KR20190000521A - Electrochromic device and preparing method thereof - Google Patents

Electrochromic device and preparing method thereof Download PDF

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KR20190000521A
KR20190000521A KR1020170079624A KR20170079624A KR20190000521A KR 20190000521 A KR20190000521 A KR 20190000521A KR 1020170079624 A KR1020170079624 A KR 1020170079624A KR 20170079624 A KR20170079624 A KR 20170079624A KR 20190000521 A KR20190000521 A KR 20190000521A
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South Korea
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electrochromic device
present
substrate
oxide
electrode layer
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KR1020170079624A
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Korean (ko)
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정동근
반원진
권성률
임현아
박윤수
김보람
한경만
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성균관대학교산학협력단
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Publication of KR20190000521A publication Critical patent/KR20190000521A/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/041—Carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
    • 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
    • G02F1/1503—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 caused by oxidation-reduction reactions in organic liquid solutions, e.g. viologen solutions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Nonlinear Science (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)

Abstract

The present invention relates to an electrochromic device comprising: a substrate; a patterned electrode layer formed on the substrate; an electron transport layer formed on the patterned electrode layer; and a colored layer formed on the electron transport layer. Excellent discoloration efficiency can be secured.

Description

ELECTROCHROMIC DEVICE AND PREPARING METHOD THEREOF BACKGROUND OF THE INVENTION 1. Field of the Invention [0001]

The present invention relates to an electrochromic device and a method of manufacturing the electrochromic device.

Smart glass selectively transmits / absorbs sunlight, so that the temperature inside buildings and transportation means can be appropriately maintained, which can contribute to energy saving. In order to selectively transmit sunlight, it is necessary to control the color of the transparent glass, which can be realized through an electrochromic material whose color changes by electrical energy. Examples of the discoloring material include metal oxides such as WOx, NbOx, and NiOx, which are inorganic materials having characteristics that change from a transparent color to a color capable of absorbing visible light by reduction. By introducing these metal oxides in the form of a transparent thin film between substrates such as glass and connecting the electrodes to both sides so as to apply electric energy thereto, a smart device, for example, smart glass having an electrochromic property can be manufactured. In order to commercialize such a smart glass, it is desirable to have high transparency before electrochromatography, high color efficiency upon discoloration, fast response speed, and high stability with constant discoloration even in repeated discoloration. Particularly, it is difficult to use a device in which the degree of discoloration decreases with repetitive discoloration, as a smart glass.

The electron transport layer is applied to an organic electronic device such as an organic light emitting device (OLED) or an organic solar cell (OSC), and is formed of LiF, Alq 3 or the like. Such an interface layer is introduced to improve the efficiency of a device through electron tunneling effect and bandgap control, and is generally formed in the form of a thin film having a thickness of 5 to 20 nm.

Especially, unlike the conventional smart glass, the electro-discolored smart glass has an electrochromic effect that changes the color by electric energy. Therefore, it selectively transmits the sunlight to maintain the temperature inside the building and the transportation means to save energy .

Therefore, various electronic color-changing smart glasses are currently being studied. As an example, Korean Patent No. 10-1137371 discloses a technique for controlling the thickness of an electrochromic smart glass film to be thinner by forming a layer of an organic coloring material only on one of two opposite surfaces of a silver nanowire layer . However, the existing electrochromic smart glass including the same has a problem that the response speed is slow, it is difficult to selectively block the sunlight, the efficiency is low, and the manufacturing cost is high. Therefore, development of an electrochromic smart glass which solves the above problems is demanded.

It is an object of the present invention to provide an electrochromic device.

It is another object of the present invention to provide a method of manufacturing an electrochromic device.

It should be understood, however, that the technical scope of the embodiments of the present invention is not limited to the above-described technical problems, and other technical problems may exist.

As a technical means for achieving the above-mentioned technical object, a first aspect of the present invention provides a semiconductor device comprising: a substrate; A patterned electrode layer formed on the substrate; An electron transport layer formed on the patterned electrode layer; And a coloring layer formed on the electron transporting layer; And an electrochromic device.

According to an embodiment of the present invention, the electrode layer is formed on a material selected from the group consisting of poly (3,4-ethylenedioxythiophene, PEDOT), polystyrene sulfonate (PSS), and combinations thereof. But it is not limited thereto.

 According to an embodiment of the present invention, the pattern may be one in which any one shape selected from the group consisting of a rectangle, a rectangle, a pyramid, a circle, a cylinder, a square, and combinations thereof is repeatedly located, but the present invention is not limited thereto .

According to one embodiment of the invention, the electron transporting layer comprises an oxide of a metal selected from the group consisting of aluminum, titanium, tin, zinc, tungsten, zirconium, gallium, indium, yttrium, niobium, tantalum, vanadium, But is not limited thereto.

According to an embodiment of the present invention, the substrate is made of indium tin oxide (ITO), fluorine tin oxide (FTO), ZnO-Ga 2 O 3 , ZnO-Al 2 O 3 , tin oxide, But is not limited to, a glass substrate or a plastic substrate containing a material selected from the group consisting of combinations of the above.

 As a technical means for achieving the above technical object, the second aspect of the present invention provides a method of manufacturing a semiconductor device, comprising: forming a patterned electrode layer on a substrate; Forming an electron transport layer on the formed patterned electrode layer; And forming a coloring layer on the electron transporting layer formed. The present invention also provides a method of manufacturing an electrochromic device.

The above-described task solution is merely exemplary and should not be construed as limiting the present disclosure. In addition to the exemplary embodiments described above, there may be additional embodiments in the drawings and the detailed description of the invention.

According to a first aspect of the present invention, A patterned electrode layer formed on the substrate; An electron transport layer formed on the patterned electrode layer; And a coloring layer formed on the electron transporting layer; Can be provided.

Conventional electrochromic smart glasses have excellent durability and are being developed and researched, but they have a disadvantage of slow response time and high manufacturing cost.

 Smart glass using WOx, a reducing coloring material, on the existing single electrode has a high transmittance when discolored, making it difficult to selectively block sunlight. In addition, discoloration and discoloration take a long time, which leads to a long reaction time to the sunlight and low efficiency.

The present invention relates to an electrochromic device manufactured by forming an electrode layer by patterning on a substrate and widening its surface, depositing and applying an electron transporting layer, and then depositing a coloring layer on the electron transporting layer. The electrochromic device exhibited lower transmittance when discolored than the conventional WOx, which was used only as a discoloration layer, and a faster response time than discoloration and decolorization.

Therefore, the electrochromic device according to the present invention can be used in a glass wall of a building and a flow device to appropriately maintain the internal temperature and save energy. In addition, it can be used in various fields such as flexible display and smart window.

FIG. 1 (a) is a schematic view of a patterned electrochromic device according to an embodiment of the present invention, and FIG. 1 (b) is a schematic view of the patterned electrochromic device.
FIG. 2A is a result of checking the permeability through the area measurement of the control group, and FIG. 2B is a result of checking the permeability through the area measurement of the electrochromic device according to one embodiment of the present application.
3 is a result of checking the solar light transmittance upon discoloration and discoloration of the electrochromic device according to an embodiment of the present invention. Fig. 3 (a) is a result of a control group, and Fig. 3 (b) This is the result of the discoloration element.
4 is a result of checking the reaction time of the electrochromic device according to an embodiment of the present invention, wherein FIG. 4 (a) is a result of a control group and FIG. 4 (b) is a result of the electrochromic device according to the present invention .
FIG. 5 shows the result of checking the discoloration efficiency index. FIG. 5 (a) shows the result of the control group, and FIG. 5 (b) shows the results of the electrochromic device according to the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention.

It should be understood, however, that the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In the drawings, the same reference numbers are used throughout the specification to refer to the same or like parts.

Throughout this specification, when a part is referred to as being "connected" to another part, it is not limited to a case where it is "directly connected" but also includes the case where it is "electrically connected" do.

It will be appreciated that throughout the specification it will be understood that when a member is located on another member "top", "top", "under", "bottom" But also the case where there is another member between the two members as well as the case where they are in contact with each other.

Throughout this specification, when an element is referred to as "including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise.

As used herein, the terms "about," " substantially, "and the like are used herein to refer to or approximate the numerical value of manufacturing and material tolerances inherent in the stated sense, Accurate or absolute numbers are used to prevent unauthorized exploitation by unauthorized intruders of the mentioned disclosure. Also, throughout the present specification, the phrase " step "or" step "does not mean" step for.

Throughout this specification, the term "combination thereof" included in the expression of the machine form means one or more combinations or combinations selected from the group consisting of the constituents described in the expression of the machine form, And the like.

Throughout this specification, the description of "A and / or B" means "A, B, or A and B".

Hereinafter, the electrochromic device and the method of manufacturing the electrochromic device of the present invention will be described in detail with reference to embodiments, examples and drawings. However, the present invention is not limited to these embodiments and examples and drawings.

According to a first aspect of the present invention, A patterned electrode layer formed on the substrate; An electron transport layer formed on the patterned electrode layer; And a coloring layer formed on the electron transporting layer; And an electrochromic device including the electrochromic device.

According to an embodiment of the present invention, the electrode layer is formed on a material selected from the group consisting of poly (3,4-ethylenedioxythiophene, PEDOT), polystyrene sulfonate (PSS), and combinations thereof. But it is not limited thereto.

The carbon nanotubes (CNTs) are formed in a hexagonal shape having six carbon atoms and connected to each other to form a tubular shape. The diameter of the tube is only a few to several tens of nanometers, which is called carbon nanotubes. It has electrical conductivity similar to copper, has the same thermal conductivity as diamond, and has a strength 100 times better than steel. Carbon fibers can be broken even if they are deformed by only 1%, while carbon nanotubes can withstand 15% deformation. In this study, the electrode was used because of its electrical conductivity.

The poly (3,4-ethylenedioxythiophene, PEDOT) and polystyrene sulfonate (PSS) were used as a solvent for spraying CNT onto a substrate and as an electrode together with CNT. Since PEDOT and PSS (PEDOT; PSS) exhibit considerably high electric conductivity and transparency, they are attracting attention as applications to photoelectronic devices. In particular, they are cheap and flexible and can be mass-produced like roll-to-roll.

  PEDOT is not soluble in almost all solvents, but it can be dispersed in water by using PSS as a counter ion. PSS acts as a very good oxidant, charge compensator, and a plate for polymerisation. PEDOT-PSS has a thiophene skeleton and is hydrophilic when combined with a sulfonate. PEDOT: PSS is used as antistatic film or hole injection layer due to high work function, high hole affinity and good transparency. Since the PSS is almost colorless, the light transmittance is mainly affected by PEDOT.

In addition, it acts as a hole conduction layer in an organic solar cell and has the effect of flattening the surface of the substrate by removing pinholes on the surface when coated on the substrate.

According to an embodiment of the present invention, the pattern may be one in which any one shape selected from the group consisting of a rectangle, a rectangle, a pyramid, a circle, a cylinder, a square, and combinations thereof is repeatedly located, but the present invention is not limited thereto .

Any one of the shapes selected from the group is repeatedly disposed, thereby increasing the surface area of the electrode, thereby improving the response speed and the index of discoloration efficiency of the device.

According to one embodiment of the present invention, the electron transporting layer may include, but not limited to, a porous metal oxide particle layer. For example, it may include, but is not limited to, an organic semiconductor, an inorganic semiconductor, or a mixture thereof.

According to one embodiment of the invention, the electron transporting layer comprises an oxide of a metal selected from the group consisting of aluminum, titanium, tin, zinc, tungsten, zirconium, gallium, indium, yttrium, niobium, tantalum, vanadium, But is not limited thereto.

For example, the metal oxide is copper aluminum oxide (Al 2 O 3), titanium dioxide (TiO 2), tin oxide (SnO 2), titanium (Ⅱ) chloride (TiCl 2), zinc oxide (ZnO), oxidation ( (NiO), cobalt (II) oxide (CoO), indium oxide (In 2 O 3 ), tungsten oxide (WO 3 ), magnesium oxide (MgO), calcium oxide (CaO ), lanthanum oxide (La 2 O 3), neodymium oxide (Nd 2 O 3), yttrium oxide (Y 2 O 3), cerium oxide (CeO 2), lead oxide (PbO), zirconium oxide (ZrO 2), iron oxide (Fe 2 O 3 ), bismuth oxide (Bi 2 O 3 ), vanadium pentoxide (V 2 O 5 ), vanadium oxide (V 2 ), oxalated niobium (Nb 2 O 5 ) ) Cobalt (II) (Co 3 O 4 ), aluminum (Al 2 O 3 ), and combinations thereof.

According to one embodiment of the disclosure, the substrate may be a conductive transparent substrate, but is not limited thereto.

According to one embodiment of the present invention, the conductive transparent substrate is made of indium tin oxide (ITO), fluorine tin oxide (FTO), ZnO-Ga2O3, ZnO-Al2O3, tin oxide, zinc oxide, glass, But not limited to, a glass substrate or a plastic substrate containing a material selected from the group consisting of The conductive transparent substrate is not particularly limited as long as it is a conductive and transparent material. For example, the plastic substrate may be selected from the group consisting of polyethylene terephthalate, polyethylene naphthalate, polycarbonate, polypropylene, polyimide, triacetylcellulose, and combinations thereof. . For example, the conductive transparent substrate may include, but is not limited to, doped with a metal selected from the group consisting of Group 3 metals, such as Al, Ga, In, Ti, and combinations thereof .

According to a second aspect of the present invention, there is provided a method comprising: forming a patterned electrode layer on a substrate; Forming an electron transport layer on the formed patterned electrode layer; And forming a coloring layer on the electron transporting layer formed. The present invention also provides a method of manufacturing an electrochromic device.

The second aspect of the present invention relates to a method of manufacturing an electrochromic device according to the first aspect of the present invention, and a detailed description thereof will be omitted. However, the description of the first aspect of the present invention May be applied equally to the second aspect of the present invention even if the description thereof is omitted.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.

≪ Example 1 > Preparation of electrochromic device

The electrochromic device of the present invention was manufactured using indium tin oxide (ITO) which is a conductive transparent substrate (5 x 5 cm).

Trichlorethylene (TCE), acetone, ethanol, and DI water were ultrasonically cleaned in the order of 10 minutes each for cleaning the ITO glass. After washing, ITO glass was patterned to widen the surface area of the electrode. 0.5 wt% of a mixture of CNT and PEDOT: PSS was spin-coated at 500 rpm for 5 seconds, 1200 rpm for 55 seconds, ) And heat-treated at 150 ° C for 20 minutes. Thereafter, Al 2 O 3 was deposited to a thickness of 1 nm on the patterned electrode using atomic layer deposition (ALD) to form an electron transport layer. Then, the color change material WO 3 15 wt% was spin-coated with ink for 5 seconds at 500 rpm, 5 seconds at 1000 rpm, 10 seconds at 2000 rpm, and 5 seconds at 1000 rpm for a total of 25 seconds, Lt; / RTI > The prepared electrochromic device of the present invention is shown in Fig.

<Experimental Example 1>

The transmittance of the electrochromic device prepared in Example 1 was confirmed. For this purpose, cyclic voltammetry was performed to confirm the permeability through area measurement. Referring to FIGS. 2A and 2B, it was confirmed that the electrochromic device of the present invention had a wider surface area than that of the control group (a device in which only WOx was deposited on an ITO glass). Therefore, it was confirmed that the electrochromic device of the present invention had an excellent transmittance.

<Experimental Example 2>

The discoloration of the electrochromic device manufactured in Example 1 and the sunlight transmittance at discoloration were confirmed by Delta OD (Delta Optical Density).

Referring to FIGS. 3 (a) and 3 (b), in the comparative example, 97.39% of discoloration and 33.98% of color development were obtained, and the electrochromic device of the present invention showed discoloration of 86.23% and color development of 26.89%. Therefore, it was confirmed that the electrochromic device of the present invention had a lower difference in discoloration and coloration, so that the solar transmittance was lower.

<Experimental Example 3>

In addition, the response speed of the electrochromic device manufactured in Example 1 was confirmed. For this, the response time of color development and discoloration was confirmed by comparing the reaction time of the electrochromic device of the present invention with that of the comparative example.

As a result, as shown in Figs. 4 (a) and 4 (b), it was confirmed that the color development time and the decoloration time of the comparative example were 27.88 s and 15.66 s, respectively. On the other hand, it was confirmed that the electrochromic device of the present invention exhibited a shorter reaction time than the comparative example, with a color development time of 17.80 s and a decolorization time of 7.16 s. Therefore, it was confirmed that the response speed is about twice as fast.

<Experimental Example 4>

Next, the discoloration efficiency index of the electrochromic device manufactured in Example 1 was confirmed and shown in FIG.

Referring to FIGS. 5A and 5B, the coloring efficiency of the comparative example was 15.57 Cm 2 / C, but the electrochromic device of the present invention showed a coloring efficiency of 45.97 Cm 2 / C. Therefore, it was confirmed that the electrochromic device of the present invention exhibits about 3 times better discoloration efficiency than the device of the comparative example.

It will be understood by those skilled in the art that the foregoing description of the embodiments is for illustrative purposes and that those skilled in the art will readily understand that various changes may be made without departing from the spirit and scope of the invention.

It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. For example, each component described as a single entity may be distributed and implemented, and components described as being distributed may also be implemented in a combined form. The scope of the present invention is defined by the appended claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be interpreted as being included in the scope of the present invention.

Claims (6)

Board;
A patterned electrode layer formed on the substrate;
An electron transport layer formed on the patterned electrode layer; And
A coloring layer formed on the electron transporting layer; And an electrochromic device. The method according to claim 1,
Wherein the electrode layer is formed by dispersing carbon nanotubes on a material selected from the group consisting of poly (3,4-ethylenedioxythiophene, PEDOT), polystyrene sulfonate (PSS), and combinations thereof. device. The method according to claim 1,
Wherein the pattern is repeatedly positioned in any one shape selected from the group consisting of a rectangle, a rectangle, a pyramid, a circle, a cylinder, a square, and combinations thereof. The method according to claim 1,
Wherein the electron transport layer comprises an oxide of a metal selected from the group consisting of aluminum, titanium, tin, zinc, tungsten, zirconium, gallium, indium, yttrium, niobium, tantalum, vanadium, device. The method according to claim 1,
The substrate is selected from the group consisting of indium tin oxide (ITO), fluorine tin oxide (FTO), ZnO-Ga 2 O 3 , ZnO-Al 2 O 3 , tin oxide, zinc oxide, glass, Wherein the electrochromic device comprises a glass substrate or a plastic substrate containing a material which is a material for forming the electrochromic device. Forming a patterned electrode layer on a substrate;
Forming an electron transport layer on the formed patterned electrode layer; And
And forming a coloring layer on the formed electron transport layer.

KR1020170079624A 2017-06-23 2017-06-23 Electrochromic device and preparing method thereof KR20190000521A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113745407A (en) * 2021-07-29 2021-12-03 暨南大学 Acid-induced color-changing electron transport layer, acid-induced color-changing organic solar cell integrated device and preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113745407A (en) * 2021-07-29 2021-12-03 暨南大学 Acid-induced color-changing electron transport layer, acid-induced color-changing organic solar cell integrated device and preparation method
CN113745407B (en) * 2021-07-29 2024-03-15 暨南大学 Acid-induced color electron transfer layer, acid-induced color organic solar cell integrated device and preparation method

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