CN114035389A - Electrochromic thin film structure capable of inhibiting self-fading/self-coloring and expanding potential window, and electrochromic device - Google Patents

Electrochromic thin film structure capable of inhibiting self-fading/self-coloring and expanding potential window, and electrochromic device Download PDF

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CN114035389A
CN114035389A CN202111313419.9A CN202111313419A CN114035389A CN 114035389 A CN114035389 A CN 114035389A CN 202111313419 A CN202111313419 A CN 202111313419A CN 114035389 A CN114035389 A CN 114035389A
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electrochromic
layer
lithium
film structure
self
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CN114035389B (en
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刘涌
曾宇
莫建良
韩高荣
徐刚
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Zhejiang University ZJU
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    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect
    • G02F1/153—Constructional details
    • G02F1/161—Gaskets; Spacers; Sealing of cells; Filling or closing of cells
    • 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
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect
    • G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
    • G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
    • G02F1/1524—Transition metal compounds

Abstract

The invention discloses an electrochromic film structure capable of inhibiting self-fading/self-coloring and expanding a potential window and an electrochromic device adopting the electrochromic film structure. The electrochromic thin film structure comprises a substrate, a transparent conducting layer, an electrochromic layer, a barrier layer and a liquid-phase electrolyte layer which are sequentially superposed, or the substrate, the transparent conducting layer, the electrochromic layer, the barrier layer and the solid-phase electrolyte layer which are sequentially superposed; the barrier layer is made of Si or SiO2‑x、SiO2、Ti、TiO2‑x、TiO20 < x < 2. The invention introduces a barrier layer between the conventional electrochromic layer and the liquid phase/solid phase electrolyte layer to inhibit the spontaneous coloring and fading behaviors of the material caused by balancing the electrochemical potential of the interface,the optical memory effect of the electrochromic material after coloring and fading is improved, and meanwhile, the material is protected from irreversible side reaction under the condition of over-high potential, so that the stability is improved.

Description

Electrochromic thin film structure capable of inhibiting self-fading/self-coloring and expanding potential window, and electrochromic device
Technical Field
The invention relates to the field of electrochromism, in particular to an electrochromic thin film structure capable of inhibiting self-fading/self-coloring and expanding a potential window, an electrochromic device and a method for inhibiting electrochromism from fading/self-coloring and expanding the potential window.
Background
Under the action of an external electric field, the electrochromic film generates reversible redox reaction, and stable optical modulation can be realized along with the embedding and the removing of ions.
The intelligent window for regulating and controlling visible light and infrared light based on electrochromism can reduce energy consumption of buildings while realizing indoor light and temperature comfort, so that the intelligent window has great market prospect and energy-saving significance.
Electrochromic materials are generally classified into cathodic electrochromic materials and anodic electrochromic materials according to reactions upon coloring.
A typical electrochromic device structure includes 5 layers, respectively a transparent conductive layer, a cathode electrochromic layer, an electrolyte layer, an anode electrochromic layer, and a transparent conductive layer.
Because the electrochromic layer and the electrolyte layer in the five-layer structure are in direct contact, the conditions that the electric double layer is gradually eliminated and the electrochemical potential of the electrolyte layer in direct contact with the surface of the electrochromic layer is changed exist after the electric double layer is established and the electric field is removed in the electrochemical reaction process, the electrochromic layer can perform self-fading and self-coloring actions for balancing the electrochemical potential, and the use of the device is not facilitated.
In addition, in order to pursue high modulation amplitude and response speed, higher overpotential is adopted for excitation, but impurities such as water molecules and the like and materials generate side reaction at the same time, and the materials are irreversibly damaged.
Therefore, it is necessary to overcome the self-fading and self-coloring behavior of the electrochromic device, obtain good optical memory effect, and achieve stable operation under a wide potential window.
Chinese patent CN109375446A proposes a method for maintaining the color fading state of electrochromic device by pulse voltage. The patent specification describes in detail driving an electrochromic device with a final voltage of increasing and larger absolute value a little beyond the preset state, and then maintaining the state of the device using a voltage pulse smaller than the absolute value of the driving voltage. The present invention is mainly aimed at maintaining a certain colored or faded state under the condition of not excessive potential, but the maintenance of the colored or faded state by applying the potential for a long time can greatly increase the energy consumption.
Chinese patent CN108037628A introduces an electrochromic film with stable performance and a preparation method thereof. The patent specification describes in detail that the electrochromic properties are degraded by depositing a protective layer barrier on the cross section of the electrochromic thin film system to block water molecules and gas molecular impurities in the environment from entering the electrochromic thin film; simultaneously introducing a transition layer Ta between the electrolyte layer and the electrochromic layer2O5Reducing leakage current improves the color memory effect and improves cycling stability. But Ta2O5The thickness of the transition layer is 200-250 nm, and the price of the material is higher than that of silicon and the like.
Disclosure of Invention
Aiming at the technical problems and the defects existing in the field, the invention provides an electrochromic film structure capable of inhibiting electrochromic self-fading/self-coloring and expanding a potential window, wherein a barrier layer is introduced between a conventional electrochromic layer and a solid-phase/liquid-phase electrolyte layer, the barrier layer prevents the electrochromic layer from being in direct contact with the solid-phase/liquid-phase electrolyte layer, inhibits the spontaneous coloring and fading behaviors of the material caused by balancing the electrochemical potential of an interface, improves the optical memory effect of the electrochromic material after coloring and fading, simultaneously protects the material from irreversible side reaction under the condition of over-high potential, and improves the stability.
An electrochromic film structure that suppresses self-fading/self-coloring and expands the potential window, comprising:
a substrate, a transparent conductive layer, an electrochromic layer, a barrier layer, a liquid-phase electrolyte layer, or,
the substrate, the transparent conducting layer, the electrochromic layer, the barrier layer and the solid electrolyte layer are sequentially superposed;
the barrier layer is made of Si and SiO2-x、SiO2、Ti、TiO2-x、TiO2Any one or more of (a), wherein 0 < x < 2;
the total thickness of the barrier layer is 1-500 nm.
In the electrochromic film structure, the barrier layer can be prepared by means of magnetron sputtering and other methods commonly used in the field.
In a preferred embodiment, in the electrochromic film structure, the barrier layer is made of a Si material and has a thickness of 1-30 nm. The inventor researches and discovers that when the barrier layer is made of Si materials, the barrier layer can play an excellent effect of inhibiting self-fading/self-coloring and expanding a potential window under the condition of an ultrathin thickness of 1-30 nm.
In a preferred embodiment, in the electrochromic thin film structure, the substrate is made of a highly transparent material, and specifically may be one or more of a glass substrate, a sapphire substrate, an aluminum oxynitride substrate, a spinel substrate, and a transparent polymer, and is preferably a glass substrate.
In a preferred example, in the electrochromic thin film structure, the material of the transparent conductive layer is an oxide, and specifically, the material may be one or more of Indium Tin Oxide (ITO), fluorine-doped tin oxide (FTO), and Aluminum Zinc Oxide (AZO), and is preferably fluorine-doped tin oxide (FTO).
In a preferred embodiment, in the electrochromic film structure, the thickness of the transparent conductive layer is 250 to 350 nm.
In a preferred embodiment, in the electrochromic thin film structure, the material of the electrochromic layer is an electrochromic material, and specifically may be tungsten oxide (WO)3-yY is 0-1), molybdenum oxide (MoO)3)、NiO、Ni2O3、Nb2O5、TiO2、Ir2O3、V2O5、Rh2O3、CoOz(1. ltoreq. z. ltoreq.1.5), preferably cathode discoloration material tungsten oxide (WO)3-y，0≤y≤1)。
In a preferred embodiment, in the electrochromic film structure, the thickness of the electrochromic layer is 200 to 400 nm.
In a preferred embodiment of the electrochromic film structure, the liquid-phase electrolyte layer is a propylene carbonate solution of lithium perchlorate (a solution of lithium perchlorate dissolved in propylene carbonate), wherein the concentration of lithium perchlorate is preferably 0.5M.
In a preferred embodiment, in the electrochromic thin film structure, the material of the solid electrolyte layer is one or more of metal lithium, lithium cobaltate, lithium phosphate, lithium nitride phosphate, lithium iron phosphate, lithium silicate, lithium aluminate, lithium aluminum silicate, lithium chromate, lithium boron sulfate, lithium vanadate, lithium nickel vanadate, lithium tantalate, lithium nitride, lithium titanate, lithium nickelate, lithium manganate, lithium carbonate, nickel oxide, vanadium oxide, molybdenum oxide, titanium oxide, chromium oxide, and tantalum oxide.
The invention also provides an electrochromic device capable of inhibiting self-fading/self-coloring and expanding a potential window, and the electrochromic device adopts the electrochromic film structure.
As a general inventive concept, the present invention also provides a method of suppressing electrochromic self-fading/self-coloring and extending a potential window, comprising: setting a barrier layer with the total thickness of 1-500 nm between an electrochromic layer and a liquid-phase electrolyte layer or between the electrochromic layer and a solid-phase electrolyte layer of an electrochromic device, wherein the barrier layer is made of Si and SiO2-x、SiO2、Ti、TiO2-x、TiO2Any one or more of them, wherein 0 < x < 2.
Compared with the prior art, the invention has the main advantages that:
according to the invention, the barrier layer with a specific thickness is introduced between the traditional electrochromic layer and the liquid phase/solid phase electrolyte layer, so that the electrochromic layer can be prevented from directly contacting the electrolyte layer with an electrochemical potential difference, ions are inhibited from spontaneously embedding and separating from the material, the electrochromic optical memory effect is improved, and the material is prevented from side reaction under a high over potential.
Drawings
FIG. 1 is a graph of the coloration of an electrochromic tungsten oxide film with and without a barrier layer at-1.8V for 60 seconds, followed by standing for 120 seconds with a spectral change in transmittance at 550 nm;
FIG. 2 is a graph of the change in transmittance spectrum at 550nm for a tungsten oxide electrochromic film with and without a barrier layer at 1.8V for 90s and then left for 120 s;
FIG. 3 is a graph of the change in transmittance spectrum at 550nm for a tungsten oxide electrochromic film with a barrier layer painted 90s at-2.0V and left at rest for 120s, faded at 2.0V for 120s and left at rest for 120 s;
FIG. 4 shows the transmittance of an electrochromic film of tungsten oxide with and without a barrier layer in the colored state and the bleached state in the wavelength range of 300 to 800nm, measured at a potential window of-2.0V for 90s and at a potential window of 2.0V for 120 s.
Detailed Description
The invention is further described with reference to the following drawings and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are conducted under conditions not specified, usually according to conventional conditions, or according to conditions recommended by the manufacturer.
Example 1
The electrochromic thin film structure with the barrier layer comprises a substrate, a transparent conductive oxide layer, an electrochromic layer, a barrier layer and a liquid-phase electrolyte layer which are sequentially superposed, wherein:
the substrate is a glass substrate;
the transparent conductive oxide layer is made of fluorine-doped tin oxide (FTO) and has the thickness of 300 nm;
the electrochromic layer is made of cathode electrochromic material tungsten oxide and is 350nm thick;
the barrier layer is made of Si and has the thickness of 15 nm;
the liquid-phase electrolyte layer is a solution obtained by dissolving lithium perchlorate in propylene carbonate, wherein the concentration of the lithium perchlorate is 0.5M.
And a metal Pt electrode is arranged in the liquid-phase electrolyte layer to be used as a counter electrode.
Compared with the electrochromic film structure with the barrier layer, the electrochromic film structure without the barrier layer is different only in that no barrier layer is arranged, and the rest parts are the same.
To determine whether the barrier layer inhibited the self-fading and self-coloring behavior, as shown in fig. 1 and 2, the cathodic electrochromic material tungsten oxide with and without barrier layer, respectively, was tested in a three-electrode system with tungsten oxide as the working electrode, metallic Pt electrode as the counter electrode, and Ag/AgCl as the reference electrode. A process of coloring by applying 60s at a potential of-1.8V and fading by applying 90s at a potential of 1.8V.
After the voltage is removed after coloring and fading, the sample is kept standing for a fixed time, and in the sample without the barrier layer, the sample undergoes self-fading after coloring, 2.2% of modulation amplitude is lost, and the transmittance is stable and only fluctuates by 0.4% compared with the sample with the barrier layer. The sample without the barrier layer after fading underwent severe self-coloration behavior during standing, with a reduction in transmission of 11.9%, while the sample with the barrier layer after standing exhibited no more than a 0.1% change in transmission.
Example 2
The same electrochromic film structure with a barrier layer and the same electrochromic film structure without a barrier layer as in example 1 were used.
Samples with and without a barrier layer were applied at-2.0V for 90s and 2.0V for 120s, respectively, to verify whether the barrier layer would still function under conditions of an excessively large potential window and an excessively long application time (i.e., using an excitation condition at a potential greater than the usual potential and a potential longer than the usual time, the conventionally applied potential would not exceed the open circuit potential by ± 1.5V, for pursuing a large modulation amplitude and a fast response), and to maintain the stability of the sample.
As shown in fig. 3, the sample with the barrier layer still has excellent optical memory effect. As shown in FIG. 4, the initial transmittance at 300 to 800nm, and the colored and bleached state transmittances in the window of the excessive potential are shown for both samples. The result shows that the sample without the barrier layer has serious irreversible damage, and the barrier layer is verified to improve the stability of the material under an expanded potential window.
Example 3
Compared with the electrochromic film structure with the barrier layer in the embodiment 1, the electrochromic film structure is only different in that the material of the barrier layer is SiO2The thickness was 20nm, and the rest were the same.
Example 4
Compared with the electrochromic film structure with the barrier layer in the embodiment 1, the electrochromic film structure is only different in that the material of the barrier layer is TiO2The thickness was 13nm, and the rest were the same.
Example 5
Compared with the electrochromic film structure with the barrier layer in the embodiment 1, the electrochromic film structure is only different in that the material of the barrier layer is Ti, the thickness is 10nm, and the rest is the same.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention as defined by the appended claims.

Claims (9)

1. An electrochromic film structure capable of suppressing self-discoloration/self-coloring and extending a potential window, comprising:
a substrate, a transparent conductive layer, an electrochromic layer, a barrier layer, and a liquid-phase electrolyte layer, which are sequentially stacked, or,
the substrate, the transparent conducting layer, the electrochromic layer, the barrier layer and the solid electrolyte layer are sequentially superposed;
the barrier layer is made of Si and SiO2-x、SiO2、Ti、TiO2-x、TiO2Any one or more of (a), wherein 0 < x < 2;
the total thickness of the barrier layer is 1-500 nm.
2. The electrochromic film structure of claim 1, wherein the barrier layer is made of Si and has a thickness of 1-30 nm.
3. The electrochromic thin film structure of claim 1, wherein the substrate is one or more of a glass substrate, a sapphire substrate, an aluminum oxynitride substrate, a spinel substrate, and a transparent polymer.
4. The electrochromic thin film structure according to claim 1, wherein the material of the transparent conductive layer is one or more of an oxide, in particular Indium Tin Oxide (ITO), fluorine-doped tin oxide (FTO), Aluminum Zinc Oxide (AZO);
the thickness of the transparent conducting layer is 250-350 nm.
5. Electrochromic film structure according to claim 1, characterized in that the material of the electrochromic layer is an electrochromic material, in particular WO3-y、MoO3、NiO、Ni2O3、Nb2O5、TiO2、Ir2O3、V2O5、Rh2O3、CoOzWherein y is more than or equal to 0 and less than or equal to 1, and z is more than or equal to 1 and less than or equal to 1.5;
the thickness of the electrochromic layer is 200-400 nm.
6. The electrochromic film structure of claim 1, wherein the liquid electrolyte layer is a solution of lithium perchlorate in propylene carbonate.
7. The electrochromic film structure of claim 1, wherein the material of the solid electrolyte layer is one or more of metallic lithium, lithium cobaltate, lithium phosphate, lithium nitride phosphate, lithium iron phosphate, lithium silicate, lithium aluminate, lithium aluminum silicate, lithium chromate, lithium boron sulfate, lithium vanadate, lithium nickel vanadate, lithium tantalate, lithium nitride, lithium titanate, lithium nickelate, lithium manganate, lithium carbonate, nickel oxide, vanadium oxide, molybdenum oxide, titanium oxide, chromium oxide, and tantalum oxide.
8. An electrochromic device capable of suppressing self-fading/self-coloring and extending a potential window, characterized by using the electrochromic film structure according to any one of claims 1 to 7.
9. A method of inhibiting electrochromic self-fade/self-coloration and extending the potential window, comprising: setting a barrier layer with the total thickness of 1-500 nm between an electrochromic layer and a liquid-phase electrolyte layer or between the electrochromic layer and a solid-phase electrolyte layer of an electrochromic device, wherein the barrier layer is made of Si and SiO2-x、SiO2、Ti、TiO2-x、TiO2Any one or more of them, wherein 0 < x < 2.
CN202111313419.9A 2021-11-08 2021-11-08 Electrochromic thin film structure capable of inhibiting self-fading/self-coloring and expanding potential window, and electrochromic device Active CN114035389B (en)

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