基于光子晶体的结构色纤维制备及其显色性能研究
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摘要
大自然中的许多材料,如蛋白石、蝴蝶翅膀和孔雀羽毛,可显示出独特绚丽的色彩,这种依靠光与物体表面周期性纳米结构的相互作用而产生的色彩,被称为“结构色”,而这种表面结构我们称之为“光子晶体”。众所周知,传统染料的制备和染色过程对人类和环境会造成严重的负面影响。如果将光子晶体的制备与纤维的染色相结合,势必能够制备出一种光子染料,并获得无污染的染色过程。实现以上设想必须研究两个重要过程,一是制备类似大自然中的结构显色材料；二是如何有效地将这些材料与纤维或织物结合,模拟或设计一条纤维染色的工艺路线。本论文以构筑结构色纤维为主要研究内容,以调控其反射光谱范围和构筑速度为主要研究手段,通过Stober法、乳液聚合法、溶剂热法、共沉淀法分别制备了二氧化硅(Si02)、聚甲基丙烯酸甲酯(PMMA)、四氧化三铁(Fe3O4@C和ZnO)、硫化锌(ZnS)胶体球,并用来构筑三维光子晶体,深入探讨了毛细管力、电场力、磁场力对结构色光谱范围和形成时间的影响,并对结构色纤维在颜色传感器领域的应用进行了探索。
在平面薄膜表面制备结构色,一般采用传统重力沉积的方式,这种方法沉积速度慢、耗时长,大大降低了制备结构色的效率；如果要在弧形的纤维表面制备一层结构色,由于沉降方向和距离的差异,这种方法并不适用；在宏观开放空间条件下采用热蒸发诱导胶体球自组装制备的三维光子晶体表面缺陷较多,质量仍有待提高。本文采用微空间中热蒸发诱导胶体球自组装的方式在玻璃纤维表面制备了三维光子晶体结构,使得玻璃纤维在自然光的照射下显示结构色,在组装过程中,整个系统中毛细管力起主导作用。以Stober法制备了粒径可控的Si02胶体球,制备的胶体球具有单分散性好、表面电荷多的特点,能较好地分散于高纯水与乙醇的混合溶剂中；通过调节热蒸发温度和混合溶剂的比例,在纤维表面可以得到从单层到多层的胶体晶体层,Si02胶体球在纤维表面呈现面心立方结构,并获得长程有序的结构。通过光纤光谱测试,结构色纤维的反射光范围为473nm～528nm。
由于玻璃纤维缺乏柔韧性,作为具有独特结构色性能的纤维在实际应用中有很大的局限性,而织物所用的高分子纤维克服了这一劣势。本文借助微空间中热蒸发自组装的方法在尼龙(PA)纤维的表面制备Si02球和PMMA球组装的胶体晶体结构,使得纤维在自然光的照射下显示结构色,并在此基础上研究了胶体晶体纤维对溶剂的颜色响应特性。研究发现Si02胶体球组装纤维显示蓝、绿、红色,对应的反射光谱波长分别为493nm、534nm、682nm(对应胶体球粒径分别为：215nm、240nm、295nm);探讨了PMMA胶体球组装的PA纤维对乙醇水溶液的颜色响应特性,结果显示随着乙醇百分含量增加,光谱反射峰从521nm到566nm逐渐移动。制备的结构色纤维可通过简单的光学显微镜观察到颜色响应性,可作为一种微型裸眼传感器使用。
虽然通过毛细管力组装胶体球在组装方式上有很大的优势,但是组装时间仍然是几十分钟级别,如果寻找一种外场响应组装的方式,或许能够大大降低组装的时间,提高制备结构色纤维的效率。本文以电泳沉积的方式将PMMA胶体球组装在碳纤维的表面,形成圆柱状的纤维结构。通过施加一定的电压和改变电泳时间,得到覆盖可见光波长范围的结构色碳纤维,将组装胶体晶体的时间由几十分钟提高到几十秒钟；设计了连续电泳装置,并在纤维表面连续沉积PMMA胶体球,制备了长程的结构色纤维。由于该装置具有连续沉积的特点,或许会成为工业上生产结构色纤维可借鉴的便捷手段。
带电荷的胶体球能在电场的作用下发生自组装,那么利用磁性胶体球是否也能得到结构色纤维呢。本文先用溶剂热法制备了Fe3O4@C磁性颗粒,研究了磁性颗粒在外磁场的诱导下可以沿着磁力线方向有序排列,同时还保持它们的链间距不会改变,其在液体中的组装可形成磁响应的布拉格反射器；其次基于微流体的空间限域效应,将磁场控制、光聚合相结合制备了反射波长为450nm、520nm、640nm的蓝绿红结构色纤维。结构色纤维具有良好的机械性能,纤维与聚合物之间有一定的化学键合作用,其断裂应力大于原来纤维,为128.9cN。
本文还利用溶剂热法制备了ZnO及Ni掺杂的ZnO胶体球,研究了ZnO的形貌变化,结果表明随着Ni掺杂浓度的提高,Zn1-xNixO粒径逐渐降低,最终形成片状结构组装的纳米球；以共沉淀法制备了ZnS和ZnS@SiO2胶体球,发现通过低温法制备的ZnS球平均粒径为450nm；提出用高折射率的ZnS@SiO2胶体球组装电场可控结构色纤维的新思路,以此为基础可以设计基于纤维的结构色微器件。
Many materials in nature, such as opal, butterfly wings and peacock feathers, show the unique and brilliant colors. The color called "structural color" depends on the interaction of light with periodic surface of nano-structures, and the surface structure is named for photonic crystals. When light waves are modulated by periodic structures, photonic band gap will also appear. If energy could not land in a photonic band gap, it will not be able to continue to spread. Generally speaking, the color of the reflected light will change with the gap in different positions, so there are bright colors. As we all know, various important problems have been discovered in the process of coloration, including an increase in the amount of environmental pollution by the dye industry. Ways of utilizing strong structural color effects may be explored to solve this problem.To achieve the above ideas, two important processes must be studied, one is the preparation of structural colored dyes similar to the materials in the nature; the other is how to efficiently combine these with fiber or fabric combination, and design a fiber dyeing process.In this thesis, in order to prepare the structurally colored fiber with a rapid self-assmbled speed and good optical properties, SiO2PMMA, Fe3O4@C, ZnO and ZnS spheres have been prepared through the stober method, emulsion polymerization, solvothermal and coprecipitation method, respectively. The capillary force, electric field force and magnetic field force have been employed to assemble the colloidal spheres for photonic crystals on the fiber. The application of structurally colored fiber in the field of color sensor is also explored.
Generally, traditional gravity sedimentation is employed for preparation of the structurally colored films on the plane surface. However, this method shows slow deposition rate and time-consuming, which greatly reduce the efficiency of preparation of structural color. Especially it is not applicable for the cuving surface of the fiber. In the open space, three dimensional photonic crystals usually show a lot of surface defects prepared by thermal evaporation self-assembly method.In second chapter, structurally colored fiber was fabricated by an isothermal heating evaporation-induced self-assembly method.Under ambient white light illumination, the fibers appear colored due to optical reflectance, which is determined by the lattice constants of the photonic crystals. SiO2with180nm,215nm and240nm in diameter were prepared by the stober method. The colloidal spheres show good monodispersity and massive surface charges, which can be dispersed in water and ethanol. By adjusting the thermal evaporation temperature and the ratio in mixed solvents, colloidal crystal layers are tunable from monolayer to multilayer. SiO2colloidal spheres exhibit a face-centered cubic structure on the surface of the fiber with a long-range order. Through the fiber spectroscopy and optical microscope test, structure color fiber displays structural colors from473nm to528nm.
Due to the lack of flexibility of glass fiber, it is limited as a colored fiber in the practical application, while the polymer fiber can overcome this disadvantage. In the third chapter, SiO2and PMMA spheres were assembled on nylon (PA) fiber by the thermal evaporation method in micro-space. The fiber displays the diffraction color in natural light. And on the basis of abovementioned researches, we explore the response characteristics of fiber to the solvent with different concentrations. The study found the fiber shows red, blue, green color with reflected spectra for493nm,534nm,682nm, respectively (corresponding colloidal spheres size:215nm,240nm,295nm). The response characteristics on PMMA colloidal spheres assembled PA fiber to the ethanol solution show that spectral reflectance peaks shift gradually from521nm to566nm with the increase of ethanol content. The fiber can be as a naked eye sensor with a valuable application.
Although there are a lot of advantages using capillary force assembled colloidal spheres on the fiber, the process has still needed a lot of minutes. One promising way is to introduce an external field-stimuli photonic structure onto the fiber. In the fourth chapter, structurally colored fiber was fabricated by an electrophoretic deposition method on carbon fiber. The fiber structures look like cylindrical. By applying a voltage and changing electrophoresis time, these fibers exhibit structural colors with reflectance spectra stretch-tunable in the range of visible light. The assembly time of colloidal crystal is improved from a few minutes to tens of seconds. We further developed a horizontal and continuous process to fabricate long range structurally colored fiber. Given the advantages of the device, it may be as a reference of fiber dyeing in the industry.
Colloidal spheres with charges can be assembled in the electric field.The magnetic colloid spheres may be also getting colored fiber under the magnetic field.In the fifth chapter, we firstly have prepared Fe3O4@C magnetic particles using solvothermal method. The magnetic particles can be ordered in the direction of magnetic force lines under an external magnetic field. A bragg reflector has been fabricated by assemble the magnetic chains in the acetone. By emulsifying magnetic particles, and combining a micro-fluidic system with magnetic self-assembly and photopolymerization, we have synthesized a magnetochromatic fiber film with fixed structure colors. The structurally colored fiber shows good mechanical properties due to a chemical bonding between fiber and polymer, and the fracture stress is128.9cN and overmatchs the original fiber.
ZnO and Ni doped ZnO colloidal spheres were prepared by solvothermal method. We studied the morphology changes of ZnO spheres by controlling the Ni2+doping concentrations. The results show that the size of Zn1-xNixO decreased with increasing Ni doping concentration, eventually forming nanoparticles assembled by nano-sheet. ZnS and ZnS@SiO2colloidal spheres were prepared by the coprecipitation method in a low temperature. ZnS spheres are uniform with an average diameter of450nm.A new idea of structurally colored fiber controllable with electric field is presented.We think the periodic structures can be changed through the electrophoretic force, and then color performance of colloidal crystals can be adjusted by changing the electric field. The imagination may serve as a way for a display micro-device based on structurally colored fiber.
在平面薄膜表面制备结构色,一般采用传统重力沉积的方式,这种方法沉积速度慢、耗时长,大大降低了制备结构色的效率；如果要在弧形的纤维表面制备一层结构色,由于沉降方向和距离的差异,这种方法并不适用；在宏观开放空间条件下采用热蒸发诱导胶体球自组装制备的三维光子晶体表面缺陷较多,质量仍有待提高。本文采用微空间中热蒸发诱导胶体球自组装的方式在玻璃纤维表面制备了三维光子晶体结构,使得玻璃纤维在自然光的照射下显示结构色,在组装过程中,整个系统中毛细管力起主导作用。以Stober法制备了粒径可控的Si02胶体球,制备的胶体球具有单分散性好、表面电荷多的特点,能较好地分散于高纯水与乙醇的混合溶剂中；通过调节热蒸发温度和混合溶剂的比例,在纤维表面可以得到从单层到多层的胶体晶体层,Si02胶体球在纤维表面呈现面心立方结构,并获得长程有序的结构。通过光纤光谱测试,结构色纤维的反射光范围为473nm～528nm。
由于玻璃纤维缺乏柔韧性,作为具有独特结构色性能的纤维在实际应用中有很大的局限性,而织物所用的高分子纤维克服了这一劣势。本文借助微空间中热蒸发自组装的方法在尼龙(PA)纤维的表面制备Si02球和PMMA球组装的胶体晶体结构,使得纤维在自然光的照射下显示结构色,并在此基础上研究了胶体晶体纤维对溶剂的颜色响应特性。研究发现Si02胶体球组装纤维显示蓝、绿、红色,对应的反射光谱波长分别为493nm、534nm、682nm(对应胶体球粒径分别为：215nm、240nm、295nm);探讨了PMMA胶体球组装的PA纤维对乙醇水溶液的颜色响应特性,结果显示随着乙醇百分含量增加,光谱反射峰从521nm到566nm逐渐移动。制备的结构色纤维可通过简单的光学显微镜观察到颜色响应性,可作为一种微型裸眼传感器使用。
虽然通过毛细管力组装胶体球在组装方式上有很大的优势,但是组装时间仍然是几十分钟级别,如果寻找一种外场响应组装的方式,或许能够大大降低组装的时间,提高制备结构色纤维的效率。本文以电泳沉积的方式将PMMA胶体球组装在碳纤维的表面,形成圆柱状的纤维结构。通过施加一定的电压和改变电泳时间,得到覆盖可见光波长范围的结构色碳纤维,将组装胶体晶体的时间由几十分钟提高到几十秒钟；设计了连续电泳装置,并在纤维表面连续沉积PMMA胶体球,制备了长程的结构色纤维。由于该装置具有连续沉积的特点,或许会成为工业上生产结构色纤维可借鉴的便捷手段。
带电荷的胶体球能在电场的作用下发生自组装,那么利用磁性胶体球是否也能得到结构色纤维呢。本文先用溶剂热法制备了Fe3O4@C磁性颗粒,研究了磁性颗粒在外磁场的诱导下可以沿着磁力线方向有序排列,同时还保持它们的链间距不会改变,其在液体中的组装可形成磁响应的布拉格反射器；其次基于微流体的空间限域效应,将磁场控制、光聚合相结合制备了反射波长为450nm、520nm、640nm的蓝绿红结构色纤维。结构色纤维具有良好的机械性能,纤维与聚合物之间有一定的化学键合作用,其断裂应力大于原来纤维,为128.9cN。
本文还利用溶剂热法制备了ZnO及Ni掺杂的ZnO胶体球,研究了ZnO的形貌变化,结果表明随着Ni掺杂浓度的提高,Zn1-xNixO粒径逐渐降低,最终形成片状结构组装的纳米球；以共沉淀法制备了ZnS和ZnS@SiO2胶体球,发现通过低温法制备的ZnS球平均粒径为450nm；提出用高折射率的ZnS@SiO2胶体球组装电场可控结构色纤维的新思路,以此为基础可以设计基于纤维的结构色微器件。
Many materials in nature, such as opal, butterfly wings and peacock feathers, show the unique and brilliant colors. The color called "structural color" depends on the interaction of light with periodic surface of nano-structures, and the surface structure is named for photonic crystals. When light waves are modulated by periodic structures, photonic band gap will also appear. If energy could not land in a photonic band gap, it will not be able to continue to spread. Generally speaking, the color of the reflected light will change with the gap in different positions, so there are bright colors. As we all know, various important problems have been discovered in the process of coloration, including an increase in the amount of environmental pollution by the dye industry. Ways of utilizing strong structural color effects may be explored to solve this problem.To achieve the above ideas, two important processes must be studied, one is the preparation of structural colored dyes similar to the materials in the nature; the other is how to efficiently combine these with fiber or fabric combination, and design a fiber dyeing process.In this thesis, in order to prepare the structurally colored fiber with a rapid self-assmbled speed and good optical properties, SiO2PMMA, Fe3O4@C, ZnO and ZnS spheres have been prepared through the stober method, emulsion polymerization, solvothermal and coprecipitation method, respectively. The capillary force, electric field force and magnetic field force have been employed to assemble the colloidal spheres for photonic crystals on the fiber. The application of structurally colored fiber in the field of color sensor is also explored.
Generally, traditional gravity sedimentation is employed for preparation of the structurally colored films on the plane surface. However, this method shows slow deposition rate and time-consuming, which greatly reduce the efficiency of preparation of structural color. Especially it is not applicable for the cuving surface of the fiber. In the open space, three dimensional photonic crystals usually show a lot of surface defects prepared by thermal evaporation self-assembly method.In second chapter, structurally colored fiber was fabricated by an isothermal heating evaporation-induced self-assembly method.Under ambient white light illumination, the fibers appear colored due to optical reflectance, which is determined by the lattice constants of the photonic crystals. SiO2with180nm,215nm and240nm in diameter were prepared by the stober method. The colloidal spheres show good monodispersity and massive surface charges, which can be dispersed in water and ethanol. By adjusting the thermal evaporation temperature and the ratio in mixed solvents, colloidal crystal layers are tunable from monolayer to multilayer. SiO2colloidal spheres exhibit a face-centered cubic structure on the surface of the fiber with a long-range order. Through the fiber spectroscopy and optical microscope test, structure color fiber displays structural colors from473nm to528nm.
Due to the lack of flexibility of glass fiber, it is limited as a colored fiber in the practical application, while the polymer fiber can overcome this disadvantage. In the third chapter, SiO2and PMMA spheres were assembled on nylon (PA) fiber by the thermal evaporation method in micro-space. The fiber displays the diffraction color in natural light. And on the basis of abovementioned researches, we explore the response characteristics of fiber to the solvent with different concentrations. The study found the fiber shows red, blue, green color with reflected spectra for493nm,534nm,682nm, respectively (corresponding colloidal spheres size:215nm,240nm,295nm). The response characteristics on PMMA colloidal spheres assembled PA fiber to the ethanol solution show that spectral reflectance peaks shift gradually from521nm to566nm with the increase of ethanol content. The fiber can be as a naked eye sensor with a valuable application.
Although there are a lot of advantages using capillary force assembled colloidal spheres on the fiber, the process has still needed a lot of minutes. One promising way is to introduce an external field-stimuli photonic structure onto the fiber. In the fourth chapter, structurally colored fiber was fabricated by an electrophoretic deposition method on carbon fiber. The fiber structures look like cylindrical. By applying a voltage and changing electrophoresis time, these fibers exhibit structural colors with reflectance spectra stretch-tunable in the range of visible light. The assembly time of colloidal crystal is improved from a few minutes to tens of seconds. We further developed a horizontal and continuous process to fabricate long range structurally colored fiber. Given the advantages of the device, it may be as a reference of fiber dyeing in the industry.
Colloidal spheres with charges can be assembled in the electric field.The magnetic colloid spheres may be also getting colored fiber under the magnetic field.In the fifth chapter, we firstly have prepared Fe3O4@C magnetic particles using solvothermal method. The magnetic particles can be ordered in the direction of magnetic force lines under an external magnetic field. A bragg reflector has been fabricated by assemble the magnetic chains in the acetone. By emulsifying magnetic particles, and combining a micro-fluidic system with magnetic self-assembly and photopolymerization, we have synthesized a magnetochromatic fiber film with fixed structure colors. The structurally colored fiber shows good mechanical properties due to a chemical bonding between fiber and polymer, and the fracture stress is128.9cN and overmatchs the original fiber.
ZnO and Ni doped ZnO colloidal spheres were prepared by solvothermal method. We studied the morphology changes of ZnO spheres by controlling the Ni2+doping concentrations. The results show that the size of Zn1-xNixO decreased with increasing Ni doping concentration, eventually forming nanoparticles assembled by nano-sheet. ZnS and ZnS@SiO2colloidal spheres were prepared by the coprecipitation method in a low temperature. ZnS spheres are uniform with an average diameter of450nm.A new idea of structurally colored fiber controllable with electric field is presented.We think the periodic structures can be changed through the electrophoretic force, and then color performance of colloidal crystals can be adjusted by changing the electric field. The imagination may serve as a way for a display micro-device based on structurally colored fiber.
引文
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