易分散、良溶性新型光限幅材料的制备与研究
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摘要
随着激光技术在工业,医学,军事等领域的广泛应用,特别是激光武器正式投入装备以来,激光防护技术和材料的研究成为了我国必须高度重视和快速发展的一项研究课题。在各种激光防护材料之中,基于三阶非线性光学原理的材料有着最为突出的性能。但目前研究的无机防护材料,由于其纳米颗粒具有很强的团聚倾向,在溶剂中分散不均匀;而在有机防护材料体系中,含有大共轭或刚性结构的材料居多,导致其溶解性较差,这些都直接影响了材料的成膜及器件化,导致其无法走向实际应用。因此本论文从探讨新型易分散、良溶性激光防护材料角度入手,分别制备了有机/无机纳米复合材料、金属纳米杂化材料、微胶囊包裹纳米材料和有机材料,这几类材料均具有良好的溶解性、分散性和光限幅性能,为材料的成膜、器件化及实际应用提供了基础。
本论文主要工作如下:
(1)首次报道了通过断裂链转移聚合法(RAFT)和Au-S成键的方法,制备了具有良好单分散性且粒径均一的Au-PAVS(聚9-(4-乙烯基苯乙烯基)蒽)二聚体纳米颗粒。在制备了亲水改性后的(聚9-(4-乙烯基苯乙烯基)蒽)的微球后,将金纳米颗粒与(聚9-(4-乙烯基苯乙烯基)蒽)微球表面的巯基键合,然后在THF中将(聚9-(4-乙烯基苯乙烯基)蒽)微球分散,以这种国内外还未见报道的方法制备了二聚体纳米颗粒。所制备的颗粒在粒径和形态等方面都有着较好的均一性,单分散性,为制备具有光限幅性能的薄膜和器件创造了良好的应用前景。经过光限幅测试表明,这种有机/无机纳米复合的二聚体纳米颗粒具有与酞菁锌相近的光限幅性能,当入射光强由0.3 J/cm~2线性增加至6 J/cm~2时,二聚体溶液的透过率随入射光强增加迅速降低,最终降至30%。通过泵浦测试可以发现,其产生光限幅机理是基于纳米材料的激发态吸收。
(2)以半RAFT法制备了聚9-(4-乙烯基苯乙烯基)蒽-乙二醇两亲性嵌段聚合物,通过自组装的方法成功包裹了溶解性较差的酞菁锌、卟啉以及C60等物质,形成了三种新的光限幅材料,在水中均具有很好的分散性。包裹体系的水溶液均具有与原来酞菁锌、卟啉以及C60相近的光限幅性能,经过包裹后的酞菁锌样品当入射能量达到6J/cm~2时输出能量为1.3 J/cm~2。相对于普通酞菁锌样品降低了近四成。被包裹的卟啉的输出能量则比未包裹的降低了16.7%。而原来不溶于水的C60经包裹后在水中也具有了在甲苯中相近的光限幅性能。由于在包裹后,三类物质都具有良好的分散性、易溶性,为实际应用奠定了基础。
(3)通过以金、银纳米颗粒和不同形态的FePt和Fe_2O_3的纳米材料作为构建材料,分别制备了FePt-Au和Ag-Fe_2O_3杂化纳米结构体,FePt-Au由FePt纳米线和金纳米颗粒构成,Ag-Fe_2O_3则由Fe_2O_3和银纳米颗粒构成。通过研究表明,杂化纳米结构可以通过原料形态和前躯体的状态来控制,通过利用纳米线,纳米棒及纳米微球等形态,还可实现多种其他纳米杂化结构材料的制备。该方法所制备的纳米杂化结构体具有粒径均一,形态规整的特点,在溶液中也具有良好的分散性。同时通过将不同的纳米材料进行杂化,在国内外首次研究了它们的光限幅性能,利用Au与FePt,Ag与Fe_2O_3在非线性光学性能上的互补性,使杂化材料具有良好的非线性光学性能和光限幅性能。如,FePt-Au随着入射光强度的增加,能够产生显著的非线性吸收,当入射能量达到5J/cm~2时,透过率仅为30%左右。而Ag-Fe_2O_3样品非线性透射下降速度远远高于Fe_2O_3样品。当入射能量达到5J/cm~2时,透过率仅为31%左右,而Fe_2O_3样品的透射则有46%。
(4)制备了含腙式结构的1,8-萘酰亚胺衍生物,并在其结构上引入不同长度的四种柔性碳链,解决了萘酰亚胺自身难溶的问题,得到了溶解性优异的1,8-萘酰亚胺衍生物。通过加入给电子基团腙式结构与主体萘酰亚胺结构结合形成强烈的“推-拉电子体系”,从而使得体系中的电子极易发生跃迁,产生较强的三阶非线性性能和与C60相近的光限幅性能。同时通过泵浦测试发现,其光限幅性能是基于激发态所产生。
In the past decades, laser technology is widely used in industry, medicine and military fields. Recently, based on the laser technology, the laser weapon was developed and put into use, from then on, the research of laser protection technology and materials became highly importance and should take it seriously and act aggressively. Among the various kinds of optical protective materials, the materials based on the third order nonlinear optics have the most outstanding performance. Unfortunately, the materials that ever used in laser protection field still exist some certain shortages. The inorganic materials is unevenly scattered in solvent because of the intense tend to aggregate of the nano particles; Meanwhile the organic materials have lower solubility because of their unique structures. The purpose of this work is focused on the exploitation of new laser protection materials, which prepared various organic/inorganic nano composite materials, metallic nano hybrid materials, microcapsule parcel nanometer materials and organic materials. The similarity of these materials has perfect solubility, dispersibility and optical limiting properties, which in favor of making films and industry applications of the materials.
Our work in this thesis can be summarized as following:
(1) First reported the preparing of nano particles of monodisperse and narrow distribution range Au-PAVS heterodimer via reversible addition-fragmentation chain transfer (RAFT) polymerization and Au-S methods. Then the nanoparticle of golden was immobilized on the surface of the PAVS via the bonds with the mercaptoacetic in the surface of the PAVS and it was dispersed in THF to prepare monodisperse Au-PAVS heterodimer. The results of optical limiting properties of the Au-PAVS heterodimer compared with PcZn shows the similar optical limiting properties. The conclusion can be obtained that the mechnism of the optical limmiting is excited state absorption according to the experimental resutlts of pump-probe technique.
(2) The amphiphilic block copolymer of PAVS-b-PEG was synthesized via semi-RAFT polymerization, then the poor water soluble materials such as PcZn, porphyrin and C60 was successfully encapsulated with the PAVS via self-assembly to obtain water soluble and nonlinear optics material. All of the three encapsulations had good nonlinear properties and were appropriate for application in the area of optical limiting.
(3) Studied the third-order nonlinearity performance and optical limiting of metallic nano hybrid materials. The FePt-Au and Ag-Fe_2O_3 composites hybrid materials were prepared by nucleation growth, both of the two composites have good dispersivity and controllable forms in solvent. We first reported that the structure of the nano composite hybrid materials could be controlled by the form of the raw material and the predecessor and the form of various nanowires, nanorods and nanooarticles was also obtained. Meanwhile, since the complementarity of the Au/FePt and Ag/Fe_2O_3 in the nonlinear optics properties, the prepared nano hybrid materials had excellent optical performance and were appropriate for application in the area of optical limiting.
(4) To resolve the poor solunility of the 1,8-naphthalimide, we prepared several derivants of 1,8-naphthalimides which contained various alkane chains via the introduction of the hydrazone to the 1,8-naphthalimides. The formation of the intense“push-pull”via the combination of the introduced electron-donating group and the structure of the naphthalimide making the electron in the system could be easily transit,as a result, the obtained materials showed strong third nonlinear optics and optical limit. According to the result, the optical limit of the prepared materials was based on the excited state absorption.
本论文主要工作如下:
(1)首次报道了通过断裂链转移聚合法(RAFT)和Au-S成键的方法,制备了具有良好单分散性且粒径均一的Au-PAVS(聚9-(4-乙烯基苯乙烯基)蒽)二聚体纳米颗粒。在制备了亲水改性后的(聚9-(4-乙烯基苯乙烯基)蒽)的微球后,将金纳米颗粒与(聚9-(4-乙烯基苯乙烯基)蒽)微球表面的巯基键合,然后在THF中将(聚9-(4-乙烯基苯乙烯基)蒽)微球分散,以这种国内外还未见报道的方法制备了二聚体纳米颗粒。所制备的颗粒在粒径和形态等方面都有着较好的均一性,单分散性,为制备具有光限幅性能的薄膜和器件创造了良好的应用前景。经过光限幅测试表明,这种有机/无机纳米复合的二聚体纳米颗粒具有与酞菁锌相近的光限幅性能,当入射光强由0.3 J/cm~2线性增加至6 J/cm~2时,二聚体溶液的透过率随入射光强增加迅速降低,最终降至30%。通过泵浦测试可以发现,其产生光限幅机理是基于纳米材料的激发态吸收。
(2)以半RAFT法制备了聚9-(4-乙烯基苯乙烯基)蒽-乙二醇两亲性嵌段聚合物,通过自组装的方法成功包裹了溶解性较差的酞菁锌、卟啉以及C60等物质,形成了三种新的光限幅材料,在水中均具有很好的分散性。包裹体系的水溶液均具有与原来酞菁锌、卟啉以及C60相近的光限幅性能,经过包裹后的酞菁锌样品当入射能量达到6J/cm~2时输出能量为1.3 J/cm~2。相对于普通酞菁锌样品降低了近四成。被包裹的卟啉的输出能量则比未包裹的降低了16.7%。而原来不溶于水的C60经包裹后在水中也具有了在甲苯中相近的光限幅性能。由于在包裹后,三类物质都具有良好的分散性、易溶性,为实际应用奠定了基础。
(3)通过以金、银纳米颗粒和不同形态的FePt和Fe_2O_3的纳米材料作为构建材料,分别制备了FePt-Au和Ag-Fe_2O_3杂化纳米结构体,FePt-Au由FePt纳米线和金纳米颗粒构成,Ag-Fe_2O_3则由Fe_2O_3和银纳米颗粒构成。通过研究表明,杂化纳米结构可以通过原料形态和前躯体的状态来控制,通过利用纳米线,纳米棒及纳米微球等形态,还可实现多种其他纳米杂化结构材料的制备。该方法所制备的纳米杂化结构体具有粒径均一,形态规整的特点,在溶液中也具有良好的分散性。同时通过将不同的纳米材料进行杂化,在国内外首次研究了它们的光限幅性能,利用Au与FePt,Ag与Fe_2O_3在非线性光学性能上的互补性,使杂化材料具有良好的非线性光学性能和光限幅性能。如,FePt-Au随着入射光强度的增加,能够产生显著的非线性吸收,当入射能量达到5J/cm~2时,透过率仅为30%左右。而Ag-Fe_2O_3样品非线性透射下降速度远远高于Fe_2O_3样品。当入射能量达到5J/cm~2时,透过率仅为31%左右,而Fe_2O_3样品的透射则有46%。
(4)制备了含腙式结构的1,8-萘酰亚胺衍生物,并在其结构上引入不同长度的四种柔性碳链,解决了萘酰亚胺自身难溶的问题,得到了溶解性优异的1,8-萘酰亚胺衍生物。通过加入给电子基团腙式结构与主体萘酰亚胺结构结合形成强烈的“推-拉电子体系”,从而使得体系中的电子极易发生跃迁,产生较强的三阶非线性性能和与C60相近的光限幅性能。同时通过泵浦测试发现,其光限幅性能是基于激发态所产生。
In the past decades, laser technology is widely used in industry, medicine and military fields. Recently, based on the laser technology, the laser weapon was developed and put into use, from then on, the research of laser protection technology and materials became highly importance and should take it seriously and act aggressively. Among the various kinds of optical protective materials, the materials based on the third order nonlinear optics have the most outstanding performance. Unfortunately, the materials that ever used in laser protection field still exist some certain shortages. The inorganic materials is unevenly scattered in solvent because of the intense tend to aggregate of the nano particles; Meanwhile the organic materials have lower solubility because of their unique structures. The purpose of this work is focused on the exploitation of new laser protection materials, which prepared various organic/inorganic nano composite materials, metallic nano hybrid materials, microcapsule parcel nanometer materials and organic materials. The similarity of these materials has perfect solubility, dispersibility and optical limiting properties, which in favor of making films and industry applications of the materials.
Our work in this thesis can be summarized as following:
(1) First reported the preparing of nano particles of monodisperse and narrow distribution range Au-PAVS heterodimer via reversible addition-fragmentation chain transfer (RAFT) polymerization and Au-S methods. Then the nanoparticle of golden was immobilized on the surface of the PAVS via the bonds with the mercaptoacetic in the surface of the PAVS and it was dispersed in THF to prepare monodisperse Au-PAVS heterodimer. The results of optical limiting properties of the Au-PAVS heterodimer compared with PcZn shows the similar optical limiting properties. The conclusion can be obtained that the mechnism of the optical limmiting is excited state absorption according to the experimental resutlts of pump-probe technique.
(2) The amphiphilic block copolymer of PAVS-b-PEG was synthesized via semi-RAFT polymerization, then the poor water soluble materials such as PcZn, porphyrin and C60 was successfully encapsulated with the PAVS via self-assembly to obtain water soluble and nonlinear optics material. All of the three encapsulations had good nonlinear properties and were appropriate for application in the area of optical limiting.
(3) Studied the third-order nonlinearity performance and optical limiting of metallic nano hybrid materials. The FePt-Au and Ag-Fe_2O_3 composites hybrid materials were prepared by nucleation growth, both of the two composites have good dispersivity and controllable forms in solvent. We first reported that the structure of the nano composite hybrid materials could be controlled by the form of the raw material and the predecessor and the form of various nanowires, nanorods and nanooarticles was also obtained. Meanwhile, since the complementarity of the Au/FePt and Ag/Fe_2O_3 in the nonlinear optics properties, the prepared nano hybrid materials had excellent optical performance and were appropriate for application in the area of optical limiting.
(4) To resolve the poor solunility of the 1,8-naphthalimide, we prepared several derivants of 1,8-naphthalimides which contained various alkane chains via the introduction of the hydrazone to the 1,8-naphthalimides. The formation of the intense“push-pull”via the combination of the introduced electron-donating group and the structure of the naphthalimide making the electron in the system could be easily transit,as a result, the obtained materials showed strong third nonlinear optics and optical limit. According to the result, the optical limit of the prepared materials was based on the excited state absorption.
引文
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