蝶翅分级结构功能氧化物的制备与耦合性能探索研究
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摘要
材料是人类文明的物质基础,现代高科技的迅猛发展对材料的性能提出了更多更高的要求。材料的性能不仅取决于其化学组分,更与其自身的结构,特别是从宏观到微观的分级结构密切相关。同一组分,不同结构的材料往往表现出截然不同的性能特征。因此材料分级结构与性能之间的耦合效应是当前材料科学领域中新兴和备受关注的重要研究领域之一。一方面对已有材料的结构及其性能进行研究表征,另一方面不断设计制备具有新的优越性能的分级结构材料。在材料分级结构的设计研究中,自然给了我们很多优秀范例与深刻启迪。长期的进化过程中,自然界生物形成了多种复杂的分级精细结构。生物体以最经济、最优化的方式构筑和组合了维持它们生存、生长的结构和组分。同时,这些丰富的分级精细结构与其材质相互耦合,呈现了结构功能的一体化。
蝴蝶翅膀(以下简称蝶翅)正是这样一种利用其自身分级精细结构实现各种优异性能的典型实例。这些以甲壳素为主要成分的蝶翅结构不仅具有所适配的机械强度及自清洁的表面性质,同时形成蝶翅的甲壳素薄膜与填充期间的空气具有不同的折射率,对入射的光线产生散射、干涉、衍射乃至光子晶体等光学作用,使得蝶翅能够呈现出不同的颜色,满足其求偶捕食等生存需要。除了颜色的变化,某些蝶翅鳞片还具有特殊的捕捉光的能力。蝶翅以简单的组分,复杂多变的分级结构实现了其赖以生存的各种功能,而这些复杂分级结构目前是人类无法精确制备和实现的。这些结构不仅对蝴蝶本身有着重要的生物意义,更给了材料研究很多新的启发与指导。以这些具有特殊多级精细微观结构的蝶翅为模板,基于遗态材料的制备思想,人工变更其组分,将甲壳素基体替换为各种具有优越物理特性的其他组分,就可以合成各种兼具原始蝶翅分级结构与新组分特性的新材料,使材料达到既具有原始蝶翅的分级结构,同时由于组分的替换产生了新的性能,达到一种“形似而神高”的境界。而对这些结构进行模拟计算,则可以预测出转变为不同组分后可能获得的新性能,为进一步的深入研究提供了理论指导和应用途径。
在本研究中,选用具有精细分级结构的蝶翅作为生物模板,以氧化锌和二氧化钛功能材料为例,合成了一系列具有蝶翅分级结构的氧化物材料。首先研究制备过程中各种工艺参数对于自然精细分级结构与形态的保真性、成分转变可控性的影响规律,并对制备得到的蝶翅结构遗态氧化锌和二氧化钛材料的性能进行了研究,同时通过对蝶翅结构的计算模拟进一步地研究蝶翅结构与性能之间的耦合关系。并在此基础上,通过工艺的改进将蝶翅的多级精细结构制备成染料敏化太阳能电池光阳极,并探讨了具有多级精细结构改善染料敏化太阳能电池光阳极效率的可行性和机理,为今后分级结构和材料特性的耦合效应来设计和提高染料敏化太阳能电池的性能提供了方法,主要研究内容和结果如下:
1.针对原始蝶翅成分及其热分解性能的分析,设计优化和确立了针对甲壳素基体的遗态功能氧化物的制备方法。经过对蝶翅基体的前处理,合适配方与浓度前驱体的配制,浸渍环境参数(温度,时间等)的调节。特别是浸渍后干燥及烧结工艺,根据蝶翅模板与前驱体成及浸渍后蝶翅模板的热分解规律的研究,提出了分步烧结工艺方法来制备蝶翅结构遗态材料。采用这一烧结工艺不仅提高了蝶翅结构遗态材料的烧得率,同时改善了其微观结构的完好性,将原始蝶翅结构仅完美地保留在遗态功能氧化物之中。由于这一方法针对蝶翅主要成分为甲壳素进行设计,所以推广至其他甲壳素基遗态材料的制备中。
2.针对尺度在微米级的蝶翅鳞片,采用显微光学研究方法,研究不同显微结构对于其显微反射谱线的影响。本章研究,通过实验证实了色素色与结构色之间的差异,同时考察结构色鳞片不同位置的颜色差异。分析结果发现显示结构色的鳞片,不同位置显示不同的颜色,其鳞片内部、外部及鳞片相互叠加处显示的颜色均有所不同,这些发现一方面证实了蝶翅结构与光之间存在的耦合效应,另一方面指导蝶翅模型的建立与光学特性的模拟。
3.在研究和分析多种蝶翅显微结构特征的基础上,建立了蝶翅结构的二维复格子模型。基于严格耦合波方法,计算模拟了本研究工作中涉及的各种具有交叉格子结构鳞片的光学特性,模拟计算的结果与实验数据有较好的拟合性。在此基础上,进一步的并对各种结构参数(包括窗口大小以及翅脊与翅肋的宽度)以及基体折射率对于模型的光反射谱线的影响规律进行了探讨。利用模拟计算得到的蝶翅多级精细结构与光之间的耦合关系可以为进一步设计优化具有类蝶翅结构,既具有交叉格子结构的光功能器件提供理论参考依据。
4.制备了具有不同种多级精细结构的氧化锌蝶翅遗态材料,分析其显微结构发光性能。在对结构参数计量分析和研究的基础上,探讨了其不同于一般氧化锌材料的发光机制。研究结果表明蝶翅显微结构与氧化锌基体的耦合效应影响了其发光特性,其机理是由于蝶翅内部显微结构形成的微谐振腔导致的随机激发现象调控了氧化锌的发光性质。蝶翅结构的氧化锌材料,不仅可以影响原有发光峰的强度,特别是黄绿色波段(500-600nm)激发光,还可以改变发光峰的位置,如在某些蝶翅结构氧化锌材料中发现了发光峰蓝移的现象。
5.鉴于上述研究基础并结合光生伏打效应,本研究在相当完整制备多级精细蝶翅结构的基础上,进一步优化工艺。将具有蝶翅结构的二氧化钛制备于导电玻璃表面上,制备出了染料敏化太阳能电池光阳极。制备得到的蝶翅结构光阳极具有高于普通多孔二氧化钛的光吸收曲线,在可见光区域的平均吸收率增加超过300%,使其具有较高的光捕获性能,从而增加了光载流子产生的几率。进一步的氮吸附与压汞仪检测结果表明蝶翅结构的光阳极结构具有较高的比表面积和良好的孔径分布,这些都有利于染料的吸附加载与再生。综合这些性能,可以推论具有蝶翅结构的光阳极在光捕获性能、染料吸附性能有着优于普通多孔二氧化钛薄膜光阳极的特性,这一研究结果为今后利用分级结构和材料特性的耦合效应来设计和提高染料敏化太阳能电池的结构提供了新思路和依据。
Scientists are always amazed by the biological materials evolved millions of years, which are characterized by unique structures and morphologies. These materials possessed the integrated functions with the hierarchical microstructures coupled with the components. Occurred on the earth in Tertiary period 25 MYA (around million years ago), the butterfly family possesses the largest number of species (about 100 000 species), which also have the most complicated hierarchical microstructures on their wings. A butterfly's wing is a uniquely visual exhibition, not only of the aesthetics of nature, but of the machinery of evolution and of inspiration of research. They are made of scales which are quite small and form two or more layers over the wing membrane.
Allured by butterfly wings special and complex hierarchical microstructures, this paper dedicated to studying on the transformation and characteristics of the inorganic butterfly wings. Based on the morph-genetic materials fabrication theory, a series of functional oxides with butterfly wings’microstructure are obtained in this study. This study was divided into five parts as follows:
1. Design a special fabrication method of morph-genetic oxides with butterfly wings microstructure, based on the careful study of the components and thermo-properties of the original butterfly wings. The influences of synthesis’parameters on the morphology and elements of the morph-genetic oxides are carefully analyzed, such as the pretreatment methods, proper concentration of precursors, environment parameters (Temperature and Time etc.) of soaking method and so on. The key factor of fabrication method is the calcination roadmap, for the original butterfly wings templates and the precursors have different thermal decomposition manner. By adjusting all of the parameters mentioned above, integrate and precise butterfly wings microstructure could be maintained in the morph-genetic oxides.
2. Using microspectrameters, the optical properties of the original butterfly wings and morph-genetic ZnO materials are studied on the micro areas on the samples. The results show that the wings with different microstructures have different colours. Also the inner, outer and the overlap area of the scales have variety colours, which are due to the interaction of the hierarchical structures and the lights.
3. Based on the measurements and statistics of the microstructures from different scales, a two-dimension crossingrib structure module was build up. Using Gsolver5.1, all the optical properties of the scales involved in the paper were calculated and simulated. The influences of the microstructure size parameters and the refraction index on the optical properties are carefully studied. Coupling relations between the hierarchical microstructure and the lights could be used for the design of optical functional devices with butterfly wings structure in the future.
4. The cathodoluminescence properties of the morph-genetic ZnO are analyzed. Using random emitted theory, the unusual cathodoluminescence behaviors of the morph-genetic ZnO are explained based on the measurements and statistics of the microstructure parameters. Not only the emitting intensities can be influenced, but also the emitting peaks positions are changed due to the coupling effect between the microstructures and emitting lights.
5. A novel photoanode structure inspired by butterfly wing scales is fabricated with potential application on solar cell. Quasi-honeycomb like structure, shallow concavities structure and cross-ribbing structure were synthesized to a fluorine-doped tin oxide-coated glass substrate using butterfly wings as biotemplates. The morphology of the photoanodes, which were maintained from the original butterfly wings, was characterized by scanning and transmission electron microscopes. The calcined butterfly wings structures photoanodes were fully crystalline with arranged ridges and ribs consisting of nanoparticles. Analysis of visible light absorption spectra measurements indicates that the light-harvesting efficiencies of the quasi-honeycomb like structure photoanode were higher than the normal titania photoanode without biotemplates owing to the special microstructures.
According the researches mentioned above, the butterfly wings hierarchical microstructures are maintained integrately and precisely in the morph-genetic oxides. Some novel properties of the morph-genetic oxides are studies for potential applications in optical devices, such as DSSC. Also, the fabrication method may be applied to other metal oxide systems that could eventually lead to the production of optical, magnetic or electric devices or components as building blocks for nanoelectronic, magnetic or photonic integrated systems.
蝴蝶翅膀(以下简称蝶翅)正是这样一种利用其自身分级精细结构实现各种优异性能的典型实例。这些以甲壳素为主要成分的蝶翅结构不仅具有所适配的机械强度及自清洁的表面性质,同时形成蝶翅的甲壳素薄膜与填充期间的空气具有不同的折射率,对入射的光线产生散射、干涉、衍射乃至光子晶体等光学作用,使得蝶翅能够呈现出不同的颜色,满足其求偶捕食等生存需要。除了颜色的变化,某些蝶翅鳞片还具有特殊的捕捉光的能力。蝶翅以简单的组分,复杂多变的分级结构实现了其赖以生存的各种功能,而这些复杂分级结构目前是人类无法精确制备和实现的。这些结构不仅对蝴蝶本身有着重要的生物意义,更给了材料研究很多新的启发与指导。以这些具有特殊多级精细微观结构的蝶翅为模板,基于遗态材料的制备思想,人工变更其组分,将甲壳素基体替换为各种具有优越物理特性的其他组分,就可以合成各种兼具原始蝶翅分级结构与新组分特性的新材料,使材料达到既具有原始蝶翅的分级结构,同时由于组分的替换产生了新的性能,达到一种“形似而神高”的境界。而对这些结构进行模拟计算,则可以预测出转变为不同组分后可能获得的新性能,为进一步的深入研究提供了理论指导和应用途径。
在本研究中,选用具有精细分级结构的蝶翅作为生物模板,以氧化锌和二氧化钛功能材料为例,合成了一系列具有蝶翅分级结构的氧化物材料。首先研究制备过程中各种工艺参数对于自然精细分级结构与形态的保真性、成分转变可控性的影响规律,并对制备得到的蝶翅结构遗态氧化锌和二氧化钛材料的性能进行了研究,同时通过对蝶翅结构的计算模拟进一步地研究蝶翅结构与性能之间的耦合关系。并在此基础上,通过工艺的改进将蝶翅的多级精细结构制备成染料敏化太阳能电池光阳极,并探讨了具有多级精细结构改善染料敏化太阳能电池光阳极效率的可行性和机理,为今后分级结构和材料特性的耦合效应来设计和提高染料敏化太阳能电池的性能提供了方法,主要研究内容和结果如下:
1.针对原始蝶翅成分及其热分解性能的分析,设计优化和确立了针对甲壳素基体的遗态功能氧化物的制备方法。经过对蝶翅基体的前处理,合适配方与浓度前驱体的配制,浸渍环境参数(温度,时间等)的调节。特别是浸渍后干燥及烧结工艺,根据蝶翅模板与前驱体成及浸渍后蝶翅模板的热分解规律的研究,提出了分步烧结工艺方法来制备蝶翅结构遗态材料。采用这一烧结工艺不仅提高了蝶翅结构遗态材料的烧得率,同时改善了其微观结构的完好性,将原始蝶翅结构仅完美地保留在遗态功能氧化物之中。由于这一方法针对蝶翅主要成分为甲壳素进行设计,所以推广至其他甲壳素基遗态材料的制备中。
2.针对尺度在微米级的蝶翅鳞片,采用显微光学研究方法,研究不同显微结构对于其显微反射谱线的影响。本章研究,通过实验证实了色素色与结构色之间的差异,同时考察结构色鳞片不同位置的颜色差异。分析结果发现显示结构色的鳞片,不同位置显示不同的颜色,其鳞片内部、外部及鳞片相互叠加处显示的颜色均有所不同,这些发现一方面证实了蝶翅结构与光之间存在的耦合效应,另一方面指导蝶翅模型的建立与光学特性的模拟。
3.在研究和分析多种蝶翅显微结构特征的基础上,建立了蝶翅结构的二维复格子模型。基于严格耦合波方法,计算模拟了本研究工作中涉及的各种具有交叉格子结构鳞片的光学特性,模拟计算的结果与实验数据有较好的拟合性。在此基础上,进一步的并对各种结构参数(包括窗口大小以及翅脊与翅肋的宽度)以及基体折射率对于模型的光反射谱线的影响规律进行了探讨。利用模拟计算得到的蝶翅多级精细结构与光之间的耦合关系可以为进一步设计优化具有类蝶翅结构,既具有交叉格子结构的光功能器件提供理论参考依据。
4.制备了具有不同种多级精细结构的氧化锌蝶翅遗态材料,分析其显微结构发光性能。在对结构参数计量分析和研究的基础上,探讨了其不同于一般氧化锌材料的发光机制。研究结果表明蝶翅显微结构与氧化锌基体的耦合效应影响了其发光特性,其机理是由于蝶翅内部显微结构形成的微谐振腔导致的随机激发现象调控了氧化锌的发光性质。蝶翅结构的氧化锌材料,不仅可以影响原有发光峰的强度,特别是黄绿色波段(500-600nm)激发光,还可以改变发光峰的位置,如在某些蝶翅结构氧化锌材料中发现了发光峰蓝移的现象。
5.鉴于上述研究基础并结合光生伏打效应,本研究在相当完整制备多级精细蝶翅结构的基础上,进一步优化工艺。将具有蝶翅结构的二氧化钛制备于导电玻璃表面上,制备出了染料敏化太阳能电池光阳极。制备得到的蝶翅结构光阳极具有高于普通多孔二氧化钛的光吸收曲线,在可见光区域的平均吸收率增加超过300%,使其具有较高的光捕获性能,从而增加了光载流子产生的几率。进一步的氮吸附与压汞仪检测结果表明蝶翅结构的光阳极结构具有较高的比表面积和良好的孔径分布,这些都有利于染料的吸附加载与再生。综合这些性能,可以推论具有蝶翅结构的光阳极在光捕获性能、染料吸附性能有着优于普通多孔二氧化钛薄膜光阳极的特性,这一研究结果为今后利用分级结构和材料特性的耦合效应来设计和提高染料敏化太阳能电池的结构提供了新思路和依据。
Scientists are always amazed by the biological materials evolved millions of years, which are characterized by unique structures and morphologies. These materials possessed the integrated functions with the hierarchical microstructures coupled with the components. Occurred on the earth in Tertiary period 25 MYA (around million years ago), the butterfly family possesses the largest number of species (about 100 000 species), which also have the most complicated hierarchical microstructures on their wings. A butterfly's wing is a uniquely visual exhibition, not only of the aesthetics of nature, but of the machinery of evolution and of inspiration of research. They are made of scales which are quite small and form two or more layers over the wing membrane.
Allured by butterfly wings special and complex hierarchical microstructures, this paper dedicated to studying on the transformation and characteristics of the inorganic butterfly wings. Based on the morph-genetic materials fabrication theory, a series of functional oxides with butterfly wings’microstructure are obtained in this study. This study was divided into five parts as follows:
1. Design a special fabrication method of morph-genetic oxides with butterfly wings microstructure, based on the careful study of the components and thermo-properties of the original butterfly wings. The influences of synthesis’parameters on the morphology and elements of the morph-genetic oxides are carefully analyzed, such as the pretreatment methods, proper concentration of precursors, environment parameters (Temperature and Time etc.) of soaking method and so on. The key factor of fabrication method is the calcination roadmap, for the original butterfly wings templates and the precursors have different thermal decomposition manner. By adjusting all of the parameters mentioned above, integrate and precise butterfly wings microstructure could be maintained in the morph-genetic oxides.
2. Using microspectrameters, the optical properties of the original butterfly wings and morph-genetic ZnO materials are studied on the micro areas on the samples. The results show that the wings with different microstructures have different colours. Also the inner, outer and the overlap area of the scales have variety colours, which are due to the interaction of the hierarchical structures and the lights.
3. Based on the measurements and statistics of the microstructures from different scales, a two-dimension crossingrib structure module was build up. Using Gsolver5.1, all the optical properties of the scales involved in the paper were calculated and simulated. The influences of the microstructure size parameters and the refraction index on the optical properties are carefully studied. Coupling relations between the hierarchical microstructure and the lights could be used for the design of optical functional devices with butterfly wings structure in the future.
4. The cathodoluminescence properties of the morph-genetic ZnO are analyzed. Using random emitted theory, the unusual cathodoluminescence behaviors of the morph-genetic ZnO are explained based on the measurements and statistics of the microstructure parameters. Not only the emitting intensities can be influenced, but also the emitting peaks positions are changed due to the coupling effect between the microstructures and emitting lights.
5. A novel photoanode structure inspired by butterfly wing scales is fabricated with potential application on solar cell. Quasi-honeycomb like structure, shallow concavities structure and cross-ribbing structure were synthesized to a fluorine-doped tin oxide-coated glass substrate using butterfly wings as biotemplates. The morphology of the photoanodes, which were maintained from the original butterfly wings, was characterized by scanning and transmission electron microscopes. The calcined butterfly wings structures photoanodes were fully crystalline with arranged ridges and ribs consisting of nanoparticles. Analysis of visible light absorption spectra measurements indicates that the light-harvesting efficiencies of the quasi-honeycomb like structure photoanode were higher than the normal titania photoanode without biotemplates owing to the special microstructures.
According the researches mentioned above, the butterfly wings hierarchical microstructures are maintained integrately and precisely in the morph-genetic oxides. Some novel properties of the morph-genetic oxides are studies for potential applications in optical devices, such as DSSC. Also, the fabrication method may be applied to other metal oxide systems that could eventually lead to the production of optical, magnetic or electric devices or components as building blocks for nanoelectronic, magnetic or photonic integrated systems.
引文
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