无添加剂贵金属纳米颗粒的合成及应用研究
发布时间：2018-09-19 08:40
【摘要】：近年来,金属纳米颗粒由于其独特的物理和化学性质,在许多领域引起了广泛的重视,成为材料科学的研究热点。在各种各样的金属纳米颗粒中,贵金属纳米颗粒赢得了研究者的重点关注,它们因为具有新颖、奇异的性质,而被广泛应用于催化、电子学、光谱学等领域。随着社会经济的发展,“绿色化学”这一概念越来越受到人们的关注,绿色、环保的化学合成方法也越来越符合大众的需求。传统的贵金属纳米颗粒的合成方法,主要是化学液相还原法,过程中需要加入还原剂、表面活性剂等添加剂。为响应绿色化学的要求,我们采用辐照的方法,在不添加任何添加剂的条件下,直接制备了贵金属纳米颗粒并研究了其应用。具体内容如下:(1)利用gamma射线辐照,在不添加任何还原剂和保护剂的情况下,直接合成了均匀稳定的金纳米颗粒,并通过扫描电镜,X-射线粉末衍射仪,紫外-可见吸收光谱仪进行表征分析。将所制备的金纳米颗粒应用于电化学检测,以葡萄糖和多巴胺作为被检测分子,研究其电化学行为。实验结果表明,金纳米颗粒修饰的电极表现出优异的电化学性能,对葡萄糖和多巴胺的检测具有高灵敏度性,并且具有良好的重复性和稳定性。(2)以同样的方法合成了银纳米颗粒,同时研究了金纳米颗粒和银纳米颗粒的表面增强拉曼性能。用所合成的纳米颗粒分别制作表面增强拉曼基底,以罗丹明6G作为客体分子,采用液体测试方式分别检测了基底的表面增强拉曼性能。结果显示,金纳米颗粒制备的基底可清晰检测到浓度为1×10-7 M的罗丹明6G分子,银纳米颗粒基底能清晰检测到1×10-9 M的罗丹明6G分子。所制备活性基底不仅具有高灵敏性,也具有高稳定性和重复性。随机选取100点收集拉曼信号,每个点都能采集到清晰的罗丹明6G的信号,且主要峰的峰强的相对标准偏差均小于20%。(3)通过辐照还原的方法从氧化银颗粒中直接还原出银纳米颗粒,并原位检测其SERS活性。首先,通过湿化学法,在不添加稳定剂的情况下合成氧化银纳米颗粒。同时,采用液-液界面自组装的方法,用所合成的氧化银纳米颗粒制作表面增强拉曼基底。分别以罗丹明6G和4-巯基苯甲酸作为被检测物质,研究了所制备的表面增强拉曼基底的性能。实验结果显示,随着时间的累积,客体分子的特征峰越来越明显,峰强也逐渐增加,当时间累积到一定程度后,特征峰强度不再变化,基本处于平稳状态。曝光一定时间后,随机连续收集多个点的拉曼信号,每个点都能获得高灵敏度的拉曼信号,且具有较好的重现性。以上结果表明,所制备的贵金属纳米颗粒具有较好的电化学性质和表面增强拉曼性能。辐照合成法作为一种可行的绿色、环保制备手段,可广泛应用于其他材料的合成,应用前景广阔。
[Abstract]:In recent years, metal nanoparticles have attracted extensive attention in many fields because of their unique physical and chemical properties. Among all kinds of metal nanoparticles, noble metal nanoparticles have attracted the attention of researchers. They have been widely used in catalysis, electronics, spectroscopy and other fields because of their novel and strange properties. With the development of social economy, people pay more and more attention to the concept of "green chemistry". The traditional method of synthesis of noble metal nanoparticles is mainly chemical liquid phase reduction, and additives such as reductant and surfactant are needed in the process. In order to meet the requirements of green chemistry, we have prepared noble metal nanoparticles directly and studied their applications by irradiation without adding any additives. The main contents are as follows: (1) the uniform and stable gold nanoparticles were synthesized by gamma irradiation without adding any reducer and protectant, and the X-ray powder diffractometer was used. UV-vis absorption spectrometer was used for characterization and analysis. The prepared gold nanoparticles were used for electrochemical detection. Glucose and dopamine were used as the detected molecules to study their electrochemical behavior. The results showed that the gold nanoparticles modified electrode showed excellent electrochemical performance and high sensitivity to the detection of glucose and dopamine. Silver nanoparticles were synthesized in the same way and the surface enhanced Raman properties of gold nanoparticles and silver nanoparticles were studied. The surface-enhanced Raman substrates were prepared from the synthesized nanoparticles, and the surface-enhanced Raman properties of the substrates were measured by liquid test using Rhodamine 6G as guest molecule. The results show that the concentration of Rhodamine 6G is 1 脳 10 ~ (-7) M and that of Rhodamine 6G of 1 脳 10 ~ (-9) M can be clearly detected on the substrate prepared by gold nanoparticles, while that of Rhodamine 6G at a concentration of 1 脳 10 ~ (-7) M can be clearly detected on the silver nanoparticles substrate. The prepared active substrate not only has high sensitivity, but also has high stability and repeatability. At random, 100 points were selected to collect Raman signals. Each point could collect a clear Rhodamine 6G signal, and the relative standard deviation of peak strength of the main peak was less than 20. (3) Silver nanoparticles were directly reduced from silver oxide particles by irradiation reduction. The SERS activity was detected in situ. First, silver oxide nanoparticles were synthesized by wet chemical method without adding stabilizer. At the same time, the surface-enhanced Raman substrate was fabricated by using the synthesized silver oxide nanoparticles by the liquid-liquid interface self-assembly method. Using Rhodamine 6G and 4-mercaptobenzoic acid as the detected substances, the properties of the surface-enhanced Raman substrates were studied. The experimental results show that with the accumulation of time the characteristic peak of the guest molecule becomes more and more obvious and the peak strength increases gradually. When the time accumulates to a certain extent the intensity of the characteristic peak does not change and is basically in a stable state. After exposure for a certain time, the Raman signals of multiple points are collected at random, each point can obtain a high sensitivity Raman signal, and it has good reproducibility. The results show that the prepared noble metal nanoparticles have good electrochemical properties and surface-enhanced Raman properties. As a feasible green and environmentally friendly preparation method, irradiation synthesis can be widely used in the synthesis of other materials.
【学位授予单位】：苏州大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O614.12;TB383.1
本文编号：2249620
[Abstract]:In recent years, metal nanoparticles have attracted extensive attention in many fields because of their unique physical and chemical properties. Among all kinds of metal nanoparticles, noble metal nanoparticles have attracted the attention of researchers. They have been widely used in catalysis, electronics, spectroscopy and other fields because of their novel and strange properties. With the development of social economy, people pay more and more attention to the concept of "green chemistry". The traditional method of synthesis of noble metal nanoparticles is mainly chemical liquid phase reduction, and additives such as reductant and surfactant are needed in the process. In order to meet the requirements of green chemistry, we have prepared noble metal nanoparticles directly and studied their applications by irradiation without adding any additives. The main contents are as follows: (1) the uniform and stable gold nanoparticles were synthesized by gamma irradiation without adding any reducer and protectant, and the X-ray powder diffractometer was used. UV-vis absorption spectrometer was used for characterization and analysis. The prepared gold nanoparticles were used for electrochemical detection. Glucose and dopamine were used as the detected molecules to study their electrochemical behavior. The results showed that the gold nanoparticles modified electrode showed excellent electrochemical performance and high sensitivity to the detection of glucose and dopamine. Silver nanoparticles were synthesized in the same way and the surface enhanced Raman properties of gold nanoparticles and silver nanoparticles were studied. The surface-enhanced Raman substrates were prepared from the synthesized nanoparticles, and the surface-enhanced Raman properties of the substrates were measured by liquid test using Rhodamine 6G as guest molecule. The results show that the concentration of Rhodamine 6G is 1 脳 10 ~ (-7) M and that of Rhodamine 6G of 1 脳 10 ~ (-9) M can be clearly detected on the substrate prepared by gold nanoparticles, while that of Rhodamine 6G at a concentration of 1 脳 10 ~ (-7) M can be clearly detected on the silver nanoparticles substrate. The prepared active substrate not only has high sensitivity, but also has high stability and repeatability. At random, 100 points were selected to collect Raman signals. Each point could collect a clear Rhodamine 6G signal, and the relative standard deviation of peak strength of the main peak was less than 20. (3) Silver nanoparticles were directly reduced from silver oxide particles by irradiation reduction. The SERS activity was detected in situ. First, silver oxide nanoparticles were synthesized by wet chemical method without adding stabilizer. At the same time, the surface-enhanced Raman substrate was fabricated by using the synthesized silver oxide nanoparticles by the liquid-liquid interface self-assembly method. Using Rhodamine 6G and 4-mercaptobenzoic acid as the detected substances, the properties of the surface-enhanced Raman substrates were studied. The experimental results show that with the accumulation of time the characteristic peak of the guest molecule becomes more and more obvious and the peak strength increases gradually. When the time accumulates to a certain extent the intensity of the characteristic peak does not change and is basically in a stable state. After exposure for a certain time, the Raman signals of multiple points are collected at random, each point can obtain a high sensitivity Raman signal, and it has good reproducibility. The results show that the prepared noble metal nanoparticles have good electrochemical properties and surface-enhanced Raman properties. As a feasible green and environmentally friendly preparation method, irradiation synthesis can be widely used in the synthesis of other materials.
【学位授予单位】：苏州大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O614.12;TB383.1
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