CN113885265A - All-solid-state inorganic electrochromic composite film system intelligent glass assembly and preparation method thereof - Google Patents

All-solid-state inorganic electrochromic composite film system intelligent glass assembly and preparation method thereof Download PDF

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Publication number
CN113885265A
CN113885265A CN202111124959.2A CN202111124959A CN113885265A CN 113885265 A CN113885265 A CN 113885265A CN 202111124959 A CN202111124959 A CN 202111124959A CN 113885265 A CN113885265 A CN 113885265A
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film
glass
layer
thickness
solid
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汤永康
甘治平
李刚
沈洪雪
王金磊
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CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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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
    • G02F1/1523—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 inorganic material
    • G02F1/1524—Transition metal compounds
    • 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
    • G02F1/1523—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 inorganic material
    • G02F1/1525—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 inorganic material characterised by a particular ion transporting layer, e.g. electrolyte

Abstract

The invention relates to an all-solid-state inorganic electrochromic composite film system intelligent glass component and a preparation method thereof, and is characterized in that: (1) two pieces of transparent conductive film glass are used as substrates, the transparent conductive film glass is ITO or FTO coated glass, and one piece of WO with the thickness of 100-500 nm is prepared on one piece of conductive glass by a magnetron sputtering method3The base film is used as an electrochromic layer, and a NiO base film with the thickness of 100-500 nm is prepared on another piece of conductive glass by a magnetron sputtering method and is used as an ion storage layer; (2) WO prepared separately by wet-chemical sol-gel process3Preparing Li + doped AlPO with the thickness of 100-500 nm on the base and NiO base film4The film is used as an ion transmission layer; (3) the two glasses were doped with wet-chemical Li + -AlPO4The films are bonded together as a medium, and the wet chemical ion transmission layer in the middle of the glass component is cured by heat treatment. The invention has the advantages that: using bidirectional patchesThe preparation method has the advantages of simple and efficient component acquisition and lower cost.

Description

All-solid-state inorganic electrochromic composite film system intelligent glass assembly and preparation method thereof
Technical Field
The invention belongs to the field of intelligent glass material structures and designs, relates to an all-solid-state inorganic intelligent glass component, and particularly relates to an all-solid-state inorganic intelligent glass component which is laminated by taking a wet chemical inorganic ion transmission layer as an adhesive medium, and a preparation method thereof.
Background
Electrochromism means that the optical properties (transmission, reflection, absorption and the like) of the material can be stably and reversibly changed under the action of an applied electric field or current. The electrochromic material has good physical and chemical properties and reversible optical performance as a novel functional material, can be used for manufacturing devices such as displays, dimming glasses, information storage and the like, has wide application prospects in various fields such as information, electronics, energy, buildings, national defense and the like, and has important significance for energy conservation and environmental protection. Especially, the electrochromic intelligent glass prepared by utilizing the electrochromic material has the advantages of low energy consumption, quick response, manual control and the like, is researched and popularized more, has light absorption and transmission adjustability under the action of an electric field, can selectively absorb or reflect external heat radiation and reduce internal heat diffusion, reduces a large amount of energy which is required to be consumed by keeping an office building and a civil house cool in summer and warm in winter, simultaneously achieves the purposes of improving the natural illumination degree and preventing peeping, solves the problem of urban light pollution which is continuously worsened in modern times, and has huge application market.
Electrochromic intelligent glass can be divided into two main categories, namely organic or inorganic electrochromic glass, wherein all-solid-state inorganic electrochromic glass is particularly concerned in the application industrialization process due to the relatively fast color change response time, relatively large color change amplitude, long cycle life and strong weather resistance, however, an all-solid-state inorganic electrochromic component is generally composed of five layers of films on glass, wherein two layers are transparent conductive films, and in addition, an electrochromic layer, an ion transmission layer and an ion storage layer are respectively arranged. The conventional electrochromic layer and ion storage layer are WO3With NiO-based film and ion transport layer of LiTaO3Films, usually prepared by magnetron sputtering, WO3Has higher preparation efficiency with NiO-based thin film layer, and LiTaO3The preparation of the layer has extremely low preparation efficiency due to the property of the target material, so that the energy consumption is huge, and the whole body isThe efficiency of the production of the module is affected, resulting in high production costs.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an all-solid-state inorganic electrochromic composite film system intelligent glass component and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the all-solid-state inorganic electrochromic composite film system intelligent glass component comprises a glass substrate and is characterized by having the following structure: an ITO or FTO thin film layer and WO with the thickness of 100-500 nm are sequentially arranged on a glass substrate from bottom to top3Thin film layer and Li + doped AlPO with thickness of 100-500 nm4The film layer, a NiO-based film layer with the thickness of 100-500 nm, an ITO or FTO film layer and a glass substrate.
Further, said WO3The film is pure WO3Films or WO3Doped with Ti2+、Ag+、Mo6+A thin film of plasma.
Further, the NiO-based film is a pure NiO film or NiO-doped Li+、Al3+、Na+、K+、Mg2+、Ca2+A thin film of plasma.
Further, said WO3The thickness of the thin film layer is 200-300 nm, and Li + doped AlPO4The thickness of the thin film layer is 200-350 nm, and the thickness of the NiO-based thin film layer is 200-350 nm.
Further, said WO3The thickness of the thin film layer is 220-280 nm, and Li + doped AlPO4The thickness of the thin film layer is 250-300 nm, and the thickness of the NiO-based thin film layer is 240-320 nm.
A preparation method of an all-solid-state inorganic electrochromic composite film system intelligent glass component is characterized by comprising the following steps:
(1) preparing a film system electrochromic layer and an ion storage layer: two pieces of transparent conductive film glass are used as substrates, the transparent conductive film glass is ITO or FTO coated glass, and one piece of WO with the thickness of 100-500 nm is prepared on one piece of conductive glass by a magnetron sputtering method3Base film as electrochromic layerPreparing a NiO-based film with a thickness of 100-500 nm as an ion storage layer on the other piece of conductive glass by a magnetron sputtering method;
(2) preparing a membrane inorganic ion transmission layer: WO prepared separately by wet-chemical sol-gel process3Preparing Li + doped AlPO with the thickness of 100-500 nm on the base and NiO base film4The thin film serves as an ion transport layer (electrolyte layer);
(3) preparing an electrochromic assembly: the two glasses were doped with wet-chemical Li + -AlPO4The films are bonded together as a medium, and then the wet chemical ion transmission layer in the middle of the glass component is cured by heat treatment (150-400 ℃) to obtain the all-solid-state inorganic electrochromic composite film system intelligent glass component.
Further, in the step (1), the magnetron sputtering power is 500-2200W, and the sputtering pressure is 0.2-2.0 Pa; the flow ratio of argon to oxygen is 10: 1-1: 1.
Further, the Li + doped AlPO of the step (2)4The preparation method of the film comprises the following steps: dip drawing, spin coating, knife coating, roll coating, and the like.
The invention organically combines magnetron sputtering coating with liquid phase method coating, and prepares the ion transmission Li + doped AlPO by the liquid phase method4The wet sol film of the inorganic ion transmission layer is used as a bonding medium, the bonding medium of two pieces of glass of the assembly is a homogeneous inorganic material, and the homogeneous material is subjected to heat treatment to mutually permeate and transfer mass so as to be solidified into a solid inorganic ion transmission layer. Meanwhile, the ion transmission layer of the electrochromic component prepared by the wet chemical sol-gel method can fully exert the advantage of loose structure of the thin film prepared by the liquid phase method, further improve the ion transmission rate of the component during working, and further improve the electrochromic efficiency of the component; simultaneously combined with high efficiency WO3The NiO-based thin film layer is prepared by a magnetron sputtering method, so that low LiTaO is avoided3The layer magnetron sputtering preparation efficiency saves energy consumption, thereby reducing the preparation cost of the whole assembly.
The effective gains of the present invention are:
1. the inorganic electrochromic intelligent glass component can be directly obtained by utilizing the bidirectional patch mode, so that the packaging process required after the traditional inorganic electrochromic intelligent glass component film system is prepared in a layer-by-layer accumulation manner is saved, and the component is simpler and more convenient to obtain;
2. compared with the traditional preparation method, the preparation method is more efficient and lower in cost, and provides a new idea for future industrialization; the intelligent glass prepared by the invention has good application prospect in the fields of building windows, curtain walls, ornaments, intelligent automobiles, consumer electronics, information display and the like.
Drawings
FIG. 1 is a simplified diagram of the process for preparing the electrochromic layer and the ion storage layer of the film system in step (1) of the present invention;
FIG. 2 is a simplified diagram of the process for preparing the inorganic ion transport layer of the membrane system in step (2) of the present invention;
FIG. 3 is a schematic diagram of the preparation process of the electrochromic assembly in step (3) of the present invention.
Detailed Description
The following examples further describe the present invention with reference to the accompanying drawings, but the examples should not be construed as limiting the present invention.
Example 1
(1) Preparing a film system electrochromic layer and an ion storage layer: as shown in fig. 1, two pieces of transparent conductive film glass are used as substrates, the transparent conductive film glass is ITO or FTO coated glass, and the sheet resistance of the film is 20 Ω/sq; preparation of WO on one of the conductive glasses by magnetron sputtering3The base film is used as an electrochromic layer, the sputtering target material is a metal W target or a metal W, Ti alloy target and the like (the doping amount of alloy elements except the metal W is 10%), the sputtering power is 1200W, and the sputtering pressure is 1.0 Pa; the flow ratio of argon gas to oxygen gas is 10:1, and the preparation thickness is controlled to be 300 nm; preparing a NiO-based film on the other piece of conductive glass as an ion storage layer by a magnetron sputtering method, wherein a sputtering target material is a metal Ni target or a metal Ni and Al alloy target and the like (the doping amount of alloy elements except the metal Ni is 15%), the sputtering power is 1000W, and the sputtering pressure is 1.0 Pa; the flow ratio of argon gas to oxygen gas is 10:1, and the preparation thickness is controlled to be 300 nm;
(2) preparing a membrane inorganic ion transmission layer: using isopropanol as solvent, aluminium isopropoxide,Preparation of Li + doped AlPO by using lithium perchlorate and phosphoric acid as precursors4Coating sol with Li + doping concentration of 20%, as shown in figure 2, and WO prepared from the sol prepared by sol-gel method3Preparation of Li + doped AlPO on base and NiO base film4Thin film as ion transport layer (electrolyte layer), Li + doped AlPO4The preparation method of the film comprises the following steps: dipping, lifting, spin coating, blade coating, roller coating and the like, and controlling the single-side preparation thickness to be 300 nm;
(3) preparing an electrochromic assembly: as shown in FIG. 3, two pieces of the above-prepared AlPO doped with Li + in wet chemistry4The films are bonded together as a medium, then a wet chemical ion transmission layer in the middle of the glass component is cured by heat treatment at the temperature of 250 ℃, and finally the all-solid-state inorganic electrochromic composite film system intelligent glass component is obtained.
Example 2
(1) Preparing a film system electrochromic layer and an ion storage layer: as shown in the attached figure 1, two pieces of transparent conductive film glass are used as substrates, the transparent conductive film glass is ITO or FTO coated glass, and the sheet resistance of the film is 8 Ω/sq; preparation of WO on one of the conductive glasses by magnetron sputtering3The base film is used as an electrochromic layer, the sputtering target material is a metal W target or a metal W, Ti alloy target and the like (the doping amount of alloy elements except the metal W is 5%), the sputtering power is 800W, and the sputtering pressure is 0.5 Pa; the flow ratio of argon gas to oxygen gas is 2:1, and the preparation thickness is controlled to be 150 nm; preparing a NiO-based film on the other piece of conductive glass as an ion storage layer by a magnetron sputtering method, wherein a sputtering target material is a metal Ni target or a metal Ni and Al alloy target and the like (the doping amount of alloy elements except metal Ni is 5%), the sputtering power is 800W, and the sputtering pressure is 0.5 Pa; the flow ratio of argon gas to oxygen gas is 2:1, and the preparation thickness is controlled to be 150 nm;
(2) preparing a membrane inorganic ion transmission layer: preparation of Li + doped AlPO by using isopropanol as solvent and aluminum isopropoxide, lithium perchlorate and phosphoric acid as precursors4Coating sol with Li + doping concentration of 20%, as shown in figure 2, and WO prepared from the sol prepared by sol-gel method3Preparation of Li + doped AlPO on base and NiO base film4Thin film as ion transport layer (electrolyte layer), Li + doped AlPO4The preparation method of the film comprises the following steps: dipping, lifting, spin coating, blade coating, roller coating and the like, and controlling the single-side preparation thickness to be 150 nm;
(3) preparing an electrochromic assembly: as shown in FIG. 3, two pieces of the above-prepared AlPO doped with Li + in wet chemistry4The films are bonded together as a medium, then a wet chemical ion transmission layer in the middle of the glass component is cured by heat treatment at the temperature of 250 ℃, and finally the all-solid-state inorganic electrochromic composite film system intelligent glass component is obtained.
Example 3
(1) Preparing a film system electrochromic layer and an ion storage layer: as shown in the attached figure 1, two pieces of transparent conductive film glass are used as substrates, the transparent conductive film glass is ITO or FTO coated glass, and the sheet resistance of the film is 35 Ω/sq; preparation of WO on one of the conductive glasses by magnetron sputtering3The base film is used as an electrochromic layer, the sputtering target material is a metal W target or a metal W, Ti alloy target and the like (the doping amount of alloy elements except the metal W is 18 percent), the sputtering power is 2000W, and the sputtering pressure is 1.8 Pa; the flow ratio of argon to oxygen gas is 8:1, and the preparation thickness is controlled to be 450 nm; preparing a NiO-based film on the other piece of conductive glass as an ion storage layer by a magnetron sputtering method, wherein a sputtering target material is a metal Ni target or a metal Ni and Al alloy target and the like (the doping amount of alloy elements except the metal Ni is 25%), the sputtering power is 2000W, and the sputtering pressure is 1.8 Pa; the flow ratio of argon to oxygen gas is 8:1, and the preparation thickness is controlled to be 450 nm;
(2) preparing a membrane inorganic ion transmission layer: preparation of Li + doped AlPO by using isopropanol as solvent and aluminum isopropoxide, lithium perchlorate and phosphoric acid as precursors4Coating sol with Li + doping concentration of 20%, as shown in figure 2, and WO prepared from the sol prepared by sol-gel method3Preparation of Li + doped AlPO on base and NiO base film4Thin film as ion transport layer (electrolyte layer), Li + doped AlPO4The preparation method of the film comprises the following steps: dipping, lifting, spin coating, blade coating, roller coating and the like, and controlling the preparation thickness of a single surface to be 450 nm;
(3) electrochromic component preparation: as shown in FIG. 3, two pieces of the above-prepared AlPO doped with Li + in wet chemistry4The films are bonded together as a medium, then a wet chemical ion transmission layer in the middle of the glass component is cured by heat treatment at the temperature of 250 ℃, and finally the all-solid-state inorganic electrochromic composite film system intelligent glass component is obtained.

Claims (9)

1. The all-solid-state inorganic electrochromic composite film system intelligent glass component comprises a glass substrate and is characterized by having the following structure: an ITO or FTO thin film layer and WO with the thickness of 100-500 nm are sequentially arranged on a glass substrate from bottom to top3Thin film layer and Li + doped AlPO with thickness of 100-500 nm4The film layer, a NiO-based film layer with the thickness of 100-500 nm, an ITO or FTO film layer and a glass substrate.
2. The all-solid-state inorganic electrochromic composite film system intelligent glass assembly according to claim 1, wherein: said WO3The film is pure WO3Films or WO3Doped with Ti2+、Ag+、Mo6+A film of ions.
3. The all-solid-state inorganic electrochromic composite film-based smart glass assembly according to claim 1 or 2, wherein: the NiO-based film is a pure NiO film or NiO-doped Li+、Al3+、Na+、K+、Mg2+、Ca2+A film of ions.
4. The all-solid-state inorganic electrochromic composite film-based smart glass assembly according to claim 1 or 2, wherein: said WO3The thickness of the thin film layer is 200-300 nm, and Li + doped AlPO4The thickness of the thin film layer is 200-350 nm, and the thickness of the NiO-based thin film layer is 200-350 nm.
5. The all-solid-state inorganic electrochromic composite film-based smart glass assembly according to claim 1 or 2, wherein: said WO3The thickness of the thin film layer is 220-280 nm, and Li + doped AlPO4The thickness of the thin film layer is 250-300 nm, and the thickness of the NiO-based thin film layer is 240-320 nm.
6. A preparation method of an all-solid-state inorganic electrochromic composite film system intelligent glass component is characterized by comprising the following steps:
(1) preparing a film system electrochromic layer and an ion storage layer: two pieces of transparent conductive film glass are used as substrates, the transparent conductive film glass is ITO or FTO coated glass, and one piece of WO with the thickness of 100-500 nm is prepared on one piece of conductive glass by a magnetron sputtering method3The base film is used as an electrochromic layer, and a NiO base film with the thickness of 100-500 nm is prepared on another piece of conductive glass by a magnetron sputtering method and is used as an ion storage layer;
(2) preparing a membrane inorganic ion transmission layer: WO prepared separately by wet-chemical sol-gel process3Preparing Li + doped AlPO with the thickness of 100-500 nm on the base and NiO base film4The film is used as an ion transmission layer;
(3) preparing an electrochromic assembly: the two glasses were doped with wet-chemical Li + -AlPO4The films are bonded together as a medium, and then the wet chemical ion transmission layer in the middle of the glass component is cured by heat treatment to obtain the all-solid-state inorganic electrochromic composite film system intelligent glass component.
7. The method for preparing the all-solid-state inorganic electrochromic composite film system intelligent glass assembly according to claim 6, wherein the method comprises the following steps: in the step (1), the magnetron sputtering power is 500-2200W, and the sputtering pressure is 0.2-2.0 Pa; the flow ratio of argon to oxygen is 10: 1-1: 1.
8. The method for preparing the all-solid-state inorganic electrochromic composite film system intelligent glass assembly according to claim 6 or 7, wherein the method comprises the following steps: the Li + doped AlPO of the step (2)4The preparation method of the film comprises the following steps: dip-drawing, spin-coating, knife-coating, roll-coating.
9. The method for preparing the all-solid-state inorganic electrochromic composite film system intelligent glass assembly according to claim 6 or 7, wherein the method comprises the following steps: the temperature of the heat treatment in the step (3) is 150-400 ℃.
CN202111124959.2A 2021-09-25 2021-09-25 All-solid-state inorganic electrochromic composite film system intelligent glass assembly and preparation method thereof Pending CN113885265A (en)

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