KR20160098537A - Electrochromic layer, method of fabricating the same, and electrochromic device comprising the same - Google Patents

Electrochromic layer, method of fabricating the same, and electrochromic device comprising the same Download PDF

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Publication number
KR20160098537A
KR20160098537A KR1020150014504A KR20150014504A KR20160098537A KR 20160098537 A KR20160098537 A KR 20160098537A KR 1020150014504 A KR1020150014504 A KR 1020150014504A KR 20150014504 A KR20150014504 A KR 20150014504A KR 20160098537 A KR20160098537 A KR 20160098537A
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South Korea
Prior art keywords
thin film
electrochromic
electrochromic thin
electrode
antimony
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KR1020150014504A
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Korean (ko)
Inventor
김형섭
이선영
안성훈
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한양대학교 에리카산학협력단
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Priority to KR1020150014504A priority Critical patent/KR20160098537A/en
Publication of KR20160098537A publication Critical patent/KR20160098537A/en

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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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  • Physics & Mathematics (AREA)
  • Nonlinear Science (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)

Abstract

A method for producing an electrochromic thin film is provided. The method for producing an electrochromic thin film includes the steps of preparing a source powder containing antimony (Sb), tin (Sn), and oxygen (O) in a powder storage tank, Using the difference to accelerate the source powder and providing the accelerated source powder on the substrate in the chamber to produce an electrochromic thin film comprising antimony doped tin oxide on the substrate, .

Description

TECHNICAL FIELD The present invention relates to an electrochromic thin film, a method of manufacturing the electrochromic thin film, and an electrochromic device including the electrochromic thin film, a method of fabricating the same, and an electrochromic device,

The present invention relates to an electrochromic thin film, a method of manufacturing the same, and an electrochromic device including the same. More particularly, the present invention relates to an electrochromic thin film comprising antimony-doped tin oxide using a source powder containing antimony, tin, And a method of manufacturing the electrochromic thin film, and an electrochromic device comprising the electrochromic thin film.

The term " electrochromic material " refers to a phenomenon in which the color reversibly varies in the direction of the electric field when a voltage is applied, and the electrochromic material is a material in which the optical characteristics of the material can be reversibly changed Materials.

That is, an oxidation and reduction reaction occurs due to the applied voltage, and a colorless phenomenon occurs in a reduced state and a colorless phenomenon in an oxidized state is referred to as a cathodic coloration. A colorless phenomenon occurs in a reduced state, Is referred to as anodic coloration. Typically, WO 3 , MoO 3 , and TIO 3 are known as reducing coloring materials, and V 2 O 5 and IrO 2 are known as oxidation-coloring materials.

Currently, the display market and the industry are being driven by organic light emitting displays or liquid crystal displays, but display devices using an electrochromic device capable of low energy driving and less burden on the eyes are being researched and developed.

For example, in Korean Patent Laid-Open Publication No. 10-2006-0020110 (Applicant, LG Chem, Application No. 10-2004-0068865), a conductive zinc oxide layer is disposed between a transparent electrode layer and an electrochromic material layer to form a transparent electrode layer and an electrochromic material Discloses a display device in which stability and durability are improved by increasing the conductivity and interface contact area between layers.

Korean Patent Publication No. 10-2006-0020110

SUMMARY OF THE INVENTION The present invention provides a highly reliable electrochromic thin film, a method of manufacturing the electrochromic thin film, and an electrochromic device including the electrochromic thin film.

Another object of the present invention is to provide an electrochromic thin film having improved electrochromic efficiency, a method for producing the electrochromic thin film, and an electrochromic device including the same.

Another technical problem to be solved by the present invention is to provide a method of manufacturing an electrochromic thin film which is easy to manufacture in a large area and is environmentally friendly.

The technical problem to be solved by the present invention is not limited to the above.

In order to solve the above technical problems, the present invention provides a method for producing an electrochromic thin film

According to one embodiment, the method for producing an electrochromic thin film includes the steps of preparing a source powder containing antimony (Sb), tin (Sn), and oxygen (O) in a powder storage tank, Accelerating the source powder using a pressure difference between the storage tank and the chamber, and providing the accelerated source powder onto the substrate in the chamber to deposit an electrochromic thin film comprising antimony doped tin oxide on the substrate Lt; / RTI >

According to one embodiment, the interior of the chamber may include an atmospheric environment.

According to one embodiment, the electrochromic thin film may include a porous material.

According to one embodiment, the particles of the source powder may be observed in the electrochromic thin film.

In order to solve the above technical problems, the present invention provides an electrochromic device.

According to one embodiment, the electrochromic device comprises a first electrode, a second electrode facing the first electrode, an ion storage layer between the first electrode and the second electrode, an ion storage layer between the first electrode and the second electrode, An electrochromic thin film disposed between the first electrode and the second electrode, the electrochromic thin film including tin oxide doped with antimony, and an electrolyte disposed between the electrochromic thin film and the ion storage layer and comprising phosphoric acid.

According to one embodiment, the electrolyte may not contain a lithium salt.

According to one embodiment, the electrochromic thin film may include a change in transmittance of incident light to a specific wavelength band of 35%.

According to an embodiment of the present invention, a porous electrochromic thin film having tin oxide doped with antimony may be formed on a substrate using a source powder containing antimony, tin and oxygen. As a result, the discoloration efficiency of the electrochromic thin film can be increased.

In addition, the electrochromic thin film can be manufactured by a dry process. Accordingly, a method of manufacturing an electrochromic thin film that is easy to manufacture in a large area, and is environmentally friendly and highly reliable can be provided.

Further, according to the embodiment of the present invention, an electrochromic device can be manufactured using an electrochromic thin film containing tin oxide doped with antimony and an electrolyte including phosphoric acid. Thus, an electrochromic device having improved color fading efficiency can be provided.

1 is a flowchart illustrating a method of manufacturing an electrochromic device according to an embodiment of the present invention.
2 is a view for explaining an apparatus for manufacturing an electrochromic thin film according to a method of manufacturing an electrochromic thin film according to an embodiment of the present invention.
3 is a view for explaining an apparatus for producing an electrochromic thin film according to an embodiment of the present invention.
4 is a view for explaining the surface of an electrochromic thin film produced according to the method of manufacturing an electrochromic thin film according to an embodiment of the present invention.
FIG. 5 is a view for explaining a change in transmittance of an electrochromic device having an electrochromic thin film according to an embodiment of the present invention. Referring to FIG.
6 is a graph illustrating a change in transmittance according to wavelength of an electrochromic device having an electrochromic thin film manufactured according to an electrochromic thin film according to an embodiment of the present invention.
7 is a graph for explaining a change in transmittance according to wavelength of an electrochromic device according to a comparative example according to an embodiment of the present invention.
8 is a graph for explaining a characteristic change according to an electrolyte included in an electrochromic device according to a comparative example according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the technical spirit of the present invention is not limited to the embodiments described herein but may be embodied in other forms. Rather, the embodiments disclosed herein are provided so that the disclosure can be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

In this specification, when an element is referred to as being on another element, it may be directly formed on another element, or a third element may be interposed therebetween. Further, in the drawings, the thicknesses of the films and regions are exaggerated for an effective explanation of the technical content.

Also, while the terms first, second, third, etc. in the various embodiments of the present disclosure are used to describe various components, these components should not be limited by these terms. These terms have only been used to distinguish one component from another. Thus, what is referred to as a first component in any one embodiment may be referred to as a second component in another embodiment. Each embodiment described and exemplified herein also includes its complementary embodiment. Also, in this specification, 'and / or' are used to include at least one of the front and rear components.

The singular forms "a", "an", and "the" include plural referents unless the context clearly dictates otherwise. It is also to be understood that the terms such as " comprises "or" having "are intended to specify the presence of stated features, integers, Should not be understood to exclude the presence or addition of one or more other elements, elements, or combinations thereof.

In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

1 is a flowchart illustrating a method of manufacturing an electrochromic device according to an embodiment of the present invention.

Referring to FIG. 1, a source powder is prepared (S110). The source powder may include antimony (Sb), tin (Sn), and oxygen (O). According to one embodiment, the source powder may be a tin oxide powder doped with antimony. The source powder may be prepared in a powder storage tank.

Using the pressure difference between the powder storage tank and the chamber connected to the powder storage tank, the source powder may be accelerated (S120). According to one embodiment, the source powder in the powder storage tank can be sprayed, and the sprayed source powder is supersonically accelerated by a pressure difference between the powder storage tank and the chamber, Can be injected into the chamber.

The accelerated source powder is provided on a substrate in the chamber, and an electrochromic thin film may be fabricated on the substrate (130). The electrochromic thin film is formed by adsorbing the accelerated source powder on the substrate and may include tin oxide doped with antimony. The substrate may be transparent and have conductivity. For example, the substrate may be an FTO.

According to an embodiment of the present invention, the source powder comprising antimony, tin and oxygen is accelerated by a pressure difference between the powder storage tank and the chamber, and the accelerated source powder is provided on the substrate , The electrochromic thin film including a porous tin oxide doped with antimony may be formed on the substrate. Accordingly, the surface area of the electrochromic thin film can be increased, thereby increasing the area in which the discoloration reaction can be performed, thereby providing a method of manufacturing an electrochromic thin film having improved discoloration efficiency.

If the antimony-doped tin oxide thin film is formed by a dip coating method, a spray coating method, or a sol-gel method, unlike the embodiment of the present invention described above, And chemicals may be used in the preparation of tin-containing solutions. In addition, when a tin oxide thin film doped with antimony is prepared using a solution containing antimony and tin, cracks are generated in the tin oxide thin film doped with antimony due to the volume expansion.

In addition, when a tin oxide thin film doped with antimony is prepared by the sputtering method, the production cost may be increased due to the high vacuum condition, and the composition of the antimony doped tin oxide thin film is not easily controlled. Further, when a tin oxide thin film doped with antimony is produced by the pulse laser deposition method, it is not easy to increase the area and the laser is difficult to control.

However, as described above, according to the embodiment of the present invention, an electrochromic thin film including tin oxide doped with antimony on the substrate can be manufactured using the source powder, dryly. Accordingly, a method of manufacturing an electrochromic thin film that is easy to manufacture in a large area, and is environmentally friendly and highly reliable can be provided.

Hereinafter, an apparatus for manufacturing an electrochromic thin film in the method of manufacturing an electrochromic thin film according to an embodiment of the present invention described above will be described with reference to FIG.

2 is a view for explaining an apparatus for manufacturing an electrochromic thin film according to a method of manufacturing an electrochromic thin film according to an embodiment of the present invention.

2, an apparatus for manufacturing an electrochromic thin film includes a chamber 100, a stage 110, a nozzle 120, a camera 130, a control unit 132, a chamber pressure regulating unit 140, An air compressor 210, a filter 220, a regulator 230, a powder storage tank 240, and a spray generator 242.

The stage 110 may be disposed in the chamber 100. The substrate 112 may be seated on the stage 110. The stage 110 may be configured to move in first and second directions parallel to the paper surface and in a third direction perpendicular to the paper surface.

The air compression unit 210 may compress air to provide compressed air. Dust, oil, and the like can be removed while the compressed air passes through the filter 220. The compressed air may be supplied to the powder storage tank 240 through the regulator 230.

A source powder 244 may be stored in the powder storage tank 240. The source powder 244 may include antimony, tin, and oxygen, as described with reference to FIG.

The spray generator 242 may be disposed in the powder storage tank 240. By the spray generator 242, the source powder 244 stored in the powder storage tank 240 can be sprayed. The sprayed source powder 244 is sprayed onto the substrate 112 in the chamber 100 by the compressed air provided from the air compression unit 210 and is supplied to the powder storage tank 240, (100). ≪ / RTI >

The chamber pressure regulator 140 and the pump 142 may maintain the inside of the chamber 100 in a low vacuum state. Thus, the pressure difference between the powder storage tank 240 and the chamber 100 is maintained substantially constant, and the difference in pressure accelerates the sprayed source powder 244, May be provided on the substrate 112, via the substrate 120. According to one embodiment, the interior of the chamber 100 may be an atmospheric environment. The chamber pressure regulator 140 may be controlled by the controller 132.

1, an electrochromic thin film containing tin oxide doped with antimony is prepared on the substrate 112 by the source powder 244 injected onto the substrate 112 .

The camera 130 may photograph the electrochromic thin film formed on the substrate 112 and transmit the photographed thin film to the controller 132. The user can observe the formation process of the electrochromic thin film through the controller 132.

Hereinafter, an electrochromic device including an electrochromic thin film manufactured according to the method for manufacturing an electrochromic thin film according to the embodiment of the present invention will be described with reference to FIG.

3 is a view for explaining an apparatus for producing an electrochromic thin film according to an embodiment of the present invention.

3, the electrochromic device includes a first electrode 310, a second electrode 320, an ion storage layer 330, an electrochromic thin film 340, an electrolyte 340, a first substrate 360, A second substrate 370, and a voltage supply unit 380. [0043]

The first electrode 310 and the second electrode 320 may be opposed to each other. The first electrode 310 and the second electrode 320 may be transparent oxide thin films (TCO). The first electrode 310 and the second electrode 320 may be formed of the same material.

The ion storage layer 330 may be disposed between the first electrode 310 and the second electrode 320. The ion storage layer 330 may be formed of a polymeric material (e.g., PEDOT), or a metal oxide (e.g., V 2 O 5 ).

The electrochromic thin film 340 may be disposed between the ion storage layer 330 and the first electrode 310. The electrochromic thin film 340 may include antimony-doped tin oxide prepared by the method described with reference to FIG. In addition, the electrochromic thin film 340 may be manufactured using the manufacturing apparatus described with reference to Fig.

The electrolyte 350 may be disposed between the electrochromic thin film 340 and the ion storage layer 330. The electrolyte 350 may include phosphoric acid (P 2 O 5 H 2 O). According to one embodiment, the electrolyte 350 may not include a lithium salt.

According to an embodiment of the present invention, the electrochromic thin film 340 includes antimony-doped tin oxide, and the electrolyte 350 may not include a lithium salt and may include phosphoric acid. Therefore, the discoloration efficiency of the electrochromic thin film 340 can be improved.

The first and second electrodes 310 and 320, the ion storage layer 330, the electrochromic thin film 340, and the first and second electrodes 310 and 320 are formed between the first substrate 360 and the second substrate 370, An electrolyte 350 may be disposed. The first substrate 360 and the second substrate 370 may be a transparent substrate (e.g., glass).

The voltage supplier 380 may be connected to the first electrode 310 and the second electrode 320 to apply a voltage to the electrochromic thin film 340. By the voltage applied to the electrochromic thin film 340, the electrochromic thin film 340 may be oxidized and / or reduced to be discolored.

For example, when the light 390 is incident on one surface of the second substrate 370, the incident light 390 passes through the electrochromic thin film 340, It can be released on one side. The transmittance according to the wavelength of the electrochromic thin film 340 is changed according to the polarity and / or the level of the voltage applied from the voltage supplier 380 so that the wavelength and intensity of the emitted light 392 can be adjusted have.

Hereinafter, characteristics of the electrochromic thin film and the electrochromic device including the electrochromic thin film according to the present invention will be described.

4 is a view for explaining the surface of an electrochromic thin film produced according to the method of manufacturing an electrochromic thin film according to an embodiment of the present invention.

Referring to FIG. 4, an antimony thin film of antimony-doped tin oxide (ATO) was formed on an FTO substrate using antimony-doped tin oxide powder to a thickness of 830 nm. 4 (a) is a measurement of the thickness variation of the ATO electrochromic thin film, and FIG. 4 (b) is a SEM photograph of the ATO electrochromic thin film.

As can be seen from FIG. 4, the surface roughness of the ATO electrochromic thin film was measured to be 290 nm, and it was confirmed that the ATO electrochromic thin film consisted of the tin oxide powder particles doped with antimony and had porosity. In other words, through the SEM photograph, the antimony-doped tin oxide powder particles were observed in the ATO electrochromic thin film.

FIG. 5 is a view for explaining a change in transmittance of an electrochromic device having an electrochromic thin film according to an embodiment of the present invention. Referring to FIG.

Referring to FIG. 5, an electrochromic device according to an embodiment of the present invention was manufactured using the ATO electrochromic thin film prepared by the method described with reference to FIG. 4, and a phosphoric acid electrolyte. The electrochromic device was placed on an object, and the degree of penetration of the object was observed according to whether or not a voltage was applied to the ATO electrochromic thin film.

As shown in FIG. 5, it can be seen that the transmittance of the electrochromic device changes depending on the voltage applied to the ATO electrochromic thin film, and the degree of transmission of the object changes.

6 is a graph for explaining a change in transmittance according to a wavelength of an electrochromic device having an electrochromic thin film produced according to a method for producing an electrochromic thin film according to an embodiment of the present invention. FIG. 8 is a graph for explaining a change in characteristics according to an electrolyte included in an electrochromic device according to a comparative example according to an embodiment of the present invention. FIG. 8 is a graph for explaining a change in transmittance according to a wavelength of an electrochromic device according to a comparative example. Graph.

6 to 8, an ATO electrochromic thin film prepared by the method described with reference to FIG. 4, and an electrolyte in which 0.1 M LIClO 4 and PC (propylene carbonate) are mixed, To prepare an electrochromic device according to a comparative example.

6 and 7, for the electrochromic device according to the embodiment of the present invention manufactured by the method described with reference to Fig. 5 and the electrochromic device according to the above-described comparative example, The change in transmittance according to wavelength was measured when bleached and voltage were applied (colored).

8, in the case of the electrochromic device according to the comparative example of the present invention, the change in the transmittance with respect to the pulse voltage is shown in Fig. 8B while the concentration of LiClO 4 is changed to 0.1M, 0.4M, and 0.8M, Respectively.

6 and 7, it can be seen that the variation of the transmittance of the electrochromic device according to the embodiment of the present invention is changed up to 35% in the wavelength band of 630 nm. In addition, the coloring efficiency of the electrochromic device according to the embodiment of the present invention was measured to be 15.5 cm 2 / C. It can also be seen that the amount of change in transmittance in a relatively high wavelength band is smaller than the amount of change in transmittance in a relatively low wavelength band.

On the other hand, in the case of the electrochromic device according to the comparative example of the present invention, it can be confirmed that the variation of the transmittance is about 10% in the 630 nm wavelength band. As can be seen from FIG. 8, even if the concentration of the lithium salt (LiClO 4 ) contained in the electrolyte is changed, it can be confirmed that the change amount of the permeability is about 8 to 10%. In particular, when the concentration of the lithium salt (LiClO 4 ) is increased, it is confirmed that the reliability of the change in the transmittance is lowered.

It is concluded that the electrochromic device including the ATO electrochromic thin film and the phosphorus-containing electrolyte and the electrolyte containing no lithium salt improves the reliability of the electrochromic device, , Respectively.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the scope of the present invention is not limited to the disclosed exemplary embodiments. It will also be appreciated that many modifications and variations will be apparent to those skilled in the art without departing from the scope of the invention.

100: chamber 110: stage
112: substrate 120: nozzle
132: controller 140: chamber pressure regulator
142: pump 210: air compression unit
220: filter 230: regulator
240: Powder storage tank 242: Spray generator
244: source powder 310, 320: first and second electrodes
330: ion storage layer 340: electrochromic thin film
350: electrolyte

Claims (7)

Preparing a source powder in a powder storage tank containing antimony (Sb), tin (Sn), and oxygen (O);
Accelerating the source powder using a pressure difference between the powder storage tank and the chamber; And
Providing the accelerated source powder on a substrate in the chamber to produce an electrochromic thin film comprising antimony doped tin oxide on the substrate.
The method according to claim 1,
Wherein the inside of the chamber is an air atmosphere.
The method according to claim 1,
Wherein the electrochromic thin film is porous.
The method according to claim 1,
Wherein the particles of the source powder are observed in the electrochromic thin film.
A first electrode;
A second electrode facing the first electrode;
An ion storage layer between the first electrode and the second electrode;
An electrochromic thin film disposed between the ion storage layer and the first electrode and comprising tin oxide doped with antimony; And
An electrochromic device disposed between the electrochromic thin film and the ion storage layer, the electrochromic device comprising an electrolyte containing phosphoric acid.
6. The method of claim 5,
Wherein the electrolyte does not contain a lithium salt.
6. The method of claim 5,
Wherein the electrochromic thin film has a change in transmittance of incident light in a specific wavelength band of 35%.
KR1020150014504A 2015-01-29 2015-01-29 Electrochromic layer, method of fabricating the same, and electrochromic device comprising the same KR20160098537A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20200025069A (en) * 2018-08-29 2020-03-10 한양대학교 에리카산학협력단 Electrochromic device with improved continuous driving characteristics and method for manufacturing the same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060020110A (en) 2004-08-31 2006-03-06 주식회사 엘지화학 Electrochromic device comprising zinc oxide and process for fabricating the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060020110A (en) 2004-08-31 2006-03-06 주식회사 엘지화학 Electrochromic device comprising zinc oxide and process for fabricating the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20200025069A (en) * 2018-08-29 2020-03-10 한양대학교 에리카산학협력단 Electrochromic device with improved continuous driving characteristics and method for manufacturing the same

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