聚合电解质控制下的纳米材料的合成及机理研究
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摘要
本论文较系统地研究了聚电解质在纳米材料合成中对晶体形貌的调控作用。将聚电解质引入到了有机微晶的合成过程中,采用有机小分子功能染料作为研究对象,构筑了三维等级结构。为有机小分子晶体的形貌控制提供了新的思路。研究了聚电解质和有机小分子功能材料的协同作用,在二者的共同调节下合成了球霰石相的碳酸钙空心球结构,丰富了生物模拟矿化制备无机生物材料的方法。本文还将聚电解质引入到了无机纳米材料氧化锌的合成过程中,采用二步法合成出了结构新颖功能性更强的氧化锌纳米空心管结构。研究结果归纳如下:
1.以阳离子聚电解质聚氢氯化丙烯胺(PAH)和阴离子聚电解质聚苯乙烯磺酸钠(PSS)作为调控荧光素晶体形貌的改性剂,通过调节体系反应条件(比如聚合物和原料浓度、超声、摇床辅助手段等),得到了荧光素晶体新颖的类似珊瑚的等级结构,单分散的多孔球和类浮雕状等尺寸形貌可控的有机晶体。讨论聚氢氯化丙烯胺等对荧光素溶液的紫外吸收光谱的影响。特别值得提出的是,其形成机理同样可以用聚合物调节无机材料晶体结构的机理来解释。进一步扩展了聚合物模板法在有机晶体生长调控中的应用。
2.采用生物矿化方法,利用聚氢氯化丙烯胺和染料罗丹明B(Rhodamine B)的协同作用,控制合成出了球霰石相的CaCO_3空心球。而且经过更长时间的转化过程,部分的球霰石相会转化为特殊四面体形貌的方解石。通过多组对比实验,充分证明了聚电解质和有机小分子的协同作用,说明引入了功能小分子后可以改善聚电解质对晶体的调控性能。这种多调控剂的协调作用有可能为合成特殊结构材料提供一种新的合成途径。
3.利用聚丙烯酸(PAA)作结构引导剂在低温(60°C)条件下,通过两步合成法在玻璃衬底上生长了ZnO纳米管。这种纳米管内部松散多孔,因此可以用于催化,传感器,能量存储或储氢材料。通过改变聚丙烯酸浓度以及其他添加剂的协同作用,合成了各种有趣的纳米管。这对可控调节ZnO的发光性能有重要的意义。此外,还较详细阐述了此种合成方法的可能的生长机制。
In this dissertation, the polyelectrolytes with different functional groups have been used to control the morphology of nano structured materials. The polyelectrolyte has been introduced to synthesize organic microcrystals and 3D hierarchical superstructures can be fabricated by using simply functional organic molecules as starting materials. Therefore, a new approach has been developed to control the morphology of small molecular weight organic materials. The cooperative effect of polyelectrolyte and simple functional organic molecules has been discussed. Furthermore, vaterite hollow spheres of calcium carbonate were prepared. So it enriched the biomineralization method to synthesize inorganic biomaterials. In addition, polyelectrolyte was utilized in preparing zinc oxide hollow nanotubes by two-step method. The main results can be summarized as follows:
1. Poly(allylamine hydrochloride) (PAH) and poly(sodium 4-styrenesulfonate) (PSS) have been used as crystal growth modifiers and directing reagents to prepare fluorescein crystals with novel coral-like hierarchical superstructures by adjusting reaction parameters including the concentrations of polymer and starting materials, shaking and ultrasonic treatments. The optical property can be adjusted by changing the size of fluorescein crystals and the adding of PAH. It should be mentioned that, the mechanism of controlled synthesis of organic materials under control of polyelectrolytes is similar to that works in inorganic system.
2. By taking advantage of the cooperative effects of PAH and Rhodamine B, vaterite hollow spheres can be synthesized. Part of vaterite will transform into calcite tetrahedrons. Through several parallel experiments, it fully proves the cooperative effect between polyelectrolyte and organic dye. Therefore, it suggests that the performance of polyelectrolyte can be further improved by simple functional molecules. The novel biomimetic method by use of multi-modifiers brings a novel pathway to prepare well-defined functional biominerals.
3. ZnO nanotubes (NTs) can be synthesized on glass substrate by two-step method using Poly(acrylic acid ) (PAA) as a structure direct reagent at low temperature (60℃). The interior of the ZnO tube is loose and porous, which demonstrates its potential applications in catalysis, sensor and energy. The influence of the concentration of PAA and the cooperation of PAA, Zn~(2+) and Hexamethylenetetramine (HMT) were discussed. The PL peaks of these tubular products show regular shift compared with ZnO NRs which act as the template in the first-step synthesis procedure. A possible growth mechanism of this unusual synthesis method to fabricate the ZnO NTs has been proposed.
1.以阳离子聚电解质聚氢氯化丙烯胺(PAH)和阴离子聚电解质聚苯乙烯磺酸钠(PSS)作为调控荧光素晶体形貌的改性剂,通过调节体系反应条件(比如聚合物和原料浓度、超声、摇床辅助手段等),得到了荧光素晶体新颖的类似珊瑚的等级结构,单分散的多孔球和类浮雕状等尺寸形貌可控的有机晶体。讨论聚氢氯化丙烯胺等对荧光素溶液的紫外吸收光谱的影响。特别值得提出的是,其形成机理同样可以用聚合物调节无机材料晶体结构的机理来解释。进一步扩展了聚合物模板法在有机晶体生长调控中的应用。
2.采用生物矿化方法,利用聚氢氯化丙烯胺和染料罗丹明B(Rhodamine B)的协同作用,控制合成出了球霰石相的CaCO_3空心球。而且经过更长时间的转化过程,部分的球霰石相会转化为特殊四面体形貌的方解石。通过多组对比实验,充分证明了聚电解质和有机小分子的协同作用,说明引入了功能小分子后可以改善聚电解质对晶体的调控性能。这种多调控剂的协调作用有可能为合成特殊结构材料提供一种新的合成途径。
3.利用聚丙烯酸(PAA)作结构引导剂在低温(60°C)条件下,通过两步合成法在玻璃衬底上生长了ZnO纳米管。这种纳米管内部松散多孔,因此可以用于催化,传感器,能量存储或储氢材料。通过改变聚丙烯酸浓度以及其他添加剂的协同作用,合成了各种有趣的纳米管。这对可控调节ZnO的发光性能有重要的意义。此外,还较详细阐述了此种合成方法的可能的生长机制。
In this dissertation, the polyelectrolytes with different functional groups have been used to control the morphology of nano structured materials. The polyelectrolyte has been introduced to synthesize organic microcrystals and 3D hierarchical superstructures can be fabricated by using simply functional organic molecules as starting materials. Therefore, a new approach has been developed to control the morphology of small molecular weight organic materials. The cooperative effect of polyelectrolyte and simple functional organic molecules has been discussed. Furthermore, vaterite hollow spheres of calcium carbonate were prepared. So it enriched the biomineralization method to synthesize inorganic biomaterials. In addition, polyelectrolyte was utilized in preparing zinc oxide hollow nanotubes by two-step method. The main results can be summarized as follows:
1. Poly(allylamine hydrochloride) (PAH) and poly(sodium 4-styrenesulfonate) (PSS) have been used as crystal growth modifiers and directing reagents to prepare fluorescein crystals with novel coral-like hierarchical superstructures by adjusting reaction parameters including the concentrations of polymer and starting materials, shaking and ultrasonic treatments. The optical property can be adjusted by changing the size of fluorescein crystals and the adding of PAH. It should be mentioned that, the mechanism of controlled synthesis of organic materials under control of polyelectrolytes is similar to that works in inorganic system.
2. By taking advantage of the cooperative effects of PAH and Rhodamine B, vaterite hollow spheres can be synthesized. Part of vaterite will transform into calcite tetrahedrons. Through several parallel experiments, it fully proves the cooperative effect between polyelectrolyte and organic dye. Therefore, it suggests that the performance of polyelectrolyte can be further improved by simple functional molecules. The novel biomimetic method by use of multi-modifiers brings a novel pathway to prepare well-defined functional biominerals.
3. ZnO nanotubes (NTs) can be synthesized on glass substrate by two-step method using Poly(acrylic acid ) (PAA) as a structure direct reagent at low temperature (60℃). The interior of the ZnO tube is loose and porous, which demonstrates its potential applications in catalysis, sensor and energy. The influence of the concentration of PAA and the cooperation of PAA, Zn~(2+) and Hexamethylenetetramine (HMT) were discussed. The PL peaks of these tubular products show regular shift compared with ZnO NRs which act as the template in the first-step synthesis procedure. A possible growth mechanism of this unusual synthesis method to fabricate the ZnO NTs has been proposed.
引文
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