氨酸做为稳定剂，合成了水溶性的CdS: Eu纳米粒子，实验中通过调节pH值，反应时间等一系列反应参数对纳米粒子进行优化，获得最佳的实验条件。将上述所制得的CdS: Eu纳米粒子作为荧光探针，基于淬灭原理，完成了在一定线性范围内对微量Hg~(2+)离子的定量检测。通过对反应条件的优化，得出在最佳实验条件下，Hg~(2+)离子在5×10-8~1×10-3mol·L~(-1)的浓度范围内与荧光强度呈现良好的线性关系，线性相关系数为0.9994。
In this dissertation, the work is mainly focused on the synthesis and opticalproperties of chalcogenides nanoparticles fabricated in aqueous and oil phase. Thenanoparticles are characterized by the measurement of TEM, HRTEM, XRD, FTIR,UV, and PL. We also studied the effect of the experimental conditions on opticalproperties of nanoparticles and the growth mechanism.
1. The CdS: Eu nanoparticles have been prepared by autoclave in ethyleneglycol. The PL of the CdS: Eu nanoparticles are affected by reaction time, reactiontemperature, storage time, storage conditions and different compositions. Meanwhile,the PL intensity, PL wavelength of CdS: Eu nanoparticles can be tuned under differentpH values. The PL intensity of the CdS: Eu nanoparticles decreased, when CdS: Eunanoparticles were coated by TGA. Then, the PL of CdS: Eu nanoparticles isimproved by adding the charge composition ions
2. The PL of CdS: Eu nanoparticals is improved by coating a shell of ZnS. Inaddition, The PL of the CdS: Eu nanoparticles are affected by the reaction conditions.And the biocompatibility of the CdS: Eu and CdS: Eu/ZnS nanoparticles weremeasured by hemolytic test, which indicated that they are biocompatible. It isimportant for nanoparticles as biomarkers in biological detection and diagnosis.
3. The CdS: Eu nanoparticles have been prepared in methylglycol. The PL ofthe CdS: Eu nanoparticles are affected by molar ratio of Cd/S, reaction time andreaction temperature. The PL of CdS: Eu nanoparticles is improved by adding thedifferent charge composition ions, such as Li~+、Na~+、K~+. And the PL of CdS: Eunanoparticles are strongest by adding Li~+, and the PL of CdS: Eu nanoparticles areweakest by adding K~+.
4. The CdS: Eu nanoparticles have been prepared by aqueous precipitation. ThePL of the CdS: Eu nanoparticles are affected by reaction time, pH values. Then, Themethod for the determination of Hg~(2+)ion using CdS: Eu nanoparticles as thefluorescent probes were developed. The response of nanoparticles fluorescence probeswas linearly proportional to the concentration of Hg~(2+)ions ranging from5×10-8to1×10-3mol·L-1. The reaction mechanism of the fluorescent quenching was nvestigated. Furthermore, the method was successfully applied to the determine Hg~(2+)ions in different real samples.
1.用乙二醇做为配体溶剂，溶剂热法制备了CdS: Eu纳米粒子。讨论在不同反应时间、反应温度和不同掺杂浓度对合成CdS: Eu纳米粒子光学性质的影响，并研究了纳米粒子的稳定性。通过对反应体系pH值的研究，我们发现溶液的酸碱性影响着生成CdS: Eu纳米粒子的荧光强度和荧光波长。我们将所制备的CdS:Eu纳米粒子中加入电荷补偿剂（Na~+），制备出了CdS: Eu, Na纳米粒子，其荧光强度明显增强。此外，我们还利用巯基乙酸（TGA）对纳米粒子的表面进行修饰，并研究了TGA用量对纳米粒子的荧光性质的影响。
2.我们将所制备的CdS: Eu纳米粒子为内核，在其表面包覆了ZnS壳层，得到发光强度高、稳定性好的CdS:Eu/ZnS核壳型纳米粒子。通过调节反应温度、反应时间和反应物配比等实验参数来调节CdS: Eu/ZnS核壳型纳米粒子的光学性质。此外，我们将CdS: Eu/ZnS核壳型纳米粒子做了体外溶血实验，结果表明，CdS: Eu/ZnS纳米粒子的生物相容性明显好于单一的CdS: Eu纳米粒子。
3.用乙二醇甲醚做为配体溶剂，利用胶体化学法低温下制备了CdS: Eu纳米粒子。讨论了不同前驱体的配比、不同反应时间和不同反应温度对CdS:Eu纳米粒子光学性质的影响。实验中分别加入了三种电荷补偿剂Li~+、Na~+和K~+离子，随着三种电荷补偿剂的加入，纳米粒子的荧光强度都有不同程度的增强，加入Li~+离子的荧光强度最大，而K~+最小，并讨论了电荷补偿剂的作用机理。
4.用L-半胱氨酸做为稳定剂，合成了水溶性的CdS: Eu纳米粒子，实验中通过调节pH值，反应时间等一系列反应参数对纳米粒子进行优化，获得最佳的实验条件。将上述所制得的CdS: Eu纳米粒子作为荧光探针，基于淬灭原理，完成了在一定线性范围内对微量Hg~(2+)离子的定量检测。通过对反应条件的优化，得出在最佳实验条件下，Hg~(2+)离子在5×10-8~1×10-3mol·L~(-1)的浓度范围内与荧光强度呈现良好的线性关系，线性相关系数为0.9994。
In this dissertation, the work is mainly focused on the synthesis and opticalproperties of chalcogenides nanoparticles fabricated in aqueous and oil phase. Thenanoparticles are characterized by the measurement of TEM, HRTEM, XRD, FTIR,UV, and PL. We also studied the effect of the experimental conditions on opticalproperties of nanoparticles and the growth mechanism.
1. The CdS: Eu nanoparticles have been prepared by autoclave in ethyleneglycol. The PL of the CdS: Eu nanoparticles are affected by reaction time, reactiontemperature, storage time, storage conditions and different compositions. Meanwhile,the PL intensity, PL wavelength of CdS: Eu nanoparticles can be tuned under differentpH values. The PL intensity of the CdS: Eu nanoparticles decreased, when CdS: Eunanoparticles were coated by TGA. Then, the PL of CdS: Eu nanoparticles isimproved by adding the charge composition ions
2. The PL of CdS: Eu nanoparticals is improved by coating a shell of ZnS. Inaddition, The PL of the CdS: Eu nanoparticles are affected by the reaction conditions.And the biocompatibility of the CdS: Eu and CdS: Eu/ZnS nanoparticles weremeasured by hemolytic test, which indicated that they are biocompatible. It isimportant for nanoparticles as biomarkers in biological detection and diagnosis.
3. The CdS: Eu nanoparticles have been prepared in methylglycol. The PL ofthe CdS: Eu nanoparticles are affected by molar ratio of Cd/S, reaction time andreaction temperature. The PL of CdS: Eu nanoparticles is improved by adding thedifferent charge composition ions, such as Li~+、Na~+、K~+. And the PL of CdS: Eunanoparticles are strongest by adding Li~+, and the PL of CdS: Eu nanoparticles areweakest by adding K~+.
4. The CdS: Eu nanoparticles have been prepared by aqueous precipitation. ThePL of the CdS: Eu nanoparticles are affected by reaction time, pH values. Then, Themethod for the determination of Hg~(2+)ion using CdS: Eu nanoparticles as thefluorescent probes were developed. The response of nanoparticles fluorescence probeswas linearly proportional to the concentration of Hg~(2+)ions ranging from5×10-8to1×10-3mol·L-1. The reaction mechanism of the fluorescent quenching was nvestigated. Furthermore, the method was successfully applied to the determine Hg~(2+)ions in different real samples.
引文
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