柔性衬底WO_3-MoO_3电致变色薄膜溶胶—凝胶制备及性能研究
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摘要
电致变色材料在军事伪装及太阳能利用等领域具有广阔应用前景。目前人们对以平板玻璃为基板的电致变色器件研究逐步成熟,部分产品已推向市场。但其耐冲击性差、极易破碎,很难应用于具有复杂表面的武器装备。开展柔性电致变色器件的研究,对扩大电致变色材料在军事等领域的应用,具有重要意义。本文对柔性电致变色器件相关材料的制备技术进行了研究,初步组装了以PET为衬底,以ITO薄膜为透明电极,以WO_3-MoO_3薄膜为电致变色层,以TiO_2薄膜为离子储存层,以PMMA-PC-LiClO_4为电解质,结构为PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO_4/TiO_2/ITO/PET的柔性全固态电致变色器件,并对WO_3-MoO_3混合氧化物薄膜的电致变色机理和动力学过程进行了分析和探讨。
以金属W粉、Mo粉以及H_2O_2等为原料,合成了水相WO_3、MoO_3和WO_3-MoO_3溶胶,采用正交试验对WO_3溶胶的稳定性和在PET/ITO衬底上的成膜性进行了研究。结果表明,制备同时具有长期稳定性和良好成膜性WO_3溶胶的最佳配比为:W(g):H_2O_2(mL):C_2H_5OH(mL):HAc(mL)=1:5.5:5:1.3。WO_3-MoO_3混合溶胶具有比单一溶胶更好的稳定性和成膜性,最佳配比为WO_3:MoO_3=9:1(摩尔比)。制备后的溶胶宜贮存在较低温度下,而镀膜则应在干燥的环境、温度适中的条件下进行。MoO_3溶胶加入WO_3溶胶后,增大了溶胶体系的斥力位能,同时减小了引力位能,致使溶胶体系的势垒升高,从而提高了其稳定性。
采用FT-IR、TG-DTA、XRD及SEM等多种手段对WO_3-MoO_3薄膜的成分和结构进行了表征。结果发现,WO_3-MoO_3干凝胶结合水的脱离温度及双氧键的裂解温度与MoO_3干凝胶大致相当,而晶化温度与WO_3干凝胶的晶化温度基本相同;WO_3-MoO_3薄膜250℃以下热处理时呈非晶态,350℃热处理后,混合薄膜析出面心立方结构的WO_3·0.5H_2O晶体,当温度升高到450℃,薄膜中除了含有WO_3·0.5H_2O外,还析出W_(0.53)Mo_(0.47)O_3,H_(0.56)Mo_(0.25)W_(0.75)O_3和Mo_9O_(26)等多种晶体。
采用可见光分光光度计、电化学工作站等研究了热处理温度、薄膜厚度、原子配比及衬底材料对WO_3-MoO_3薄膜电致变色性能的影响,结合XPS等对其电致变色机理以及着/退色动力学过程进行了分析和探讨。结果表明,衬底材料对WO_3-MoO_3薄膜光学调制性能的影响不大,但塑料基薄膜的着色阈值电位略高于玻璃基薄膜;随WO_3-MoO_3/ITO/PET薄膜厚度的增加,制备态时的透过率略有减小,着色阈值电位降低,可见光调制幅度和储存电荷的能力增大;随着Mo含量的增加,WO_3-MoO_3/ITO/PET薄膜对可见光的调制幅度先增加后减小,在30atm%时达到最大值。
制备态的纯WO_3和MoO_3薄膜中仅含有六价金属离子;WO_3-MoO_3混合薄膜中氧空位增加,除含有六价离子外,还存在W~(5+)和Mo~(5+)。当Li~+和e~-注入WO_3-MoO_3薄膜后,注入的e~-占据空的W_(5d)、W_(6s)、Mo_(4d)和Mo_(5s)轨道,并在费米能级附近富集,将部分W~(6+)还原成W~(5+)和W~(4+),同时将部分Mo~(6+)和部分Mo~(5+)还原成Mo~(4+)。注入的e~-在WO_3-MoO_3薄膜中相邻价态的相邻离子间跃迁,产生不同的能量吸收,从而使其呈现出灰色变色特征。电场反向,Li~+和e~-从WO_3-MoO_3薄膜中抽取,W~(4+)和Mo~(4+)又被氧化成高价态,薄膜退色。
当着色电位低于阈值电位时,主要是电化学控制过程;当着色电位高于阈值电位时,Li~+在膜内的扩散为控制步骤。在±1.5V的阶跃电位下,WO_3-MoO_3/ITO/PET薄膜150s后达到饱和致色,经75s后达到完全退色。WO_3-MoO_3薄膜具有较好的开路记忆能力,但在空气中自然退色48h后,不再具有可逆的电致变色效应。
以钛酸四丁酯、乙醇、冰醋酸和蒸馏水等为原料,合成了稳定期在2个月以上,在PET/ITO和Glass/ITO衬底上成膜性能良好的TiO_2溶胶。随热处理温度的升高,Li~+在TiO_2薄膜中的注入和抽取更为容易,薄膜所注入和抽取的电荷密度减小,循环可逆性增强,对可见光的调制能力降低,着色/退色时间先降低后升高,350℃时达到最小值;塑料基TiO_2薄膜与相同条件下制备的玻璃基薄膜电色性能相似,都具有较弱的阴极电致变色效应和较强的Li~+储存能力,但循环可逆性较低;随厚度的增加,TiO_2薄膜离子贮存能力增大,循环可逆性减小,光学调制幅度增大,电化学响应时间缩短。塑料基TiO_2薄膜的电化学响应时间、离子储存能力与WO_3-MoO_3薄膜相匹配,且变色前后透过率都较高,可用作对电极。
采用原位聚合法合成了PMMA-PC-LiClO_4凝胶电解质,研究了LiClO_4/PC浓度和MMA单体含量对凝胶电解质室温电导率的影响。结果表明:凝胶室温离子电导率随LiClO_4/PC浓度的增加先增加后减小,浓度为1mol/L时达到最大值;随MMA单体加入量的增加,凝胶电解质膜的离子电导率减小,机械强度升高。MMA单体的加入量为50%,LiClO_4/PC浓度为1mol/L时,凝胶电解质的室温电导率为1.43×10~(-3)S/cm。PMMA-PC-LiClO_4凝胶电解质在可见光范围内的透过率大于85%,电化学稳定窗口为4.5V,满足电致变色器件在光学和电化学等方面的要求。
组装了结构为PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO_4/TiO_2/ITO/PET的柔性全固态电致变色小型器件,样品面积为5×2.5cm~2,厚度为0.4mm;器件在波长600nm处,着色和退色时的透过率分别为25%和56%,K值为0.58,饱和着色时间约为180s,完全退色时间约为120s;在全可见光波段,△T_(vis)为28%;循环寿命约为600次。
Electrochromic materials could be applied widely in the field of the military camouflage and solor energy usage due to its changing of colour and heating absorbtion with the applied voltage. Presently, the study on the electrochromic devices based on plate glass is active, and some products are on sale. However, it is difficult for these devices to use in the weapons equipments with complex surfaces because of their frangibility and poor toughness. Therefore, it is an important significance of developing the plastic electrochromic divice. In this paper, the preparation technologies about the corresponding materials for the plastic electrochromic divice were devoped, and the electrochromic cell sample with the laminated structure of PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO4/TiO_2/ITO/PET was fabricated. The electrochromic mechanism and dynamics of the WO_3-MoO_3 hybrid oxide films were discussed.
Tungsten powder, molybdium powder and hydrogen peroxide were used to prepare the aquous WO_3, MoO_3 and WO_3-MoO_3 sols. The stability and film formability of the sols on the PET/ITO substrates were studied. It is shown that the optimizing ratio to prepare WO_3 sol is W(g):H_2O_2(mL):C_2H_5OH(mL):HAc(mL)= 1:5.5:5:1.3. It is better for the hybrid sol to be saved at low temperature and the film to be fabricated at a moderate temperature in a dry atmosphere. The stable time of the WO3 sols with the addition of MoO_3 sols becomes longer because the potencial wall of the hybrid sols increases with the repelling potential increasing and the suction potential decreasing.
The compositions and structures of the WO_3-MoO_3 films were analysed by the means of FT-IR, TG-DTA, XRD, SEM et al.The results show that the deviating temperature of the bonded water and dividing temperature of the peroxide bond of the hybrid gels are equal to those of the MoO_3 gels, while their crystalized temperature is same as the WO_3 gels. The WO_3-MoO_3 films annealed under 250℃is amorphous. The bcc crystal of WO_3·0.5H_2O is formed when the heat treatment temperature is 350℃.When the heat treatment temperature increases to 450℃,several kinds of crystal separated out from the hybrid oxide films, such as WO_3·0.5H_2O,W_(0.53)Mo_(0.47)O_3,H_(0.56)Mo_(0.25)W_(0.75)O_3,Mo_9O_(26) and so on.
Effects of the heat treatment temperature, thickness, composition and substrate materials of the hybrid oxide films on the electrochromic properties were studied by the spectrophotometer and the electrochemical workstation. The electrochromic mechanism and the dynamic process were also analysed by XPS. It is shown that the substrates have little effect on the properties of modulating the visual light, but the threshold potential of the film based on PET/ITO is higher than that of Glass/ITO slightly. With increasing of thickness of the hybrid films, both the transmittance of the prepared films and the threshold potential decrease, while the magnitude of the modulating light and the inserted charge density incease. At the same time, the changing of light transmittance between the coloured film and the bleached film increases at first, and then decreases with the increasing of the molybdenum, and gets to maximum with 30atm% Mo atoms.
Only W~(6+) appears in the as-prepared WO_3 films made by the sol-gel method. With the addition of molybdenum, the five valences of W and Mo come forth from the as-prepared hybrid oxide film because of the increasing of oxygen cavity. At the coloured state, some W~(6+) deoxidize to W~(5+) and W~(4+),and partial Mo~(6+) and Mo~(5+) deoxidize to Mo~(4+).Different energy absorbance is caused when the inserted electrons hop between the border atoms with border valence, and as a result, the hybrid oxide films become grey. When bleaching, both W and Mo atoms revert to the as-prepared state, and the hybrid oxide film becomes transparent again. The results of the electrochromic dynamic reveal that the control step during the colouring process is the diffusing speed of the inserted lithium ions. The colouring speed is slower than the bleaching speed. The hybrid oxide film remains the colouring state for 48 hours under open circuit, but its electrochromism becomes irreversible.
Titanium oxide sol was synthesized with Ti(OBu)_4, ethanol, acetic acid and deion water, which could remain stable for over two months. Nanotitanium oxide films were prepared on the PET/ITO and Glass/ITO substrates by the sol-gel method. The structure and electrochromic properties of the films were characterised and compared. It is shown that the titanium dioxide particles of the TiO_2/ITO/PET film are bigger than those of the TiO_2/ITO/Glass film. With the annealing temperature increasing, the K value of the TiO_2/ITO/PET film increases from 0.56 to 0.97 and the lifetime from less than 50 cycles to more than 10000 cycles, while its intercalation charge density decreases from 14.12mC/cm~2 to 6.61 mC/cm~2.Both the TiO_2/ITO/PET film and the TiO_2/ITO/Glass film reveal weak cathodic colouration and strong capability of saving lithium ions. The electrochemical response time and the saving ions capability of the TiO_2/ITO/PET film are matching to those of the WO_3-MoO_3/ITO/PET film. Furthermore, the TiO_2/ITO/PET film remains high transmittance at the state of colouring and bleaching, so it can be used as a count electrode of the electrochromic WO_3-MoO_3 film.
The gel electrolyte of the PMMA-PC-LiClO_4 system was prepared by the in-suit polymerization method. Effects of concentration of the lithium salt and content of the MMA monomer on the room conductance of the gel electrolyte were discussed. The results reveal that the room conductance gets to maximum of 1.43×10~(-3)S/cm when the concentration of LiClO_4/PC is 1mol/L and the content of MMA is 50%.The transmittance of the gel electrolyte is over 85% and the electrochemical property remains stable under 4.5V, so it can meet the requirement of the electrochromic device.
The all-solid flexible electrochromic cell sample with the laminated structure of PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO_4/TiO_2/ITO/PET was fabricated in this paper. It is 5×2.5cm~2 in size,and 0.4mm in thickness. The electrochromic properties of the cell were tested. The transmittance variation between the coloured state and the bleached state is 31% at the wavelength of 600nm and the K value is 0.58. The colouring time and the bleaching time are about 180s and 120s, respectively.
以金属W粉、Mo粉以及H_2O_2等为原料,合成了水相WO_3、MoO_3和WO_3-MoO_3溶胶,采用正交试验对WO_3溶胶的稳定性和在PET/ITO衬底上的成膜性进行了研究。结果表明,制备同时具有长期稳定性和良好成膜性WO_3溶胶的最佳配比为:W(g):H_2O_2(mL):C_2H_5OH(mL):HAc(mL)=1:5.5:5:1.3。WO_3-MoO_3混合溶胶具有比单一溶胶更好的稳定性和成膜性,最佳配比为WO_3:MoO_3=9:1(摩尔比)。制备后的溶胶宜贮存在较低温度下,而镀膜则应在干燥的环境、温度适中的条件下进行。MoO_3溶胶加入WO_3溶胶后,增大了溶胶体系的斥力位能,同时减小了引力位能,致使溶胶体系的势垒升高,从而提高了其稳定性。
采用FT-IR、TG-DTA、XRD及SEM等多种手段对WO_3-MoO_3薄膜的成分和结构进行了表征。结果发现,WO_3-MoO_3干凝胶结合水的脱离温度及双氧键的裂解温度与MoO_3干凝胶大致相当,而晶化温度与WO_3干凝胶的晶化温度基本相同;WO_3-MoO_3薄膜250℃以下热处理时呈非晶态,350℃热处理后,混合薄膜析出面心立方结构的WO_3·0.5H_2O晶体,当温度升高到450℃,薄膜中除了含有WO_3·0.5H_2O外,还析出W_(0.53)Mo_(0.47)O_3,H_(0.56)Mo_(0.25)W_(0.75)O_3和Mo_9O_(26)等多种晶体。
采用可见光分光光度计、电化学工作站等研究了热处理温度、薄膜厚度、原子配比及衬底材料对WO_3-MoO_3薄膜电致变色性能的影响,结合XPS等对其电致变色机理以及着/退色动力学过程进行了分析和探讨。结果表明,衬底材料对WO_3-MoO_3薄膜光学调制性能的影响不大,但塑料基薄膜的着色阈值电位略高于玻璃基薄膜;随WO_3-MoO_3/ITO/PET薄膜厚度的增加,制备态时的透过率略有减小,着色阈值电位降低,可见光调制幅度和储存电荷的能力增大;随着Mo含量的增加,WO_3-MoO_3/ITO/PET薄膜对可见光的调制幅度先增加后减小,在30atm%时达到最大值。
制备态的纯WO_3和MoO_3薄膜中仅含有六价金属离子;WO_3-MoO_3混合薄膜中氧空位增加,除含有六价离子外,还存在W~(5+)和Mo~(5+)。当Li~+和e~-注入WO_3-MoO_3薄膜后,注入的e~-占据空的W_(5d)、W_(6s)、Mo_(4d)和Mo_(5s)轨道,并在费米能级附近富集,将部分W~(6+)还原成W~(5+)和W~(4+),同时将部分Mo~(6+)和部分Mo~(5+)还原成Mo~(4+)。注入的e~-在WO_3-MoO_3薄膜中相邻价态的相邻离子间跃迁,产生不同的能量吸收,从而使其呈现出灰色变色特征。电场反向,Li~+和e~-从WO_3-MoO_3薄膜中抽取,W~(4+)和Mo~(4+)又被氧化成高价态,薄膜退色。
当着色电位低于阈值电位时,主要是电化学控制过程;当着色电位高于阈值电位时,Li~+在膜内的扩散为控制步骤。在±1.5V的阶跃电位下,WO_3-MoO_3/ITO/PET薄膜150s后达到饱和致色,经75s后达到完全退色。WO_3-MoO_3薄膜具有较好的开路记忆能力,但在空气中自然退色48h后,不再具有可逆的电致变色效应。
以钛酸四丁酯、乙醇、冰醋酸和蒸馏水等为原料,合成了稳定期在2个月以上,在PET/ITO和Glass/ITO衬底上成膜性能良好的TiO_2溶胶。随热处理温度的升高,Li~+在TiO_2薄膜中的注入和抽取更为容易,薄膜所注入和抽取的电荷密度减小,循环可逆性增强,对可见光的调制能力降低,着色/退色时间先降低后升高,350℃时达到最小值;塑料基TiO_2薄膜与相同条件下制备的玻璃基薄膜电色性能相似,都具有较弱的阴极电致变色效应和较强的Li~+储存能力,但循环可逆性较低;随厚度的增加,TiO_2薄膜离子贮存能力增大,循环可逆性减小,光学调制幅度增大,电化学响应时间缩短。塑料基TiO_2薄膜的电化学响应时间、离子储存能力与WO_3-MoO_3薄膜相匹配,且变色前后透过率都较高,可用作对电极。
采用原位聚合法合成了PMMA-PC-LiClO_4凝胶电解质,研究了LiClO_4/PC浓度和MMA单体含量对凝胶电解质室温电导率的影响。结果表明:凝胶室温离子电导率随LiClO_4/PC浓度的增加先增加后减小,浓度为1mol/L时达到最大值;随MMA单体加入量的增加,凝胶电解质膜的离子电导率减小,机械强度升高。MMA单体的加入量为50%,LiClO_4/PC浓度为1mol/L时,凝胶电解质的室温电导率为1.43×10~(-3)S/cm。PMMA-PC-LiClO_4凝胶电解质在可见光范围内的透过率大于85%,电化学稳定窗口为4.5V,满足电致变色器件在光学和电化学等方面的要求。
组装了结构为PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO_4/TiO_2/ITO/PET的柔性全固态电致变色小型器件,样品面积为5×2.5cm~2,厚度为0.4mm;器件在波长600nm处,着色和退色时的透过率分别为25%和56%,K值为0.58,饱和着色时间约为180s,完全退色时间约为120s;在全可见光波段,△T_(vis)为28%;循环寿命约为600次。
Electrochromic materials could be applied widely in the field of the military camouflage and solor energy usage due to its changing of colour and heating absorbtion with the applied voltage. Presently, the study on the electrochromic devices based on plate glass is active, and some products are on sale. However, it is difficult for these devices to use in the weapons equipments with complex surfaces because of their frangibility and poor toughness. Therefore, it is an important significance of developing the plastic electrochromic divice. In this paper, the preparation technologies about the corresponding materials for the plastic electrochromic divice were devoped, and the electrochromic cell sample with the laminated structure of PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO4/TiO_2/ITO/PET was fabricated. The electrochromic mechanism and dynamics of the WO_3-MoO_3 hybrid oxide films were discussed.
Tungsten powder, molybdium powder and hydrogen peroxide were used to prepare the aquous WO_3, MoO_3 and WO_3-MoO_3 sols. The stability and film formability of the sols on the PET/ITO substrates were studied. It is shown that the optimizing ratio to prepare WO_3 sol is W(g):H_2O_2(mL):C_2H_5OH(mL):HAc(mL)= 1:5.5:5:1.3. It is better for the hybrid sol to be saved at low temperature and the film to be fabricated at a moderate temperature in a dry atmosphere. The stable time of the WO3 sols with the addition of MoO_3 sols becomes longer because the potencial wall of the hybrid sols increases with the repelling potential increasing and the suction potential decreasing.
The compositions and structures of the WO_3-MoO_3 films were analysed by the means of FT-IR, TG-DTA, XRD, SEM et al.The results show that the deviating temperature of the bonded water and dividing temperature of the peroxide bond of the hybrid gels are equal to those of the MoO_3 gels, while their crystalized temperature is same as the WO_3 gels. The WO_3-MoO_3 films annealed under 250℃is amorphous. The bcc crystal of WO_3·0.5H_2O is formed when the heat treatment temperature is 350℃.When the heat treatment temperature increases to 450℃,several kinds of crystal separated out from the hybrid oxide films, such as WO_3·0.5H_2O,W_(0.53)Mo_(0.47)O_3,H_(0.56)Mo_(0.25)W_(0.75)O_3,Mo_9O_(26) and so on.
Effects of the heat treatment temperature, thickness, composition and substrate materials of the hybrid oxide films on the electrochromic properties were studied by the spectrophotometer and the electrochemical workstation. The electrochromic mechanism and the dynamic process were also analysed by XPS. It is shown that the substrates have little effect on the properties of modulating the visual light, but the threshold potential of the film based on PET/ITO is higher than that of Glass/ITO slightly. With increasing of thickness of the hybrid films, both the transmittance of the prepared films and the threshold potential decrease, while the magnitude of the modulating light and the inserted charge density incease. At the same time, the changing of light transmittance between the coloured film and the bleached film increases at first, and then decreases with the increasing of the molybdenum, and gets to maximum with 30atm% Mo atoms.
Only W~(6+) appears in the as-prepared WO_3 films made by the sol-gel method. With the addition of molybdenum, the five valences of W and Mo come forth from the as-prepared hybrid oxide film because of the increasing of oxygen cavity. At the coloured state, some W~(6+) deoxidize to W~(5+) and W~(4+),and partial Mo~(6+) and Mo~(5+) deoxidize to Mo~(4+).Different energy absorbance is caused when the inserted electrons hop between the border atoms with border valence, and as a result, the hybrid oxide films become grey. When bleaching, both W and Mo atoms revert to the as-prepared state, and the hybrid oxide film becomes transparent again. The results of the electrochromic dynamic reveal that the control step during the colouring process is the diffusing speed of the inserted lithium ions. The colouring speed is slower than the bleaching speed. The hybrid oxide film remains the colouring state for 48 hours under open circuit, but its electrochromism becomes irreversible.
Titanium oxide sol was synthesized with Ti(OBu)_4, ethanol, acetic acid and deion water, which could remain stable for over two months. Nanotitanium oxide films were prepared on the PET/ITO and Glass/ITO substrates by the sol-gel method. The structure and electrochromic properties of the films were characterised and compared. It is shown that the titanium dioxide particles of the TiO_2/ITO/PET film are bigger than those of the TiO_2/ITO/Glass film. With the annealing temperature increasing, the K value of the TiO_2/ITO/PET film increases from 0.56 to 0.97 and the lifetime from less than 50 cycles to more than 10000 cycles, while its intercalation charge density decreases from 14.12mC/cm~2 to 6.61 mC/cm~2.Both the TiO_2/ITO/PET film and the TiO_2/ITO/Glass film reveal weak cathodic colouration and strong capability of saving lithium ions. The electrochemical response time and the saving ions capability of the TiO_2/ITO/PET film are matching to those of the WO_3-MoO_3/ITO/PET film. Furthermore, the TiO_2/ITO/PET film remains high transmittance at the state of colouring and bleaching, so it can be used as a count electrode of the electrochromic WO_3-MoO_3 film.
The gel electrolyte of the PMMA-PC-LiClO_4 system was prepared by the in-suit polymerization method. Effects of concentration of the lithium salt and content of the MMA monomer on the room conductance of the gel electrolyte were discussed. The results reveal that the room conductance gets to maximum of 1.43×10~(-3)S/cm when the concentration of LiClO_4/PC is 1mol/L and the content of MMA is 50%.The transmittance of the gel electrolyte is over 85% and the electrochemical property remains stable under 4.5V, so it can meet the requirement of the electrochromic device.
The all-solid flexible electrochromic cell sample with the laminated structure of PET/ITO/WO_3-MoO_3/PMMA-PC-LiClO_4/TiO_2/ITO/PET was fabricated in this paper. It is 5×2.5cm~2 in size,and 0.4mm in thickness. The electrochromic properties of the cell were tested. The transmittance variation between the coloured state and the bleached state is 31% at the wavelength of 600nm and the K value is 0.58. The colouring time and the bleaching time are about 180s and 120s, respectively.
引文
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