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WO2018199570A1 - Film transmettant la lumière et élément électrochromique le comprenant - Google Patents

Film transmettant la lumière et élément électrochromique le comprenant Download PDF

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Publication number
WO2018199570A1
WO2018199570A1 PCT/KR2018/004672 KR2018004672W WO2018199570A1 WO 2018199570 A1 WO2018199570 A1 WO 2018199570A1 KR 2018004672 W KR2018004672 W KR 2018004672W WO 2018199570 A1 WO2018199570 A1 WO 2018199570A1
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WO
WIPO (PCT)
Prior art keywords
film
layer
light
electrochromic
transmittance
Prior art date
Application number
PCT/KR2018/004672
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English (en)
Korean (ko)
Inventor
김용찬
김기환
Original Assignee
주식회사 엘지화학
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from KR1020180045418A external-priority patent/KR102202928B1/ko
Application filed by 주식회사 엘지화학 filed Critical 주식회사 엘지화학
Priority to JP2019557574A priority Critical patent/JP7051183B2/ja
Priority to EP18790688.8A priority patent/EP3617771B1/fr
Priority to US16/604,841 priority patent/US11409178B2/en
Priority to CN201880026866.6A priority patent/CN110573953B/zh
Publication of WO2018199570A1 publication Critical patent/WO2018199570A1/fr

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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
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B26/00—Optical devices or arrangements for the control of light using movable or deformable optical elements
    • G02B26/02—Optical devices or arrangements for the control of light using movable or deformable optical elements for controlling the intensity of light

Definitions

  • the present application relates to a light transmitting film and an electrochromic device including the same.
  • Electrochromic refers to a phenomenon in which the optical properties of the electrochromic material are changed by a reversible electrochemical oxidation or reduction reaction, and the device using the phenomenon is called an electrochromic device.
  • the change in the optical properties of the device can be realized through the color change of the layer or film containing the electrochromic material.
  • WO 3 which is almost colorless and transparent as an electrochromic material
  • a reduction reaction occurs when electrolyte ions and electrons are moved by voltage application, and the color of the layer or film including the electrochromic material becomes blue. It is colored.
  • an oxidation reaction occurs in the layer or film, the layer or film is discolored to its original transparent state. In order for such discoloration to be fully realized in the device, not only the electrochromic layer or film in the discolored state, but also other layer or film configurations laminated together must have sufficient transparency (transmittance).
  • One object of the present application is to provide a light transmissive film that can be used in an electrochromic device.
  • Another object of the present application is to provide a light transmissive film capable of reversible discoloration depending on the voltage applied.
  • Still another object of the present application is to provide a light transmissive film for electrochromic device having excellent durability.
  • Still another object of the present application is to provide an electrochromic device including a transmissive film capable of reversible discoloration according to an applied voltage.
  • the present application relates to a light transmissive film.
  • the term “transmittance” may mean a case where the optical characteristic such as color change occurring in the electrochromic device is transparent enough to clearly recognize, and there is no external factor such as, for example, potential application.
  • the state that is, the decoloring state described below
  • the light transmittance of the film itself is at least 60% or more. More specifically, the lower limit of light transmittance of the light transmitting film of the present application may be 60% or more, 70% or more, or 75% or more, and the upper limit of the light transmittance may be 95% or less, 90% or less, or 85% or less.
  • light in the present application may mean visible light in the wavelength range of 380 nm to 780 nm, and more specifically, visible light in the 550 nm wavelength.
  • the transmittance can be measured using a known haze meter (HM).
  • the light transmissive film may include an oxynitride.
  • the light transmissive film may be an oxynitride having one layer or film form or a laminate of an oxynitride having a layer or film form and another layer or film configuration.
  • oxynitride is used differently from oxide or nitride.
  • the oxynitride may include two or more metals selected from Ti, Nb, Mo, Ta, and W.
  • the oxynitride of the light transmissive film may include Mo and Ti at the same time.
  • nitrides, oxides or oxynitrides containing only Mo are poor in adhesion to adjacent thin films, and nitrides, oxides or oxynitrides containing only Ti are poor in durability, such as decomposing upon application of potential.
  • nitrides or oxynitrides containing any one of the metals listed above, such as Ti alone or Mo only are for example 40% or less, 35% or less or 30% or less, even when no potential is applied.
  • the difference in the transmittance at the time of coloration and the transmittance at the time of decolorization such as the difference in the apparent optical properties of the coloration and decolorization required in the electrochromic device. Difficult to show
  • the oxynitride may be represented by the following formula (1).
  • a means an element content ratio of Mo
  • b means an element content ratio of Ti
  • x means an element content ratio of O
  • y means an element content ratio of N
  • the term "element content ratio" in the present application may be atomic%, and may be measured by X-ray photoelectron spectroscopy (XPS).
  • XPS X-ray photoelectron spectroscopy
  • the light transmissive film may be a variable transmittance film that transmits light when a predetermined voltage is applied.
  • the permeability variable properties result from the reduction discoloration properties of the oxynitrides described above.
  • the oxynitride included in the film has a light transmittance close to colorless in an intact state without an electrochemical reaction, but when a predetermined voltage is applied, discoloration, ie, coloration, occurs at a predetermined level or more with a reduction reaction with the electrolyte ions.
  • the oxynitride is a reducing discoloration material.
  • the film is an electrochromic transmittance variable film having a light transmittance of 60% or more when decoloring (or discoloring) and having a light transmittance of less than 60% when coloring.
  • the light transmissive film can be colored under voltage application conditions of -2V or less, for example -2.5V or less or -3V or less. That is, the colored level of the light transmissive film may be 2 V, 2.5 V or 3 V.
  • the term “colored level” refers to an electrochemical reaction caused by a transmissive film or a predetermined voltage applied to a half-cell including the film and the conductive layer, and as a result, the translucent film is colored.
  • the transmittance of the film may be reduced, such as “minimum size (absolute value)” of a voltage that may cause coloration of the film.
  • the coloring level i.e., the minimum magnitude (absolute value) of the voltage causing coloring
  • the coloring level of a light transmissive film can change to some extent according to a specific structure in 2 V or more range. When colored, the light transmissive film may have a color of (dark) gray or black color.
  • the coloring level of oxides including any one of known color change materials for example, Ti, Nb, Mo, Ta, and W, is about 1V, the light-transmitting film of the present application may be said to have excellent durability against high voltage. Can be.
  • the upper limit of the voltage magnitude (absolute value) applied for coloring of the film is not particularly limited, but may be, for example, 6 V or less. If it exceeds 6V, the light transmissive film, or another structure adjacent thereto, may deteriorate.
  • the thickness of the light transmissive film may be 150 nm or less.
  • the light transmissive film may have a thickness of 140 nm or less, 130 nm or less, or 120 nm or less.
  • the lower limit of the thickness of the light transmissive film is not particularly limited, but may be, for example, 10 nm or more, 20 nm or more, or 30 nm or more. If it is less than 10 nm, the film stability is not good.
  • the light refractive index of the light transmitting film may be in the range of 1.5 to 3.0 or 1.8 to 2.8.
  • the visible light refractive index is in the above range, the light-transmitting film may implement visibility with respect to the appropriate transparency and optical properties change.
  • the method for forming the light transmissive film is not particularly limited.
  • a known deposition method such as sputter deposition can be used in forming the light transmitting film.
  • the present application relates to an electrochromic device.
  • the device may include an electrode layer, a light transmitting film, and an electrolyte (layer).
  • the form in which the element includes an electrode layer, a light transmitting film, and an electrolyte (layer) is not particularly limited.
  • the device may sequentially include an electrode layer, a light transmitting film, and an electrolyte (layer).
  • the light transmissive film used for the electrochromic device may have the same configuration as mentioned above. Since the translucent film which has the said structure can have a visible light transmittance of 60% or more, it is suitable as a film for electrochromic elements. Further, as described above, since it can be colored when a predetermined voltage is applied, it can also be used as a so-called electrochromic layer. Specifically, the light-transmitting film may have a transmittance of 60% or more by itself when decolorized, that is, uncolored, and when colored, transmittance of less than 60%, for example, 45% or less, 30, while the transmittance becomes low. It can have a transmittance of less than or equal to 20%. In one example, the light transmissive film may have a light transmittance difference of 20% or more or 30% or more during coloring and decolorization.
  • the electrochromic device may also have a visible light transmittance of 60% or more, more specifically in the range of 60% to 95%.
  • the electrochromic device may have a light transmittance difference of 10% or more, 20% or more, or 30% or more in coloration and decolorization.
  • the electrode layer may include a conductive compound, metal mesh, or OMO (oxide / metal / oxide).
  • ITO Indium Tin Oxide
  • IGO indium galium oxide
  • FTO Fluor doped Tin Oxide
  • AZO Alium doped Zinc Oxide
  • GZO Ga doped Zinc Oxide
  • ATO Antimony doped Tin Oxide
  • IZO Indium doped Zinc Oxide
  • NTO Niobium doped Titanium Oxide
  • ZnO zink oxide
  • CTO Cesium Tungsten Oxide
  • the materials listed above are not limited to the material of the transparent conductive compound.
  • the metal mesh used for the electrode layer may include Ag, Cu, Al, Mg, Au, Pt, W, Mo, Ti, Ni, or an alloy thereof, and may have a lattice form.
  • the materials usable for the metal mesh are not limited to the metal materials listed above.
  • the electrode layer may comprise oxide / metal / oxide (OMO). Since the OMO has a lower surface resistance than the transparent conductive oxide represented by ITO, it is possible to improve the electrical properties of the electrochromic device by reducing the color change rate.
  • OMO oxide / metal / oxide
  • the OMO may include a top layer, a bottom layer, and a metal layer provided between the two layers.
  • the upper layer may mean a layer located relatively farther from the translucent film among the layers constituting the OMO.
  • the top and bottom layers of an OMO electrode include Sb, Ba, Ga, Ge, Hf, In, La, Se, Si, Ta, Se, Ti, V, Y, Zn, Zr or oxides of these alloys. can do.
  • the type of each metal oxide included in the upper layer and the lower layer may be the same or different.
  • the thickness of the top layer may range from 10 nm to 120 nm or from 20 nm to 100 nm.
  • the visible light refractive index of the upper layer may be in the range of 1.0 to 3.0 or 1.2 to 2.8.
  • the thickness of the lower layer may range from 10 nm to 100 nm or from 20 nm to 80 nm.
  • the visible light refractive index of the lower layer may be in the range of 1.3 to 2.7 or 1.5 to 2.5.
  • the metal layer included in the OMO electrode may include a low resistance metal material.
  • a low resistance metal material for example, one or more of Ag, Cu, Zn, Au, Pd, and alloys thereof may be included in the metal layer.
  • the metal layer may have a thickness in the range of 3 nm to 30 nm or in the range of 5 nm to 20 nm.
  • the metal layer may have a visible light refractive index of 1 or less or 0.5 or less. When having a refractive index and a thickness in the above range, an appropriate level of optical properties can be imparted to the electrode layer and the device.
  • the electrode layer of the above configuration may have a thickness of 50 nm to 400 nm or less.
  • the light transmittance can be appropriately implemented within the thickness range.
  • the device may include another electrode layer.
  • the electrode layer may be referred to as first and second electrode layers according to positions relative to other configurations.
  • the device may sequentially include a first electrode layer, an electrolyte layer, the light transmissive film, and a second electrode layer.
  • the configuration of each electrode layer is the same as mentioned above.
  • the electrolyte layer may be configured to provide electrolyte ions involved in the electrochromic reaction.
  • Electrolyte ions may be monovalent cations, such as H + , Li + , Na + , K + , Rb + , or Cs + , which are inserted into the light transmissive film and which may be involved in the discoloration reaction.
  • the kind of electrolyte is not particularly limited.
  • liquid electrolytes, gel polymer electrolytes or inorganic solid electrolytes can be used without limitation.
  • the electrochromic film composition can include a compound capable of providing a monovalent cation such as H + , Li + , Na + , K + , Rb + , or Cs +
  • the composition of the specific compound used in the electrolyte layer Is not particularly limited.
  • the electrolyte may be LiClO 4 , LiBF 4 , LiAsF 6 , or LiPF 6 It may include a lithium salt compound, such as, or a sodium salt compound such as NaClO 4 .
  • the electrolyte layer may include a carbonate compound as a solvent. Since a carbonate type compound has high dielectric constant, ionic conductivity can be improved.
  • a solvent such as propylene carbonate (PC), ethylene carbonate (EC), dimethyl carbonate (DMC), diethyl carbonate (DEC) or ethylmethyl carbonate (EMC) may be used as the carbonate-based compound.
  • the electrolyte layer may be polyvinylidene fluoride (PVdF), polyacrylonitrile (PAN), polymethyl methacrylate ( Polymethyl methacrylate (PMMA), Polyvinyl chloride (PVC), Polyethylene oxide (PEO), Polypropylene oxide (PPO), Poly (vinylidene fluoride-hexafluoro fluoropropylene) ( Poly (vinylidene fluoride-hexafluoro propylene), PVdF-HFP), polyvinylacetate (Polyvinyl acetate, PVAc), polyoxyethylene (Polyoxyethylene, POE), polyamideimide (Polyamideimide, PAI) and the like may be included.
  • PVdF polyvinylidene fluoride
  • PAN polyacrylonitrile
  • PMMA Polymethyl methacrylate
  • PVC Polyethylene oxide
  • PPO Polypropylene oxide
  • PVdF-HFP Polyvinylacetate
  • the thickness of the electrolyte layer may range from 10 ⁇ m to 200 ⁇ m.
  • the electrochromic device of the present application may further include a second electrochromic layer.
  • the device may further include a second electrochromic layer between the first electrode layer and the electrolyte.
  • the electrochromic translucent film may be referred to as a first electrochromic layer.
  • the second electrochromic layer may have a color change characteristic different from that of the first electrochromic layer. That is, the second electrochromic layer may include an oxidative discoloring material that may be colored when oxidized. As such, when the color development (color change) characteristics of the color change material used in each of the first and second electrochromic layers are different, the second electrochromic layer is different from the first electrochromic layer during oxidation and reduction for electrochromic. You can set the charge balance of.
  • the oxidative discoloration material included in the second electrochromic layer such as LiNiOx, IrO 2 , NiO, V 2 O 5 , LixCoO 2 , Rh 2 O 3 or CrO 3 , Cr, Mn, Fe, Oxides of Co, Ni, Rh, or Ir; Hydroxides of Cr, Mn, Fe, Co, Ni, Rh, or Ir; And prussian blue.
  • the thickness of the second electrochromic layer may range from 50 nm to 450 nm.
  • the electrochromic device may further include a substrate.
  • the substrate may be located on the outer side of the device, for example on the outer side of the first and / or second electrode layer.
  • the substrate may also have a visible light transmittance of 60% to 95%. If the transmittance
  • glass or polymer resins can be used. More specifically, a polyester film such as polycarbonate (PC), polyethylene (phthalene naphthalate) (PEN) or polyethylene (ethylene terephthalate) (PET), an acrylic film such as poly (methyl methacrylate) (PMMA), or polyethylene (PE) Or a polyolefin film such as PP (polypropylene) may be used, but is not limited thereto.
  • the electrochromic device may further include a power source.
  • the manner of electrically connecting the power source to the device is not particularly limited and may be appropriately made by those skilled in the art.
  • a film having not only light transmittance but also reversible discoloration according to an applied voltage and excellent in resistance to high voltage may be provided.
  • Example 1 is a graph showing a state in which the laminate of the present application Example 1 is driven without degradation in durability when a voltage of ⁇ 5 V is applied.
  • ITO having a light transmittance of about 90% was formed on one surface of glass (galss) having a light transmittance of about 98%.
  • an oxynitride (Mo a Ti b O x N y ) layer containing Mo and Ti was formed on the one surface of ITO (as opposed to the glass position) by sputter deposition to form a thickness of 30 nm (Preparation Example 1).
  • the weight percent ratio of the target of Mo and Ti was 1: 1, the deposition power was 100 W, the process pressure was deposited at 15 mTorr, and each flow rate of Ar, N 2 and O 2 was 30 sccm, 5 sccm, and 5 sccm.
  • Nitrogen nitride layer was formed in the same manner as in Example 1, except that the flow rate of nitrogen was 10 sccm during deposition and the content ratio was changed as shown in Table 1 (Preparation Example 2).
  • Nitrogen nitride layer was formed in the same manner as in Example 1, except that the flow rate of nitrogen was 15 sccm during deposition, and the content ratio was changed as shown in Table 1 (Preparation Example 3).
  • An oxide layer was formed in the same manner as in Example 1 except that the flow rate of nitrogen was 0 sccm during deposition and the content ratio was changed as shown in Table 1 (Preparation Example 4).
  • the oxynitride layers of Comparative Examples 1 to 3 have very low transmittance, while the oxynitride layer of Example 1 has a transmittance of about 90%.
  • the oxynitride or the light-transmitting laminate including the same used in Example 1 can be used as a member for the electrochromic device.
  • Example 2 The laminate prepared in Example 1 (glass / ITO / oxynitride (Mo a Ti b O x N y ) (half-cell) was immersed in an electrolyte containing LiClO 4 (1M) and propylene carbonate (PC), 25 Coloring voltage of ⁇ 3 V and decolorization voltage of +3 V were applied alternately at 50 ° C. for 50 seconds, respectively.
  • the currents, transmittances, and discoloration times at the time of coloration and decolorization measured over time are as shown in Table 2. .
  • the laminate including the light-transmitting film of the present application has a discoloration characteristic when a potential having a size of 3 V or more is applied.
  • Fig. 1 is a graph showing the state in which the laminate (electrochromic device) of Example 2 is driven when a driving potential of ⁇ 5 V is applied. 1, it can be seen that the laminate including the light-transmitting film of the present application exhibits uniform cycle characteristics even when a relatively high driving potential is applied and operates without deterioration in durability.

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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

La présente invention concerne un film transmettant la lumière et un élément le comprenant. Le film présente une transmissivité de lumière, permet un chromisme réversible en fonction d'une tension appliquée et présente une excellente durabilité dans une plage de tension de pilotage de chromisme.
PCT/KR2018/004672 2017-04-24 2018-04-23 Film transmettant la lumière et élément électrochromique le comprenant WO2018199570A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2019557574A JP7051183B2 (ja) 2017-04-24 2018-04-23 透光性フィルムおよびこれを含むエレクトロクロミック素子
EP18790688.8A EP3617771B1 (fr) 2017-04-24 2018-04-23 Film transmettant la lumière et élément électrochromique le comprenant
US16/604,841 US11409178B2 (en) 2017-04-24 2018-04-23 Light-transmitting film and an electrochromic device comprising the same
CN201880026866.6A CN110573953B (zh) 2017-04-24 2018-04-23 透光膜和包括其的电致变色装置

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2017-0052047 2017-04-24
KR20170052047 2017-04-24
KR10-2018-0045418 2018-04-19
KR1020180045418A KR102202928B1 (ko) 2017-04-24 2018-04-19 투광성 필름 및 이를 포함하는 전기변색소자

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WO2018199570A1 true WO2018199570A1 (fr) 2018-11-01

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PCT/KR2018/004672 WO2018199570A1 (fr) 2017-04-24 2018-04-23 Film transmettant la lumière et élément électrochromique le comprenant

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WO (1) WO2018199570A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060089643A (ko) * 2005-02-04 2006-08-09 신에쓰 가가꾸 고교 가부시끼가이샤 반투명 적층막, 포토마스크 블랭크, 포토마스크 및 이들의제조방법
US7099062B2 (en) * 2001-09-26 2006-08-29 Forskarpatent I Uppsala Ab Electrochromic film and device comprising the same
KR101271371B1 (ko) * 2011-07-11 2013-06-07 주식회사 피케이엘 평판 디스플레이 소자의 제조에 사용되는 그레이 톤 마스크 및 그 제조방법
KR101501104B1 (ko) * 2012-12-28 2015-03-10 전자부품연구원 스마트 윈도우용 유연한 다기능성 적층체 필름
KR20160104584A (ko) * 2015-02-26 2016-09-05 주식회사 엘지화학 전도성 구조체 및 이의 제조방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7099062B2 (en) * 2001-09-26 2006-08-29 Forskarpatent I Uppsala Ab Electrochromic film and device comprising the same
KR20060089643A (ko) * 2005-02-04 2006-08-09 신에쓰 가가꾸 고교 가부시끼가이샤 반투명 적층막, 포토마스크 블랭크, 포토마스크 및 이들의제조방법
KR101271371B1 (ko) * 2011-07-11 2013-06-07 주식회사 피케이엘 평판 디스플레이 소자의 제조에 사용되는 그레이 톤 마스크 및 그 제조방법
KR101501104B1 (ko) * 2012-12-28 2015-03-10 전자부품연구원 스마트 윈도우용 유연한 다기능성 적층체 필름
KR20160104584A (ko) * 2015-02-26 2016-09-05 주식회사 엘지화학 전도성 구조체 및 이의 제조방법

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