CN114859612A - Aerogel composite electrochromic glass and preparation method thereof - Google Patents
Aerogel composite electrochromic glass and preparation method thereof Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 49
- 239000011521 glass Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 90
- 238000011049 filling Methods 0.000 claims abstract description 12
- 230000004888 barrier function Effects 0.000 claims abstract description 10
- 238000010345 tape casting Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 99
- 239000007789 gas Substances 0.000 claims description 88
- 238000004544 sputter deposition Methods 0.000 claims description 48
- 239000011248 coating agent Substances 0.000 claims description 44
- 238000000576 coating method Methods 0.000 claims description 44
- 238000005266 casting Methods 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 18
- 239000005329 float glass Substances 0.000 claims description 18
- 229910003002 lithium salt Inorganic materials 0.000 claims description 15
- 159000000002 lithium salts Chemical class 0.000 claims description 15
- 239000013077 target material Substances 0.000 claims description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 230000002745 absorbent Effects 0.000 claims description 11
- 239000002250 absorbent Substances 0.000 claims description 11
- 239000005341 toughened glass Substances 0.000 claims description 11
- 239000005340 laminated glass Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000002390 adhesive tape Substances 0.000 claims description 9
- 230000000873 masking effect Effects 0.000 claims description 9
- 238000002845 discoloration Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000004014 plasticizer Substances 0.000 claims description 8
- 239000003381 stabilizer Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 6
- 238000005546 reactive sputtering Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 5
- 229910001120 nichrome Inorganic materials 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 229920005549 butyl rubber Polymers 0.000 claims description 3
- 239000002274 desiccant Substances 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 3
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000004663 powder metallurgy Methods 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229940124543 ultraviolet light absorber Drugs 0.000 claims description 3
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000007766 curtain coating Methods 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 11
- 239000010410 layer Substances 0.000 description 97
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 5
- 238000004040 coloring Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 239000004965 Silica aerogel Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 238000003384 imaging method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000000007 visual effect Effects 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
- G02F1/1514—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
-
- 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
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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
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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
- G02F1/155—Electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
- Y02B80/22—Glazing, e.g. vaccum glazing
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides aerogel composite electrochromic glass and a preparation method thereof, wherein the aerogel composite electrochromic glass comprises a first substrate, a PVB tape casting film layer, a second substrate and an aerogel filling layer which are sequentially arranged, and the technical scheme is as follows: the first substrate comprises a first substrate, a first anti-reflection medium film layer, a barrier layer, a conducting layer, a first transparent conducting layer and a cathode color changing layer which are sequentially and compositely arranged, and the second substrate comprises a second substrate, a second anti-reflection medium film layer, a second transparent conducting film layer and an anode color changing layer which are sequentially and compositely arranged; the application discloses aerogel composite electrochromic glass solves the light transmittance control problem, and especially visible light and near infrared light are in different wavelength bands, and better realization is automatic regulation and control colour, is adjusted luminance and is adjusted the temperature.
Description
Technical Field
The invention belongs to the technical field of color-changing film glass, and particularly relates to aerogel composite electrochromic glass and a preparation method thereof.
Background
The color-changing glass can automatically adjust the transmittance of visible light and infrared light, meet the requirements of developing different energy-saving glasses in different latitude areas, and cannot meet the energy-saving requirements in winter and summer at the same time. And the electrochromic is a phenomenon that the polarity and the strength of an applied electric field cause reversible oxidation or reduction reaction of a material, so that the color of the material is changed. The electrochromic intelligent glass can adjust the transmittance of visible light and has a barrier effect on infrared light, so that the temperature of an interlayer region can be adjusted, and corresponding electrochromic devices comprise an intelligent window, a reflector, a display and the like according to the properties of adjustable transmission, adjustable reflection, and adjustable information display and radiation of the electrochromic material.
In recent years, energy saving and environmental protection are concerned, the temperature in buildings or vehicles is raised due to strong solar radiation, people can continuously think of trying to use air conditioners, the energy consumption applied to buildings accounts for the total energy consumption in the world in recent years, and the same building energy consumption also accounts for a larger proportion of the total energy consumption; the wavelength range of visible light is about 380-780 nm, the solar spectrum mainly comprises 300-2500 nm, and the energy is mainly concentrated in the wavelength range; light in the wavelength range of 780-2500 nm is called near infrared light, the wavelength energy of the part accounts for about 50% of the total energy of the solar spectrum, the part of light does not help human visual imaging, if a material can shield the near infrared light in an environment requiring a lower temperature, has high visible light transmittance, and can shield part of harmful ultraviolet rays, the material can play a role in reducing energy consumption of buildings and vehicles, and a more comfortable environment is provided.
Disclosure of Invention
In order to solve the problem of light transmission performance control, particularly to better realize automatic color regulation, light regulation and temperature regulation of visible light and near infrared light in different wavelength bands, the invention provides aerogel composite electrochromic glass.
The second purpose of the invention is to provide a preparation method of the aerogel composite electrochromic glass.
The invention discloses aerogel composite electrochromic glass, which comprises a first substrate, a PVB tape casting film layer, a second substrate and an aerogel filling layer which are sequentially arranged, and is characterized in that: the first substrate comprises a first substrate, a first anti-reflection medium film layer, a barrier layer, a conducting layer, a first transparent conducting layer and a cathode color changing layer which are sequentially and compositely arranged, and the second substrate comprises a second substrate, a second anti-reflection medium film layer, a second transparent conducting film layer and an anode color changing layer which are sequentially and compositely arranged.
Preferably, the first antireflection dielectric film layer is Nb 2 O 5 The barrier layer is a NiCr film layer, the conducting layer is an Ag layer, the first transparent conducting layer is an ITO film layer, and the cathode color changing layer is a WO film layer 3 And (5) film layer. The barrier layer is used for blocking water vapor from entering and can promote the silver layer of the conductive layer to be oxidized.
Preferably, the second antireflection dielectric film layer is TiO 2 The second transparent conductive film layer is an ITO layer, and the anode color changing layer is a NiO layer.
Preferably, the PVB casting film layer (3) is mainly composed of PVB resin, lithium salt, a plasticizer, an ultraviolet absorbent and a stabilizer, wherein the lithium salt is one or more of lithium perchlorate, lithium carbonate and lithium niobate. Through melt blending and extrusion, the dispersibility of lithium salt in a PVB base material is improved, and the concentration of lithium ions is stabilized, so that the conductivity of the material is controlled better.
Preferably, the aerogel filling layer comprises an aluminum frame and a toughened glass layer, and SiO is filled between the aluminum frame and the toughened glass layer 2 An aerogel.
Preferably, the cathode discoloration layer is doped WO 3 The film thickness is 450 nm and 600 nm.
Preferably, the anode discoloration layer is an NIO-doped film layer, and the thickness of the film is 200-300 nm.
Preferably, the PVB casting film layer is prepared by the following method:
(1) adding PVB resin (300-;
(2) in the extrusion casting process, the PVB conductive master batch is added into PVB resin according to the proportion of 20 percent to prepare the high-conductivity PVB film with the thickness of 1mm and the conductivity of 10 -5 -10 -7 S/cm。
Preferably, the first substrate is toughened or semi-toughened or non-toughened glass with the thickness of 3-10mm, and Bi is arranged on the first substrate 4 O 6 And the second substrate is toughened, semi-toughened or non-toughened glass and has a thickness of 3-10 mm. Is provided with Bi 4 O 6 The priming layer can effectively prevent water vapor from corroding the electrochromic layer, the service life is prolonged, and the product quality is guaranteed.
A preparation method of aerogel composite electrochromic glass comprises the following steps:
the method comprises the following steps: preparing a first substrate: selecting high-quality float glass, cleaning the float glass with deionized water, conveying the float glass to a magnetron sputtering coating machine, arranging an RF plasma cleaning device in a buffer chamber of the coating machine, and spraying an optical absorbent after plasma cleaning to prepare a first substrate;
step two, preparing the bottom layer Bi 4 O 6 Layer (b): the first substrate after the first step is sent into a coating area, a bismuth target is sputtered by magnetron sputtering, reactive sputtering is carried out by a direct current power supply, and Ar gas and O are used 2 As sputtering gas, the gas flow rate is 100SCCM:120SCCM, the film thickness is 20-40nm, and the bottom layer is obtained;
step three, preparing a first antireflection dielectric film layer: the substrate after the second step is sent to the next coating area, and is reactively sputtered by a direct current power supply, and Ar gas and O for selecting a high-refractive-index material Nb 2 As sputtering gas, gas flow 100SCCM:120SCCM to prepare a first anti-reflection dielectric film layer with the film thickness of 40-60 nm;
step four, preparing a barrier layer: the substrate after the third step is sent into the next coating area, a direct current power supply sputters a NiCr target, Ar gas is used as sputtering gas, the gas flow is 120SCCM, and the film thickness is 4-6 nm;
step five, preparing a conductive layer: and (5) conveying the substrate after the step four into a next coating area, sputtering an Ag target by using a direct-current power supply, using Ar as sputtering gas, and ensuring that the gas flow is 120SCCM and the film thickness is 8-10 nm.
Step six, preparing a first transparent conductive layer: the substrate after the step five is sent into the next coating area, ITO target material is sputtered in an alternating current mode, the temperature in the cavity is 300-450 ℃, and Ar gas and O gas in the step 2 As sputtering gas, gas flow 100SCCM:120SCCM, the film thickness is 80-100 nm;
step seven, preparing a cathode discoloring layer:
(1) and adjusting the target material: co-sputtering by magnetron sputtering method with sputtering sources at 120 deg.C, loading tungsten and molybdenum targets on the sputtering sources, and using Ar gas and O 2 As sputtering gas, the gas flow rate was 100SCCM:120SCCM, adjusting the power of each target to obtain different doping proportions;
(2) and preparing a doped target material: mixing WO 3 、MO 3 The powder is mixed according to the doping proportion in the fourth step, and is prepared into doped WO by adopting a powder metallurgy method 3 A target material;
(3) and masking: covering two adjacent sides of the substrate subjected to the sixth step by using an oxygen-free adhesive tape with the width of 10 mm;
(4) preparing a cathode discoloring layer: the substrate after the mask is finished is sent to the next coating area to be coated with the doped WO 3 Film with Ar gas, O 2 As sputtering gas, the gas flow rate was 100SCCM: 10SCCM to obtain doped WO 3 A film; the film thickness is 450-;
obtaining a first substrate after the seventh step;
step eight, preparing a second substrate of the second substrate: selecting high-quality float glass, cleaning the float glass with deionized water, conveying the float glass to a magnetron sputtering coating machine, arranging an RF plasma cleaning device in a buffer chamber of the coating machine, and spraying an optical absorbent after plasma cleaning to prepare a second substrate;
step nine, preparing a second anti-reflection medium film layer: sending the second substrate after the step eight into a coating area, carrying out magnetron sputtering on titanium, carrying out reactive sputtering by using a direct-current power supply, using Ar gas and O2 as sputtering gases, wherein the gas flow is 100SCCM:120SCCM, and the film thickness is 20-40 nm;
step ten, preparing a second transparent conductive layer: the substrate after the ninth step is sent to the next coating area for alternating current sputtering of the ITO target material, the chamber is heated to 300 ℃ and 450 ℃, and Ar gas and O in the step 2 As sputtering gas, gas flow 100SCCM:120SCCM, film thickness 150-;
eleven, masking: covering two adjacent sides of the substrate after the step ten by using an oxygen-free adhesive tape with the width of 10 mm;
step twelve, preparing an anode color changing layer: feeding the substrate after the mask of the step eleven into a next coating area, carrying out direct current sputtering on a nickel target, and preparing an NIO-doped thin film by using Ar gas as sputtering gas with the gas flow of 120 SCCM; the film thickness is 200-300 nm;
completing the step twelve to obtain a second substrate;
step thirteen, laying electrodes: removing the masking adhesive tapes of the first substrate and the second substrate, coating conductive silver paste, and leading out a conductive wire;
fourteen, preparing a PVB casting film layer;
step fifteen, packaging the electrochromic glass: sequentially stacking a first substrate, a PVB tape casting film layer and a second substrate in sequence, and then preparing the electrochromic laminated glass by adopting autoclave autoclaved molding;
sixthly, filling SiO (silicon dioxide) in an area enclosed by the aluminum frame and the toughened glass layer by using an aluminum frame (the aluminum frame contains a drying agent) which is coated with butyl rubber and has the thickness of 8-10mm on the electrochromic laminated glass after the step fifteen is finished 2 And filling the aerogel with hollow structural adhesive to form the aerogel composite electrochromic glass.
Compared with the prior art, the invention has the following advantages:
(1) the aerogel composite electrochromic glass has the advantages that the electrochromic layer is divided into the cathode electrochromic layer and the anode electrochromic layer due to different pressurizing, when voltage is applied, ions are injected into the layers to generate a color change phenomenon, under the action of an external electric field, the cathode electrochromic film layer and the anode electrochromic film layer can be simultaneously colored, so that the colored color is deepened, the bleached transmittance is higher, the silica aerogel is a novel amorphous solid material which is gathered by nanometer-level particles and takes air as a dispersion medium, the solvent in the original framework is removed from the aerogel through a special production process, thereby having the advantages of high porosity, translucence, low refractive index and the like, and combining the functions of the cathode and anode discoloring layers by utilizing the characteristics of the aerogel, by adjusting the filling amount of the aerogel, the visible light transmittance of the aerogel glass is better applied to the temperature and light adjustment of the composite electrochromic glass; electrochromic and aerogel are compounded, and active energy-saving and passive energy-saving compounding is realized. When the color-changing glass is used for electrochromic laminated glass, different colors can be obtained by introducing different voltages to the electrochromic glass, so that the efficient selectivity of a spectrum is ensured, and the colors, the light modulation and the temperature regulation can be automatically regulated and controlled;
(2) according to the preparation method of the aerogel composite electrochromic glass, the nano silver layer is added on the bottom layer of the ITO film, so that the conductivity of the electrochromic glass is improved; the multiple dielectric layers are compounded, so that the fading state visible light transmittance of the electrochromic glass is greatly improved, and the visible light modulation range of the electrochromic glass is enlarged; the cathode and anode discoloring layers are covered with coating films, so that the acid-base etching of the film after the coating is reduced, and the conductivity of the electrode is improved.
Drawings
FIG. 1 shows the sequence of the layers of the electrochromic glass.
Detailed Description
The following description of the preparation method of an aerogel composite electrochromic glass according to the present invention with reference to examples 1 to 4 is provided:
a preparation method of aerogel composite electrochromic glass comprises the following steps:
the method comprises the following steps: preparation of the first substrate 11: selecting high-quality float glass, cleaning the float glass with deionized water, conveying the float glass to a magnetron sputtering coating machine, arranging an RF plasma cleaning device in a buffer chamber of the coating machine, and spraying an optical absorbent after plasma cleaning to prepare a first substrate 11;
step two, preparing the bottom layer Bi 4 O 6 Layer (b): the first substrate to complete the first step11, feeding the mixture into a coating area, carrying out magnetron sputtering on a bismuth target, carrying out reactive sputtering by using a direct current power supply, and carrying out Ar gas and O 2 As sputtering gas, the gas flow is 100SCCM to 120SCCM, and the film thickness is 20-40nm, so as to obtain a bottom layer;
step three, preparing a first antireflection dielectric film layer 12: the substrate after the second step is sent to the next coating area, and is reactively sputtered by a direct current power supply, and Ar gas and O for selecting a high-refractive-index material Nb 2 As sputtering gas, gas flow 100SCCM:120SCCM to prepare a first anti-reflection dielectric film layer 12 with the film thickness of 40-60 nm;
step four, preparing a barrier layer 13: the substrate after the third step is sent into the next coating area, a direct current power supply sputters a NiCr target, Ar gas is used as sputtering gas, the gas flow is 120SCCM, and the film thickness is 4-6 nm;
step five, preparing the conductive layer 14: and (4) conveying the substrate subjected to the step four into a next coating area, sputtering an Ag target by using a direct-current power supply, using Ar as sputtering gas, wherein the gas flow is 120SCCM, and the film thickness is 8-10 nm.
Step six, preparing the first transparent conductive layer 15: the substrate after the step five is sent into the next coating area, ITO target material is sputtered in an alternating current mode, the temperature in the cavity is 300-450 ℃, and Ar gas and O gas in the step 2 As sputtering gas, gas flow 100SCCM:120SCCM, the film thickness is 80-100nm, and the film sheet resistance is 8-10 ohm;
step seven, preparing a cathode discoloring layer 16:
(1) and adjusting the target material: co-sputtering by magnetron sputtering method with sputtering sources at 120 deg.C, loading tungsten and molybdenum targets on the sputtering sources, and using Ar gas and O 2 As sputtering gas, the gas flow rate was 100SCCM:120SCCM, and adjusting the power of each target to obtain different doping proportions;
(2) and preparing a doped target material: mixing WO 3 、MO 3 The powder is mixed according to the doping proportion in the fourth step, and is prepared into doped WO by adopting a powder metallurgy method 3 A target material;
(3) and masking: covering two adjacent sides of the substrate subjected to the sixth step by using an oxygen-free adhesive tape with the width of 10 mm;
(4) preparation of the cathodic coloration layer 16: the substrate after the mask is finished is sent to the next coating area and is coated with the doped WO 3 Film(s)With Ar gas, O 2 As sputtering gas, the gas flow rate was 100SCCM: 10SCCM to obtain doped WO 3 A film; the film thickness is 450-;
obtaining a first substrate 1 after the seventh step;
step eight, preparing the second substrate 21 of the second substrate 2: selecting high-quality float glass, cleaning the float glass with deionized water, conveying the float glass to a magnetron sputtering coating machine, arranging an RF plasma cleaning device in a buffer chamber of the coating machine, and spraying an optical absorbent after plasma cleaning to prepare a second substrate 21;
step nine, preparing a second antireflection dielectric film layer 22: sending the second substrate 21 subjected to the step eight into a coating area, carrying out magnetron sputtering on titanium, carrying out reactive sputtering by using a direct-current power supply, using Ar gas and O2 as sputtering gases, wherein the gas flow is 100SCCM:120SCCM, and the film thickness is 20-40 nm;
step ten, preparing a second transparent conductive layer 23: the substrate after the ninth step is sent to the next coating area for alternating current sputtering of the ITO target material, the chamber is heated to 300 ℃ and 450 ℃, and Ar gas and O in the step 2 As sputtering gas, gas flow 100SCCM:120SCCM, film thickness of 150-;
eleven, masking: covering two adjacent sides of the substrate after the step ten by using an oxygen-free adhesive tape with the width of 10 mm;
step twelve, preparing an anode discoloration layer 24: feeding the substrate after the mask of the step eleven into a next coating area, carrying out direct current sputtering on a nickel target, and preparing an NIO-doped thin film by using Ar gas as sputtering gas with the gas flow of 120 SCCM; the film thickness is 200-300 nm;
completing the step twelve to obtain a second substrate 2;
step thirteen, laying electrodes: removing the masking adhesive tapes on the first substrate 1 and the second substrate 2, coating conductive silver paste, and leading out conductive wires;
fourteen, preparing a PVB casting film layer 3;
(1) uniformly mixing PVB resin, lithium salt, a plasticizer, an ultraviolet light absorber and a stabilizer in a high-speed mixer, and preparing PVB conductive master batch by adopting a method of melt blending and extrusion of a double-screw extruder;
(2) in the extrusion casting process, adding the PVB conductive master batch into PVB resin according to the proportion of 20% to prepare a high-conductivity PVB film with the thickness of 1 mm;
step fifteen, packaging the electrochromic glass: sequentially stacking a first substrate 1, a PVB casting film 3 and a second substrate 2, and then preparing electrochromic laminated glass by autoclave steam-pressure molding;
sixthly, filling SiO (silicon dioxide) in an area enclosed by the aluminum frame 41 and the toughened glass layer 42 by using an aluminum frame 41 (the aluminum frame contains a drying agent) which is coated with butyl rubber and has the thickness of 8-10mm on the electrochromic laminated glass after the step fifteen is finished 2 And filling the aerogel with hollow structural adhesive to form the aerogel composite electrochromic glass.
Table 1: thickness of each dielectric layer of examples 1-4
In example 1 preparation of a cathodically coloring layer, WO 3 、MO 3 The powder doping ratio is 1: 2; during preparation of the PVB casting film layer, 600g of PVB resin, 300g of lithium salt, 150g of plasticizer, 15g of ultraviolet absorbent and 20g of stabilizer are used, the lithium salt is composed of lithium carbonate and lithium niobate according to the weight ratio of 1:1, and the actual measured conductivity of the prepared PVB casting film is 10 -5 S/cm；
In example 2 preparation of a cathodically coloring layer, WO 3 、MO 3 The powder doping ratio is 1.2: 2; when the PVB casting film layer is prepared, 500g of PVB resin, 200g of lithium salt, 150g of plasticizer, 15g of ultraviolet absorbent and 20g of stabilizer are used, the lithium salt is composed of lithium perchlorate and lithium niobate according to the weight ratio of 1:1, and the actual measured conductivity of the prepared PVB casting film is 10 -5 S/cm；
In example 3 preparation of a cathodically coloring layer, WO 3 、MO 3 The powder doping ratio is 1.5: 2; when the PVB casting film layer is prepared, the PVB resin is 300g, the lithium salt is 200g, the plasticizer is 150g, the ultraviolet absorbent is 15g, the stabilizer is 20g, the lithium salt is lithium niobate, and the actually measured conductivity of the prepared PVB casting film is 10 -5 S/cm；
In example 4 preparation of a cathodically coloring layer, WO 3 、MO 3 The powder doping ratio is 1: 2; when the PVB casting film layer is prepared, the PVB resin is 400g, the lithium salt is 200g, the plasticizer is 150g, the ultraviolet absorbent is 15g, the stabilizer is 20g, the lithium salt is lithium niobate, and the actually measured conductivity of the prepared PVB casting film is 10 -5 S/cm。
With the conditions of examples 1-4 above, the aerogel composite electrochromic glass obtained was prepared and evaluated for the following properties:
table 2: comparison of product Performance test results obtained in examples 1-4
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Visible light transmittance% | 25.5％ | 37.2％ | 36.5％ | 25.8％ |
| Transmittance of infrared ray% | 5.5％ | 7.2％ | 6.5％ | 5.8％ |
| Reflectance% | 2.3％ | 2.0％ | 2.1％ | 1.8％ |
The aerogel composite electrochromic glass has the advantages that the electrochromic layer is divided into the cathode electrochromic layer and the anode electrochromic layer due to different pressurizing, when voltage is applied, ions are injected into the layers to generate a color change phenomenon, under the action of an external electric field, the cathode electrochromic film layer and the anode electrochromic film layer can be simultaneously colored, so that the colored color is deepened, the bleached transmittance is higher, the silica aerogel is a novel amorphous solid material which is gathered by nanometer-level particles and takes air as a dispersion medium, the solvent in the original framework is removed from the aerogel through a special production process, thereby having the advantages of high porosity, translucence, low refractive index and the like, and combining the functions of the cathode and anode discoloring layers by utilizing the characteristics of the aerogel, by adjusting the filling amount of the aerogel, the visible light transmittance of the aerogel glass is better applied to the temperature and light adjustment of the composite electrochromic glass; electrochromic and aerogel are compounded, and active energy-saving and passive energy-saving compounding is realized. When the color-changing glass is used for electrochromic laminated glass, different colors can be provided by introducing different voltages to the electrochromic glass, so that the efficient selectivity of a spectrum is ensured, and the color, the light modulation and the temperature adjustment can be automatically regulated and controlled.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The utility model provides a compound electrochromic glass of aerogel, includes first substrate (1), PVB curtain coating film layer (3), second substrate (2) and aerogel filling layer (4) that set gradually, its characterized in that: the first substrate (1) comprises a first substrate (11), a first anti-reflection medium film layer (12), a barrier layer (13), a conducting layer (14), a first transparent conducting layer (15) and a cathode discoloration layer (16) which are sequentially and compositely arranged, and the second substrate (2) comprises a second substrate (21), a second anti-reflection medium film layer (22), a second transparent conducting film layer (23) and an anode discoloration layer (24) which are sequentially and compositely arranged.
2. An aerogel composite electrochromic glass as in claim 1, wherein: the first anti-reflection medium film layer (12) is Nb 2 O 5 The barrier layer (13) is a NiCr film layer, the conducting layer (14) is an Ag layer, the first transparent conducting layer (15) is an ITO film layer, and the cathode discoloration layer (16) is WO 3 And (5) film layer.
3. An aerogel composite electrochromic glass as in claim 1, wherein: the second anti-reflection medium film layer (22) is TiO 2 The second transparent conductive film layer (23) is an ITO layer, and the anode discoloration layer (24) is an NIO layer.
4. An aerogel composite electrochromic glass as in claim 1, wherein: the PVB casting film layer (3) is mainly composed of PVB resin, lithium salt, a plasticizer, an ultraviolet light absorber and a stabilizer, wherein the lithium salt is one or more of lithium perchlorate, lithium carbonate and lithium niobate.
5. An aerogel composite electrochromic glass as in claim 1, wherein: aerogel filling layer (4) includes aluminium frame (41) and toughened glass layer (42), it has SiO to fill between aluminium frame (41) and toughened glass layer (42) 2 An aerogel.
6. An aerogel composite electrochromic glass as in claim 1, wherein: the cathode discoloration layer (16) is doped with WO 3 The film thickness is 450 nm and 600 nm.
7. An aerogel composite electrochromic glass as in claim 1, wherein: the anode discoloring layer (25) is an NIO-doped film layer, and the thickness of the film is 200-300 nm.
8. An aerogel composite electrochromic glass according to claim 4, wherein: the preparation method of the PVB casting film layer (3) comprises the following steps:
(1) uniformly mixing PVB resin, lithium salt, a plasticizer, an ultraviolet light absorber and a stabilizer in a high-speed mixer, and preparing PVB conductive master batch by adopting a method of melt blending and extrusion of a double-screw extruder;
(2) in the extrusion casting process, the PVB conductive master batch is added into PVB resin according to the proportion of 20 percent to prepare the high-conductivity PVB film with the thickness of 1 mm.
9. An aerogel composite electrochromic glass as in claim 1, wherein: the first substrate (11) is toughened, semi-toughened or non-toughened glass, and Bi is arranged on the first substrate 4 O 6 The second substrate (21) is toughened, semi-toughened or non-toughened glass.
10. The preparation method of the aerogel composite electrochromic glass is characterized by comprising the following steps of:
the method comprises the following steps: preparing a first substrate: selecting high-quality float glass, cleaning the float glass with deionized water, conveying the float glass to a magnetron sputtering coating machine, arranging an RF plasma cleaning device in a buffer chamber of the coating machine, and spraying an optical absorbent after plasma cleaning to prepare a first substrate;
step two, preparing the bottom layer Bi 4 O 6 Layer (b): will complete the first stepA substrate is sent into a coating area, a bismuth target is magnetically sputtered, a direct current power supply is used for reactive sputtering, Ar gas and O are used 2 As sputtering gas, the gas flow rate is 100SCCM:120SCCM, the film thickness is 20-40nm, and the bottom layer is obtained;
step three, preparing a first antireflection dielectric film layer: the substrate after the second step is sent to the next coating area, and is reactively sputtered by a direct current power supply, and Ar gas and O for selecting a high-refractive-index material Nb 2 As sputtering gas, gas flow 100SCCM:120SCCM to prepare a first anti-reflection dielectric film layer with the film thickness of 40-60 nm;
step four, preparing a barrier layer: the substrate after the third step is sent into the next coating area, a direct current power supply sputters a NiCr target, Ar gas is used as sputtering gas, the gas flow is 120SCCM, and the film thickness is 4-6 nm;
step five, preparing a conductive layer: and (5) conveying the substrate after the step four into a next coating area, sputtering an Ag target by using a direct-current power supply, using Ar as sputtering gas, and ensuring that the gas flow is 120SCCM and the film thickness is 8-10 nm.
Step six, preparing a first transparent conductive layer: the substrate after the step five is sent into the next coating area, the ITO target material is sputtered in an alternating current mode, and the inside of the cavity is heated by 300- O C, Ar gas, O of the step 2 As sputtering gas, gas flow 100SCCM:120SCCM, the film thickness is 80-100 nm;
step seven, preparing a cathode discoloring layer:
(1) and adjusting the target material: co-sputtering by magnetron sputtering method with sputtering sources at 120 deg.C, loading tungsten and molybdenum targets on the sputtering sources, and using Ar gas and O 2 As sputtering gas, the gas flow rate was 100SCCM:120SCCM, adjusting the power of each target to obtain different doping proportions;
(2) and preparing a doped target material: mixing WO 3 、MO 3 The powder is mixed according to the doping proportion in the fourth step, and is prepared into doped WO by adopting a powder metallurgy method 3 A target material;
(3) and masking: covering two adjacent sides of the substrate subjected to the sixth step by using an oxygen-free adhesive tape with the width of 10 mm;
(4) preparing a cathode discoloring layer: the substrate after the mask is finished is sent to the next coating area and is coated with the doped WO 3 Film with Ar gas, O 2 As a sputtering gasBody, gas flow 100SCCM: 10SCCM to obtain doped WO 3 A film; the film thickness is 450-;
obtaining a first substrate after the seventh step;
step eight, preparing a second substrate of the second substrate: selecting high-quality float glass, cleaning the float glass with deionized water, conveying the float glass to a magnetron sputtering coating machine, arranging an RF plasma cleaning device in a buffer chamber of the coating machine, and spraying an optical absorbent after plasma cleaning to prepare a second substrate;
step nine, preparing a second anti-reflection medium film layer: sending the second substrate after the step eight into a coating area, carrying out magnetron sputtering on titanium, carrying out reactive sputtering by using a direct-current power supply, using Ar gas and O2 as sputtering gases, wherein the gas flow is 100SCCM:120SCCM, and the film thickness is 20-40 nm;
step ten, preparing a second transparent conductive layer: the substrate after the ninth step is sent to the next coating area for alternating current sputtering of the ITO target material, and the chamber is heated by 300- O C, in this step, Ar gas and O2 were used as sputtering gases, and the gas flow rate was 100SCCM:120SCCM, film thickness 150-;
eleven, masking: covering two adjacent sides of the substrate after the step ten by using an oxygen-free adhesive tape with the width of 10 mm;
step twelve, preparing an anode color changing layer: conveying the substrate after the mask of the step eleven into a next coating area, carrying out direct current sputtering on a nickel target, and preparing an NIO-doped thin film by using Ar gas as sputtering gas with the gas flow of 120 SCCM; the film thickness is 200-300 nm;
completing the step twelve to obtain a second substrate;
step thirteen, laying electrodes: removing the masking adhesive tapes on the first substrate and the second substrate, coating conductive silver paste, and leading out a conductive wire;
fourteen, preparing a PVB casting film layer;
step fifteen, packaging the electrochromic glass: sequentially stacking a first substrate, a PVB tape casting film layer and a second substrate in sequence, and then preparing the electrochromic laminated glass by adopting autoclave autoclaved molding;
sixthly, placing the electrochromic laminated glass coated with the butyl rubber on the electrochromic laminated glass in the step fifteen, wherein the thickness of the electrochromic laminated glass is 8An aluminum frame (the aluminum frame contains a drying agent) with the thickness of 10mm, and a region enclosed by the aluminum frame and the toughened glass layer is filled with SiO 2 And filling the aerogel with hollow structural adhesive to form the aerogel composite electrochromic glass.
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