有序无机纳米线薄膜的可控组装及组装体功能研究
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摘要
近年来,一维纳米材料的合成方法和技术已经取得飞速进步。所谓纳米线是其直径在纳米尺度的一类纳米材料结构。当纳米线直径的尺寸等于或小于物质的本征长度,如波尔半径、光波波长、声子自由程等,量子效应变得非常显著。同时由于其拥有大比表面积以及二维受限一维导通的特性,纳米线具有很多独特的光学、电学、磁学性质,也是一种理想的能量传输材料,使其可以传输电子、光子、声子等量子化粒子,促进其在技术领域的应用。一维纳米材料的物理化学性质不仅取决于自身的形状和尺寸,也取决于组装体的协同作用。一维纳米材料结构表面或界面的功能化和通过纳米基元组装实现不同功能的集成是解决纳米材料未来应用的关键科学问题之一,对一维纳米材料的表面与界面进行人工的、可控的功能化从而改变一维纳米材料表面和界面性质,不但可以改进一维纳米材料的本征性能,而且可以创造出新的纳米特性和功能。因此,开展一维纳米材料的组装和功能集成的基础研究具有重要的理论和实际的意义。
本论文将着重探讨纳米线做为组装基元的可控合成、规模化组装、以及纳米线组装体的功能研究。通过利用微波、水热等合成手段,可控合成高质量的纳米线,并对其直径和长度进行调控；同时利用气液界面的朗格缪尔—布吉特技术、液液界面、毛细管诱导、电子束诱导等方法组装纳米线,成功制备了多种有序的纳米线薄膜；并且系统研究了有序的纳米线功能薄膜器件化制备。论文取得的研究成果总结如下：
1、发展了碲纳米线制备技术,探索了其形态、尺度调控的规律。利用微波辅助,在15分种内,成功制备了直径在20纳米,长度在几百微米的单晶碲纳米线,并研究了聚乙烯吡咯烷酮的用量、溶液酸碱度、反应时间、表面活性剂种类对产物的影响；于室温下,使用同步辐射真空紫外光源研究了高度亲水性的碲纳米线的荧光性质。因合成的碲纳米线具有很强的反应活性,我们还使用紫外吸收光谱实时追踪技术,研究了其在水中的稳定性,讨论了不同合成方法对其反应活性的影响。除了微波反应,我们还通过向反应体系中加入丙酮和调控反应时间,首次成功制备了尺寸均一的碲纳米晶、纳米棒、纳米线、纳米管等,为今后研究其化学转化制备一系列碲化物和贵金属纳米结构等提供了良好的前驱物,并为实现其可控组装奠定了物质基础。
2、发展了超细纳米线及不同维度纳米构筑单元的可控组装技术,成功制备了不同功能的宏观尺度纳米线组装体。利用首先利用朗格缪尔—布吉特(Langmuir-Blodgett)法采用双亲性溶剂与非极性溶剂混合液来分散亲水性碲纳米线,克服了传统朗格缪尔技术需要前期疏水化处理步骤的缺陷,从而可有效可控地组装高长径比(大于104)的一维柔性纳米材料,节约了时间和能源,并通过层层组装的转移方式,通过控制层数达到对纳米线薄膜厚度的控制,通过控制相邻两层膜的夹角而得到具有有序周期性结构的纳米线薄膜；还可以把组装形成的有序纳米线膜转移到任意衬底上,包括硅片、云母等光滑基片或滤纸等不平整衬底上；在此工作基础上,我们利用一维碲纳米线薄膜的化学反应特性,简单高效地宏量制备了有序的碲化物纳米线薄膜,以及得到碲.碲化物异质纳米线薄膜并灵活连续的控制了纳米线薄膜的组分。液液界面是一个经济有效的自组装平台,我们在前人的工作基础上,提出了一种加入新溶剂诱导的液液界面组装方法,该方法经济高效的组装银纳米有序薄膜,做为一种通用的纳米材料组装方法,可以利用液液界面组装包括,零维纳米颗粒、纳米方块、二维纳米片等各种纳米材料,并且可以实现一维纳米线和零维纳米颗粒的共组装；利用朗格缪尔—布吉特技术组装超细的钨的氧化物(w18049)纳米线,共组装组装碲纳米线.银纳米线,利用不同的纳米线具有不同的稳定性,通过刻蚀得到距离可控的纳米线组装薄膜。
3、发展了毛细管诱导纳米线的组装及电子束诱导纳米线的组装技术。成功在普通毛细管内壁制备了纳米线有序组装体,并在原位电子束下,纳米线和导电碳膜卷曲行为。其中利用毛细管内溶液流动诱导银纳米线的组装,在毛细管内壁形成致密有序的银纳米线有序薄膜。通过控制流速、溶液分散浓度、组装距离等因素,纳米线薄膜的紧密程度可以调控。这个内壁有银纳米银薄膜的毛细管可以用作便携式的、可重复利用的表面增强拉曼衬底。偏振光谱证实了一维纳米线薄膜的高度有序性；利用一种新型电子束诱导方法原位快速的制备碳基的复合纳米管,包括碳.纳米线复合纳米管、碳.纳米棒复合纳米管、碳.纳米片复合纳米管、碳.纳米颗粒复合纳米管。增加辐射时间,可以得到多壁的纳米管,在纳米尺度上实现了能量的转换,达到了对弹性势能的存储。
4、发展了基于有序纳米线薄膜的几种纳米器件的制备方法；包括,有序碲纳米线的光电器件制备、有序碲化物纳米线的光电器件制备、有序碲化银纳米线薄膜的记忆器件制备、碲.碲化银异质有序纳米线记忆器件的制备、碲.金异质有序纳米线柔性电极的制备、有序w18049纳米线薄膜的电致变色器件的制备、间距可控的有序纳米线薄膜的柔性透明电极的制备、贵金属纳米线的表面增强拉曼衬底的制备。系统研究了纳米线组装体结构和性能的相互关系,实现将有序纳米线组装体在刚性的衬底和柔性的高分子衬底上的有效复合与集成,探索其在研制具有优越光磁、光导、存储器件、生物传感等多重功能的纳米功能器件中的应用。
A nanowire is a structure with a diameter of the order of a nanometer. When the diameter puts the radial dimension of the nanowire at or below certain characteristic lengths, such as the Bohr radius, the wavelength of the light, phonon mean-free path, and others, quantum mechanical effects become important. With a large surface-to-volume ratio and two-dimensional confinement, nanowires show unique optical, magnetic, and electronic properties. Macroscopic-scale nanofabrication using wire-like nanostructures has become one of the most active research areas of materials science. Integrating these nanowires in wafer scale as key components will require the development of appropriate methods to assemble these materials. Rational assembly strategies are needed not only to build complex structures with novel collective properties and device fabrication using wire-based film is sometimes pursued out of necessity.
Herein, we intend to demonstrate the process in the field of emerging nanowires. Overall, the objectives of this thesis are (i) to synthesis nanowires with controlled mophology;(ii) to assembly nanowires in wafer scale by interface, including LB technique, liquid-liquid interface;(iii) to assembly nanowires by capillary;(iv) to assembly nanowires by in situ electro beam irradiation, and (v) nanodevice fabrication based on the well-defined nanowire film.
1. Uniform and ultralong single-crystalline tellurium (Te) nanowires with a diameter of20nm and length of tens of micrometers can be rapidly synthesized by a microwave-assisted method. Besides microwave assisted method, we have carried out systematic studies to synthesis of Tellurium nanostruc-tures from sub10nm particles, nanorods, and nanowires, to nanotubes by a simple solution process.
2. Well-defined periodic mesostructures of hydrophilic ultrathin Te nanowires with aspect ratios of at least104can be produced by the Langmuir-Blodgett technique without any extra hydrophobic pretreatment or functionalization; Based on the reacity of Te nanowries, macroscale ultrathin telluride nanowire films, such as Ag2Te, Cu2Te, and PbTe, can be rapidly fabricated by chemical transformation at room temperature. Furthermore, this versatile strategy can also be used to fabricate tellurium/telluride hetero-nanowire films (Te-Ag2Te and Cu2Te-Te-Ag2Te-PbTe). The properties of the ultrathin hetero-nanowire films obtained could also be tuned by changing the composition of the hetero-nanowire films through chemical transformation. A family of water/oil interfaces is introduced to provide effective platforms for rapid fabrication of large-area self-assembled nanofi lms composed of various nanosized building blocks, including nanoparticles (NPs), nanocubes (NC), nanowires (NWs), and nanosheets, at room temperature. As a general interfacial assembly method, NWs and NPs are co-assembled at the liquid/liquid interface; well-defined W18O49nanowires were fabricated by LB technique; space control of the ordered nanowire film.
3. A new route for ordering hydrophilic Ag nanowires with high aspect ratio by flowing through a glass capillary. By controlling the flow parameters of nanowire suspensions, initially random Ag nanowires can be aligned to form nanowire arrays with tunable density, forming cambered nanowire films adhered onto the inner wall of the capillary; Fabrication of a family of curling tubular nanostructures rapidly created by a rolling up of carbonmembranes under in situ TEM electron beam irradiation. Multiwall tubes can also be created if irradiation by electron beam is performed long enough.
4. Nanodevice fabrication based on the ordered nanowire films, including ordered Tellurium, Telluride and Te-Telluride hetero-nanowire films for photoconductive nanodevice; ordered Ag2Te and Te-Ag2Te nanowries for memory device; ultrathin Te-Au hetero-nanowire based flexible electronics; ultrathin W18O49nanowire assemblies for electrochromic devices; Tunable assembly of silver nanowires for high-performance flexible transparent electrodes; Noble metal nanowrie films for for surface-enhanced Raman spectroscopy (SERS).
本论文将着重探讨纳米线做为组装基元的可控合成、规模化组装、以及纳米线组装体的功能研究。通过利用微波、水热等合成手段,可控合成高质量的纳米线,并对其直径和长度进行调控；同时利用气液界面的朗格缪尔—布吉特技术、液液界面、毛细管诱导、电子束诱导等方法组装纳米线,成功制备了多种有序的纳米线薄膜；并且系统研究了有序的纳米线功能薄膜器件化制备。论文取得的研究成果总结如下：
1、发展了碲纳米线制备技术,探索了其形态、尺度调控的规律。利用微波辅助,在15分种内,成功制备了直径在20纳米,长度在几百微米的单晶碲纳米线,并研究了聚乙烯吡咯烷酮的用量、溶液酸碱度、反应时间、表面活性剂种类对产物的影响；于室温下,使用同步辐射真空紫外光源研究了高度亲水性的碲纳米线的荧光性质。因合成的碲纳米线具有很强的反应活性,我们还使用紫外吸收光谱实时追踪技术,研究了其在水中的稳定性,讨论了不同合成方法对其反应活性的影响。除了微波反应,我们还通过向反应体系中加入丙酮和调控反应时间,首次成功制备了尺寸均一的碲纳米晶、纳米棒、纳米线、纳米管等,为今后研究其化学转化制备一系列碲化物和贵金属纳米结构等提供了良好的前驱物,并为实现其可控组装奠定了物质基础。
2、发展了超细纳米线及不同维度纳米构筑单元的可控组装技术,成功制备了不同功能的宏观尺度纳米线组装体。利用首先利用朗格缪尔—布吉特(Langmuir-Blodgett)法采用双亲性溶剂与非极性溶剂混合液来分散亲水性碲纳米线,克服了传统朗格缪尔技术需要前期疏水化处理步骤的缺陷,从而可有效可控地组装高长径比(大于104)的一维柔性纳米材料,节约了时间和能源,并通过层层组装的转移方式,通过控制层数达到对纳米线薄膜厚度的控制,通过控制相邻两层膜的夹角而得到具有有序周期性结构的纳米线薄膜；还可以把组装形成的有序纳米线膜转移到任意衬底上,包括硅片、云母等光滑基片或滤纸等不平整衬底上；在此工作基础上,我们利用一维碲纳米线薄膜的化学反应特性,简单高效地宏量制备了有序的碲化物纳米线薄膜,以及得到碲.碲化物异质纳米线薄膜并灵活连续的控制了纳米线薄膜的组分。液液界面是一个经济有效的自组装平台,我们在前人的工作基础上,提出了一种加入新溶剂诱导的液液界面组装方法,该方法经济高效的组装银纳米有序薄膜,做为一种通用的纳米材料组装方法,可以利用液液界面组装包括,零维纳米颗粒、纳米方块、二维纳米片等各种纳米材料,并且可以实现一维纳米线和零维纳米颗粒的共组装；利用朗格缪尔—布吉特技术组装超细的钨的氧化物(w18049)纳米线,共组装组装碲纳米线.银纳米线,利用不同的纳米线具有不同的稳定性,通过刻蚀得到距离可控的纳米线组装薄膜。
3、发展了毛细管诱导纳米线的组装及电子束诱导纳米线的组装技术。成功在普通毛细管内壁制备了纳米线有序组装体,并在原位电子束下,纳米线和导电碳膜卷曲行为。其中利用毛细管内溶液流动诱导银纳米线的组装,在毛细管内壁形成致密有序的银纳米线有序薄膜。通过控制流速、溶液分散浓度、组装距离等因素,纳米线薄膜的紧密程度可以调控。这个内壁有银纳米银薄膜的毛细管可以用作便携式的、可重复利用的表面增强拉曼衬底。偏振光谱证实了一维纳米线薄膜的高度有序性；利用一种新型电子束诱导方法原位快速的制备碳基的复合纳米管,包括碳.纳米线复合纳米管、碳.纳米棒复合纳米管、碳.纳米片复合纳米管、碳.纳米颗粒复合纳米管。增加辐射时间,可以得到多壁的纳米管,在纳米尺度上实现了能量的转换,达到了对弹性势能的存储。
4、发展了基于有序纳米线薄膜的几种纳米器件的制备方法；包括,有序碲纳米线的光电器件制备、有序碲化物纳米线的光电器件制备、有序碲化银纳米线薄膜的记忆器件制备、碲.碲化银异质有序纳米线记忆器件的制备、碲.金异质有序纳米线柔性电极的制备、有序w18049纳米线薄膜的电致变色器件的制备、间距可控的有序纳米线薄膜的柔性透明电极的制备、贵金属纳米线的表面增强拉曼衬底的制备。系统研究了纳米线组装体结构和性能的相互关系,实现将有序纳米线组装体在刚性的衬底和柔性的高分子衬底上的有效复合与集成,探索其在研制具有优越光磁、光导、存储器件、生物传感等多重功能的纳米功能器件中的应用。
A nanowire is a structure with a diameter of the order of a nanometer. When the diameter puts the radial dimension of the nanowire at or below certain characteristic lengths, such as the Bohr radius, the wavelength of the light, phonon mean-free path, and others, quantum mechanical effects become important. With a large surface-to-volume ratio and two-dimensional confinement, nanowires show unique optical, magnetic, and electronic properties. Macroscopic-scale nanofabrication using wire-like nanostructures has become one of the most active research areas of materials science. Integrating these nanowires in wafer scale as key components will require the development of appropriate methods to assemble these materials. Rational assembly strategies are needed not only to build complex structures with novel collective properties and device fabrication using wire-based film is sometimes pursued out of necessity.
Herein, we intend to demonstrate the process in the field of emerging nanowires. Overall, the objectives of this thesis are (i) to synthesis nanowires with controlled mophology;(ii) to assembly nanowires in wafer scale by interface, including LB technique, liquid-liquid interface;(iii) to assembly nanowires by capillary;(iv) to assembly nanowires by in situ electro beam irradiation, and (v) nanodevice fabrication based on the well-defined nanowire film.
1. Uniform and ultralong single-crystalline tellurium (Te) nanowires with a diameter of20nm and length of tens of micrometers can be rapidly synthesized by a microwave-assisted method. Besides microwave assisted method, we have carried out systematic studies to synthesis of Tellurium nanostruc-tures from sub10nm particles, nanorods, and nanowires, to nanotubes by a simple solution process.
2. Well-defined periodic mesostructures of hydrophilic ultrathin Te nanowires with aspect ratios of at least104can be produced by the Langmuir-Blodgett technique without any extra hydrophobic pretreatment or functionalization; Based on the reacity of Te nanowries, macroscale ultrathin telluride nanowire films, such as Ag2Te, Cu2Te, and PbTe, can be rapidly fabricated by chemical transformation at room temperature. Furthermore, this versatile strategy can also be used to fabricate tellurium/telluride hetero-nanowire films (Te-Ag2Te and Cu2Te-Te-Ag2Te-PbTe). The properties of the ultrathin hetero-nanowire films obtained could also be tuned by changing the composition of the hetero-nanowire films through chemical transformation. A family of water/oil interfaces is introduced to provide effective platforms for rapid fabrication of large-area self-assembled nanofi lms composed of various nanosized building blocks, including nanoparticles (NPs), nanocubes (NC), nanowires (NWs), and nanosheets, at room temperature. As a general interfacial assembly method, NWs and NPs are co-assembled at the liquid/liquid interface; well-defined W18O49nanowires were fabricated by LB technique; space control of the ordered nanowire film.
3. A new route for ordering hydrophilic Ag nanowires with high aspect ratio by flowing through a glass capillary. By controlling the flow parameters of nanowire suspensions, initially random Ag nanowires can be aligned to form nanowire arrays with tunable density, forming cambered nanowire films adhered onto the inner wall of the capillary; Fabrication of a family of curling tubular nanostructures rapidly created by a rolling up of carbonmembranes under in situ TEM electron beam irradiation. Multiwall tubes can also be created if irradiation by electron beam is performed long enough.
4. Nanodevice fabrication based on the ordered nanowire films, including ordered Tellurium, Telluride and Te-Telluride hetero-nanowire films for photoconductive nanodevice; ordered Ag2Te and Te-Ag2Te nanowries for memory device; ultrathin Te-Au hetero-nanowire based flexible electronics; ultrathin W18O49nanowire assemblies for electrochromic devices; Tunable assembly of silver nanowires for high-performance flexible transparent electrodes; Noble metal nanowrie films for for surface-enhanced Raman spectroscopy (SERS).
引文
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