摘要
本论文旨在通过对化合物晶体结构的分析,设计和发展合适的反应路线实现对低维功能纳米材料的可控合成,并结合物质本征的性能,将其应用于各种电化学领域。对低维功能纳米材料的形貌,结构与性能之间的相关性进行初步探讨。本论文主要包括以下几方面的内容：
1.作者通过将静电纺丝法和煅烧技术结合,首次制备出多级结构LiV3O8纳米纤维,它是由暴露大量{100}晶面的LiV3O8纳米片相互交叉而成的。在整个合成过程中,聚乙烯醇(PVA)起到了双重作用：一是在静电纺丝过程中为纤维的形成提供模板；二是有效防止LiV3O8纳米颗粒的团聚,使其根据自身晶体自范性生长最终形成暴露{100}晶面的纳米片。另外,煅烧时间也严重影响着多级LiV3O8纳米纤维的形成。相比文献之前的报道,我们制备的这种暴露单一晶面的多级结构LiV3O8内米纤维组成的水溶液锂离子电池,表现出更高的放电比容量和更好的循环稳定性。因此,这种多级结构的LiV3O8纳米纤维将在水溶液锂离子电池领域有良好的应用前景。这是我们首次将静电纺丝技术拓展到水溶液锂离子电池电极材料的合成领域。此外,我们制备的这种纳米纤维具有特殊的亚显微结构,可能在传感器,催化以及能源存储等领域有潜在的应用价值。
2.作者首次通过机械剥离层状有机-无机杂化中间体,得到厚度仅为1.4nm的大面积WO3·2H2O超薄纳米片。与相应的块材相比,WO3·2H2O超薄纳米片具有良好的可柔性,更高的Li+扩散系数,且与基底接触更加紧密。得到的超薄纳米片成功地组装成柔性电致变色器件,表现出大的透过率差(ΔT=48%)、快速的着色/褪色响应速率(tc,90%=5.1s,tb,90%=9.7s)、较高的着色效率(120.9cm2C-1)、良好的循环稳定性以及很好的可柔性。其综合的电致变色性能要优于块材WO3·2H2O组成的电致变色器件和之前文献中报道的其它柔性电致变色器件的性能。这可以归因于WO3·2H2O超薄纳米片独特的原子结构和形貌特征.我们还通过第一性原理计算深入研究了WO3·2H2O的电致变色机理。结果表明,随着Li+的插入,WO3·2H2O经历着从半导体到金属的转变,这也正是电致变色的原因。且WO3·2H2O超薄纳米片能够有效促进半导体与金属之间的转变,从而提高着色/褪色响应速率,尤其对着色过程影响显著。本工作为二维超薄纳米片用于制备高性能柔性电致变色器件提供大量有用信息,促进了柔性便携式电子器件的发展。
3.作者通过简单的液相剥离法合成了厚度仅为2-3nm的WO3·H2O超薄纳米片,并首次将其组装成Cu/WO3·H2O超薄纳米片ITO-PET柔性非易失性阻变存储器件(ITO-PET：表面涂有氧化铟锡(ITO)的聚对苯二甲酸乙二醇酯(PET))。该器件表现出低的开关电压(+1.0V/-1.14V)、大的高低阻值比(>105)、优异的数据保持性(>105s)、耐疲劳特性(>5000次)以及良好的可柔性。通过正电子寿命谱的研究表明,合成的W03-H20超薄纳米片中存在大量的V””[OWOH2]空位簇。根据理论分析和实验数据,作者提出了金属Cu2+和V''''[OWOH2]空位簇共同作用的新型阻变存储机理。这一工作不仅对柔性非易失性阻变存储器件的发展有一定的指导意义,而且有助于深入理解阻变存储器的存储机理。
4.作者将液相剥离法和煅烧法结合首次制备出厚度大约为4nm的WO3多孔纳米薄片。为了实验对比,作者还合成了4nm厚的WO3无孔纳米薄片和无孔厚片,并分析了三者的物相和形貌。作者研究了由(010)取向的单斜相WO3·2H20超薄纳米片转化成(001)取向的单斜相WO3纳米薄片的晶体结构衍化过程。作者将合成的WO3多孔纳米薄片,无孔纳米薄片和无孔厚片分别在导电玻璃上制备成薄膜,作为光电极测试其光电催化性能。结果表明,由WO3多孔纳米薄片组成的薄膜具有更高的光电流密度,更小的界面电荷转移电阻以及良好的稳定性,这是其二维形貌和多孔结构共同作用的结果。这种具备优异性能的WO3多孔纳米薄片将可能成为一种理想的光电催化材料。
The goal of this dissertation is to design and develop novel chemical reaction routes for the controllable fabrication of low-dimensional functional nanomaterials by analyzing the crystal structural characteristics of the target products. On the basis of the intrinsic properties of the materials, these low-dimensional functional nanomaterials have been applied for various electrochemical area. The corresponding morphology-structure-property relationships have been also investigated in this dissertation. The details are summarized briefly as follows:
1. For the first time, we report a facile route to prepare the hierarchical LiV3O8nanofibers constructed by interleaving two dimensional nanosheets with exposed {100} facets using electrospinning combined with calcination. PVA is proved to play a dual role in both electrospinning and calcination process:besides it acts as the template for forming the fibers, it could prevent effectively the aggregation of LiV3O8nanoparticles, which makes them grow into small nanosheets with exposed{100} facets owing to growth characteristic habit of LiV3O8. In addition, the calcination time also affects the formation of hierarchical LiVO8nanofibers. Significantly, the fabricated LiV3O8nanofibers with hierarchitecture and exposure of the specific facets exhibit higher discharge capacity and better cycling stability than those reported in previous literature, suggesting that the hierarchical LiV3O8nanofibers have promising potential for application in ALIBs. Meanwhile, we extend the electrospinning technique to fabricate the electrode material for aqueous lithium ion batteries. The electrospun hierarchical nanofiber described in this study has been confirmed as a unique submicrostructure that will probably have potential applications in sensors, catalysis, chemical power sources, and so on.
2. We firstly synthesize large-area nanosheets of tungsten oxide dihydrate with a thickness of only about1.4nm via ultrasonic exfoliation of lamellar inorganic-organic hybrid intermediate. Compared with the bulk counterpart, WO3·2H2O ultrathin nanosheets possess more flexible feature, better interface contact with the substrate and higher Li+diffusion coefficient. The flexible electrochromic device based on WO3-2H2O ultrathin nanosheets has been successfully assembled, which exhibits large transparency contrast (△T=48%), fast coloration/bleaching response time (tc,90%=5.1s, tb,90%=9.7s), a high coloration efficiency of120.9cm2 C-1, good cycling stability and excellent flexibility. These superior electrochromic performances are strikingly higher than those of WO3-2H2O bulk-based ECD and the previously reported flexible ECDs in full consideration of various parameters, which can be ascribed to the synergetic effect between the unique atomic structure of WO3-2H2O and the morphological features of ultrathin nanosheets. The calculated density of states for WO3·2H2O and LixWO3·2H2O indicate that WO3·2H2O undergoes a transition from semiconducting to metallic state accompanied by Li+intercalation, which is the reason of electrochromism. The relationship between the structural features of ultrathin nansoheets and color-switching time is further researched, and the results manifest that WO3-2H2O ultrathin nanosheets can effectively facilitate the semiconductor-to-metal transition and increase the coloration/bleaching response speed, especially for the coloration process. It will provide plenty of valuable information for ultrathin2D nanosheets to develop the high-performance flexible electrochromic devices. The excellent electrochromic performances with the combination of flexibility make our device a prominent candidate in flexible and portable electronics.
3. We firstly report an inorganic graphene analogue, WO3·H2O ultrathin nanosheets with only2-3nm thickness, as a promising material to construct a flexible resistance switching random access memory (RRAM) device. The material possesses abundant vacancy associates V""[OWOH2] as revealed by the positron annihilation spectra, providing some new insights into switching mechanisms in the oxide-based RRAM. By virtue of the synergic advantages of metal Cu ions and vacancy associates V""[OWOH2], the as-established flexible Cu/WO3·H2O ultrathin nanosheets/ITO-PET device achieves low operating voltage (+1.0V/-1.14V), large resistance OFF/ON ratio (>105), long retention time (>105s), good endurance (>5000cycles), and excellent flexibility. The finding of the existence of distinct defects in ultrathin nanosheets undoubtedly leads to a deep understanding of the underlying nature of the resistance switching (RS) behavior, which may serve as a guide to improve the performances and promote the rapid development of RRAM.
4. We firstly synthesize porous WO3thin nanosheets with4nm thickness using liquid exfoliation combined with calcination. For comparison, nonporous WO3thin nanosheets and nonporous bulk WO3were also obtained and investigated by various characterization methods. The evolution from monoclinic WO3·2H2O ultrathin nanosheets with (010) preferred orientation to monoclinic WO3thin nanosheets with (001) preferred orientation can be eadily explained by topotactic transformation process. The porous WO3thin nanosheets, nonporous WO3thin nanosheets and nonporous bulk WO3are assembled into thin films on the conductive indium-tin-oxide (ITO) coated glasses, respectively. The fabricated thin films as the photoanodes carry out photoelectrochemical tests in a standard three-electrode configuration. The results indicate that the porous WO3thin nanosheets exhibit higher photocurrent density, lower interfacial charge-transfer resistance and better photostability than nonporous WO3thin nanosheets and nonporous bulk WO3, which attributes to the synergic effect of two-dimensional morphology and porous structures. The porous WO3thin nanosheets will be a promising photoanode material for photoelectrochemical water splitting.
引文
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