多功能含金属纳米材料的制备与性质研究
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摘要
随着科技的发展，多功能纳米材料越来越受到科学家们的重视，它们在离子检测、催化和生物成像等方面得到了广泛应用。已有的功能材料主要包括荧光功能材料，磁功能材料以及电功能材料。然而单一功能的纳米材料已经不能满足当今应用的需要，多功能复合材料尤其荧光和磁性纳米杂化材料成为研究的热点之一。无论从基础研究或应用前景上看，探索荧光和磁性纳米材料新型的合成方法，并对所得荧光和磁性纳米材料性质进行研究以及制备出多功能杂化材料无疑有重要的现实意义。因此，本论文围绕多功能含金属纳米材料及其杂化材料，开展了以下四部分工作：
在论文的第2章中，我们发展了一种弱胺还原的方法制备荧光纳米簇。采用水合肼作为还原剂，谷胱甘肽作为稳定剂情况下，温和条件下制备荧光Ag纳米簇。获得的Ag纳米簇粒径均匀，具有优良的荧光性质，其荧光发射峰位在620nm，且具有很好的稳定性和水溶性质。进一步，以合成的Ag纳米簇作为模板，采用galvanic exchange reaction方法制备了荧光Au纳米点。所得的Au纳米点粒径均匀约为2.9nm，表现出优良的荧光性质，荧光量子效率高达10%；同时制备的Au纳米点的荧光性质具有优异的稳定性，在pH=1-11较宽范围的溶液中、高浓度盐离子环境下、长时间放置以及强光照射下，其荧光性质几乎不发生改变,这归因于Au纳米点表面由谷胱甘肽稳定和Au(I)-S配合物的稳定作用；获得Au纳米点具有良好的水溶性和低的生物毒性，将其与CAL-27和MC3T3-E1细胞进行孵化，Au纳米点可以进入细胞质和细胞核，可以作为一种生物荧光探针。
在论文的第3章中，我们合成新型近红外荧光纳米簇并对其性质进行研究。近红外光具有在生物体内深的光穿透性和弱的光散射等优点。我们选用谷胱甘肽作为稳定剂，S-肼配合物作为S源，成功制备出来具有近红外荧光的Ag_2S纳米簇。获得的Ag_2S纳米簇尺寸均匀，结构稳定，其尺寸可以控制在1.6nm到4.5nm之间，相应的荧光发射波长从620nm的红光区移到720nm的近红外区。由于生物小分子谷胱甘肽作为稳定剂，Ag_2S纳米簇具有水溶性和稳定性好、生物毒性低等特点，它可以进入MC3T3–EI细胞的细胞质和细胞核，作为一种生物荧光探针将在细胞成像领域都具有很好的应用价值。
论文的第4章，我们沿用胺还原法，成功制备了一种同时具有荧光和磁性的新型EuSe稀土纳米晶。烷基胺和烷基酸为稳定剂，采用稀土铕的无机化合物与Se单质反应，一步制备具有低价态的EuSe纳米晶。所得EuSe纳米晶具有以下特点：形貌为球形，尺寸为20nm，粒径均匀，具有优良的荧光发射和铁磁性质。EuSe纳米晶的荧光发射峰位在403nm，半峰宽窄(约30nm)，色纯度高。通过调节实验条件可以制备出形貌各异的EuSe纳米晶，包括纳米棒，纳米带，球形以及中空纳米结构，这些不同形貌的纳米材料仍然保持荧光和磁性等性质。此方法避免使用复杂的稀土配合物，环境污染小，产物纯度高。另外，操作容易，重复性好，适合大批量制备低价态稀土纳米晶。作为一种新型荧光和磁性的纳米材料，EuSe纳米晶在磁光设备等方面具有很好的应用前景。利用两亲性嵌段聚合物F127，可以实现将稀土纳米晶从油相转移到水相，将在细胞荧光成像和磁成像等领域显示出应用价值。
在论文的第5章中，我们采用层层组装法制备荧光和磁性纳米杂化材料。采用紫外光还原法制备了阴离子聚电解质PAA稳定的荧光Ag纳米簇，其荧光发射峰位为570nm，粒径为1.5nm。通过一种阳离子聚电解质PAH辅助，利用库伦力等超分子作用层层组装，实现将磁性Fe_3O_4和荧光Ag纳米簇复合，制备磁性/荧光纳米杂化材料。获得以Fe_3O_4为核、外层修饰Ag纳米簇的杂化材料，保持了Fe_3O_4的磁性和Ag的纳米簇荧光性质。进一步，我们采用相近的方法，制备具有上下双模转换型荧光的Ag NCs-NaGdF_4:Yb/Tm NPs磁/光纳米杂化材料。这些磁性和荧光多功能杂化材料将在荧光成像和核磁共振生物成像等领域得到应用。
With the development of science and technology, multifunctional nanomaterialsattracted more and more attention of scientists and they have been widely used inions detection, catalysis and biological imaging. Existing functional materials arefluorescent, magnetic, and electrical function. However, nanomaterials with singlefunction can not be suitable for practical applications. Multifunctional hybridmaterials, especially magnetic and fluorescent hybrid materials become one ofresearch focus. Therefore, based on the point of view of basic research andapplications, exploring novel synthesis method and property of magnetic andfluorescent nano-materials as well as further preparing the multifunctional hybridmaterials will undoubtedly have important practical significance. In my PhD paper,around metal-containing multifunctional nanomaterials, we carry out the follow fourparts of work:
In Chapter2, we develop reduction method with weak amine to preparefluorescent nanoclusters (NCs). Using hydrazine hydrate (N2H4.2H2O) as reducingagent and glutathione (GSH) as stabling agent, fluorescent Ag NCs were synthesizedat room temperature. As-prepared Ag NCs exhibited red fluorescence with amaximum emission at620nm, and had good stability, water-soluble and uniformsize. Using presynthesized and size-specific controlled Ag nanodots (Ag NDs) astemplates, the galvanic exchange reaction was used to prepare fluorescent goldnanodots (GNDs). As-prepared GNDs with the size of2.9nm lead to propensities ofstrong fluorescence (quantum yields~10%), high stability and surface-bioactivity.The PL of resultant GNDs showed high photo-, time-, metal-and pH-stability. In pHvalues ranged from1to11, the solution of high salt concentration, exposed under450W Xenon (Xe) lamp for3h and storing under normal condition for three months,the PL of GNDs hardly changed, which were attributed to the protective surface layer of glutathione (GSH) and the presence of Au(I)-S complex on the surface ofthe gold core.. Moreover, this glutathione, as a stabilizer makes GNDs have gooddispersion in aqueous solution and low biological toxicity. In this study, the CAL-27and MC3T3-E1cells are used as a model to evaluate the fluorescence imaging ofGNDs.
Next in Chapter3, we study the novel near-infrared (NIR) NCs. In vivoapplication the NIR nanomaterials have the advantages of the deep light penetrationand weak light scattering. Using GSH as capping reagent and sulfur-hydrazinehydrate complex as S~(2-)source, NIR Ag_2S NCs were prepared. The resultant Ag_2SNCs showed tunable luminescence from visible red (624nm) to NIR (724nm)corresponding to increasing the size from1.6nm to4.5nm. GSH is a kind of smallbiomolecules with several functional groups, including carboxyl and amino groupsthat suggested resultant Ag_2S NCs had good dispersion in aqueous solution and lowbiological toxicity. These advantages made as-prepared Ag_2S NCs possess potentialapplications in biological labeling as well. At last, MC3T3-EI cells are choosed toconfirm as-prepared NIR Ag_2S NCs have good application in the field of cellimaging.
In Chapter4, we use similar amine reducing approach to prepare magnetic andfluorescent dual functional EuSe nanocrystals. Using EuCl3(H2O)6and elemental Seas Eu and Se sources, and using the alkyl amines (OLA) and alkyl acids (OA) asstabilizing agent, one-step was developed to prepare divalent EuSe nanocrystals. Theresultant EuSe nanocrystals with spherical morphology and the size of20nm showblue emission (peaking at403nm with2.8%quantum yield) and magnetic propertywith coercively (Hc) of80.2Oe at room temperature. Controlling experimentalconditions, the morphologis of EuSe nanocrystals could be tunable and nanorods,nanobelts, spherical and hollow nanoparticles can be prepared. These EuSenanocrystals with various morphologies also have fluorescent and magneticpreporties. In our approach, the amine also behaves as a reducing agent. Note thatour ready approach is highly reproducible and suitable for large-scale production, facilitating the potential in various applications including opto-magnetic devices,optical isolators, optical catalysis, and photo magnetic memories. By F127, EuSenanocrystals could be transferred to aqueous phase, which suggested the EuSenanocrystals had a broader range of applications in the field of cell imaging andmagnetic imaging.
Finally, in Chapter5, the layer by layer assembly method is used to preparefluorescent NCs and magnetic nanopartlcles (NPs) hybrid nanomaterials. Using UVreduction method, PAA, the anionic polyelectrolyte, stabilized fluorescent Ag NCswere synthesized. As-prepared PAA-Ag NCs with the size of1.5nm showfluorescence property with emission at570nm. Then, through the help of PAH, thecationic electrolyte, magnetic Fe_3O_4NPs and fluorescent PAA-Ag NCs hybridnanomaterials are prepared by layer by layer assembly. As-prepared hybridnanomaterials have the core of Fe_3O_4and the outermost layer of fluorescent PAA-AgNCs. Hence as-prepared hybrid nanomaterials show magnetic and fluorescentproperties of Fe_3O_4NPs and Ag NCs. Then, we use similar layer by layer assemblymethod to prepare paramagnetic, up and down dual model fluorescent AgNCs-NaGdF_4: Yb/Tm NPs hybrid nanomaterials. The magnetic and fluorescentmultifunctional hybrid nanomaterials could be applied in the field of biologicalimaging and magnetic resonance imaging.
在论文的第2章中，我们发展了一种弱胺还原的方法制备荧光纳米簇。采用水合肼作为还原剂，谷胱甘肽作为稳定剂情况下，温和条件下制备荧光Ag纳米簇。获得的Ag纳米簇粒径均匀，具有优良的荧光性质，其荧光发射峰位在620nm，且具有很好的稳定性和水溶性质。进一步，以合成的Ag纳米簇作为模板，采用galvanic exchange reaction方法制备了荧光Au纳米点。所得的Au纳米点粒径均匀约为2.9nm，表现出优良的荧光性质，荧光量子效率高达10%；同时制备的Au纳米点的荧光性质具有优异的稳定性，在pH=1-11较宽范围的溶液中、高浓度盐离子环境下、长时间放置以及强光照射下，其荧光性质几乎不发生改变,这归因于Au纳米点表面由谷胱甘肽稳定和Au(I)-S配合物的稳定作用；获得Au纳米点具有良好的水溶性和低的生物毒性，将其与CAL-27和MC3T3-E1细胞进行孵化，Au纳米点可以进入细胞质和细胞核，可以作为一种生物荧光探针。
在论文的第3章中，我们合成新型近红外荧光纳米簇并对其性质进行研究。近红外光具有在生物体内深的光穿透性和弱的光散射等优点。我们选用谷胱甘肽作为稳定剂，S-肼配合物作为S源，成功制备出来具有近红外荧光的Ag_2S纳米簇。获得的Ag_2S纳米簇尺寸均匀，结构稳定，其尺寸可以控制在1.6nm到4.5nm之间，相应的荧光发射波长从620nm的红光区移到720nm的近红外区。由于生物小分子谷胱甘肽作为稳定剂，Ag_2S纳米簇具有水溶性和稳定性好、生物毒性低等特点，它可以进入MC3T3–EI细胞的细胞质和细胞核，作为一种生物荧光探针将在细胞成像领域都具有很好的应用价值。
论文的第4章，我们沿用胺还原法，成功制备了一种同时具有荧光和磁性的新型EuSe稀土纳米晶。烷基胺和烷基酸为稳定剂，采用稀土铕的无机化合物与Se单质反应，一步制备具有低价态的EuSe纳米晶。所得EuSe纳米晶具有以下特点：形貌为球形，尺寸为20nm，粒径均匀，具有优良的荧光发射和铁磁性质。EuSe纳米晶的荧光发射峰位在403nm，半峰宽窄(约30nm)，色纯度高。通过调节实验条件可以制备出形貌各异的EuSe纳米晶，包括纳米棒，纳米带，球形以及中空纳米结构，这些不同形貌的纳米材料仍然保持荧光和磁性等性质。此方法避免使用复杂的稀土配合物，环境污染小，产物纯度高。另外，操作容易，重复性好，适合大批量制备低价态稀土纳米晶。作为一种新型荧光和磁性的纳米材料，EuSe纳米晶在磁光设备等方面具有很好的应用前景。利用两亲性嵌段聚合物F127，可以实现将稀土纳米晶从油相转移到水相，将在细胞荧光成像和磁成像等领域显示出应用价值。
在论文的第5章中，我们采用层层组装法制备荧光和磁性纳米杂化材料。采用紫外光还原法制备了阴离子聚电解质PAA稳定的荧光Ag纳米簇，其荧光发射峰位为570nm，粒径为1.5nm。通过一种阳离子聚电解质PAH辅助，利用库伦力等超分子作用层层组装，实现将磁性Fe_3O_4和荧光Ag纳米簇复合，制备磁性/荧光纳米杂化材料。获得以Fe_3O_4为核、外层修饰Ag纳米簇的杂化材料，保持了Fe_3O_4的磁性和Ag的纳米簇荧光性质。进一步，我们采用相近的方法，制备具有上下双模转换型荧光的Ag NCs-NaGdF_4:Yb/Tm NPs磁/光纳米杂化材料。这些磁性和荧光多功能杂化材料将在荧光成像和核磁共振生物成像等领域得到应用。
With the development of science and technology, multifunctional nanomaterialsattracted more and more attention of scientists and they have been widely used inions detection, catalysis and biological imaging. Existing functional materials arefluorescent, magnetic, and electrical function. However, nanomaterials with singlefunction can not be suitable for practical applications. Multifunctional hybridmaterials, especially magnetic and fluorescent hybrid materials become one ofresearch focus. Therefore, based on the point of view of basic research andapplications, exploring novel synthesis method and property of magnetic andfluorescent nano-materials as well as further preparing the multifunctional hybridmaterials will undoubtedly have important practical significance. In my PhD paper,around metal-containing multifunctional nanomaterials, we carry out the follow fourparts of work:
In Chapter2, we develop reduction method with weak amine to preparefluorescent nanoclusters (NCs). Using hydrazine hydrate (N2H4.2H2O) as reducingagent and glutathione (GSH) as stabling agent, fluorescent Ag NCs were synthesizedat room temperature. As-prepared Ag NCs exhibited red fluorescence with amaximum emission at620nm, and had good stability, water-soluble and uniformsize. Using presynthesized and size-specific controlled Ag nanodots (Ag NDs) astemplates, the galvanic exchange reaction was used to prepare fluorescent goldnanodots (GNDs). As-prepared GNDs with the size of2.9nm lead to propensities ofstrong fluorescence (quantum yields~10%), high stability and surface-bioactivity.The PL of resultant GNDs showed high photo-, time-, metal-and pH-stability. In pHvalues ranged from1to11, the solution of high salt concentration, exposed under450W Xenon (Xe) lamp for3h and storing under normal condition for three months,the PL of GNDs hardly changed, which were attributed to the protective surface layer of glutathione (GSH) and the presence of Au(I)-S complex on the surface ofthe gold core.. Moreover, this glutathione, as a stabilizer makes GNDs have gooddispersion in aqueous solution and low biological toxicity. In this study, the CAL-27and MC3T3-E1cells are used as a model to evaluate the fluorescence imaging ofGNDs.
Next in Chapter3, we study the novel near-infrared (NIR) NCs. In vivoapplication the NIR nanomaterials have the advantages of the deep light penetrationand weak light scattering. Using GSH as capping reagent and sulfur-hydrazinehydrate complex as S~(2-)source, NIR Ag_2S NCs were prepared. The resultant Ag_2SNCs showed tunable luminescence from visible red (624nm) to NIR (724nm)corresponding to increasing the size from1.6nm to4.5nm. GSH is a kind of smallbiomolecules with several functional groups, including carboxyl and amino groupsthat suggested resultant Ag_2S NCs had good dispersion in aqueous solution and lowbiological toxicity. These advantages made as-prepared Ag_2S NCs possess potentialapplications in biological labeling as well. At last, MC3T3-EI cells are choosed toconfirm as-prepared NIR Ag_2S NCs have good application in the field of cellimaging.
In Chapter4, we use similar amine reducing approach to prepare magnetic andfluorescent dual functional EuSe nanocrystals. Using EuCl3(H2O)6and elemental Seas Eu and Se sources, and using the alkyl amines (OLA) and alkyl acids (OA) asstabilizing agent, one-step was developed to prepare divalent EuSe nanocrystals. Theresultant EuSe nanocrystals with spherical morphology and the size of20nm showblue emission (peaking at403nm with2.8%quantum yield) and magnetic propertywith coercively (Hc) of80.2Oe at room temperature. Controlling experimentalconditions, the morphologis of EuSe nanocrystals could be tunable and nanorods,nanobelts, spherical and hollow nanoparticles can be prepared. These EuSenanocrystals with various morphologies also have fluorescent and magneticpreporties. In our approach, the amine also behaves as a reducing agent. Note thatour ready approach is highly reproducible and suitable for large-scale production, facilitating the potential in various applications including opto-magnetic devices,optical isolators, optical catalysis, and photo magnetic memories. By F127, EuSenanocrystals could be transferred to aqueous phase, which suggested the EuSenanocrystals had a broader range of applications in the field of cell imaging andmagnetic imaging.
Finally, in Chapter5, the layer by layer assembly method is used to preparefluorescent NCs and magnetic nanopartlcles (NPs) hybrid nanomaterials. Using UVreduction method, PAA, the anionic polyelectrolyte, stabilized fluorescent Ag NCswere synthesized. As-prepared PAA-Ag NCs with the size of1.5nm showfluorescence property with emission at570nm. Then, through the help of PAH, thecationic electrolyte, magnetic Fe_3O_4NPs and fluorescent PAA-Ag NCs hybridnanomaterials are prepared by layer by layer assembly. As-prepared hybridnanomaterials have the core of Fe_3O_4and the outermost layer of fluorescent PAA-AgNCs. Hence as-prepared hybrid nanomaterials show magnetic and fluorescentproperties of Fe_3O_4NPs and Ag NCs. Then, we use similar layer by layer assemblymethod to prepare paramagnetic, up and down dual model fluorescent AgNCs-NaGdF_4: Yb/Tm NPs hybrid nanomaterials. The magnetic and fluorescentmultifunctional hybrid nanomaterials could be applied in the field of biologicalimaging and magnetic resonance imaging.
引文
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