超分子聚合物/无机纳米粒子有序组装体的结构与性能
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摘要
纳米复合材料的机械、光学、电和磁等各项性能不仅取决于各组成的性质，还取决于纳米复合材料的结构及无机纳米粒子在共聚物微区中的组装和排列。超分子聚合物通过微观相分离可以形成丰富的微观结构，在这个过程中可诱导无机纳米粒子组装。功能性纳米粒子的可控分级有序组装在基础研究和应用技术等领域都具有重要的意义，是目前聚合物/无机纳米粒子复合材料领域一个重要的方向和生长点。
本论文基于超分子诱导无机纳米粒子自组装的方法，以嵌段共聚物、小分子氢键试剂和无机纳米粒子为研究对象，系统地研究了嵌段共聚物、小分子和无机纳米粒子三元体系的组装行为，阐明了超分子聚合物/无机纳米粒子复合材料各种有序结构形成的原因及不同形态间转变的机制，从而得到了具有特定功能和新颖有序结构的自组装复合材料，为功能性复合材料的设计和制备提供了实验和理论依据：
首先，嵌段共聚物聚苯乙烯-聚乙烯基吡啶（PS-b-P4VP）中的P4VP与十五烷基苯酚（PDP）通过氢键相互作用得到了梳状超分子。采用表面接枝技术使球形无机纳米粒子均匀分散在超分子聚合物不同嵌段的微区，实现了纳米粒子在超分子体系中有序排列；调节纳米粒子的尺寸和加入量，对其在微区中的位置及纳米粒子间距进行了调控，并通过解组装的方法破坏共聚物与小分子氢键试剂形成的氢键，从而得到单个分散的包覆有无机纳米粒子的杂化胶束；阐明了共聚物微区的均方根末端距与纳米粒子直径的比例对纳米粒子在共聚物微区中的分布规律及对体系中纳米粒子平动熵和嵌段共聚物构象熵的影响规律。
系统研究了无机纳米粒子和小分子PDP的含量对共聚物/金纳米粒子复合物形态（层状、棒状和球状等）的影响规律及形态转变规律；通过同时向体系中加入金纳米粒子和小分子氢键试剂，使体系在增加纳米粒子含量的同时可保持复合组装体的形态；在此基础上，得到了纳米粒子与氢键试剂含量对共聚物组装体结构影响的相图。
其次，研究了表面聚合物配体性质对金纳米棒在聚合物棒状微区中分散的影响，结果表明采用分子量不同的二元PS同时修饰金纳米棒，使金棒与聚合物基体产生足够的浸润性，从而使金纳米棒良好地分散在共聚物微区中；研究了纳米粒子的含量、长径比和棒状胶束的直径对金纳米棒的空间位置和取向的影响；结果表明，长金棒形成平行于棒状微区轴向的排列，而短棒则形成垂直于棒状微区的排列，表明二维受限对棒状纳米粒子取向有重要影响；紫外分光光度计和有限差分时域模拟结果表明，金棒的有序组装及组装结构的改变对杂化胶束光学性质有重要的影响。
再次，研究了新型的纳米粒子三嵌段体在超分子P4VP(PDP)体系中形成超晶格的堆积行为。结果表明，调节各组分的参数（包括纳米粒子的几何结构、纳米粒子配体的种类及分子量），各向异性的纳米粒子可以形成大面积自支撑二维、三维超晶格结构。对比了纳米粒子表面配体性质和几何形态对超级晶格自组装结构的影响，提出了可能的形态转变机理。
最后，研究了乳液液滴界面不稳定条件下的自组装从而得到了核中包覆有金纳米粒子的共聚物胶束。通过改变表面活性剂十二烷基硫酸钠的浓度，成功制备出形态可调的囊泡、棒、球状复合胶束。该方法可同时实现对光电材料C60和聚-3-已基噻吩的有效包覆。
本工作丰富了人们对超分子聚合物与无机纳米粒子自组装行为的理解，为从分子层面理解、设计、制备和优化有序结构纳米复合材料提供了理论基础和实验依据。
The properties of nanocomposites depend not only on the individual building blocks,but also on the organization and spatial arrangement of individual blocks within the host.Block copolymer, which can microphase separate into a variety of periodically orderednanostructures, have shown their potential for organizing inorganic nanoparticles inbulk/thin film. Supramolecular block polymers can further provide more versatile routes tocontrol spatial arrangement of the nanoparticles over multiple length scales. Arrangementof nanoparticles to form ordered arrays with single particle precision over macroscopicdistances will not only enable a basic understanding of the physical properties of this newfamily of material, but also pave the way for next-generation nanoparticle-based devices.
In this thesis, we systematically investigated the self-assembly behaviors ofsupermolecular polymers and nanoparticles. The purposes of this thesis include predictingthe underlying rules of self-assembled structures with the variation of the content ofindividual blocks within the host, understanding the origin of the formation of the orderednanostructures, elucidating of the mechanism for the morphological transitions betweendifferent structures, and providing guidelines for design and fabrication of novelnanocomposites.
Polystyrene-poly(4-vinyl pyridine)(PS20K-b-P4VP17K) and pentadecylphenol (PDP)were dissolved in chloroform to form PS-P4VP(PDP)x(x represents ratio of PDP to P4VP)comb-coil supramolecules. NPs were synthesized and functionalized with a thiol-end PS.Upon addition of PS-coated NPs to the supramolecules, hierarchical structures, whereNPs were selectively incorporated in PS cylindrically confined phases withinP4VP(PDP)1.0matrices were formed. Isolated wormlike micelles with uniformly dispersedgold NPs along the centerline were obtained by removal of small molecule PDP. Thisversatile approach allows us to fine tune interparticle distance and micellar morphology byvarying the content of nanoparticles and/or hydrogen bonding agent in the supramolecularassemblies. Spatial distribution of NPs in micellar core depends on D/R0(D denotes theoverall diameter of PS-coated Au NPs, R0is the root-mean-square end-to-end distance of host block of the block copolymer). And the relationship between translational entropy ofthe particles and polymer conformation entropy were estabilished.
The NP loading and the PDP addition effect on the hybrid aggregate morphology withspherical, cylindrical, or nano-sheet morphologies were systematically investigated. Thebalance between the NP loading and the PDP addition maintains the same micellarmorphology while achieves high NP loading. Based on the data above, effect of theamount of PDP and NP loading on the hybrid micellar morphology were summarized in aphase diagram.
We describe an effective approach to disperse and orient nanorods (NRs) withincylindrically confined microdomains of block copolymer (BCP)-based supramolecularself-assemblies by tethering two populations of the same homopolymer brushes withdifferent lengths on the surface of the NRs. The mismatch of binary polymer brushes withdifferent lengths on the surface of the NRs was used to effectively improve the dispersionof the NRs within polymer matrix, due to the enhanced wetting of the brushes bysurrounding mismatch polymers. Location and orientation of the NRs can be tailored byvarying the content of NRs, the aspect ratio of the NRs, or the diameter of the cylindricalnano-objects. UV-visible spectroscopy measurements and finite-difference time-domain(FDTD) calculations confirm that our approach provides a simple yet versatile route tocontrol the optical properties of the hybrid nano-objects via the tunable assembly of theNRs.
The hydrophilic gold nanorod grafted with a hydrophobic polymer at both ends wasconsidered as ABA triblock copolymer. We reported on a different approach to fabricatelarge-area, free-standing2D,3D superlattice through combining phase separation, stericrepulsion and long range attractive interaction between nanoparticles. The packingbehavior of the metal nanoparticle can be controlled by varying the geometries ofnanoparticles or the ligands on the surface of nanoparticles. The self-assemblymechanisms have been discussed.
Finally, we introduce a facile way to fabricate hybrid micelles through interfacialinstabilities of oil-in-water emulsion droplets containing polystyrene-b-poly(ethyleneoxide) and PS-grafted Au nanoparticles. Hybrid micellar morphology can be tuned fromvesicles to wormlike micelles and to spherical micelles via varying the concentration of surfactant sodium dodecyl sulfate. In addition, our experimental technique can beextended to encapsulate fullerene(C60) and polythiophene.
These findings will provide an understanding of the nature of the self-assembly ofsupramolecular polymers and nanoparticles, and help engineers to design orderednanostructured functional materials and optimize the fabrication process.
本论文基于超分子诱导无机纳米粒子自组装的方法，以嵌段共聚物、小分子氢键试剂和无机纳米粒子为研究对象，系统地研究了嵌段共聚物、小分子和无机纳米粒子三元体系的组装行为，阐明了超分子聚合物/无机纳米粒子复合材料各种有序结构形成的原因及不同形态间转变的机制，从而得到了具有特定功能和新颖有序结构的自组装复合材料，为功能性复合材料的设计和制备提供了实验和理论依据：
首先，嵌段共聚物聚苯乙烯-聚乙烯基吡啶（PS-b-P4VP）中的P4VP与十五烷基苯酚（PDP）通过氢键相互作用得到了梳状超分子。采用表面接枝技术使球形无机纳米粒子均匀分散在超分子聚合物不同嵌段的微区，实现了纳米粒子在超分子体系中有序排列；调节纳米粒子的尺寸和加入量，对其在微区中的位置及纳米粒子间距进行了调控，并通过解组装的方法破坏共聚物与小分子氢键试剂形成的氢键，从而得到单个分散的包覆有无机纳米粒子的杂化胶束；阐明了共聚物微区的均方根末端距与纳米粒子直径的比例对纳米粒子在共聚物微区中的分布规律及对体系中纳米粒子平动熵和嵌段共聚物构象熵的影响规律。
系统研究了无机纳米粒子和小分子PDP的含量对共聚物/金纳米粒子复合物形态（层状、棒状和球状等）的影响规律及形态转变规律；通过同时向体系中加入金纳米粒子和小分子氢键试剂，使体系在增加纳米粒子含量的同时可保持复合组装体的形态；在此基础上，得到了纳米粒子与氢键试剂含量对共聚物组装体结构影响的相图。
其次，研究了表面聚合物配体性质对金纳米棒在聚合物棒状微区中分散的影响，结果表明采用分子量不同的二元PS同时修饰金纳米棒，使金棒与聚合物基体产生足够的浸润性，从而使金纳米棒良好地分散在共聚物微区中；研究了纳米粒子的含量、长径比和棒状胶束的直径对金纳米棒的空间位置和取向的影响；结果表明，长金棒形成平行于棒状微区轴向的排列，而短棒则形成垂直于棒状微区的排列，表明二维受限对棒状纳米粒子取向有重要影响；紫外分光光度计和有限差分时域模拟结果表明，金棒的有序组装及组装结构的改变对杂化胶束光学性质有重要的影响。
再次，研究了新型的纳米粒子三嵌段体在超分子P4VP(PDP)体系中形成超晶格的堆积行为。结果表明，调节各组分的参数（包括纳米粒子的几何结构、纳米粒子配体的种类及分子量），各向异性的纳米粒子可以形成大面积自支撑二维、三维超晶格结构。对比了纳米粒子表面配体性质和几何形态对超级晶格自组装结构的影响，提出了可能的形态转变机理。
最后，研究了乳液液滴界面不稳定条件下的自组装从而得到了核中包覆有金纳米粒子的共聚物胶束。通过改变表面活性剂十二烷基硫酸钠的浓度，成功制备出形态可调的囊泡、棒、球状复合胶束。该方法可同时实现对光电材料C60和聚-3-已基噻吩的有效包覆。
本工作丰富了人们对超分子聚合物与无机纳米粒子自组装行为的理解，为从分子层面理解、设计、制备和优化有序结构纳米复合材料提供了理论基础和实验依据。
The properties of nanocomposites depend not only on the individual building blocks,but also on the organization and spatial arrangement of individual blocks within the host.Block copolymer, which can microphase separate into a variety of periodically orderednanostructures, have shown their potential for organizing inorganic nanoparticles inbulk/thin film. Supramolecular block polymers can further provide more versatile routes tocontrol spatial arrangement of the nanoparticles over multiple length scales. Arrangementof nanoparticles to form ordered arrays with single particle precision over macroscopicdistances will not only enable a basic understanding of the physical properties of this newfamily of material, but also pave the way for next-generation nanoparticle-based devices.
In this thesis, we systematically investigated the self-assembly behaviors ofsupermolecular polymers and nanoparticles. The purposes of this thesis include predictingthe underlying rules of self-assembled structures with the variation of the content ofindividual blocks within the host, understanding the origin of the formation of the orderednanostructures, elucidating of the mechanism for the morphological transitions betweendifferent structures, and providing guidelines for design and fabrication of novelnanocomposites.
Polystyrene-poly(4-vinyl pyridine)(PS20K-b-P4VP17K) and pentadecylphenol (PDP)were dissolved in chloroform to form PS-P4VP(PDP)x(x represents ratio of PDP to P4VP)comb-coil supramolecules. NPs were synthesized and functionalized with a thiol-end PS.Upon addition of PS-coated NPs to the supramolecules, hierarchical structures, whereNPs were selectively incorporated in PS cylindrically confined phases withinP4VP(PDP)1.0matrices were formed. Isolated wormlike micelles with uniformly dispersedgold NPs along the centerline were obtained by removal of small molecule PDP. Thisversatile approach allows us to fine tune interparticle distance and micellar morphology byvarying the content of nanoparticles and/or hydrogen bonding agent in the supramolecularassemblies. Spatial distribution of NPs in micellar core depends on D/R0(D denotes theoverall diameter of PS-coated Au NPs, R0is the root-mean-square end-to-end distance of host block of the block copolymer). And the relationship between translational entropy ofthe particles and polymer conformation entropy were estabilished.
The NP loading and the PDP addition effect on the hybrid aggregate morphology withspherical, cylindrical, or nano-sheet morphologies were systematically investigated. Thebalance between the NP loading and the PDP addition maintains the same micellarmorphology while achieves high NP loading. Based on the data above, effect of theamount of PDP and NP loading on the hybrid micellar morphology were summarized in aphase diagram.
We describe an effective approach to disperse and orient nanorods (NRs) withincylindrically confined microdomains of block copolymer (BCP)-based supramolecularself-assemblies by tethering two populations of the same homopolymer brushes withdifferent lengths on the surface of the NRs. The mismatch of binary polymer brushes withdifferent lengths on the surface of the NRs was used to effectively improve the dispersionof the NRs within polymer matrix, due to the enhanced wetting of the brushes bysurrounding mismatch polymers. Location and orientation of the NRs can be tailored byvarying the content of NRs, the aspect ratio of the NRs, or the diameter of the cylindricalnano-objects. UV-visible spectroscopy measurements and finite-difference time-domain(FDTD) calculations confirm that our approach provides a simple yet versatile route tocontrol the optical properties of the hybrid nano-objects via the tunable assembly of theNRs.
The hydrophilic gold nanorod grafted with a hydrophobic polymer at both ends wasconsidered as ABA triblock copolymer. We reported on a different approach to fabricatelarge-area, free-standing2D,3D superlattice through combining phase separation, stericrepulsion and long range attractive interaction between nanoparticles. The packingbehavior of the metal nanoparticle can be controlled by varying the geometries ofnanoparticles or the ligands on the surface of nanoparticles. The self-assemblymechanisms have been discussed.
Finally, we introduce a facile way to fabricate hybrid micelles through interfacialinstabilities of oil-in-water emulsion droplets containing polystyrene-b-poly(ethyleneoxide) and PS-grafted Au nanoparticles. Hybrid micellar morphology can be tuned fromvesicles to wormlike micelles and to spherical micelles via varying the concentration of surfactant sodium dodecyl sulfate. In addition, our experimental technique can beextended to encapsulate fullerene(C60) and polythiophene.
These findings will provide an understanding of the nature of the self-assembly ofsupramolecular polymers and nanoparticles, and help engineers to design orderednanostructured functional materials and optimize the fabrication process.
引文
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