CN109298578A - A kind of compound electrochomeric glass and its processing method - Google Patents

A kind of compound electrochomeric glass and its processing method Download PDF

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Publication number
CN109298578A
CN109298578A CN201811439957.0A CN201811439957A CN109298578A CN 109298578 A CN109298578 A CN 109298578A CN 201811439957 A CN201811439957 A CN 201811439957A CN 109298578 A CN109298578 A CN 109298578A
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CN
China
Prior art keywords
film
compound
electrochomeric glass
sputtering device
conductive layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811439957.0A
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Chinese (zh)
Inventor
汪剑飞
唐业波
孙大富
汤占刚
王本初
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Dongguan Yintaifeng Optical Technology Co Ltd
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Dongguan Yintaifeng Optical Technology Co Ltd
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Publication date
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Priority to CN201811439957.0A priority Critical patent/CN109298578A/en
Publication of CN109298578A publication Critical patent/CN109298578A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL 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
    • G02F1/00Devices 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
    • G02F1/01Devices 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 
    • G02F1/15Devices 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
    • G02F1/1514Devices 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
    • G02F1/1523Devices 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
    • G02F1/1525Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material characterised by a particular ion transporting layer, e.g. electrolyte
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL 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
    • G02F1/00Devices 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
    • G02F1/01Devices 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 
    • G02F1/15Devices 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
    • G02F1/153Constructional details

Abstract

System of the present invention provides a kind of compound electrochomeric glass and its processing method, including glass substrate, and the face sputter coating by cathode magnetic control sputtering device in glass substrate forms ion conductive layer;By rotary magnetron sputtering device, sputter coating forms composite electrochromic film on ion conductive layer, and rotary magnetron sputtering device includes rotating cathode target tube, and rotating cathode target tube is equipped with WOxAnd NiOxTarget, WOxAnd NiOxDuty ratio be respectively 70% and 30%;By cathode magnetic control sputtering device, sputter coating forms transparent conductive film on composite electrochromic film.The present invention can effectively improve the type of form and aspect, ensure the color display category and the purity of color of electrochomeric glass, the electrochromic response time is short, signal can be responded rapidly to be changed, whole light transmission effect is good, the electrochromic effect quality of electrochomeric glass is high, and membrane structure is stablized.

Description

A kind of compound electrochomeric glass and its processing method
Technical field
The present invention relates to electrochomeric glass, a kind of compound electrochomeric glass and its processing method are specifically disclosed.
Background technique
Electrochomeric glass refers to that the optical properties of material are stablized under the action of extra electric field, reversible color becomes The phenomenon that change, cashes the reversible change for color and transparency in appearance.Electrochromic material can add outside lower driving Under voltage and current effect, reversible color change is issued, is that reversible variation occurs for the valence state of material and component, makes material Optical property changes or keeps to change, while electrochromic material also needs good ionic conductivity, higher Contrast, the electric color performance of discoloration efficiency and cycle period etc..
In the prior art, electrochomeric glass mainly includes glass substrate, ion conductive layer, tungsten oxide film and transparent leads Electrolemma, the form and aspect of this electrochomeric glass are single, the electrochromic response time is long, transmitted colors are not pure, this electroluminescent The application range of photo chromic glass is small, cannot achieve the discoloration regulatory function of high quality.
Summary of the invention
Based on this, it is necessary to it is directed to prior art problem, a kind of compound electrochomeric glass and its processing method are provided, Form and aspect are various, the response time is short, transmission effects are good.
To solve prior art problem, the present invention discloses a kind of compound electrochomeric glass, including glass substrate, glass The side of substrate is successively arranged ion conductive layer, composite electrochromic film and transparent conductive film, and composite electrochromic film is tungsten gold Belong to the cosputtering composite film of oxide and nickel metal oxide.
Further, ion conductive layer is LiPON layer.
Further, composite electrochromic film is the cosputtering composite film of tungstic acid and nickel monoxide.
Further, transparent conductive film is indium oxide tin film.
Further, glass substrate with a thickness of 1~6mm.
Further, ion conductive layer with a thickness of 15~50nm.
Further, composite electrochromic film with a thickness of 50~200nm.
Further, transparent conductive film with a thickness of 15~35nm.
Invention additionally discloses a kind of processing methods of compound electrochomeric glass, successively the following steps are included:
A, the face sputter coating by cathode magnetic control sputtering device in glass substrate forms ion conductive layer;
B, by rotary magnetron sputtering device, sputter coating forms composite electrochromic film on ion conductive layer, and rotary magnetron splashes Injection device includes rotating cathode target tube, and rotating cathode target tube is equipped with WOxAnd NiOxTarget, WOxAnd NiOxDuty score It Wei 70% and 30%;
C, by cathode magnetic control sputtering device, sputter coating forms transparent conductive film on composite electrochromic film.
Further, in step B, the sputtering voltage frequency of rotary magnetron sputtering device is 30~60kHz.
The invention has the benefit that the present invention discloses a kind of compound electrochomeric glass and its processing method, setting Special WOx, NiOx cosputtering electrochromism membrane structure, can effectively improve the type of form and aspect, it is ensured that electrochomeric glass The purity of color display category and color, the electrochromic response time is short, can respond rapidly to signal and be changed, whole Light transmission effect is good, can effectively ensure that normal light transmission, the electrochromic effect quality of electrochomeric glass are high and thin Membrane structure is stablized, long service life.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of compound electrochomeric glass in the present invention.
Fig. 2 is the operation schematic diagram of rotary magnetron sputtering device used in processing method in the present invention.
Appended drawing reference are as follows: glass substrate 10, ion conductive layer 11, composite electrochromic film 12, transparent conductive film 13, rotation Cathode targets pipe 20.
Specific embodiment
To further understand the features of the present invention, technological means and specific purposes achieved, function, below with reference to Present invention is further described in detail with specific embodiment for attached drawing.
With reference to Fig. 1, Fig. 2.
The embodiment of the present invention discloses a kind of compound electrochomeric glass, including glass substrate 10, and the one of glass substrate 10 Side is successively arranged ion conductive layer 11, composite electrochromic film 12 and transparent conductive film 13, and composite electrochromic film 12 is tungsten gold Belonging to the cosputtering composite film of oxide and nickel metal oxide, the electrochromic response time of composite electrochromic film 12 is short, Transmitted colors are pure.
Special WOx, NiOx cosputtering electrochromism membrane structure is arranged in the present invention, can effectively improve the type of form and aspect, Ensure the color display category and the purity of color of electrochomeric glass, the electrochromic response time is short, can respond rapidly to Signal is changed, and whole light transmission effect is good, can effectively ensure normal light transmission, electrochomeric glass it is electroluminescent Color changeable effect quality is high, and membrane structure is stablized, long service life.
In the present embodiment, ion conductive layer 11 is LiPON layer, i.e., ion conductive layer 11 is LiPON layers.
In the present embodiment, composite electrochromic film 12 be tungstic acid and nickel monoxide cosputtering composite film, three The mixed proportion of tungsten oxide and nickel monoxide is 7:3, and the stable structure of composite electrochromic film 12 can effectively ensure whole Color purity, and light transmission is good.
In the present embodiment, transparent conductive film 13 is indium oxide tin film, i.e., transparent conductive film 13 is ito film.
In the present embodiment, glass substrate 10 with a thickness of 1~6mm.
Based on the above embodiment, ion conductive layer 11 with a thickness of 15~50nm.
Based on the above embodiment, composite electrochromic film 12 with a thickness of 50~200nm.
Based on the above embodiment, transparent conductive film 13 with a thickness of 15~35nm.
The processing method that a kind of compound electrochomeric glass is also disclosed in the embodiment of the present invention, successively the following steps are included:
A, the face sputter coating by cathode magnetic control sputtering device in glass substrate 10 forms ion conductive layer 11, in this step The cathode targets of cathode magnetic control sputtering device are LiPON or PEO-LiClO4, glass substrate 10 connects anode, cathode targets connection Cathode, electronics collide under electric field action with ar atmo, so that ionization forms argon ion and new electronics, new electronics flies to glass Glass substrate 10, argon ion accelerates to fly to cathode targets under electric field action, and with the surface of high-energy bombarding cathode target, makes yin Pole target sputters, and cathode targets atom or molecule sputter deposited onto formation ion conductive layer 11 on glass substrate 10;
B, by rotary magnetron sputtering device, sputter coating forms composite electrochromic film 12, rotary magnetic on ion conductive layer 11 Control sputtering equipment includes rotating cathode target tube 20, and rotating cathode target tube 20 is equipped with WOxAnd NiOxTarget, WOxAnd NiOx's Duty ratio is respectively 70% and 30%, and the ion conductive layer 11 of glass substrate 10 is towards rotating cathode target tube 20, glass substrate 10 connection anodes, rotating cathode target tube 20 connect cathode, and electronics collides under electric field action with ar atmo, to ionize It forms argon ion and new electronics, new electronics flies to glass substrate 10, argon ion accelerates to fly to target under electric field action, and with height Energy bombards the surface of rotating cathode target tube 20, sputters target, target atom or molecule sputter deposited onto glass base On the ion conductive layer 11 of plate 10, rotating cathode target tube 20 is constantly rotated in sputtering process, WOxAnd NiOxWith 70% and 30% Duty ratio deposited on ion conductive layer 11 and form composite electrochromic film 12;
C, by cathode magnetic control sputtering device, sputter coating forms transparent conductive film 13, this step on composite electrochromic film 12 The cathode targets of middle cathode magnetic control sputtering device are ITO, FTO or AZO, and the composite electrochromic film 12 of glass substrate 10 is towards yin Pole target, glass substrate 10 connect anode, and cathode targets connect cathode, and electronics collides under electric field action with ar atmo, To which ionization forms argon ion and new electronics, new electronics flies to glass substrate 10, and argon ion accelerates to fly to yin under electric field action Pole target, and with the surface of high-energy bombarding cathode target, sputter cathode targets, cathode targets atom or molecule sputtering It deposits on the composite electrochromic film 12 of glass substrate 10, forms transparent conductive film 13.
In the present embodiment, in step B, the sputtering voltage frequency of rotary magnetron sputtering device is 30~60kHz, preferably Ground, sputtering voltage frequency are 40kHz, it can be ensured that the adhesion effect of composite electrochromic film 12, composite electrochromic film 12 Uniformity is good, and color changeable effect is good.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (10)

1. a kind of compound electrochomeric glass, which is characterized in that including glass substrate (10), the one of the glass substrate (10) Side is successively arranged ion conductive layer (11), composite electrochromic film (12) and transparent conductive film (13), the composite electrochromic Film (12) is the cosputtering composite film of tungsten metal oxidic and nickel metal oxide.
2. a kind of compound electrochomeric glass according to claim 1, which is characterized in that the ion conductive layer (11) For LiPON layer.
3. a kind of compound electrochomeric glass according to claim 1, which is characterized in that the composite electrochromic film It (12) is the cosputtering composite film of tungstic acid and nickel monoxide.
4. a kind of compound electrochomeric glass according to claim 1, which is characterized in that the transparent conductive film (13) For indium oxide tin film.
5. a kind of compound electrochomeric glass according to claim 1, which is characterized in that the glass substrate (10) With a thickness of 1~6mm.
6. a kind of compound electrochomeric glass according to claim 5, which is characterized in that the ion conductive layer (11) With a thickness of 15~50nm.
7. a kind of compound electrochomeric glass according to claim 6, which is characterized in that the composite electrochromic film (12) with a thickness of 50~200nm.
8. a kind of compound electrochomeric glass according to claim 7, which is characterized in that the transparent conductive film (13) With a thickness of 15~35nm.
9. a kind of processing method of compound electrochomeric glass, which is characterized in that successively the following steps are included:
A, the face sputter coating by cathode magnetic control sputtering device in glass substrate (10) forms ion conductive layer (11);
B, by rotary magnetron sputtering device, sputter coating forms composite electrochromic film on the ion conductive layer (11) (12), the rotary magnetron sputtering device includes rotating cathode target tube (20), and the rotating cathode target tube (20) is equipped with WOxAnd NiOxTarget, WOxAnd NiOxDuty ratio be respectively 70% and 30%;
C, by the cathode magnetic control sputtering device, sputter coating forms electrically conducting transparent on the composite electrochromic film (12) Film (13).
10. a kind of processing method of compound electrochomeric glass according to claim 9, which is characterized in that step B In, the sputtering voltage frequency of the rotary magnetron sputtering device is 30~60kHz.
CN201811439957.0A 2018-11-29 2018-11-29 A kind of compound electrochomeric glass and its processing method Pending CN109298578A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111796466A (en) * 2020-07-02 2020-10-20 深圳市诚德利科技有限公司 Rare earth metal electrochromic film electrode and preparation method and application thereof
CN113896566A (en) * 2021-08-24 2022-01-07 北京工业大学 Multifunctional color anti-counterfeiting film preparation method based on rotation parameter control

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5321544A (en) * 1991-09-04 1994-06-14 Sun Active Glass Electrochromics, Inc. Electrochromic structures and methods
US5442478A (en) * 1990-10-30 1995-08-15 The Regents, University Of California Electrochromic device using mercaptans and organothiolate compounds
CN101833211A (en) * 2010-04-01 2010-09-15 中国科学院宁波材料技术与工程研究所 Intelligent dimming glass
CN205405029U (en) * 2016-02-26 2016-07-27 研创应用材料(赣州)股份有限公司 High electrochromic film who changes speed
CN108227328A (en) * 2018-01-30 2018-06-29 林嘉佑 A kind of automatically controlled all solid state intelligent dimming device of modified form
CN108254989A (en) * 2016-12-29 2018-07-06 宁波祢若电子科技有限公司 Full-solid electrochromic window and solid-state electrochromic mirror and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5442478A (en) * 1990-10-30 1995-08-15 The Regents, University Of California Electrochromic device using mercaptans and organothiolate compounds
US5321544A (en) * 1991-09-04 1994-06-14 Sun Active Glass Electrochromics, Inc. Electrochromic structures and methods
CN101833211A (en) * 2010-04-01 2010-09-15 中国科学院宁波材料技术与工程研究所 Intelligent dimming glass
CN205405029U (en) * 2016-02-26 2016-07-27 研创应用材料(赣州)股份有限公司 High electrochromic film who changes speed
CN108254989A (en) * 2016-12-29 2018-07-06 宁波祢若电子科技有限公司 Full-solid electrochromic window and solid-state electrochromic mirror and preparation method thereof
CN108227328A (en) * 2018-01-30 2018-06-29 林嘉佑 A kind of automatically controlled all solid state intelligent dimming device of modified form

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111796466A (en) * 2020-07-02 2020-10-20 深圳市诚德利科技有限公司 Rare earth metal electrochromic film electrode and preparation method and application thereof
CN113896566A (en) * 2021-08-24 2022-01-07 北京工业大学 Multifunctional color anti-counterfeiting film preparation method based on rotation parameter control

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