CN113064308A - Electric control toning glass - Google Patents
Electric control toning glass Download PDFInfo
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- CN113064308A CN113064308A CN201911275014.3A CN201911275014A CN113064308A CN 113064308 A CN113064308 A CN 113064308A CN 201911275014 A CN201911275014 A CN 201911275014A CN 113064308 A CN113064308 A CN 113064308A
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- ion conductor
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- 239000011521 glass Substances 0.000 title claims abstract description 44
- 239000010410 layer Substances 0.000 claims abstract description 200
- 239000010416 ion conductor Substances 0.000 claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000011241 protective layer Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims description 32
- 229910052758 niobium Inorganic materials 0.000 claims description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 229910052741 iridium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 230000008859 change Effects 0.000 abstract description 8
- 239000013077 target material Substances 0.000 description 30
- 238000000151 deposition Methods 0.000 description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 238000000034 method Methods 0.000 description 19
- 239000007789 gas Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 14
- 239000001301 oxygen Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 14
- 238000004544 sputter deposition Methods 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 10
- 238000001755 magnetron sputter deposition Methods 0.000 description 10
- 230000008021 deposition Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- GDMRBHLKSYSMLJ-UHFFFAOYSA-N [F].O=[Si] Chemical compound [F].O=[Si] GDMRBHLKSYSMLJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Images
Classifications
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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
-
- 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
-
- 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
Abstract
The embodiment of the invention discloses an electric control toning glass, which comprises a substrate, and a first transparent conducting layer, a first main toning layer, a first ion conductor layer, a first auxiliary toning layer, a second transparent conducting layer, a second auxiliary toning layer, a second ion conductor layer, a second main toning layer, a third transparent conducting layer and a protective layer which are sequentially formed on the same side of the substrate. The electrically-controlled toning glass can improve the color change uniformity of the glass in large-area product devices.
Description
Technical Field
The invention relates to the technical field of glass, in particular to electric control toning glass.
Background
In the current industrialization process of the electric control toning glass, the electric control toning product has a plurality of defects on the color changing uniformity and the color changing cycle life of large-area product devices, and the inorganic color changing material is mainly WO3A material. WO3The material is a well-known high-efficiency cathode color-changing material, and WO is controlled through chemical oxidation and reduction reactions3The valence state change of the medium W can realize the absorption regulation and control effect on the spectrum. However, the existing electric control color mixing products have the defects of large-area non-uniform color change, short cycle life and the like, and after the products are circulated for a certain number of times, the color changing function near the electrode is seriously attenuated or even does not change color, thereby greatly influencing the application of the products in engineering.
Disclosure of Invention
In order to solve the above problems, embodiments of the present invention provide an electrically controlled toning glass to improve the color change uniformity of the electrically controlled toning glass in large-area product devices.
Specifically, the embodiment of the invention provides an electronic control toning glass, which comprises a substrate, and a first transparent conducting layer, a first main toning layer, a first auxiliary toning layer, a first ion conductor layer, a second transparent conducting layer, a second main toning layer, a second ion conductor layer, a second auxiliary toning layer, a third transparent conducting layer and a protective layer which are sequentially formed on the same side of the substrate.
In one embodiment of the present invention, the materials of the first and second main color modulation layers are respectively selected from oxides of at least two combinations of W, Mo, Nb, Ti, and Ta.
In one embodiment of the present invention, the materials of the first main color modulation layer and the second main color modulation layer are the same.
In one embodiment of the present invention, the first main color modulation layer and the second main color modulation layer have a thickness ranging from 30nm to 500nm, respectively.
In one embodiment of the present invention, the materials of the first auxiliary color modulation layer and the second auxiliary color modulation layer are respectively selected from oxides of combinations of at least two elements of Ni, V, Co, Ir, Fe, and Mn.
In one embodiment of the invention, the materials of the first and second auxiliary color modulation layers are the same.
In one embodiment of the present invention, the first and second auxiliary color modulation layers have a thickness ranging from 20nm to 500nm, respectively.
In one embodiment of the present invention, the materials of the first transparent conductive layer, the second transparent conductive layer and the third transparent conductive layer are respectively selected from one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO and Ag; the thickness ranges of the first transparent conducting layer and the second transparent conducting layer are respectively 1-1100 nm; the thickness range of the third transparent conducting layer is 10-1000 nm.
In one embodiment of the present invention, the materials of the first ion conductor layer and the second ion conductor layer are respectively selected from one or a combination of at least two of H, Li, Na, K and Mg; the thickness ranges of the first ion conductor layer and the second ion conductor layer are 10nm-100nm respectively.
In one embodiment of the present invention, the material of the protective layer is selected from an oxide or nitride or oxynitride of one of Si, Ti, Zn, Sn, Nb, Ta; the thickness range of the protective layer is 0.2-100 nm.
One or more of the above technical solutions may have the following advantages or beneficial effects: the electric control toning glass provided by the embodiment of the invention adopts a specific film layer structure in which the main toning layer and the auxiliary toning layer are adjacent and are in interval combination with each other, can actively adjust energy-saving parameters according to environmental changes, and improves the color change uniformity of an electric control toning product in a large-area product device. In addition, the electrically-controlled color-mixing glass prepared by the preparation method provided by the embodiment of the invention through a specific preparation process has more stable color and better large-area color uniformity, simplifies the production process, reduces the production cost and improves the production efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an electrically controlled toning glass provided by an embodiment of the invention.
Fig. 2 is a schematic flow chart of a method for preparing the electrically-controlled toning glass provided by the embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.
As shown in fig. 1, an embodiment of the present invention provides an electrically controlled toning glass 700. The electrically controlled toning glass 700 includes, for example, a substrate 10, and a first transparent conductive layer 11, a first main toning layer 12, a first auxiliary toning layer 13, a first ion conductor layer 14, a second transparent conductive layer 21, a second main toning layer 22, a second ion conductor layer 23, a second auxiliary toning layer 24, a third transparent conductive layer 30, and a protective layer 40, which are formed in this order on the same side of the substrate 10.
The electric control toning glass provided by the embodiment of the invention adopts a specific film layer structure combining adjacent arrangement of the main and auxiliary toning layers and interval arrangement of the main and auxiliary toning layers, can realize active adjustment of energy-saving parameters according to environmental changes, and improves the color change uniformity of an electric control toning product in large-area product devices.
Specifically, the substrate 10 may be, for example, a glass substrate or other substrate having a similar function. Specifically, the glass substrate is, for example, float glass, ultra-white glass, a high-alumina glass material, or the like. The thickness of the substrate 10 may range, for example, from 0.05 to 25 mm.
The materials of the first transparent conductive layer 11, the second transparent conductive layer 21, and the third transparent conductive layer 30 are respectively selected from one or a combination of at least two of FTO (fluorine silicon oxide), ITO (indium tin oxide), IGZO (indium gallium zinc oxide), AZO (aluminum zinc oxide), GZO (gallium zinc oxide), and Ag. The combination of at least two herein may be, for example, a combination of two such as AZO and GZO, or a combination of three such as FTO, ITO, GZO, even more, and the like. Preferably, at least two of the first transparent conductive layer 11, the second transparent conductive layer 21, and the third transparent conductive layer 30 are made of the same material. The thickness ranges of the first transparent conductive layer 11 and the second transparent conductive layer 21 are 1-1100nm respectively. The thickness of the third transparent conductive layer 30 ranges from 10 to 1000 nm. Preferably, the thickness of the first transparent conductive layer 11, the second transparent conductive layer 21 and the third transparent conductive layer 30 are in the range of 10-300nm, respectively. Further preferably, at least two of the first transparent conductive layer 11, the second transparent conductive layer 21, and the third transparent conductive layer 30 have the same thickness.
The first main color modulation layer 12 and the second main color modulation layer 22 are main spectrum adjustment function layers. The materials of the first main color modulation layer 12 and the second main color modulation layer 22 are inorganic color-changing materials respectively. The inorganic colour change material may for example be selected from oxides of combinations of at least two elements of W, Mo, Nb, Ti, Ta, for example oxides of any two of W, Mo, Nb, Ti, Ta such as WMoOx, wnbo x, or oxides of the three combinations WMoTiOx, WNbTaOx, or even more combinations. The stoichiometric ratio of the oxide may be sufficient oxygen or less than the stoichiometric ratio of oxygen. Preferably, the materials of the first and second main color modulation layers 12 and 22 are the same. The first main color modulation layer 12 and the second main color modulation layer 22 have a thickness range of 30 to 500nm, respectively. Preferably, the thicknesses of the first and second main color modulation layers 12 and 22 are equal.
The materials of the first ion conductor layer 14 and the second ion conductor layer 23 are respectively selected from one or a combination of at least two of H, Li, Na, K, and Mg, for example, a combination of two thereof such as Li and Na, a combination of three thereof such as Na, K, and Mg, and even more. Preferably, the materials of the first ion conductor layer 14 and the second ion conductor layer 23 are the same. The thicknesses of the first ion conductor layer 14 and the second ion conductor layer 23 are respectively 10nm-100 nm. Preferably, the thicknesses of the first ion conductor layer 14 and the second ion conductor layer 23 are equal.
The first auxiliary color adjusting layer 13 and the second auxiliary color adjusting layer 24 are spectrum auxiliary adjusting function layers. The materials of the first auxiliary color adjusting layer 13 and the second auxiliary color adjusting layer 24 are respectively selected from oxides of at least two combinations of Ni, V, Co, Ir, Fe and Mn. Specifically, the materials of the first and second auxiliary color adjusting layers 13 and 24, respectively, may be, for example, a combination of two of Ni, V, Co, Ir, Fe, Mn such as NiVOx, NiCoOx, NiIrOx, NiFeOx, or a combination of three, or even a combination of more. The stoichiometric ratio of the oxide may be sufficient oxygen or less than the stoichiometric ratio of oxygen. Preferably, the materials of the first auxiliary color adjusting layer 13 and the second auxiliary color adjusting layer 24 are the same. The thickness ranges of the first auxiliary color adjusting layer 13 and the second auxiliary color adjusting layer 24 are 20nm-500nm respectively. Preferably, the thicknesses of the first auxiliary color modulation layer 13 and the second auxiliary color modulation layer 24 are equal.
The material of the protective layer 40 is selected from an oxide or nitride or oxynitride of one of Si, Ti, Zn, Sn, Nb, and Ta. For example, the material of the protective layer 40 may be Si3N4。Si3N4The high-temperature ceramic material has the advantages of high hardness, high melting point, stable chemical property, strong corrosion resistance, mechanical scratch resistance and high-temperature oxidation resistance, and can play a good role in protection when being used as a protective layer. The thickness of the protective layer is 0.2-100 nm.
In addition, the embodiment of the invention also provides a preparation method of the electric control toning glass, for example, the preparation method is used for preparing the electric control toning glass 700. The preparation method of the electric control toning glass comprises the following steps:
s11: a substrate is provided. And cleaning and drying the substrate.
S12: a first transparent conductive layer is formed on a substrate. Specifically, the substrate is heated to a preset temperature, wherein the preset temperature range is, for example, 280-300 ℃, one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO, and Ag is used as a target material, and the first transparent conductive layer is obtained by deposition under a preset vacuum sputtering gas pressure. The preset vacuum sputtering pressure is, for example, 1.0E-3～9.0E-3mbar. Preferably, the first transparent conductive layer can also be a pre-prepared conductive film layer. This allows better index matching between the layers.
S13: a first main color modulation layer is formed on the first transparent conductive layer. The oxide of at least two of W, Mo, Nb, Ti and Ta is used as the target material. The stoichiometric ratio of the oxide may be sufficient oxygen or less than the stoichiometric ratio of oxygen. And (3) depositing the target material under a preset vacuum sputtering pressure to obtain a first main color control layer. Preferably, the first main color modulation layer may also be formed using a plurality of target sites at the same time, so that a better bonding force between the film layers may be obtained.
S14: a first auxiliary color modulation layer is formed on the first main color modulation layer. Specifically, oxide of at least two combinations of Ni, V, Co, Ir, Fe and Mn is used as a target material, and the target material is deposited under the condition of preset vacuum sputtering air pressure to obtain a first auxiliary color control layer. The stoichiometric ratio of the oxide in the target material may be sufficient oxygen or less than the stoichiometric ratio of oxygen. Preferably, the first auxiliary toning layer can also be formed by adopting a plurality of target positions at the same time so as to obtain better binding force between the film layers.
S15: a first ion conductor layer is formed on the first auxiliary color modulation layer. One or a combination of at least two of H, Li, Na, K and Mg is used as a target material, and the target material is deposited under the condition of preset vacuum sputtering air pressure to obtain a first ion conductor layer. Preferably, the first ion conductor layer can also be formed by using a plurality of target sites at the same time, so as to obtain better bonding force between films.
S16: and forming a second transparent conductive layer on the first ion conductor layer. Specifically, one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO and Ag is used as a target material, and the target material is deposited under the condition of preset vacuum sputtering air pressure to obtain the second transparent conductive layer. Preferably, the second transparent conductive layer can also be a pre-prepared conductive film layer. This allows better index matching between the layers.
S17: and forming a second main color modulation layer on the second transparent conductive layer. The oxide of at least two of W, Mo, Nb, Ti and Ta is used as the target material. And (3) depositing the target material under a preset vacuum sputtering pressure to obtain a second main color control layer. Preferably, the second main color modulation layer can also be formed simultaneously using a plurality of target sites, so that a better bonding force between the film layers can be obtained.
S18: and forming a second ion conductor layer on the second main color modulation layer. And taking one or the combination of at least two of H, Li, Na, K and Mg as a target material, and depositing the target material under the condition of preset vacuum sputtering air pressure to obtain a second ion conductor layer. Preferably, the second ion conductor layer can also be formed by using a plurality of target sites at the same time, so as to obtain better bonding force between films.
S19: and forming a second auxiliary color modulation layer on the second ion conductor layer. Specifically, at least two oxides of Ni, V, Co, Ir, Fe and Mn are used as target materials, and the target materials are deposited under the condition of preset vacuum sputtering air pressure to obtain a second auxiliary color control layer. The stoichiometric ratio of the oxide in the target material may be sufficient oxygen or less than the stoichiometric ratio of oxygen. Preferably, the second auxiliary toning layer can also be formed by adopting a plurality of target positions at the same time so as to obtain better binding force between the film layers.
S20: and forming a third transparent conductive layer on the second auxiliary color adjusting layer. And taking one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO and Ag as a target material, and depositing the target material under a preset vacuum sputtering pressure to obtain the third transparent conductive layer. Preferably, the third transparent conductive layer can also be a conductive film layer prepared in advance. This allows better index matching between the layers.
S21: and forming a protective layer on the third transparent conductive layer. Taking oxide or nitride or oxynitride of one of Si, Ti, Zn, Sn, Nb and Ta as a target material, and depositing the target material under a preset vacuum sputtering pressure to obtain the protective layer. Preferably, the protective layer can also be formed simultaneously with multiple target sites to achieve better binding between the layers of the film.
In addition, the preparation method of the electric control toning glass provided by the embodiment of the invention can also comprise a heat treatment step. Specifically, a vacuum heat treatment and annealing process is performed, wherein the heat treatment temperature is, for example, 300-.
Furthermore, the method for preparing the electrically-controlled toning glass provided by the embodiment of the invention can also comprise pre-vacuum transition and parallel connection of electrodes to finish the preparation of the electrically-controlled toning glass. The pre-vacuum transition and the electrode connection can be completed by adopting the method in the prior art, and the details are not repeated here.
The following describes the process of preparing electrically controlled tinted glass in detail by means of a specific example.
[ EXAMPLES ]
The utility model provides an automatically controlled mixing of colors glass, its membranous layer structure outwards is in proper order by the base plate: substrate/ITO (150nm)/WMoOx (200nm)/NiVOx (80nm)/Li (40nm)/ITO (150nm)/WMoOx (200nm)/Li (40nm)/NiVOx (80nm)/ITO (120nm)/Si3N4(20nm)。
The process for preparing the electric control toning glass sequentially comprises the following steps:
(1) cleaning and drying the substrate, scribing a line by laser, cleaning and drying again, and placing the substrate in a vacuum sputtering area;
(2) depositing an ITO layer on a substrate in a magnetron sputtering mode, wherein the target material is an ITO rotating target, the power supply is direct current or a medium-frequency power supply with the frequency of 2000-40000Hz, the power is 1-30 KW, the process gas is argon, and the deposition is carried out at the temperature of 290 ℃;
(3) depositing a WMoOx layer on the ITO layer in a magnetron sputtering mode, wherein the used target material is a metal WMo planar target, the power supply is a direct-current power supply, the power is 1-30 KW, the process gas is a mixed gas of pure argon and oxygen, and after deposition, heating to 550 ℃ to enter the next coating area;
(4) depositing a NiVOx layer on the WMoOx layer in a magnetron sputtering mode, wherein the used target material is a metal NiV planar target, the power supply is a direct-current power supply, the power is 1-30 KW, the process gas is a mixed gas of pure argon and oxygen, and the temperature is raised to 550 ℃ after deposition at a corresponding temperature so as to enter a next coating area;
(5) depositing a Li layer on the NiVOx layer in a magnetron sputtering mode, wherein a target material is a Li rotary target, a power supply is an intermediate frequency or direct current power supply, the power is 1-30 KW, a process gas is argon, and the deposition is carried out at the temperature of 550 ℃;
(6) depositing an ITO layer on the Li layer in a magnetron sputtering mode, wherein the target material is an ITO rotating target, the power supply is a direct current or intermediate frequency power supply, the power is 1-30 KW, the process gas is argon, and the deposition is carried out at the temperature of 290 ℃;
(7) depositing a WMoOx layer on the ITO layer in a magnetron sputtering mode, wherein the used target material is a metal WMo planar target, the power supply is a direct-current power supply, the power is 1-30 KW, the process gas is a mixed gas of pure argon and oxygen, and after deposition, heating to 550 ℃ to enter the next coating area;
(8) depositing a Li layer on the WMoOx layer in a magnetron sputtering mode, wherein a target material is a Li rotating target, a power supply is an intermediate frequency or direct current power supply, the power is 1-30 KW, and a process gas is argon and is deposited at the temperature of 550 ℃;
(9) depositing a NiVOx layer on the Li layer in a magnetron sputtering mode, wherein a target material is a metal NiV plane target, a power supply is a direct-current power supply, the power is 1-30 KW, a process gas is a mixed gas of pure argon and oxygen, and the temperature is raised to 550 ℃ after deposition at a corresponding temperature so as to enter a next coating area;
(10) depositing an ITO layer on the NiVOx layer in a magnetron sputtering mode, wherein the target material is an ITO rotating target, the power supply is a direct current or intermediate frequency power supply, the power is 1-30 KW, the process gas is argon, and the deposition is carried out at the temperature of 290 ℃;
(11) depositing Si on the ITO layer by adopting a magnetron sputtering mode3N4The layer, used target are SiAl rotating target, the power is the intermediate frequency power, the power is 1 ~ 10KW, and process gas is the mist of argon gas and nitrogen gas, deposit at room temperature.
(12) Annealing process, laser scribing process, electrode layout and wiring, testing and laminating process.
In summary, the electrically-controlled color-adjusting glass provided by the embodiment of the invention adopts a specific film structure combining adjacent arrangement of the main and auxiliary color-adjusting layers and interval arrangement of the main and auxiliary color-adjusting layers, can actively adjust energy-saving parameters according to environmental changes, can improve the color-changing uniformity of the electrically-controlled color-adjusting glass in large-area product devices through adjustment and matching of an electric control system, has richer colors and wider color coordinate regions, and can be applied to the fields of automobile side window glass, high-speed train windows, airplane suspension windows, sunlight rooms, sunglasses, ski goggles and the like which need color adjustment. In addition, the preparation method of the electric control toning glass provided by the embodiment of the invention adopts a magnetron reactive sputtering deposition method to form each film layer, thereby avoiding multiple times of entering and exiting of coating equipment in the production process, simplifying the production process, further reducing the production cost and improving the production efficiency.
In addition, it should be understood that the foregoing embodiments are merely exemplary illustrations of the present invention, and the technical solutions of the embodiments can be arbitrarily combined and collocated without conflict between technical features and structural contradictions, which do not violate the purpose of the present invention.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The electric control toning glass is characterized by comprising a substrate, a first transparent conducting layer, a first main toning layer, a first auxiliary toning layer, a first ion conductor layer, a second transparent conducting layer, a second main toning layer, a second ion conductor layer, a second auxiliary toning layer, a third transparent conducting layer and a protective layer, wherein the first transparent conducting layer, the first main toning layer, the first ion conductor layer, the second transparent conducting layer, the second main toning layer, the second ion conductor layer, the second auxiliary toning layer, the third transparent conducting layer and the protective layer are.
2. The electrically controlled toning glass according to claim 1, wherein the materials of the first and second main toning layers are respectively selected from oxides of at least two combinations of W, Mo, Nb, Ti and Ta.
3. Electrically controllable tinted glass according to claim 2, characterized in that the material of the first main tinted layer and the second main tinted layer is the same.
4. The electrically controlled toning glass according to claim 1, wherein the first and second main toning layers have a thickness in the range of 30nm to 500nm, respectively.
5. The electrically controlled toning glass according to claim 1, wherein the materials of the first and second auxiliary toning layers are respectively selected from oxides of at least two element combinations of Ni, V, Co, Ir, Fe and Mn.
6. The electrically controlled toning glass according to claim 5, wherein the first and second auxiliary toning layers are made of the same material.
7. The electrically controlled toning glass according to claim 1, wherein the first and second auxiliary toning layers each have a thickness in the range of 20nm to 500 nm.
8. The electrically controlled toning glass according to claim 1, wherein the materials of the first transparent conducting layer, the second transparent conducting layer and the third transparent conducting layer are respectively selected from one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO and Ag; the thickness ranges of the first transparent conducting layer and the second transparent conducting layer are respectively 1-1100 nm; the thickness range of the third transparent conducting layer is 10-1000 nm.
9. The electrically controlled toning glass according to claim 1, wherein the materials of the first ion conductor layer and the second ion conductor layer are respectively selected from one or a combination of at least two of H, Li, Na, K and Mg; the thickness ranges of the first ion conductor layer and the second ion conductor layer are 10nm-100nm respectively.
10. Electrically controllable toning glass according to claim 1, characterised in that the material of the protective layer is selected from oxides or nitrides or oxynitrides of one of Si, Ti, Zn, Sn, Nb, Ta.
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| CN201911275014.3A CN113064308A (en) | 2019-12-12 | 2019-12-12 | Electric control toning glass |
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