摘要
伴随着全球环境污染和能源危机问题日益严重,如何有效地节约资源与保护环境以实现可持续发展是当前科技领域的重要课题。电致变色材料作为一种新型的节能材料,由于在建筑节能领域的应用前景而受到极大关注。若能突破电致变色材料在制备和应用中的诸多关键技术,开发出高性能、低成本而又实用性强的电致变色材料,则有望解决现有电致变色薄膜材料在实际应用中的瓶颈问题。本论文以WO3和NiO为主要研究对象,以调控其微观结构和形貌为手段,通过液相法制备了微纳米结构的电致变色薄膜,并通过有机复合化对其进行改性研究,主要目的是提高其光调节范围、电致变色效应速度、着色效率以及循环寿命。此外,还组装了基于凝胶电解质的NiO/WO3互补型电致变色器件,并对其电致变色性能和实用化前景进行了研究和探索。
采用简单的水热法在FTO导电基底上制备了垂直定向排列的一维WO3纳米结构阵列和自编织的W03纳米片电致变色薄膜,且所制备的WO3均为六方相结构。研究发现水热反应溶液中尿素的含量以及溶剂中水和乙腈的比例对产物最终的形貌起到关键作用,以水为溶剂,通过调节尿素含量得到了长方形的WO3纳米棒阵列,而当尿素含量不变,通过调节溶剂中水和乙腈的体积比例得到了圆柱形纳米棒阵列的WO3薄膜。与传统的纳米颗粒薄膜相比,垂直定向的纳米棒阵列结构具有较大的活性比表面积和有序的离子通道,不仅可以缩短离子的扩散路径,而且有利于电解液与纳米棒的充分接触。因此电致变色性能得到了明显改善。其中着色时间和褪色时间分别为6-9s和3～5s,着色效率最高可以达到106.8cm2/C。以乙腈为溶剂加入少量水,并同时加入尿素和草酸来调控W03的结构形貌,可以得到一种由纳米线编织而成的纳米片状结构。这种编织体结构大大增加了电化学反应的活性比表面积,因此着色效率有了明显提高,可以达到134cm2/C,然而由于这种相互交错的编制体结构会阻碍离子的嵌入和迁出,因此着色和褪色时间有所延长。
采用水热法在FTO导电基底上制备了NiO电致变色薄膜。通过调节水热反应溶液中过硫酸钾和氨水的添加量分别得到了自组装的NiO多级微米片和六方形的NiO纳米盘薄膜。对于自组装的NiO多级微米片薄膜来说,微米片之间相互交错排列所形成的大孔结构以及微米片中存在的由于纳米叶子的自组装而形成的小孔结构,不仅增大了其电化学反应的活性比表面积,而且有利于Li+的嵌入/脱出反应,因此具有良好的电致变色性能。其中,着色时间和褪色时间分别为4.6和7.2s,着色效率可以达到89.3cm2/C。此外,与文献报道的多孔的NiO纳米片薄膜相比,多级NiO微米片薄膜结构稳定、具有一定机械强度,能承受由于离子和电子的双注入和脱出所引起的晶格应力和体积变化,显示了良好的循环稳定性。
分别采用浸泡法和电化学沉积法在FTO玻璃上制备了微纳米结构的PANI电致变色薄膜。浸泡法制备PANI薄膜时,掺杂剂的种类对PANI薄膜的结构和形貌具有重要影响。当草酸作为掺杂剂时,得到的是致密的PANI纳米颗粒薄膜,当丙烯酸作为掺杂剂时,得到的是PANI微米棒薄膜,采用电化学氧化聚合制备PANI薄膜时,沉积方式对薄膜的结构形貌具有重要影响。其中,恒流和恒压沉积得到的薄膜均为致密的无定形PANI薄膜,而循环伏安法得到的是纳米棒网络结构的PANI薄膜；结合水热法和循环伏安法实现了W03和PANI在纳米层次上的结构设计。WO3/PANI复合薄膜结合了两者的优点,具有了双重的电致变色效应。与单一的W03薄膜相比,复合薄膜显示了多色性,且由于形成了施主-受主系统,加速了离子和电子的迁移速度,实现了快速响应。与单一PANI薄膜相比,复合薄膜中W03纳米棒阵列结构使得覆盖在其表面的PANI纳米短棒的活性比表面得到充分利用,从而提高了其光调制范围和着色效率。
采用水热法在FTO玻璃上制备了三种多孔结构的NiO电致变色薄膜,并结合循环伏安法在NiO多孔结构上生长了PANI纳米结构,得到了三种不同的复合电致变色薄膜。由于NiO和PANI均在正压下着色,负压下褪色,因此,NiO/PANI复合薄膜在电致变色性能上具有一定的增强效果,与互补型的WO3/PANI复合薄膜相比,具有更好的电致变色性能。其在550nm处的光调制范围可以达到62%,着色效率高达121cm2／C,着色和褪色时间分别为90和120ms。
以自编织W03纳米片薄膜和NiO多级微米片薄膜为电致变色层和离子存储层,分别组装了基于液态和固态电解质的NiO/WO3互补型电致变色器件。在NiO/WO3互补器件中,NiO不仅作为离子存储层,也起到了互补变色的作用,W03薄膜和NiO薄膜电致变色的叠加效应,使器件的电致变色性能得到提高。如基于液态电解质的器件的着色时间和褪色时间分别为1.8和3.2s,着色效率可以达到146.9cm2/C。而基于凝胶电解质的全固态器件,由于凝胶态电解质层中电子和离子的迁移受到非导电性聚合物框架结构的阻碍作用,使其迁移比较缓慢,且凝胶电解质的稳定性和机械强度比较差,导致在电致变色循环过程中,聚合物框架结构遭到破坏而坍塌,导致了不可逆循环,因此电致变色性能较差,还有待提高,距离实用化还有一定距离。
With the emergence of environmental pollution and energy crisis, effective energy conservation and environmental protection for achieving sustainable development are currently important issues in scientific community. Electrochromic (EC) materials, as one of the energy-saving materials, have attracted vast attention owing to the potential application in smart windows. Although the research is very wide for the organic/inorganic EC materials, there are many problems in the practical applications, such as the poor cycle stability, slow switching responses, low optical modulation and high power consumption, which make them difficult to meet the needs of practical applications. This thesis focused on the liquid-phase fabrication of inorganic and organic/inorganic composite EC films composed of micro/nanomaterials. The effects of the various nanostructures on the EC performance of these films were examined in detail. Finally, an all-solid-state electrochromic device based on NiＯ/WＯ3complementary structure and gel electrolyte was fabricated and its EC properties were also systematically investigated.
Vertically aligned １D WO3nanostructure and self-weaving WO3nanoflake films were grown on fluorine-doped tin oxide (FTO) coated glass substrate using a crystal-seed-assisted hydrothermal technique, respectively. Detailed mechanistic studies revealed that the composition of the precursor solution played important roles in determining the final shape and size of the WO3nanostructures. The rectangular nanorod array film can be obtained in the presence of1.2mmol urea with water as the solvent. While the cylindrical nanorods were grown by tuning the solvent composition with the urea content fixed at1.2mmol. Due to the large tunnels in the hexagonally structured WO3, and the large active surface area available for electrochemical reactions, a large optical modulation of66% at632.8nｍ and a potential of -2.0V, fast switching speeds of6.7s and3.4s for coloration and bleaching, respectively, and a high coloration efficiency of106.8cm2/C were achieved for the cylindrical nanorod array film. Interestingly, with addition of oxalic acid and urea to a mixed solvent of de-ionized water and acetonitrile, WO3nanoflakes woven from nanowires were grown. This unique nanostructure gives a coarse surface, making a larger surface area available for reactions in electrochemical processes and therefore a higher coloration efficiency of134.4cm2/C was achieved. Moreover, the braided structure is more solid than that of the previously reported nanowire arrays and may enhance the long-term cycling stability, which is a crucial parameter for practical devices. However, its coloration and bleaching times were prolonged because the intertwined structure would hinder the ion intercalation/deintercalation.
Thin films of hexagonal NiO nanoplates and hierarchical NiO micro flakes assembled from nanoleaves were grown directly on FTO-coated glass substrates using a facile and template-free hydrothermal technique. As compared to conventional nanoporous structures or other1D nanostructures, the hierarchically assembled microflakes produced a larger active surface area, which is not only limited to the large open-pore voids between the microflakes, but also to the pore structure formed by the oriented assembly of the nanoleaves. It is noteworthy that the microflakes are made of atomically thin nanoleaves, which is similar to the layered WO3and MoO3nanosheets reported in the previous literatures. Such a layered structure that made of atomically thin nanoleaves would facilitate ion intercalation/deintercalation by reducing their diffusion path lengths. Thus, the films exhibited a high optical modulation (62.5%at550nm), large coloration efficiency (89.3cm2/C at550nm by applying a low coloration voltage of-1.0V) and fast switching responses with a coloring time of4.6s and a bleaching time of7.2s. Moreover, for the hierarchically assembled NiO films, the nanoleaves were assembled into microflake through the noncovalent bonds and gave an orderly integration architecture. This structure exhibited better structural stability and mechanical properties than the randomly distributed nanoplates. Therefore, it would reduce the dissolution caused by volumetric changes and lattice stresses during the repeated Li+ insertion and extraction process and result in a good cycling durability.
The soaking method and electrochemical deposition method were used to fabricate micro/nanostructured PANI EC films. Films of PANI nanoparticles were obtained by soaking the FTO glass in a solution containing0.5mol/L aniline and0.5mol/L aqueous H2SO4with oxalic acid as a dopant.When acrylic acid was used as the dopant, the resulting films were composed of PANI microrods. For the electrochemical oxidation polymerization of PANI film, the mode of deposition had a significant impact on the morphologies of the films. The dense amorphous PANI films were prepared through the constant current or voltage mode. While the nanorods film was grown by potentiodynamic cycle at a sweep rate of100mV/s. Therefore, the potentiodynamic cycle method was used to deposit PANI nanostructures on the WO3nanorods array film. The resulting WO3/PANI composite films exhibited double electrochromic effect of WO3and PANI. Compared with the single WO3films, the composite films showed tuning-color and fast switching responses with a coloring time of800ms and a bleaching time of500ms, which is attributed to the formation of donor-acceptor systems. The composite films also exhibited a high optical modulation (42% at632.8nm), large coloration efficiency (76cm2/C by applying a low coloration voltage of0.8V) as compare to the single PANI film.
The highly porous NiO/polyaniline composite films were prepared by combining hydrothermal process and electro-polymerization. Firstly, three types of porous NiO films have been synthesized by tuning the composition of the precursor solution in hydrothermal reaction vessel. Secondly, PANI nanostructures were deposited onto the as-prepared NiO porous structures by potentiodynamic cycle method. Since NiO and PANI are both colored under positive voltage and bleached under negative voltage, the NiO/PANI composite films showed highly enhanced EC performance as compared to the WO3/PANI composite films. A large optical modulation of62% at550nm, fast switching speeds of90and120ms for coloration and bleaching, respectively, and a high coloration efficiency of121cm2/C were achieved for the composite film assembled from NiO nanoplates and polyaniline pleated structures.
An all-solid-state EC device for modulating the optical transmittance was fabricated based on NiＯ/W03complementary structure and gel electrolyte. For comparation, a corresponding device based on liquid electrolyte was also manufactured. Due to the fast ions migration velocity, the device based on liquid electrolyte showed fast switching speeds of1.8and3.2s for coloration and bleaching, respectively, and a high coloration efficiency of146.9cm2/C. However, the device based on gel electrolyte gave poor EC performance because the migration of ions in the gel electrolyte was hindered by the non-conductive polymer frame, which led to a low switching kinetics. Moreover, due to the poor chemical stability and mechanical strength of the gel electrolyte, the polymer frame would be destroyed or collapsed during the coloration/bleaching process, and led to an irreversible cycle. Thus, it is necessary to improve the EC performance of all-solid-state device in our following research work and make it feasible for practical applications.
引文
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