可聚合纳米粒子的设计合成与高折射率聚合物杂化光学材料
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摘要
为了适应现代社会对功能性光学材料日益增加的需求进而使得光学材料在信息和光电领域的应用范围得到迅速的发展，科研工作者们通过将具有特异性功能的无机纳米粒子通过一定的方法引入到传统的树脂材料中，在保持原有树脂材料性能的基础上，改善并增强整体复合材料的光学性能。
在本论文中我们主要致力于制备具有非常广泛实际应用价值的高折射率聚合物纳米杂化光学材料。无机纳米粒子虽然具有令人着迷的高折射率性质，但是由于它们具有比较大的表面，使得这些粒子在聚合物相中很容易发生团聚而最终影响材料的性能，尤其材料的透过性能。虽然利用有机小分子修饰无机纳米粒子的办法解决了纳米粒子在聚合物相中相容性的问题，但是这一办法存在着一个问题便是有机小分子修饰剂一般折射率较低其引入对材料最终的折射率有一定的影响作用。
基于这一研究背景，我们在本论文中提出了以聚合物单体作为无机纳米粒子的修饰剂，一方面起到了修饰无机纳米粒子的作用，另一方面很好的解决了无机纳米粒子与聚合物相间的过渡问题，最重要的是没有向体系中引入其他有机小分子，而且最终得到的纳米粒子表面还有可以继续聚合的官能团。围绕这一中心思想，我们制备了一系列的可聚合纳米粒子（石墨烯纳米粒子，硅纳米粒子以及硫化锌纳米粒子），基于这些“可聚合的纳米粒子”我们分别制备了微米级别的薄膜，毫米级别的自支持膜材料以及块状的体相材料。值得一提的是，当我们将可聚合硅纳米粒子引入到聚合物体系中后，最后得到1μm左右的薄膜，在可见光区具有很好的光学透过率，而且将纯聚合物的折射率由原来的1.548提高至2.312。然后我们又进一步通过平衡材料的光学性能，机械性能以及热稳定性能，将材料应用到LED封装材料上。
总之，在本论文中我们用一种简单有效的方法制备了一系列高折射率聚合物纳米复合材料，其中微米级的薄膜在减反射涂层以及光波导材料领域具有潜在的应用价值，对于自支持材料和体相材料在LED封装以及光学仪器上具有实际的应用价值。
The optical materials with high refractive index have attracted considerableattention due to its potential application in optical electronic and information storagefields, such as the LED encapsulate materials, optical waveguides, anti-reflectioncoatings, optical storage media, and volume holographics and so on. Therefore,research of high refractive index optical nanocomposites is becoming aninterdisciplinary subject.
The traditional optical organic materials have a small adjustable RI range (1.3-1.7)due to their chemical structure limitation, which restricts their practical application inthe field of optics. In the past decades, researchers incorporated inorganicnanoparticles with high refractive index into polymers to improve the refractive indexof the polymer and achieved many achievements. Generally, inorganic nanoparticlesare easily to aggregate owing to their high surface area, which will directly sacrificethe transparency of the final materials. In the past research, the inorganicnanoparticles always experienced a surface modification process, which improved thecompatibility between inorganic nanoparticles and polymer matrix. However, itdecreased the refractive index of the pristine nanoparticles at the same time. It is stillan important topic to incorporate appropriately sized nanoparticles into a polymermatrix without aggregation and thus to prepare transparent materials with a highrefractive index via a simple and effective method.
In the second Chapter, polymerizable ZnS NPs are prepared in the monomers viaa novel strategy and a series of transparent bulk nanocomposite materials are obtainedby free radical initiated in situ bulk polymerization using these polymerizable ZnSNPs. From the TEM results, we know that the obtained polymerizable ZnS NPs with asmall size of4–5nm have a good dispersion in the monomers. The FTIR and NMRresult indicate that the PA molecules were attached to the surface of the ZnS and havean interaction with the zinc ions. The obtained bulk nanocomposites have a goodtransmittance in the visible range and its refractive index can be continuouslyregulated in the range of1.527to1.598by changing the content of polymerizable ZnSNPs. The novel strategy opens a new gate to fabricate these kinds of nanocompositesand thus extend the application of the nanocomposites in optical devices.
In the third Chapter, stable GNPs with a diameter of3–5nm have beensynthesized in DMAA by the solvothermal method. The refractive index of theGNPs–PDMAA nanocomposite films could be continuously regulated in the range of1.516to1.976by the content of GNPs. Additionally, the refractive index could reach1.976with50wt%GNP content. We also obtained nanocomposite films with a higherrefractive index above2.0by improving the refractive index of the polymer matrices.Based on the polymerizable GNPs, we also prepared a series of free-standing filmswith different weight contents of GNPs, and the refractive index of theseself-supporting films can be continuously regulated in the range of1.534to1.583.And we also find that the GNPs play a key role in the mechanical properties of thenanocomposites.
In the forth Chapter, ultrahigh refractive index Si NPs-based transparentnanocomposite films are obtained by embedding quantum-sized and almost oxide-freeSi NPs into polymer matrices via an effective and convenient chemical method. Weuse vinyl-terminated monomers as the solvent, ligand, and monomer to produce thepolymerizable Si NPs. The polymerizable Si NPs further polymerizes withco-monomer to produce Si NPs-based nanocomposite films. By altering the dosage ofSi NPs, the refractive index of the films is tunable to2.3. Based on the polymerizable Si NPs, we also prepared a series of free-standing films with different weight contentsof Si NPs, and the refractive index of these self-supporting films can be continuouslyregulated in the range of1.534to1.718. And we also find that the Si NPs play a keyrole in the mechanical properties of the nanocomposites.
In the fifth Chapter, a novel kind of flexible free-standing and high refractiveindex transparent paper-like materials based on graphene and silicon nanoparticleswere prepared. The flexibility paper-like materials have a high refractive index (from1.534to1.721) and good transmittance. It has great potential application as LEDencapsulant materials. On this basis, we applied these materials in the field of LEDand exhibit outstanding light output compared with the unencapsulated LEDs. Theoptical free-standing paper-like materials, which comprise a pliable base and possessa high refractive index property, may be expected to expand its applications in otheroptoelectronic devices.
在本论文中我们主要致力于制备具有非常广泛实际应用价值的高折射率聚合物纳米杂化光学材料。无机纳米粒子虽然具有令人着迷的高折射率性质，但是由于它们具有比较大的表面，使得这些粒子在聚合物相中很容易发生团聚而最终影响材料的性能，尤其材料的透过性能。虽然利用有机小分子修饰无机纳米粒子的办法解决了纳米粒子在聚合物相中相容性的问题，但是这一办法存在着一个问题便是有机小分子修饰剂一般折射率较低其引入对材料最终的折射率有一定的影响作用。
基于这一研究背景，我们在本论文中提出了以聚合物单体作为无机纳米粒子的修饰剂，一方面起到了修饰无机纳米粒子的作用，另一方面很好的解决了无机纳米粒子与聚合物相间的过渡问题，最重要的是没有向体系中引入其他有机小分子，而且最终得到的纳米粒子表面还有可以继续聚合的官能团。围绕这一中心思想，我们制备了一系列的可聚合纳米粒子（石墨烯纳米粒子，硅纳米粒子以及硫化锌纳米粒子），基于这些“可聚合的纳米粒子”我们分别制备了微米级别的薄膜，毫米级别的自支持膜材料以及块状的体相材料。值得一提的是，当我们将可聚合硅纳米粒子引入到聚合物体系中后，最后得到1μm左右的薄膜，在可见光区具有很好的光学透过率，而且将纯聚合物的折射率由原来的1.548提高至2.312。然后我们又进一步通过平衡材料的光学性能，机械性能以及热稳定性能，将材料应用到LED封装材料上。
总之，在本论文中我们用一种简单有效的方法制备了一系列高折射率聚合物纳米复合材料，其中微米级的薄膜在减反射涂层以及光波导材料领域具有潜在的应用价值，对于自支持材料和体相材料在LED封装以及光学仪器上具有实际的应用价值。
The optical materials with high refractive index have attracted considerableattention due to its potential application in optical electronic and information storagefields, such as the LED encapsulate materials, optical waveguides, anti-reflectioncoatings, optical storage media, and volume holographics and so on. Therefore,research of high refractive index optical nanocomposites is becoming aninterdisciplinary subject.
The traditional optical organic materials have a small adjustable RI range (1.3-1.7)due to their chemical structure limitation, which restricts their practical application inthe field of optics. In the past decades, researchers incorporated inorganicnanoparticles with high refractive index into polymers to improve the refractive indexof the polymer and achieved many achievements. Generally, inorganic nanoparticlesare easily to aggregate owing to their high surface area, which will directly sacrificethe transparency of the final materials. In the past research, the inorganicnanoparticles always experienced a surface modification process, which improved thecompatibility between inorganic nanoparticles and polymer matrix. However, itdecreased the refractive index of the pristine nanoparticles at the same time. It is stillan important topic to incorporate appropriately sized nanoparticles into a polymermatrix without aggregation and thus to prepare transparent materials with a highrefractive index via a simple and effective method.
In the second Chapter, polymerizable ZnS NPs are prepared in the monomers viaa novel strategy and a series of transparent bulk nanocomposite materials are obtainedby free radical initiated in situ bulk polymerization using these polymerizable ZnSNPs. From the TEM results, we know that the obtained polymerizable ZnS NPs with asmall size of4–5nm have a good dispersion in the monomers. The FTIR and NMRresult indicate that the PA molecules were attached to the surface of the ZnS and havean interaction with the zinc ions. The obtained bulk nanocomposites have a goodtransmittance in the visible range and its refractive index can be continuouslyregulated in the range of1.527to1.598by changing the content of polymerizable ZnSNPs. The novel strategy opens a new gate to fabricate these kinds of nanocompositesand thus extend the application of the nanocomposites in optical devices.
In the third Chapter, stable GNPs with a diameter of3–5nm have beensynthesized in DMAA by the solvothermal method. The refractive index of theGNPs–PDMAA nanocomposite films could be continuously regulated in the range of1.516to1.976by the content of GNPs. Additionally, the refractive index could reach1.976with50wt%GNP content. We also obtained nanocomposite films with a higherrefractive index above2.0by improving the refractive index of the polymer matrices.Based on the polymerizable GNPs, we also prepared a series of free-standing filmswith different weight contents of GNPs, and the refractive index of theseself-supporting films can be continuously regulated in the range of1.534to1.583.And we also find that the GNPs play a key role in the mechanical properties of thenanocomposites.
In the forth Chapter, ultrahigh refractive index Si NPs-based transparentnanocomposite films are obtained by embedding quantum-sized and almost oxide-freeSi NPs into polymer matrices via an effective and convenient chemical method. Weuse vinyl-terminated monomers as the solvent, ligand, and monomer to produce thepolymerizable Si NPs. The polymerizable Si NPs further polymerizes withco-monomer to produce Si NPs-based nanocomposite films. By altering the dosage ofSi NPs, the refractive index of the films is tunable to2.3. Based on the polymerizable Si NPs, we also prepared a series of free-standing films with different weight contentsof Si NPs, and the refractive index of these self-supporting films can be continuouslyregulated in the range of1.534to1.718. And we also find that the Si NPs play a keyrole in the mechanical properties of the nanocomposites.
In the fifth Chapter, a novel kind of flexible free-standing and high refractiveindex transparent paper-like materials based on graphene and silicon nanoparticleswere prepared. The flexibility paper-like materials have a high refractive index (from1.534to1.721) and good transmittance. It has great potential application as LEDencapsulant materials. On this basis, we applied these materials in the field of LEDand exhibit outstanding light output compared with the unencapsulated LEDs. Theoptical free-standing paper-like materials, which comprise a pliable base and possessa high refractive index property, may be expected to expand its applications in otheroptoelectronic devices.
引文
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