CN107991819B - Method for improving Prussian blue electrochromic film on LiClO4Method for cyclic stability in PC electrolytes - Google Patents
Method for improving Prussian blue electrochromic film on LiClO4Method for cyclic stability in PC electrolytes Download PDFInfo
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 28
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000013225 prussian blue Substances 0.000 title claims abstract description 23
- 229960003351 prussian blue Drugs 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 13
- 125000004122 cyclic group Chemical group 0.000 title claims 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 16
- 229960000583 acetic acid Drugs 0.000 claims description 9
- 230000001351 cycling effect Effects 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims 9
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical group CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- -1 alkenyl ester Chemical class 0.000 claims 1
- 229910013684 LiClO 4 Inorganic materials 0.000 abstract description 21
- 239000010408 film Substances 0.000 abstract description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract description 6
- 239000010409 thin film Substances 0.000 abstract description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 abstract description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 abstract description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 abstract description 2
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- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 abstract description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 abstract description 2
- 235000006408 oxalic acid Nutrition 0.000 abstract description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000000970 chrono-amperometry Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
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- 239000011248 coating agent Substances 0.000 description 1
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- 230000000052 comparative effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
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- 238000004090 dissolution Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
- G02F2001/1517—Cyano complex compounds, e.g. Prussian blue
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Abstract
一种提高普鲁士蓝电致变色薄膜在LiClO4/PC电解质中的循环稳定性的方法，属于功能材料技术应用领域。在配置的LiClO4/PC电解液中滴入弱酸(可选醋酸，油酸，草酸等)，将普鲁士蓝电致变色薄膜放入到电解液中进行电致变色。可以提高循环稳定性，提高寿命。A method for improving the cycle stability of a Prussian blue electrochromic thin film in a LiClO 4 /PC electrolyte belongs to the technical application field of functional materials. Weak acid (optional acetic acid, oleic acid, oxalic acid, etc.) is dropped into the configured LiClO 4 /PC electrolyte, and the Prussian blue electrochromic film is put into the electrolyte for electrochromic. It can improve cycle stability and prolong life.
Description
技术领域technical field
本发明涉及如何提高普鲁士蓝薄膜在LiClO4/PC电解质的循环寿命的方法，属于功能材料技术应用领域。The invention relates to a method for improving the cycle life of a Prussian blue film in a LiClO 4 /PC electrolyte, and belongs to the technical application field of functional materials.
背景技术Background technique
目前在不断推进城市化的中国，建筑物的能耗占到社会总能耗的28％左右，窗户是建筑物能耗的主要途径，约30％～50％的能量通过窗户流失，同时能源和环境问题也日益凸显出来，降低能源消耗势在必行。电致变色材料作为一种新型功能材料，能过在一定外加电压作用下发生可逆的颜色变化，已广泛应用于飞机悬窗、智能窗、汽车后视镜、国防军事伪装等领域。电致变色材料是指在外加电压或电流的作用下能够可逆地改变其光学性能的材料。电致变色材料要求具有良好的离子和电子导电性、较高的对比度、变色效率和循环周期等电致变色性能。At present, in China, which is continuously promoting urbanization, the energy consumption of buildings accounts for about 28% of the total energy consumption of society. Windows are the main way of building energy consumption. About 30% to 50% of energy is lost through windows. Environmental problems have become increasingly prominent, and it is imperative to reduce energy consumption. As a new type of functional material, electrochromic material can undergo reversible color change under the action of a certain applied voltage, and has been widely used in aircraft hanging windows, smart windows, car rearview mirrors, defense and military camouflage and other fields. Electrochromic materials refer to materials that can reversibly change their optical properties under the action of an applied voltage or current. Electrochromic materials are required to have electrochromic properties such as good ionic and electronic conductivity, high contrast, color-changing efficiency and cycle time.
在众多电致变色材料中，普鲁士蓝具有响应速度快、颜色对比度高、薄膜均匀性好、制备原材料成本低的特点，并且能够在无色、蓝色、浅绿色三种颜色间变化，因此受到越来越多研究人员关注。但研究人员欲将其应用在电致变色器件中时，却发现普鲁士蓝在LiClO4/PC电解质中的循环稳定性较差，其循环寿命只有100圈左右，显然不能满足实际中的应用。普鲁士蓝在LiClO4/PC电解质中循环稳定性、耐久性差成为亟待解决的问题。使用本文中提到加入醋酸的方法，普鲁士蓝在LiClO4/PC 电解质中的循环寿命能够从100圈提高至3000圈且循环前后不出现明显衰减。而且，我们认为如果加入其它种类的弱酸也能达到相似的效果。Among many electrochromic materials, Prussian blue has the characteristics of fast response speed, high color contrast, good film uniformity, low cost of preparation raw materials, and can change among three colors: colorless, blue, and light green. More and more researchers are paying attention. However, when the researchers wanted to apply it in electrochromic devices, they found that the cycle stability of Prussian blue in LiClO 4 /PC electrolyte was poor, and its cycle life was only about 100 cycles, which obviously could not meet the practical application. The poor cycling stability and durability of Prussian blue in LiClO 4 /PC electrolyte have become an urgent problem to be solved. Using the method of adding acetic acid mentioned in this paper, the cycle life of Prussian blue in LiClO 4 /PC electrolyte can be improved from 100 cycles to 3000 cycles without significant decay before and after cycling. Furthermore, we believe that similar effects can be achieved if other kinds of weak acids are added.
发明内容SUMMARY OF THE INVENTION
本发明主要通过成本较低、操作简单的电化学沉积技术，制备出质地均匀的普鲁士蓝(PB)薄膜。通过在LiClO4/PC电解质中加入醋酸的方法，将普鲁士蓝薄膜的循环寿命从100圈提高至3000圈且不出现明显衰减。我们认为如果加入其它种类的弱酸也能达到相似的效果。The invention mainly prepares the Prussian blue (PB) thin film with uniform texture through the electrochemical deposition technology with low cost and simple operation. By adding acetic acid to LiClO 4 /PC electrolyte, the cycle life of Prussian blue films was improved from 100 cycles to 3000 cycles without obvious attenuation. We believe that similar effects can be achieved if other kinds of weak acids are added.
一种提高普鲁士蓝电致变色薄膜在LiClO4/PC电解质中的循环稳定性的方法，其特征在于，在配置的LiClO4/PC电解液中滴入弱酸；在 LiClO4/PC电解液中，LiClO4与弱酸的摩尔比为1∶1.7×1-610×10-6或 PC与弱酸的体积比为500∶1～5，将普鲁士蓝电致变色薄膜放入到电解液中进行电致变色。A method for improving the cycle stability of a Prussian blue electrochromic film in a LiClO 4 /PC electrolyte, characterized in that a weak acid is dropped into the configured LiClO 4 /PC electrolyte; in the LiClO 4 /PC electrolyte, The molar ratio of LiClO 4 to weak acid is 1:1.7×1 -6 10×10 -6 or the volume ratio of PC to weak acid is 500:1～5, put the Prussian blue electrochromic film into the electrolyte for electroplating discoloration.
上述的弱酸可选自醋酸、油酸、草酸等中的一种或几种，优选醋酸，进一步优选冰醋酸。The above-mentioned weak acid can be selected from one or more of acetic acid, oleic acid, oxalic acid, etc., preferably acetic acid, more preferably glacial acetic acid.
采用三电极体系，利用普林斯顿电化学工作站和紫外可见分光光度计在两种电解质中进行计时电流和透过率测试。PB薄膜蓝色为着色态，无色为褪色态。采用本发明的方法使得普鲁士蓝电致变色薄膜透过率稳定，不随时间增长或推移而变化衰减，循环稳定性好，寿命长。Chronoamperometry and transmittance measurements were performed in both electrolytes using a three-electrode system using a Princeton electrochemical workstation and a UV-Vis spectrophotometer. The blue color of the PB film is in the colored state, and the colorless is in the faded state. By adopting the method of the invention, the transmittance of the Prussian blue electrochromic thin film is stable, does not change and decay with the increase or passage of time, and has good cycle stability and long service life.
附图说明Description of drawings
图1制备的质地均匀的PB薄膜照片Figure 1 Photo of the prepared PB film with uniform texture
图2为PB薄膜在LiClO4/PC电解质(a)和在醋酸+LiClO4/PC电解质 (b)中的透过率曲线。Figure 2 shows the transmittance curves of PB films in LiClO 4 /PC electrolyte (a) and in acetic acid+LiClO 4 /PC electrolyte (b).
具体实施方式Detailed ways
下面结合附图和具体实施方式，进一步阐明本发明的实质性特点和显著优点，本发明决非仅局限于以下实施例，该发明对于其它种类的弱酸加入到LiClO4/PC电解质中具有相同的指导作用。The substantive features and significant advantages of the present invention will be further clarified below in conjunction with the accompanying drawings and specific embodiments. The present invention is by no means limited to the following examples. The invention has the same effect on the addition of other types of weak acids to the LiClO 4 /PC electrolyte. guiding role.
实施例1Example 1
(1)制备电沉积所需PB前驱液：将0.05mM K3Fe(CN)6、0.05mM FeCl3、0.1M KCl溶入去离子水中，磁力搅拌5min，用浓盐酸调节其 pH＝2.0，再磁力搅拌5min。(1) Preparation of PB precursor solution for electrodeposition: Dissolve 0.05mM K 3 Fe(CN) 6 , 0.05mM FeCl 3 , and 0.1M KCl in deionized water, stir magnetically for 5 minutes, adjust its pH=2.0 with concentrated hydrochloric acid, Magnetic stirring was continued for 5 min.
(2)ITO导电玻璃在使用前需依次经过丙酮、乙醇、去离子水超声波清洗，清洗后将玻璃擦干。使用恒电位仪进行镀膜，在恒流模式下，利用三电极体系进行电沉积，ITO导电玻璃连接工作电极，使用铂片作为对电极，Ag/KCl电极作为参比电极，在电流密度为10μA/cm2条件下电沉积时间为15min。工作电极和对电极平行对称排列。(2) The ITO conductive glass needs to be ultrasonically cleaned with acetone, ethanol and deionized water in sequence before use, and the glass should be wiped dry after cleaning. A potentiostat was used for coating, and a three-electrode system was used for electrodeposition in constant current mode. ITO conductive glass was connected to the working electrode, a platinum sheet was used as the counter electrode, and the Ag/KCl electrode was used as the reference electrode. The current density was 10 μA/ The electrodeposition time was 15 min under the condition of cm 2 . The working electrode and the counter electrode are arranged in parallel and symmetrically.
(3)将沉积完成的薄膜用去离子水冲洗后置于室温空气中12h。(3) The deposited film was rinsed with deionized water and then placed in air at room temperature for 12 h.
(4)配置电解质溶液：配制50ml的1mol/L的LiClO4/PC电解液 (LiClO4和PC组成的电解液，LiClO4的浓度为1mol/L)，溶解完全后加入2滴冰醋酸，使得LiClO4与弱酸的摩尔比为1∶1.7×10-6～3×10-6。(4) Configure electrolyte solution: prepare 50ml of 1 mol/L LiClO 4 /PC electrolyte (electrolyte composed of LiClO 4 and PC, the concentration of LiClO 4 is 1 mol/L), add 2 drops of glacial acetic acid after the dissolution is complete, so that The molar ratio of LiClO 4 to weak acid is 1:1.7×10 -6 to 3×10 -6 .
(5)同时配制LiClO4/PC电解液做对比测试。如果加入其它弱酸可按PC与弱酸的体积比进行试验。(5) Simultaneously prepare LiClO 4 /PC electrolyte for comparative test. If other weak acids are added, the test can be carried out according to the volume ratio of PC to weak acid.
(6)将制备好的薄膜放入电解质溶液中，采用步骤(3)三电极体系，利用普林斯顿电化学工作站和紫外可见分光光度计分别在两种电解质中进行计时电流(设为-0.05V和0.5V)和透过率测试，PB薄膜在 LiClO4/PC电解质(a)和在醋酸+LiClO4/PC电解质(b)中的透过率测试条件完全相同，结果具体见图2。(6) Put the prepared film into the electrolyte solution, adopt the three-electrode system of step (3), use the Princeton electrochemical workstation and the ultraviolet-visible spectrophotometer to carry out the chronoamperometry in the two electrolytes (set to -0.05V and 0.5V) and transmittance test, the transmittance test conditions of PB film in LiClO 4 /PC electrolyte (a) and in acetic acid + LiClO 4 /PC electrolyte (b) are exactly the same, the results are shown in Figure 2.
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