仿蝶翅微纳结构金属功能材料的制备及光响应特性研究
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摘要
金属微纳结构为当前纳米研究所关注的前沿与热点。这类金属材料在微、纳米跨尺度范围内具有多维数、多层次的形态结构分布的特点，其特有的微观形态结构赋予了其独特的光、电、磁、力、热等特性。其中，表面等离子体共振特性是金属微纳结构最重要的光学特性之一。由于在电磁波的作用下，金属微纳结构内部电子的协同振荡会在其表面激发产生表面等离激元共振效应，从而增强金属表面的局域电磁场，可在亚波长范围内形成光汇聚、光波导、光增强、光储存等光学效应。然而，要深入系统研究金属的精细分级结构与其物理性能的耦合效应的内在关系和实现今后在纳米集成光子学、生物传感、生物标记、医学成像、太阳能电池、以及表面增强光谱等领域的应用，迫切需要找到兼顾高效、低成本、可重复等特性的复杂三维金属微纳结构的制备方法。现有的“自下而上”的化学自组装手段所得金属微纳结构的一致性较差，且构型有限。而采用电子束刻蚀、聚焦离子束加工等“自上而下”的物理方法来构筑金属微纳结构，涉及复杂的制备工艺、昂贵的设备，难以兼顾高效、低成本等关键制备要素，对于构筑三维（3D）亚微米复杂分级结构更是无能为力。该现状成为揭示与3D金属微纳结构相关的新现象、新机理的巨大瓶颈，进而严重制约了此类材料的实际应用。因此，探索3D金属微纳结构的制备新方法和深入研究微纳结构构型与金属之间的耦合作用，对于充实和完善3D微纳金属结构的构型、发掘其新特性、认识其机理、推动其实用化具有重要意义。
自然界生物体经长期进化与传承，在3D微纳结构的设计与功能耦合方面提供了大量有效借鉴。鳞翅目生物（蝴蝶与蛾）的翅膀鳞片（以下统称蝶翅鳞片）为精细结构与功能一体化的典范。该生物种类多达十七余万种，其鳞片通过自然选择，进化出了多形态、多维数和跨尺度的精细微纳结构，具有复杂的光学行为，以满足其求偶、躲避天敌等生存需要。同时，这些结构受生物体基因调控，具有天然的一致性和可重复性，而每片蝶翅可提供十万以上的鳞片，赋予其天然可宏量化的特点。这种结构/功能耦合的优良设计对先进功能材料的构筑具有借鉴作用，更可直接为制备微纳结构的功能材料提供大量的天然模板。
为此，本研究启迪于自然，针对3D金属微纳结构难以制备这一关键科学问题，充分利用蝶翅鳞片微纳结构精细复杂、形貌多样、一致性好、可宏量化等独特优势，选用具有3D微纳结构的蝶翅为模板，在保持其自然精细3D结构的同时将其成分转化为不同种金属，构筑具有蝶翅鳞片微纳结构的金属功能材料（以下简称金属蝶翅）。进而系统研究了制备过程中的材质转化与结构形成、演化规律，揭示了3D金属微纳结构的光功能响应规律，阐明了材料的组分与微纳结构的耦合响应机制，为3D金属微纳结构的功能材料的研究提供了新思路和新模型。主要成果如下：
一、在国际上率先开发了一种将蝶翅鳞片转化为具有蝶翅结构的金属微纳结构功能材料的特有制备方法。通过表面功能化、化学沉积、模板酸解三步骤成功获得七种（Co、Ni、Cu、Pd、Ag、Pt、Au）具有原始蝶翅鳞片三维亚微米结构的金属功能材料，构筑起数十万种天然生物微纳结构与多种功能金属之间相结合的桥梁，极大拓展了目前金属微纳结构的构型库。由于蝶翅的主要成分甲壳素为自然界第二大类天然生物物质，该方法还可用于其它甲壳素生物微纳结构的金属功能材料的制备。
二、基于3D有序结构金属鳞片显著的光学响应特性，选择高化学稳定性的Au有序结构鳞片为表面拉曼增强光谱（Surface-enhanced Raman spectroscopy,SERS）基片，研究其对R6G分子拉曼信号的增强规律。结果表明在Au有序结构鳞片上可检出超低浓度（10~(-13)M）的R6G分子，其探测灵敏度比商用SERS基片（Klarite）提高10倍（10-12M）。同时，由于金属蝶翅鳞片结构的天然一致性，R6G拉曼光谱的相对标准差低于5.2%，优于商用Klarite基片规定的相对标准差值（10%），而同样作为一次性使用的耗材，其成本仅为Klarite的1/10。进而发现整片Au蝶翅（~10cm2）也具有检测超低浓度（10~(-13)M）R6G分子拉曼光谱的能力，为一大面积的超高灵敏的SERS基片。这些成果有望使SERS技术走出实验室并推广至各应用单位，在快速蛋白识别、爆炸物检测、农药残留物检测等领域具有广阔的应用前景。
三、为深入揭示金属蝶翅的拉曼增强机理，通过调控Cu蝶翅鳞片的微纳结构，探索了Cu蝶翅周期性结构与材质的耦合机制和光响应特性。利用物理建模和拟实计算对金属蝶翅模型内局域电场分布的特性进行拟实，结果表明金属蝶翅鳞片内尺度为20-30nm的肋（rib）结构可将电磁场局域增强区（“热点”）沿第三维方向分布，从而有效提高单位激光照射面积内“热点”的数量，显著提升了SERS性能。该结论在多种具有不同“rib”层数的金属鳞片中得到实验证实，可以为在数十万种蝶翅鳞片中寻找最优的SERS构型提供依据，更可为设计其他金属表面光增强功能器件提供指导。
四、受成果三启迪，采用具有高层“rib”结构的蝶翅鳞片为模板制备Au蝶翅金属增强荧光（Surface-enhanced fluorescence,MEF）基片，深入研究了Au鳞片结构诱导的荧光增强性质。结果表明相对于普通玻璃表面，Au蝶翅鳞片可将重要的荧光染色剂异硫氰酸荧光素(FITC)的荧光发射强度提高31倍，该性能比人工设计的同类基片提高1倍。进一步将人类宫颈癌细胞（HeLa）生长于Au蝶翅表面，在低浓度（0.1μg/mL FITC）荧光染色条件下，采用共聚焦荧光显微镜对癌细胞成功地进行了荧光成像。该发现为MEF领域开辟了一个全新的研究思路与实现途径。
本研究为今后金属微纳结构的设计、制备及结构与材质的耦合效应的探索提供了研究手段、技术支撑和实现途径，为高效表面等离子体光学器件的人工设计和构筑提供了全新的设计理念。由于三维跨尺度复杂微纳结构制备困难为当今纳米材料领域研究的一大共性问题，因此本工作对多层次、多维数乃至结构功能一体化微纳结构的研究具有重要学术意义。
Metallic sub-micrometer structures with multi-dimensions, multi-levels, andmulti-functions have attracted great attention owing to their excellent and fascinatingproperties. One of the most important optical properties of metallic sub-micrometerstructures is surface plasmon resonance. This phenomenon is induced by collectiveoscillations of free electrons driven by the electromagnetic field of incident lights. Itcan provide light concentration, optical waveguide, optical enhancement, opticalstorage, and other optical effects and thus has many potential applications in opticalintegrate circuits, biosensors, biomarkers, bioimaging, solar cells, and surface enhancedspectroscopy, et al. Great efforts have been made on the fabrication of metallicmicro/nano structures. However, most approaches need a trade off between the highcost and the high producibility. In addition, the fabrication of complicated hierarchicalthree dimensional (3D) structures at sub-micrometer levels is still a challenge at present.Such situation limits the applications of metallic sub-micrometer structures. Therefore,it is critical to develop novel fabrication techniques for the3D metallic nanostructures.
Nature has been providing us inspirations for the design of elaborated hierarchicalstructures with various functions. A butterfly wing with hierarchical sub-micrometerstructures is such a perfect example, which can provide unique photo-responseproperties.
In this work, we have fabricated seven kinds of novel metallic functional materialswith butterfly scales’ sub-micrometer structures, which are difficult to imitate bytraditional methods, and explored their photo-response properties. The main results areas follows:
1. A versatile route is designed for the fabrication of metallic functional materials(Co, Ni, Cu, Pd, Ag, Pt, Au) with sub-micrometer superstructures of butterfly wingscales. Through selective surface functionalization and standard electroless deposition,a homogeneous and morphology preserving replication of original scales intricate3Dmicrostructures is achieved. Since chitin, the main component of butterfly wing scales, is one of the richest natural macromolecular compounds, this approach can be extendedto replicate other chitin-based biostructures.
2. Using the novel Au butterfly wings (or scales) with periodic structures asSERS substrates, a detectable lower limit (10~(-13)M) of R6G concentration has beenachieved. Such a detection sensitivity is one order of magnitude higher than itscommercial counterpart (Klarite), and the SERS substrates of Au butterfly wings are10times cheaper per piece in cost than Klarite. Moreover, the Au scales exhibite goodreproducibility with a relative standard deviation (RSD)5.2%, which is comparable toKlarite. These results help bring affordable SERS substrates as consumables with highsensitivity, high reproducibility, and low cost to ordinary laboratories across the world.
3. The3D sub-micrometer Cu structures replicated from butterfly wing scales aresuccessfully tuned by modifying the Cu deposition time. An optimized Cu platingprocess (10min in Cu deposition) yields replicas with the best conformal morphologiesof original wing scales and in turn the best SERS performance. Simulation results showthat the so-called “rib-structures” in Cu butterfly wing scales present naturally piled-uphotspots where electromagnetic fields are substantially amplified, giving rise to a muchhigher hotspot density than in plain2D Cu structures. Such a mechanism is furtherverified in several Cu replicas of scales from various butterfly species. This findinghelps select the best morphologies for SERS use in175,000butterfly and moth species,and can provide a theorotical guidance for designing sub-micrometer metallicstructures for photo-response applications.
4. The Au metal enhanced fluorescence (MEF) substrates directly replicatedfrom natural butterfly (Morpho sulkowskyi) wing scales can greatly enhance thefluorescence of fluorophores (fluorscein isothiocyanate, FITC). A31fold andreproducible (relative standard deviation, or RSD=6.5%) fluorescence enhancementfactor (EF) of FITC is achieved on gold M. sulkowskyi wing scales that can be preparedwith a half time-cost in an ordinary laboratory. Such results are confirmed in abioimaging process for HeLa cells (human cervical cancer cells) grown on our goldbutterfly wings. This nature inspired strategy paves the way towards3D MEFsubstrates with over175,000butterfly scale morphologies to choose from, and mayopen a new way for MEF research areas.
In general, this work has proposed a new method for building sub-micrometer metallic materials with175,000morphologies. It also puts up a new concept andmethod for designing3D metals with sub-micrometer resolutions, and provides a vaststructural pool for the development of new physical phenomena and properties basedon these materials.
自然界生物体经长期进化与传承，在3D微纳结构的设计与功能耦合方面提供了大量有效借鉴。鳞翅目生物（蝴蝶与蛾）的翅膀鳞片（以下统称蝶翅鳞片）为精细结构与功能一体化的典范。该生物种类多达十七余万种，其鳞片通过自然选择，进化出了多形态、多维数和跨尺度的精细微纳结构，具有复杂的光学行为，以满足其求偶、躲避天敌等生存需要。同时，这些结构受生物体基因调控，具有天然的一致性和可重复性，而每片蝶翅可提供十万以上的鳞片，赋予其天然可宏量化的特点。这种结构/功能耦合的优良设计对先进功能材料的构筑具有借鉴作用，更可直接为制备微纳结构的功能材料提供大量的天然模板。
为此，本研究启迪于自然，针对3D金属微纳结构难以制备这一关键科学问题，充分利用蝶翅鳞片微纳结构精细复杂、形貌多样、一致性好、可宏量化等独特优势，选用具有3D微纳结构的蝶翅为模板，在保持其自然精细3D结构的同时将其成分转化为不同种金属，构筑具有蝶翅鳞片微纳结构的金属功能材料（以下简称金属蝶翅）。进而系统研究了制备过程中的材质转化与结构形成、演化规律，揭示了3D金属微纳结构的光功能响应规律，阐明了材料的组分与微纳结构的耦合响应机制，为3D金属微纳结构的功能材料的研究提供了新思路和新模型。主要成果如下：
一、在国际上率先开发了一种将蝶翅鳞片转化为具有蝶翅结构的金属微纳结构功能材料的特有制备方法。通过表面功能化、化学沉积、模板酸解三步骤成功获得七种（Co、Ni、Cu、Pd、Ag、Pt、Au）具有原始蝶翅鳞片三维亚微米结构的金属功能材料，构筑起数十万种天然生物微纳结构与多种功能金属之间相结合的桥梁，极大拓展了目前金属微纳结构的构型库。由于蝶翅的主要成分甲壳素为自然界第二大类天然生物物质，该方法还可用于其它甲壳素生物微纳结构的金属功能材料的制备。
二、基于3D有序结构金属鳞片显著的光学响应特性，选择高化学稳定性的Au有序结构鳞片为表面拉曼增强光谱（Surface-enhanced Raman spectroscopy,SERS）基片，研究其对R6G分子拉曼信号的增强规律。结果表明在Au有序结构鳞片上可检出超低浓度（10~(-13)M）的R6G分子，其探测灵敏度比商用SERS基片（Klarite）提高10倍（10-12M）。同时，由于金属蝶翅鳞片结构的天然一致性，R6G拉曼光谱的相对标准差低于5.2%，优于商用Klarite基片规定的相对标准差值（10%），而同样作为一次性使用的耗材，其成本仅为Klarite的1/10。进而发现整片Au蝶翅（~10cm2）也具有检测超低浓度（10~(-13)M）R6G分子拉曼光谱的能力，为一大面积的超高灵敏的SERS基片。这些成果有望使SERS技术走出实验室并推广至各应用单位，在快速蛋白识别、爆炸物检测、农药残留物检测等领域具有广阔的应用前景。
三、为深入揭示金属蝶翅的拉曼增强机理，通过调控Cu蝶翅鳞片的微纳结构，探索了Cu蝶翅周期性结构与材质的耦合机制和光响应特性。利用物理建模和拟实计算对金属蝶翅模型内局域电场分布的特性进行拟实，结果表明金属蝶翅鳞片内尺度为20-30nm的肋（rib）结构可将电磁场局域增强区（“热点”）沿第三维方向分布，从而有效提高单位激光照射面积内“热点”的数量，显著提升了SERS性能。该结论在多种具有不同“rib”层数的金属鳞片中得到实验证实，可以为在数十万种蝶翅鳞片中寻找最优的SERS构型提供依据，更可为设计其他金属表面光增强功能器件提供指导。
四、受成果三启迪，采用具有高层“rib”结构的蝶翅鳞片为模板制备Au蝶翅金属增强荧光（Surface-enhanced fluorescence,MEF）基片，深入研究了Au鳞片结构诱导的荧光增强性质。结果表明相对于普通玻璃表面，Au蝶翅鳞片可将重要的荧光染色剂异硫氰酸荧光素(FITC)的荧光发射强度提高31倍，该性能比人工设计的同类基片提高1倍。进一步将人类宫颈癌细胞（HeLa）生长于Au蝶翅表面，在低浓度（0.1μg/mL FITC）荧光染色条件下，采用共聚焦荧光显微镜对癌细胞成功地进行了荧光成像。该发现为MEF领域开辟了一个全新的研究思路与实现途径。
本研究为今后金属微纳结构的设计、制备及结构与材质的耦合效应的探索提供了研究手段、技术支撑和实现途径，为高效表面等离子体光学器件的人工设计和构筑提供了全新的设计理念。由于三维跨尺度复杂微纳结构制备困难为当今纳米材料领域研究的一大共性问题，因此本工作对多层次、多维数乃至结构功能一体化微纳结构的研究具有重要学术意义。
Metallic sub-micrometer structures with multi-dimensions, multi-levels, andmulti-functions have attracted great attention owing to their excellent and fascinatingproperties. One of the most important optical properties of metallic sub-micrometerstructures is surface plasmon resonance. This phenomenon is induced by collectiveoscillations of free electrons driven by the electromagnetic field of incident lights. Itcan provide light concentration, optical waveguide, optical enhancement, opticalstorage, and other optical effects and thus has many potential applications in opticalintegrate circuits, biosensors, biomarkers, bioimaging, solar cells, and surface enhancedspectroscopy, et al. Great efforts have been made on the fabrication of metallicmicro/nano structures. However, most approaches need a trade off between the highcost and the high producibility. In addition, the fabrication of complicated hierarchicalthree dimensional (3D) structures at sub-micrometer levels is still a challenge at present.Such situation limits the applications of metallic sub-micrometer structures. Therefore,it is critical to develop novel fabrication techniques for the3D metallic nanostructures.
Nature has been providing us inspirations for the design of elaborated hierarchicalstructures with various functions. A butterfly wing with hierarchical sub-micrometerstructures is such a perfect example, which can provide unique photo-responseproperties.
In this work, we have fabricated seven kinds of novel metallic functional materialswith butterfly scales’ sub-micrometer structures, which are difficult to imitate bytraditional methods, and explored their photo-response properties. The main results areas follows:
1. A versatile route is designed for the fabrication of metallic functional materials(Co, Ni, Cu, Pd, Ag, Pt, Au) with sub-micrometer superstructures of butterfly wingscales. Through selective surface functionalization and standard electroless deposition,a homogeneous and morphology preserving replication of original scales intricate3Dmicrostructures is achieved. Since chitin, the main component of butterfly wing scales, is one of the richest natural macromolecular compounds, this approach can be extendedto replicate other chitin-based biostructures.
2. Using the novel Au butterfly wings (or scales) with periodic structures asSERS substrates, a detectable lower limit (10~(-13)M) of R6G concentration has beenachieved. Such a detection sensitivity is one order of magnitude higher than itscommercial counterpart (Klarite), and the SERS substrates of Au butterfly wings are10times cheaper per piece in cost than Klarite. Moreover, the Au scales exhibite goodreproducibility with a relative standard deviation (RSD)5.2%, which is comparable toKlarite. These results help bring affordable SERS substrates as consumables with highsensitivity, high reproducibility, and low cost to ordinary laboratories across the world.
3. The3D sub-micrometer Cu structures replicated from butterfly wing scales aresuccessfully tuned by modifying the Cu deposition time. An optimized Cu platingprocess (10min in Cu deposition) yields replicas with the best conformal morphologiesof original wing scales and in turn the best SERS performance. Simulation results showthat the so-called “rib-structures” in Cu butterfly wing scales present naturally piled-uphotspots where electromagnetic fields are substantially amplified, giving rise to a muchhigher hotspot density than in plain2D Cu structures. Such a mechanism is furtherverified in several Cu replicas of scales from various butterfly species. This findinghelps select the best morphologies for SERS use in175,000butterfly and moth species,and can provide a theorotical guidance for designing sub-micrometer metallicstructures for photo-response applications.
4. The Au metal enhanced fluorescence (MEF) substrates directly replicatedfrom natural butterfly (Morpho sulkowskyi) wing scales can greatly enhance thefluorescence of fluorophores (fluorscein isothiocyanate, FITC). A31fold andreproducible (relative standard deviation, or RSD=6.5%) fluorescence enhancementfactor (EF) of FITC is achieved on gold M. sulkowskyi wing scales that can be preparedwith a half time-cost in an ordinary laboratory. Such results are confirmed in abioimaging process for HeLa cells (human cervical cancer cells) grown on our goldbutterfly wings. This nature inspired strategy paves the way towards3D MEFsubstrates with over175,000butterfly scale morphologies to choose from, and mayopen a new way for MEF research areas.
In general, this work has proposed a new method for building sub-micrometer metallic materials with175,000morphologies. It also puts up a new concept andmethod for designing3D metals with sub-micrometer resolutions, and provides a vaststructural pool for the development of new physical phenomena and properties basedon these materials.
引文
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