CN112748619A - Color-changing glass - Google Patents
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- CN112748619A CN112748619A CN201911044159.2A CN201911044159A CN112748619A CN 112748619 A CN112748619 A CN 112748619A CN 201911044159 A CN201911044159 A CN 201911044159A CN 112748619 A CN112748619 A CN 112748619A
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- 239000011521 glass Substances 0.000 title claims abstract description 84
- 239000010410 layer Substances 0.000 claims abstract description 129
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 239000010416 ion conductor Substances 0.000 claims abstract description 14
- 239000011241 protective layer Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims description 29
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 229910052715 tantalum Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 229910052741 iridium Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 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
- 239000005315 stained glass Substances 0.000 claims 3
- 238000012360 testing method Methods 0.000 description 24
- 238000000034 method Methods 0.000 description 20
- 230000008569 process Effects 0.000 description 17
- 239000013077 target material Substances 0.000 description 17
- 238000000151 deposition Methods 0.000 description 16
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- 238000004544 sputter deposition Methods 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 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 8
- 229910052786 argon Inorganic materials 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000007747 plating Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- GDMRBHLKSYSMLJ-UHFFFAOYSA-N [F].O=[Si] Chemical compound [F].O=[Si] GDMRBHLKSYSMLJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
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- 229910010293 ceramic material Inorganic materials 0.000 description 2
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- -1 etc.) Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 239000006121 base glass Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
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- 230000007547 defect Effects 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
- 238000010030 laminating Methods 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
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- 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
- G02F1/153—Constructional details
- G02F1/1533—Constructional details structural features not otherwise provided for
-
- 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
Abstract
The embodiment of the invention discloses color-changing glass, which comprises a substrate glass layer, and a first transparent conducting layer, a main color changing layer, an auxiliary color changing layer, an ion conductor layer, a second transparent conducting layer and a top protective layer which are sequentially arranged on the substrate glass layer. The color-changing glass can improve the color-changing uniformity of the color-changing glass in large-area product devices.
Description
Technical Field
The invention relates to the technical field of glass, in particular to color-changing glass.
Background
In the current industrialization process, the color-changing glass such as electrochromic glass 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, due to the large-area non-uniform color change, short cycle life and the like, the color change function near the electrode is seriously attenuated or even does not change color after the cycle is carried out for a certain number of times, thereby greatly influencing the application of the electrode in engineering.
Disclosure of Invention
In order to solve the above problems, embodiments of the present invention provide a color-changing glass, so as to improve color-changing uniformity of the color-changing glass in a large-area product device.
Specifically, the embodiment of the invention provides color-changing glass, which comprises a substrate glass layer, and a first transparent conductive layer, a main color layer, an auxiliary color-changing layer, an ion conductor layer, a second transparent conductive layer and a top protective layer which are sequentially arranged on the substrate glass layer.
In one embodiment of the present invention, the material of the primary coloring barrier layer is selected from oxides of at least two combinations of W, Mo, Nb, Ti and Ta, and the thickness of the primary coloring barrier layer is greater than 30nm and less than or equal to 500 nm.
In one embodiment of the present invention, the material of the auxiliary coloration layer is selected from oxides of at least two combinations of Ni, V, Co, Ir, Fe, Mn.
In one embodiment of the present invention, the thickness of the auxiliary coloration layer is greater than 20nm and equal to or less than 500 nm.
In one embodiment of the present invention, the thickness of the first transparent conductive layer is 1 to 1100 nm; the thickness of the second transparent conducting layer is 10-1000 nm.
In one embodiment of the present invention, the thicknesses of the first transparent conductive layer and the second transparent conductive layer are respectively greater than 10nm and equal to or less than 300 nm.
In one embodiment of the present invention, the materials of the first transparent conductive layer and the second transparent conductive layer are respectively selected from one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO, Ag.
In one embodiment of the invention, the material of the ion conductor layer is selected from one or a combination of at least two of H, Li, Na, K and Mg; the thickness of the ion conductor layer is greater than 10nm and less than or equal to 100 nm.
In one embodiment of the invention, the material of the top protective layer is selected from an oxide or nitride or oxynitride of one of Si, Ti, Zn, Sn, Nb, Ta.
In one embodiment of the invention, the thickness of the top protective layer is 0.2-100 nm.
The technical scheme has the following advantages: the color-changing glass provided by the embodiment of the invention adopts a specific film structure with the adjacent main color-changing layer and the adjacent auxiliary color-changing layer, can actively adjust energy-saving parameters according to environmental changes, improves the color-changing uniformity of electrochromic products in large-area product devices, and can be used for replacing building glass, automobile glass, aviation glass, decorative glass and the like.
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 a photochromic glass according to an embodiment of the present invention.
FIG. 2 is a schematic flow chart of a method for preparing a photochromic glass according to an embodiment of the present invention.
FIG. 3a is a graph showing the visible light transmittance spectra of the test sample 5 of the present invention at different color-changing positions.
Fig. 3b is a schematic diagram of the performance variation of the test sample 5 in different color-changing gears according to the present 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 all-inorganic vacuum-coated color-changeable glass 900. The color-changing glass 900 is, for example, electrochromic glass. The color-changing glass 900 includes, for example, a substrate glass layer 10, and a first transparent conductive layer 11, a main color-changing layer 12, an auxiliary color-changing layer 13, an ion conductor layer 14, a second transparent conductive layer 20, and a top protective layer 30, which are sequentially disposed on the substrate glass layer 10.
The photochromic glass provided by the embodiment of the invention adopts a specific film structure adjacent to the main photochromic layer and the auxiliary photochromic layer, can actively adjust energy-saving parameters according to environmental changes, and improves the photochromic uniformity of the photochromic glass in large-area product devices.
The substrate glass layer 10 may be float glass, ultra-white glass, high-alumina glass, medium-alumina glass, various colored glass (such as gray glass, green glass, lake blue glass, etc.), PET (Polyethylene terephthalate) film, etc. The thickness of the base glass layer 10 may be, for example, 0.02 to 25 mm.
The material of the first transparent conductive layer 11 is an inorganic color-changing material. The inorganic color-changing material is 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. The thickness of the first transparent conductive layer 11 is 1 to 1100 nm. Preferably, the thickness of the first transparent conductive layer is greater than 10nm and equal to or less than 300 nm. Preferably, the thickness of the first transparent conductive layer is greater than 10nm and equal to or less than 300 nm.
The main color changing layer 12 is a solar spectrum adjusting functional layer. The main color changing layer 12 is made of inorganic color changing material. The inorganic colour change material may for example be selected from oxides of at least two combinations of W, Mo, Nb, Ti, Ta, e.g. oxides of any two combinations of W, Mo, Nb, Ti, Ta, such as WMoOx, wnbo x, or oxides of the three combinations WMoTiOx, WNbTaOx, even more combinations. The stoichiometric ratio of the oxide may be sufficient oxygen or less than the stoichiometric ratio of oxygen. The thickness of the main dichroic layer 12 is greater than 30nm and less than or equal to 500 nm.
The material of the auxiliary discoloring layer 13 is selected from oxides of at least two combinations of Ni, V, Co, Ir, Fe and Mn. In particular, the material of the auxiliary coloration layer 13 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. The thickness of the auxiliary color-changing layer 13 is greater than 20nm and equal to or less than 500 nm.
The material of the ion conductor layer 14 is selected from: H. one or the combination of at least two of Li, Na, K and Mg. H. The combination of elements in Li, Na, K, Mg includes, for example, a combination of two elements such as Li and Na, a combination of three elements such as Na, K, Mg, and even more. The thickness of the ion conductor layer 14 is greater than 10nm and equal to or less than 100 nm.
The material of the second transparent conductive layer 20 is an inorganic color-changing material. The inorganic color-changing material is selected from one or any 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 thickness of the second transparent conductive layer 20 is 10-1000 nm. Preferably, the thickness of the second transparent conductive layer 20 is greater than 10nm and equal to or less than 300 nm.
The material of the top protective layer 30 is selected from an oxide or nitride or oxynitride of one of Si, Ti, Zn, Sn, Nb, and Ta. The thickness of the top protective layer is 0.2-100 nm. Preferably, the material of the top protective layer 30 is Si3N4。Si3N4The ceramic material is a high-temperature ceramic material, has high hardness, high melting point and stable chemical property, has strong corrosion resistance, mechanical scratch resistance and high-temperature oxidation resistance, and can play a good role in protection when being used as a top protective layer.
In addition, the embodiment of the invention also provides a preparation method of the color-changing glass, for example, the preparation method is used for preparing the color-changing glass 900. The method for preparing the color-changing glass comprises the following steps:
s11: a substrate glass layer is provided. And cleaning and drying the substrate glass layer.
S12: plating a first transparent conductive layer on the substrate glass layer. Specifically, the substrate glass layer 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 first preset vacuum sputtering gas pressure. The first predetermined 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: plating a main color changing layer 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) placing the target material under a second preset vacuum sputtering pressure for deposition to obtain the main transformer color layer. The second predetermined vacuum sputtering pressure is, for example, 1.0E-3～9.0E-3mbar. Preferably, the main color layer can also be plated by a plurality of target positions at the same time, so that better bonding force between the film layers can be obtained. The process gases employed by the plurality of target sites may or may not be uniform.
S14: plating an auxiliary color changing layer on the main color changing layer. Specifically, oxides of at least two combinations of Ni, V, Co, Ir, Fe and Mn are used as target materials, and the target materials are deposited under the condition of third preset vacuum sputtering air pressure to obtain the auxiliary discoloring layer. The third predetermined vacuum sputtering pressure is, for example, 1.0E-3～9.0E-3mbar. The stoichiometric ratio of the oxide in the target material may be sufficient oxygen or less than the stoichiometric ratio of oxygen. Preferably, the auxiliary color-changing layer can be plated by a plurality of target positions at the same time so as to obtain better bonding force between the film layers. The process gas ratios employed for the plurality of target sites may be non-uniform.
S15: and plating an ion conductor layer on the auxiliary color changing 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 fourth preset vacuum sputtering air pressure condition to obtain the ion conductor layer. The fourth predetermined vacuum sputtering pressure is, for example, 1.0E-3～9.0E-3mbar. Also, preferably, the ion conductor layer can be plated with multiple target sites simultaneously to achieve better bonding force between the films. The process gas ratios employed for the plurality of target sites may be non-uniform.
S16: plating a second transparent conductive layer on the ion conductor layer. One of FTO, ITO, IGZO, AZO, GZO and AgAnd (3) taking one or a combination of at least two as a target material, and depositing the target material under a fifth preset vacuum sputtering pressure to obtain a second transparent conductive layer. The fifth predetermined vacuum sputtering pressure is, for example, 1.0E-3～9.0E-3mbar. 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 plating a top protective layer on the second transparent conductive layer. And taking an 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 sixth preset vacuum sputtering pressure to obtain the top protective layer. The sixth predetermined vacuum sputtering pressure is, for example, 1.0E-3～9.0E-3mbar. Also, preferably, the auxiliary color-changing layer can be plated with multiple target sites simultaneously to achieve better bonding force between the layers. The process gas ratios employed for the plurality of target sites may be non-uniform.
S18: and (6) heat treatment. Specifically, a vacuum heat treatment and annealing process is performed, wherein the heat treatment temperature is, for example, 300-.
S19: and (5) carrying out pre-vacuum transition and parallel connection of electrodes to finish the preparation of the color-changing 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 color-changing glass with more neutral color-changing can be applied to the fields of building glass outer walls, interior decoration, automobile skylight glass, automobile side window glass, automobile rear windshield glass, automobile front windshield glass, automobile rearview mirrors, high-speed rail windows, airplane suspension windows, sunlight rooms, sunglasses, ski goggles and the like which need light-adjusting. The photochromic glass provided by the embodiment of the invention adopts a specific film structure, a photochromic layer and an auxiliary photochromic layer material which are adjacent to the main photochromic layer and the auxiliary photochromic layer, can actively adjust energy-saving parameters according to environmental changes, and improves the photochromic uniformity of the photochromic glass in large-area product devices. Moreover, because each layer can be formed by adopting a magnetron reactive sputtering deposition method during the production of the color-changing glass, the multiple entering and exiting of coating equipment in the production process can be avoided, the production process is simplified, the production cost can be reduced, and the production efficiency can be improved.
The process for producing the color-changeable glass will be described in detail below by way of a specific example.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The utility model provides a glass discolours, its membranous layer structure outwards is in proper order by substrate glass layer: substrate glass layer/ITO (150nm)/WMoOx (200nm)/NiVOx (80nm)/Li (40nm)/ITO (120nm)/Si3N4(20nm)。
The process for preparing the color-changing glass sequentially comprises the following steps:
(1) cleaning and drying the substrate glass layer, scribing a line by laser, cleaning and drying again, and placing in a vacuum sputtering area;
(2) depositing an ITO layer on a substrate glass layer by adopting a magnetron sputtering mode, wherein a target material is an ITO rotating target, a power supply is a direct current or intermediate frequency power supply, the frequency is 2000-40000Hz, the power is 1-30 KW, a process gas is argon, and the ITO layer is deposited 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 on the ITO layer by adopting a magnetron sputtering modeSi3N4The 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.
(8) Annealing process, laser scribing process, electrode layout and wiring, testing and laminating process.
In addition, the embodiment of the invention also tests the performance of 6 kinds of color-changing glass. The parameters of 12 test samples of 6 kinds of discolored glass are shown in Table 1. Wherein, the 1 st is 2 test samples of the color-changing glass in the prior art, the other 5 test samples are 10 test samples of the color-changing glass provided by the invention, and the materials of the main color-changing layer and the first auxiliary color-changing layer are different. The comparative data of the performance of the test samples under the same test conditions in different states are shown in table 2. Further, in this embodiment, the test sample 5 is tested at different color-changing positions, and the obtained performance parameters are shown in table 3 and fig. 3a and 3 b.
TABLE 16 parameter Table of test samples
TABLE 26 table of Performance parameters of the test specimens in different states
| Status of state | T | a*t | b*t | a*g | b*g | a*f | b*f |
| Transparent state of the prior art sample | 51.43 | -5.38 | 7.83 | -6.32 | 8.38 | 5.35 | 20.78 |
| State of the art sample staining | 5.6 | -8.55 | -30.54 | -7.54 | -10.58 | 14.36 | -17.30 |
| Test sample 1 clear state | 60.2 | -7.44 | 7.38 | 11.69 | -7.9 | 14.55 | -9.98 |
| Test sample 1 colored state | 1.1 | -0.76 | 1.77 | -0.48 | 4.27 | -6.24 | -11.79 |
| |
59.8 | -5.49 | -1.42 | -0.36 | -2.91 | 9.66 | 0.4 |
| |
3.2 | -0.79 | 1.77 | -0.48 | 4.33 | -6.15 | -11.67 |
| Test sample 3 clear state | 61.3 | -4.92 | -0.85 | 0.24 | -2.64 | 9.93 | 0.67 |
| Test sample 3 colored state | 1.9 | -0.86 | 1.7 | -0.52 | 4.36 | -6.22 | -11.74 |
| |
64.9 | -5.22 | -1.45 | -0.06 | -2.54 | 9.93 | 0.67 |
| |
1.59 | -1.1 | 1.46 | -0.76 | 4.12 | -6.46 | -11.98 |
| Test sample 5 transparent state | 66.62 | -7.24 | 7.58 | 11.99 | -7.70 | 14.45 | -9.78 |
| Test sample 5 colored state | 1.93 | 1.32 | -4.43 | 1.15 | 3.52 | -2.32 | 19.91 |
TABLE 3 Performance parameter Table for test sample 5 at different color-changing gears
As is apparent from tables 2 and 3 and fig. 3a and 3b, the color of the photochromic glass of the examples of the present invention is more excellent than that of the photochromic glass of the prior art, the visible light transmittance T of the photochromic glass of the prior art ranges from 51.43% to 5.6%, and the visible light transmittance of the photochromic glass of the examples of the present invention ranges from 66.62% to 1.93%, that is, the transmittance is increased. In addition, the visible light transmission color a x t, b x t of the photochromic glass provided by the embodiment of the invention surrounds the vicinity of the neutral color, and is nearly colorless, while the product of the photochromic glass in the prior art is yellow before transmitting the photochromic glass, transmits b x t and reaches 7.83, and displays blue b x t and reaches-30.54 after being discolored. The outdoor colors a x g and b x g of the embodiment of the invention are neutral, but the color of the color-changing glass in the prior art is relatively insufficient. Obviously, the color of the color-changing glass provided by the embodiment of the invention is more stable in the preparation process and the subsequent color-changing use process, and the large-area color uniformity is better.
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 color-changing glass is characterized by comprising a substrate glass layer, and a first transparent conducting layer, a main color changing layer, an auxiliary color-changing layer, an ion conductor layer, a second transparent conducting layer and a top protective layer which are sequentially arranged on the substrate glass layer.
2. The photochromic glass of claim 1, wherein the material of the primary photochromic layer is selected from oxides of at least two of W, Mo, Nb, Ti and Ta, and the thickness of the primary photochromic layer is greater than 30nm and less than or equal to 500 nm.
3. The photochromic glass of claim 1, wherein the material of the auxiliary photochromic layer is selected from oxides of at least two of Ni, V, Co, Ir, Fe and Mn.
4. The photochromic glass of claim 1, wherein the thickness of the auxiliary photochromic layer is greater than 20nm and equal to or less than 500 nm.
5. The stained glass according to claim 1, wherein the thickness of the first transparent conductive layer is 1-1100 nm; the thickness of the second transparent conducting layer is 10-1000 nm.
6. The color-changing glass according to claim 5, wherein the thicknesses of the first transparent conductive layer and the second transparent conductive layer are each greater than 10nm and equal to or less than 300 nm.
7. The stained glass according to claim 1, wherein the materials of the first transparent conductive layer and the second transparent conductive layer are respectively selected from one or a combination of at least two of FTO, ITO, IGZO, AZO, GZO and Ag.
8. The stained glass according to claim 1, wherein the material of the ion conductor layer is selected from one or a combination of at least two of H, Li, Na, K and Mg; the thickness of the ion conductor layer is greater than 10nm and less than or equal to 100 nm.
9. Changing glass according to claim 1, characterised in that the material of the top protective layer is selected from the group consisting of oxides or nitrides or oxynitrides of one of Si, Ti, Zn, Sn, Nb, Ta.
10. Changing glass according to claim 1, characterised in that the thickness of the top protective layer is 0.2-100 nm.
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| CN104898344A (en) * | 2015-05-08 | 2015-09-09 | 上方能源技术(杭州)有限公司 | All-solid state electrochromic device preparation method and prepared electrochromic glass |
| CN109613781A (en) * | 2019-02-02 | 2019-04-12 | 张玲 | The full-inorganic solid-state electrochromic mould group of the conductive film containing inorganic transparent |
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| US20100132988A1 (en) * | 2006-11-03 | 2010-06-03 | Saint-Gobain Glass France | Highly electrically conductive transparent layer with a metal grid having optimized electrochemical resistance |
| US20130010347A1 (en) * | 2010-01-08 | 2013-01-10 | Kazuki Tajima | All-solid-state reflective dimming electrochromic element sealed with protective layer, and dimming member comprising the same |
| US20120033287A1 (en) * | 2010-08-05 | 2012-02-09 | Soladigm, Inc. | Multi-pane electrochromic windows |
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Application publication date: 20210504 |