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WO2018188154A1 - Structure de dispositif électrochromique à couche mince à semi-conducteur intégral et son procédé de préparation - Google Patents

Structure de dispositif électrochromique à couche mince à semi-conducteur intégral et son procédé de préparation Download PDF

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Publication number
WO2018188154A1
WO2018188154A1 PCT/CN2017/084792 CN2017084792W WO2018188154A1 WO 2018188154 A1 WO2018188154 A1 WO 2018188154A1 CN 2017084792 W CN2017084792 W CN 2017084792W WO 2018188154 A1 WO2018188154 A1 WO 2018188154A1
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WIPO (PCT)
Prior art keywords
layer
oxide
lithium
electrochromic device
nano
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2017/084792
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English (en)
Chinese (zh)
Inventor
陈支勇
余小强
许冰文
黄嵚甫
蔡卫鹏
彭晟罡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jisheng Photoelectric (shenzhen) Co Ltd
Original Assignee
Jisheng Photoelectric (shenzhen) Co Ltd
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Publication of WO2018188154A1 publication Critical patent/WO2018188154A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • G02F1/153—Constructional details
    • G02F1/1533—Constructional details structural features not otherwise provided for

Definitions

  • the invention belongs to the field of electrochromic processing, and in particular relates to a structure and a preparation method of a solid full-film electrochromic device.
  • Electrochromism refers to the phenomenon that the optical properties (reflectance, transmittance, absorptivity, etc.) of a material undergo a stable and reversible color change under the action of an applied electric field, and the appearance is a reversible change in color and transparency.
  • the electrochromic smart glass has the adjustability of light absorption and transmission under the action of an electric field, and can selectively absorb or reflect the external heat radiation and the internal heat diffusion, thereby improving the natural light level and preventing peek. Therefore, electrochromic devices have a wide use value in the field of construction, anti-glare for vehicles, and sun-discoloring glasses.
  • the working area of the electrochromic device generally consists of a layer of color changing material, an ion conductor layer, and an ion storage layer.
  • the color-changing material layer, the ion conductor layer, and the ion storage layer are often required to be formed by various processes, and then need to be processed through a complicated packaging process.
  • All solid state devices employing inorganic ion storage layers can withstand longer solar radiation than all solid state devices of organic ion storage layers.
  • the lithium source in the inorganic all solid state device is derived from a lithium oxide ion conducting layer or a lithium oxide ion storage layer.
  • the prior art adopts a direct sputtering lithium oxide ion conductive layer or a lithium oxide ion storage layer, and has a low effective lithium content per unit volume in lithium oxide, difficulty in controlling the consistency of lithium oxide film layer composition, and a low sputtering rate.
  • the resulting equipment is costly and expensive.
  • the technical problem to be solved by the present invention is to overcome the bottleneck of the consistency control of the composition of the electrochromic device and the slow deposition of the lithium source compound in the prior art, thereby proposing the structure and preparation of a solid full-film electrochromic device. method.
  • the present invention discloses an all-solid-state electrochromic device (as shown in FIG. 1 ), and the electrochromic device is sent up to the next by a metal reflective layer or a transparent conductive layer, an electrochromic layer.
  • the dielectric layer, the lithium alloy layer, the ion storage layer, and the transparent conductive layer are composed.
  • the metal reflective layer is one of silver and aluminum.
  • the transparent conductive layer is one of indium tin oxide, aluminum-doped zinc oxide, and fluorine-doped tin oxide.
  • the electrochromic layer may be a transition metal oxide.
  • the transition metal oxide is one of tungsten oxide, vanadium pentoxide, ruthenium oxide, titanium oxide, ruthenium oxide, cobalt oxide, and molybdenum oxide.
  • the dielectric layer is one of silicon oxide and silicon oxynitride.
  • the lithium alloy layer is one of a lithium aluminum alloy and a lithium magnesium aluminum alloy.
  • the dielectric layer has a thickness of 10 to 500 nm; the lithium alloy layer has a thickness of 5 to 100 nm; the ion storage layer has a thickness of 300 to 1000 nm; and the electrochromic layer has a thickness of 300 to 1000 nm;
  • the metal reflective layer has a thickness of 20 to 500 nm.
  • the invention also discloses a method for preparing any of the electrochromic devices, the method steps are as follows:
  • a mask is coated to leave a wiring area, and a second transparent conductive film is plated.
  • the all-solid electrochromic device provided by the invention is composed of a multi-layer composite film layer, has a simple process, a fast coating rate, good component control, and good weather resistance of the device.
  • the target in the process can use a DC power source, which is 8-11 times higher than the conventional process using a RF power source, which greatly increases the productivity and greatly improves the color change rate of the overall device.
  • the invention breaks through the limitation that the coating rate of the lithium source layer of the existing all-solid-state electrochromic device structure is too slow, and innovatively solves the problem that the magnetic vapor deposition device has low efficiency in sputtering the lithium-lithide ceramic target by the physical vapor deposition device. It is easier to achieve large-scale production. In terms of application prospects, according to the choice of the underlying materials, it can be used in two major industries.
  • the bottom layer uses a metal reflective layer for electrochromic automotive rearview mirrors, and the bottom layer uses a transparent conductive layer for building curtain wall energy-saving glass.
  • FIG. 1 is a schematic longitudinal sectional view of an electrochromic device for an automobile rear view mirror according to an embodiment
  • FIG. 2 is a front elevational view of an automotive rearview mirror electrochromic device according to an embodiment
  • FIG. 3 is a comparative diagram of the fade color reflectance for an automotive rearview mirror electrochromic device according to an embodiment
  • FIG. 4 is a graph showing the reflectance of a car rearview mirror electrochromic device according to an embodiment as a function of time
  • FIG. 5 is a schematic longitudinal sectional structural view of an electrochromic device for building curtain wall energy-saving glass according to an embodiment
  • FIG. 6 is a comparison diagram of the effect of fading and discoloration state of the electrochromic device for building curtain wall energy-saving glass according to the embodiment
  • FIG. 7 is a view showing an effect of transmittance of an electrochromic device for building curtain wall energy-saving glass according to an embodiment at a wavelength of 850 nm as a function of response time;
  • the reference numerals are: 1-all solid state electrochromic device film.
  • Embodiment 1 This embodiment discloses an all-solid-state electrochromic device for an automobile rearview mirror (as shown in FIGS. 1 and 2), which is placed in a magnetron sputtering chamber after the mirror-size glass is chamfered.
  • a device is sequentially formed on the surface of the glass to form a device, and the electrochromic device is sequentially sent to the bottom to include:
  • a silver reflective layer, a tungsten oxide layer, a silicon oxide layer, a lithium magnesium alloy layer, a titanium-doped lithium iron phosphate layer, and an indium tin oxide layer was carried out, as shown in Figures 3 and 4, which has a large amplitude adjustment range and a fast response capability.
  • the silver reflective layer has a thickness of 60 nm; the tungsten oxide layer has a thickness of 350 nm; the silicon oxide layer has a thickness of 30 nm; the lithium magnesium alloy layer has a thickness of 20 nm; the titanium-doped lithium iron phosphate layer has a thickness of 600 nm; and the indium tin oxide layer has a thickness of 200 nm. ;
  • Embodiment 2 This embodiment discloses an all-solid-state electrochromic device.
  • the electrochromic device is sequentially provided with an aluminum reflective layer, a tungsten oxide layer, a silicon oxynitride layer, a lithium aluminum alloy layer, and a nickel oxide. , transparent conductive layer.
  • the thickness of the aluminum reflective layer is 100 nm; the thickness of the tungsten oxide layer is 400 nm; the thickness of the silicon oxynitride layer is 50 nm; the thickness of the lithium magnesium alloy layer is 25 nm; the thickness of the nickel oxide layer is 650 nm; and the thickness of the indium tin oxide layer is 200 nm;
  • Example 3 This embodiment discloses an all-solid-state electrochromic device (the overall longitudinal sectional structure of which is shown in FIG. 5).
  • the electrochromic device is sequentially provided to include an aluminum alloy reflective layer, a tungsten oxide layer, and a silicon nitrogen.
  • the thickness of the tungsten oxide is 500 nm; the lithium aluminum alloy layer is 30 nm; the silicon oxynitride layer is 100 nm; and the nickel oxide layer is 500 nm;
  • Embodiment 4 This embodiment discloses a preparation process of an all-solid-state electrochromic device for building curtain wall energy-saving glass, and the steps are as follows:
  • the 1.8 mm glass was plasma-cleaned and placed in a magnetron sputtering coating apparatus.
  • DC magnetron sputtering transparent conductive layer ITO film background vacuum degree is 1.8X10 -3 Pa, pure argon gas is introduced to the chamber gas pressure 0.3Pa, power is set to 6W/cm 2 , glass is heated at 200 ° sputtering
  • the ITO transparent conductive layer having a film thickness of 100 nm.
  • the mask plate is placed above the silver layer, and the electrochromic tungsten oxide layer is plated by a metal tungsten target by DC reactive sputtering: the background vacuum is 1.8 ⁇ 10 ⁇ 3 Pa, and the pure argon gas is introduced to the argon partial pressure of 1.3 Pa.
  • an intermediate frequency power source magnetron sputtering film is used as the ion conduction layer: the target uses a silicon-aluminum target, the instrument is pumped to a background vacuum of 1.8 ⁇ 10 -3 Pa, and the chamber is filled with oxygen to a pressure of 1.3 Pa.
  • the silicon-aluminum oxide ion-conducting layer having a radio frequency power of 2.2 W/cm 2 and a sputtered film layer thickness of 50 nm.
  • a lithium-cobalt co-doped nickel oxide film was used as the ion storage layer by DC power source magnetron sputtering: the target was 7% lithium, 5% titanium doped nickel oxide ceramic target, and the instrument was pumped to the background.
  • a transparent conductive layer ITO film was sputtered by DC magnetron: the background vacuum was 1.8 ⁇ 10 -3 Pa, the pure argon gas was introduced to the chamber gas pressure of 0.3 Pa, and the power was set to 6 W/ Cm 2 , an ITO transparent conductive layer having a sputtered film layer thickness of 100 nm.
  • the transmission curve of the device before and after discoloration was tested, as shown in Fig. 6.
  • the transmittance of the device before and after discoloration is large, and the maximum can be adjusted from 85% to 5%, which is very suitable for electrochromic building curtain wall.
  • the performance of the device as a function of response time at 850 nm was tested. As shown in Figure 7, the device has fast response capability and can achieve high transmission to high absorption changes in seconds.
  • Experimental example 3 The electrochromic device is subjected to the fading rate and the change with the corresponding time.
  • the experimental test results are shown in FIG. 3 and FIG. 4, and it can be seen that the electrochromic device obtained in the embodiment has a fast response speed and can be The state of high penetration to high light absorption is completed in a few seconds.
  • Figure 3 is a comparison of the discoloration contrast: the transmittance of the overall device under discoloration and fading.
  • the overall device has a large degree of discoloration and has a high light modulation effect.
  • Figure 4 color response time chart: The overall device response speed is very fast, can complete the state of high penetration to high light absorption in a few seconds.

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  • Physics & Mathematics (AREA)
  • Nonlinear Science (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)

Abstract

La présente invention concerne une structure d'un dispositif électrochromique à couche mince à semi-conducteur intégral et un procédé de préparation de celui-ci, appartenant au domaine du traitement électrochromique. Le dispositif électrochromique comprend, dans l'ordre de haut en bas, une couche de réflexion métallique ou une couche conductrice transparente, une couche électrochromique, une couche intermédiaire, une couche d'alliage de lithium, une couche de stockage d'ions et une couche conductrice transparente. Le dispositif électrochromique à semi-conducteur comprend des couches multiples de couches de film composite, et présente les avantages d'un procédé concis, d'une vitesse de revêtement rapide, d'une bonne commande de composant et d'une bonne résistance aux intempéries. Avec la présente invention, une avancée est réalisée dans la conception de couche de film de dispositif, la propriété selon laquelle la teneur en lithium par unité de volume efficace de lithium métallique ou d'alliage de lithium est beaucoup plus élevée que celle de composés de lithium est utilisée, et la caractéristique de la vitesse de pulvérisation cathodique de l'alliage de lithium métallique étant beaucoup plus élevée que celle de l'oxyde de lithium est également utilisée. Les objectifs d'amélioration de l'efficacité de production du dispositif, de réduction du coût de l'équipement et de prolongement de la durée de vie en cycle sont réalisés, la vitesse de réponse électrochromique du dispositif est élevée, et la compétitivité sur le marché est bonne.
PCT/CN2017/084792 2017-04-13 2017-05-18 Structure de dispositif électrochromique à couche mince à semi-conducteur intégral et son procédé de préparation Ceased WO2018188154A1 (fr)

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CN201710240528.XA CN107015412A (zh) 2017-04-13 2017-04-13 一种固态全薄膜电致变色器件的结构及制备方法
CN201710240528.X 2017-04-13

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CN112180647B (zh) * 2019-07-03 2022-11-29 中国科学院苏州纳米技术与纳米仿生研究所 包含多彩薄膜结构的装置
CN110265741A (zh) * 2019-06-14 2019-09-20 浙江工业大学 能原位观察电极材料在充放电过程中状态变化的开放式模拟锂电池的电化学池及测试方法
CN110737143A (zh) * 2019-10-30 2020-01-31 哈尔滨工业大学 一种快速响应的全固态电致变色器件及其制备方法
CN111142304B (zh) * 2019-12-25 2022-10-14 宁波祢若电子科技有限公司 一种全固态电致变色器件及其制作方法
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CN116534899B (zh) * 2023-04-17 2025-08-22 安徽精卓光显技术有限责任公司 氧化钨纳米晶、功能玻璃、电致变色器件及制备方法
CN117344276A (zh) * 2023-10-11 2024-01-05 上海交通大学深圳研究院 一种电致可见-红外响应超表面薄膜及其制备方法
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