多酸型电致变色材料的性能调控
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摘要
电致变色材料以其在显示器、灵巧窗、汽车观后镜等领域的应用潜力而引起了广泛的关注。多金属氧酸盐(多酸,英文缩写POMs),一类无机金属氧化物构成的簇合物,以其多样的结构和独特的氧化还原性能在电致变色领域展现出了广阔的发展前景。本论文工作采用交替沉积技术构筑了多酸为电活性组分的膜材料,并研究了其电致变色性能。具体内容如下:
1利用交替沉积自组装技术将单取代Dawson多酸P2W17、中性红(NR)和聚电解质(PAH)构筑成复合膜。紫外可见吸收光谱确定了复合膜的增长是非常有序的。扫描电镜照片表明薄膜表面是均匀和平整的。该薄膜可以呈现出由粉红色到蓝紫色到深蓝紫色的颜色变化,即实现了可调变颜色的过程。而且,不同的颜色也可以代表不同的存储信号。这种复合膜材料在可调变的电致变色器件和数据存储器件方面具有潜在的应用。
2采用交替沉积方法将Dawson型多酸P2W18,PAH和TiO2制备成了电致变色复合膜材料。紫外可见吸收光谱,扫描电镜,循环伏安法,计时电流用于表征了复合膜材料。紫外可见吸收光谱和循环伏安法均可证明P2W18和TiO2被成功的构筑到薄膜中。将TiO2构筑到薄膜中后,这种复合膜的电致变色稳定性明显加强了。吸光度和电流密度变化显示出薄膜的稳定性明显提高。显然,TiO2的存在加强了薄膜和基底的附着力,从而提高了膜的稳定性。这种复合膜具有较高的光反差、适当的响应时间、较低的操作电压以及良好的稳定性可能满足电致变色器件的需求。
3将交替沉积和电聚合技术结合,构筑了Dawson型多酸P2W18和聚(3,4-乙烯二氧噻吩)(PEDOT)的复合膜。首先,采用交替沉积技术将P2W18和PAH制备成膜;然后,再利用电聚合技术沉积了PEDOT膜。将P2W18和PEDOT两种阴极着色材料进行复合后,得到了电致变色性能加强的膜材料,在650 nm处的光反差为54.7%,且循环1500圈后稳定性没有明显降低。而且,其变色范围几乎覆盖整个可见区。光谱电化学表明,这两种材料均保留了各自的电致变色性能,从而提高了光反差。聚电解质PAH以盘卷的结构有利于薄膜稳定性的提高。实验结果表明:多酸在提高PEDOT变色性能方面发挥了重要作用;交替沉积和电聚合技术结合开辟了构筑多酸和PEDOT薄膜材料的新方法。
4利用交替沉积技术将Dawson型多酸P2W18、碳纳米管(CNTs)、壳聚糖(CS)三元组分构筑成了纳米复合膜。CS作为阳离子电解质用来分散CNTs,得到CS-CNTs的复合物,然后采用交替沉积法与P2W18制备成薄膜。该膜材料的电致变色性能提高了,其在620 nm的光反差可达到20.3%,着色效率为91.5%。而且,将CNTs构筑到膜中,复合膜的厚度和表面粗糙度明显增加了。显然,CNTs的存在影响了膜结构,从而提高了复合膜的光反差和着色效率。研究结果说明CNTs在提高多酸电致变色性能方面发挥着重要作用。
Electrochromic materials have received much attention in chemistry and materials science owing to their potential applications in smart windows, displays and car rear-view mirrors. Polyoxometalates (POMs) represent a well-known class of structurally well-defined metal oxide nanoclusters. POMs are promising candidates due to their diverse structures and good reversible redox activity.
In this paper, we focus on the fabrication of POMs-based film materials by layer-by-layer method (LbL) and investigation of the electrochromic performances.
1 We successfully fabricated the multilayer film composed of the polyoxometalate cluster K10[P2W17O61] (P2W17), Neutral Red (NR) and polyallylamine hydrochloride (PAH) by the LbL method. The characterization of UV-vis spectroscopy reveals that POM, PAH and NR were constantly deposited in the ultrathin films. The surface morphology was investigated by SEM, which is uniform and smooth. This composite film demonstrates color changes from deep pink to light purple, then to dark purple-blue, achieving tunable color of electrochromic material. Furthermore, the different color can be considered as different spectral signal. Therefore, the composite film may become a promising candidate for application in tunable-color electrochromic devices and data-storage devices.
2 We reported the preparation of multilayer film consisting of tungstophosphate (P2W18), PAH and TiO2 by the LbL technique. The composite film was characterized by UV-vis spectrum, scanning electron micrpscopy (SEM), cyclic voltammetry (CV) and chronoamperomtric (CA). The characterizations of UV-vis spectrum and CV confirm the incorporation of P2W18 and TiO2 into the composite film. The composite film displays enhanced electrochromic stability due to the presence of TiO2. The performance of high optical contrast, suitable response time and low operation potential and long-term stability should be promising to meet the requirement for electrochromic devices.
3 A composite film containing P2W18, PAH and poly(3,4-ethylenedioxythiophene) (PEDOT) was fabricated by smart combination of LbL with electro-polymerization methods. The multilayer film is synthesized by forming P2W18 layer with PAH using the LbL technique, followed by deposition of PEDOT layer using electro-polymerization in aqueous solution. From the experimental results, the composite film displays enhanced electrochromic performance by combination of PEDOT with P2W18, resulting in the optical contrast of 54.7% at 600 nm and the absorbance without noticeable change upon 1500 cycles. Furthermore, the film provides broader absorption throughout the visible region. Spectroelectrochemical investigation demonstrates that both PEDOT and P2W18 synchronously contribute to electrochromic coloration. The existence of polyelectrolyte PAH in a condensed, coiled conformation is responsible for enhanced stability. These results demonstrate the essential role of POMs in improving functionality on PEDOT. The smart combination of LbL and electro-polymerization methods provides a convenient means to create new materials based on both PEDOT and POMs.
4 We successfully constructed a nanocomposite film containing P2W18, carbon nanotubes (CNTs) and chitosan (CS) by LbL method. Chitosan was chosen as cationic polyelectrolyte for dispersing CNTs to form a stable CS-CNTs composite, which was assembled with anionic P2W18. The composite material displays enhanced electrochromic performance, with the optical contrast of 20.3% and coloration efficiency of 91.5 cm2 C-1 at 620 nm. Furthermore, the film displays the increased thickness and surface roughness by incorporation of CNTs into the P2W18 film. Obviously, the presence of CNTs has the strong influence on the multilayer structure, leading to high optical contrast and coloration efficiency. The results demonstrate the essential role of CNTs in enhancing electrochromism on POMs.
1利用交替沉积自组装技术将单取代Dawson多酸P2W17、中性红(NR)和聚电解质(PAH)构筑成复合膜。紫外可见吸收光谱确定了复合膜的增长是非常有序的。扫描电镜照片表明薄膜表面是均匀和平整的。该薄膜可以呈现出由粉红色到蓝紫色到深蓝紫色的颜色变化,即实现了可调变颜色的过程。而且,不同的颜色也可以代表不同的存储信号。这种复合膜材料在可调变的电致变色器件和数据存储器件方面具有潜在的应用。
2采用交替沉积方法将Dawson型多酸P2W18,PAH和TiO2制备成了电致变色复合膜材料。紫外可见吸收光谱,扫描电镜,循环伏安法,计时电流用于表征了复合膜材料。紫外可见吸收光谱和循环伏安法均可证明P2W18和TiO2被成功的构筑到薄膜中。将TiO2构筑到薄膜中后,这种复合膜的电致变色稳定性明显加强了。吸光度和电流密度变化显示出薄膜的稳定性明显提高。显然,TiO2的存在加强了薄膜和基底的附着力,从而提高了膜的稳定性。这种复合膜具有较高的光反差、适当的响应时间、较低的操作电压以及良好的稳定性可能满足电致变色器件的需求。
3将交替沉积和电聚合技术结合,构筑了Dawson型多酸P2W18和聚(3,4-乙烯二氧噻吩)(PEDOT)的复合膜。首先,采用交替沉积技术将P2W18和PAH制备成膜;然后,再利用电聚合技术沉积了PEDOT膜。将P2W18和PEDOT两种阴极着色材料进行复合后,得到了电致变色性能加强的膜材料,在650 nm处的光反差为54.7%,且循环1500圈后稳定性没有明显降低。而且,其变色范围几乎覆盖整个可见区。光谱电化学表明,这两种材料均保留了各自的电致变色性能,从而提高了光反差。聚电解质PAH以盘卷的结构有利于薄膜稳定性的提高。实验结果表明:多酸在提高PEDOT变色性能方面发挥了重要作用;交替沉积和电聚合技术结合开辟了构筑多酸和PEDOT薄膜材料的新方法。
4利用交替沉积技术将Dawson型多酸P2W18、碳纳米管(CNTs)、壳聚糖(CS)三元组分构筑成了纳米复合膜。CS作为阳离子电解质用来分散CNTs,得到CS-CNTs的复合物,然后采用交替沉积法与P2W18制备成薄膜。该膜材料的电致变色性能提高了,其在620 nm的光反差可达到20.3%,着色效率为91.5%。而且,将CNTs构筑到膜中,复合膜的厚度和表面粗糙度明显增加了。显然,CNTs的存在影响了膜结构,从而提高了复合膜的光反差和着色效率。研究结果说明CNTs在提高多酸电致变色性能方面发挥着重要作用。
Electrochromic materials have received much attention in chemistry and materials science owing to their potential applications in smart windows, displays and car rear-view mirrors. Polyoxometalates (POMs) represent a well-known class of structurally well-defined metal oxide nanoclusters. POMs are promising candidates due to their diverse structures and good reversible redox activity.
In this paper, we focus on the fabrication of POMs-based film materials by layer-by-layer method (LbL) and investigation of the electrochromic performances.
1 We successfully fabricated the multilayer film composed of the polyoxometalate cluster K10[P2W17O61] (P2W17), Neutral Red (NR) and polyallylamine hydrochloride (PAH) by the LbL method. The characterization of UV-vis spectroscopy reveals that POM, PAH and NR were constantly deposited in the ultrathin films. The surface morphology was investigated by SEM, which is uniform and smooth. This composite film demonstrates color changes from deep pink to light purple, then to dark purple-blue, achieving tunable color of electrochromic material. Furthermore, the different color can be considered as different spectral signal. Therefore, the composite film may become a promising candidate for application in tunable-color electrochromic devices and data-storage devices.
2 We reported the preparation of multilayer film consisting of tungstophosphate (P2W18), PAH and TiO2 by the LbL technique. The composite film was characterized by UV-vis spectrum, scanning electron micrpscopy (SEM), cyclic voltammetry (CV) and chronoamperomtric (CA). The characterizations of UV-vis spectrum and CV confirm the incorporation of P2W18 and TiO2 into the composite film. The composite film displays enhanced electrochromic stability due to the presence of TiO2. The performance of high optical contrast, suitable response time and low operation potential and long-term stability should be promising to meet the requirement for electrochromic devices.
3 A composite film containing P2W18, PAH and poly(3,4-ethylenedioxythiophene) (PEDOT) was fabricated by smart combination of LbL with electro-polymerization methods. The multilayer film is synthesized by forming P2W18 layer with PAH using the LbL technique, followed by deposition of PEDOT layer using electro-polymerization in aqueous solution. From the experimental results, the composite film displays enhanced electrochromic performance by combination of PEDOT with P2W18, resulting in the optical contrast of 54.7% at 600 nm and the absorbance without noticeable change upon 1500 cycles. Furthermore, the film provides broader absorption throughout the visible region. Spectroelectrochemical investigation demonstrates that both PEDOT and P2W18 synchronously contribute to electrochromic coloration. The existence of polyelectrolyte PAH in a condensed, coiled conformation is responsible for enhanced stability. These results demonstrate the essential role of POMs in improving functionality on PEDOT. The smart combination of LbL and electro-polymerization methods provides a convenient means to create new materials based on both PEDOT and POMs.
4 We successfully constructed a nanocomposite film containing P2W18, carbon nanotubes (CNTs) and chitosan (CS) by LbL method. Chitosan was chosen as cationic polyelectrolyte for dispersing CNTs to form a stable CS-CNTs composite, which was assembled with anionic P2W18. The composite material displays enhanced electrochromic performance, with the optical contrast of 20.3% and coloration efficiency of 91.5 cm2 C-1 at 620 nm. Furthermore, the film displays the increased thickness and surface roughness by incorporation of CNTs into the P2W18 film. Obviously, the presence of CNTs has the strong influence on the multilayer structure, leading to high optical contrast and coloration efficiency. The results demonstrate the essential role of CNTs in enhancing electrochromism on POMs.
引文
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