CN112394580A - All-solid-state fast response electrochromic device and preparation method thereof - Google Patents
All-solid-state fast response electrochromic device and preparation method thereof Download PDFInfo
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- CN112394580A CN112394580A CN202010970612.9A CN202010970612A CN112394580A CN 112394580 A CN112394580 A CN 112394580A CN 202010970612 A CN202010970612 A CN 202010970612A CN 112394580 A CN112394580 A CN 112394580A
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- electrochromic
- ion storage
- transition
- inert gas
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Images
Classifications
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- G—PHYSICS
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- 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
- G02F1/1525—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 characterised by a particular ion transporting layer, e.g. electrolyte
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0676—Oxynitrides
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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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
- G02F1/1514—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 all-solid-state quick response electrochromic device, which relates to the field of electrochromic and comprises a substrate, a first conducting layer, an electrochromic layer, an ion conducting layer, an ion storage layer and a second conducting layer, wherein the first conducting layer, the electrochromic layer, the ion conducting layer, the ion storage layer and the second conducting layer are sequentially arranged on the substrate; further comprising: a transition layer; the transition layer is located between the electrochromic layer and the first conducting layer or at least one of the ion storage layers, and the transition layer is an uneven conducting film layer. The invention has the technical effects that: by adding the transition layer, the conductivity of the electrode is increased. And the electron and ion mobility of the film can be adjusted by adjusting the coverage rate of the transition layer on the functional layer of the electrochromic device, so that the improvement of the coloring and fading uniformity is realized. In addition, the electrochromic glass can have wider infrared regulation and control capability.
Description
Technical Field
The invention relates to the field of electrochromism, in particular to an all-solid-state quick response electrochromism device and a preparation method thereof.
Background
Electrochromism refers to a phenomenon in which optical properties (reflectivity, transmittance, absorption, etc.) undergo a stable, reversible color change under the action of an applied electric field. Electrochromic technology has been developed for more than forty years, and Electrochromic devices (ECDs) have wide application prospects in the fields of intelligent windows, displays, spacecraft temperature control modulation, automobile no-glare rearview mirrors, weapon equipment stealth and the like due to the characteristics of continuous adjustability of transmitted light intensity, low energy loss, open-circuit memory function and the like. With the continuous improvement of the requirements of human beings on consumer products, the ECD shows huge market prospects and application values in the fields of automobiles, home appliances, aerospace, rail transit, green buildings and the like, and electrochromic products attract more and more extensive attention and attention at home and abroad and are a new generation of high-efficiency building energy-saving products after heat-absorbing glass, heat-reflecting coated glass and low-radiation glass.
In the traditional electrochromic device, the conducting layer is made of Transparent metal Oxide (TCO) film, and the conductivity and the water vapor isolation of the TCO film are worse than those of the metal film, but the metal film cannot ensure high ion transmission efficiency under the condition of ensuring high conductivity. Therefore, the TCO film is used in the conventional electrochromic device, but the problems of poor conductivity and poor water vapor isolation are not solved.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problem to be solved by the present invention is to enhance the electrical conductivity and moisture barrier properties of electrochromic devices.
In order to achieve the above object, the present invention provides an all-solid-state fast response electrochromic device, comprising a substrate, and a first conductive layer, an electrochromic layer, an ion conducting layer, an ion storage layer, and a second conductive layer sequentially disposed on the substrate; wherein a stack of the electrochromic layer up to a face of the ion storage layer is rugged.
Further, still include: a first transition layer; the first transition layer is located between the electrochromic layer and the first conducting layer, and the first transition layer is a smooth or uneven conducting film layer.
Further, still include: and the second transition layer is positioned in the ion storage layer and is an uneven conductive film layer.
Further, the first transition layer and the second transition layer are selected from one or more of the following materials: silver, aluminum, copper, nichrome.
Further, the first transition layer is a mesh-shaped conductive film layer, and a contact interface is included between the electrochromic layer and the first conductive layer.
Further, a coverage of the transition layer between the electrochromic layer and the first conductive layer on the first conductive layer is 15 to 80%.
Further, the second transition layer is a mesh-shaped conductive film layer, the ion storage layer comprises a first ion storage layer and a second ion storage layer, and a contact interface is arranged between the first ion storage layer and the second ion storage layer.
Further, the coverage of the second transition layer on the first ion storage layer is 3 to 60%.
Further, a cathodic coloring material is included in the electrochromic layer and an anodic coloring material is included in the ion storage layer.
Further, the cathodic coloring material is selected from at least one of the following materials: tungsten oxynitride, molybdenum oxynitride, niobium oxynitride, titanium oxynitride, tantalum oxynitride; the anodic coloring material is selected from at least one of the following materials: nickel oxynitride, iridium oxynitride, manganese oxynitride, cobalt oxynitride, tungsten nickel oxynitride, tungsten iridium oxynitride, tungsten manganese oxynitride, tungsten cobalt oxynitride.
Further, the substrate is a curved substrate.
The invention also provides a preparation method of the all-solid-state quick response electrochromic device, which comprises the following steps:
forming a first transition layer on the first conductive layer under the condition of isolating the outside air;
carrying out reactive sputtering on a first target material by doping an inert gas into a reaction gas, forming a first electrochromic layer on the first transition layer, and carrying out plasma etching on the first electrochromic layer by using the inert gas; doping the first target material with the reaction gas by using the inert gas for reactive sputtering, and forming a second electrochromic layer on the first electrochromic layer;
forming an ion conducting layer on the second electrochromic layer;
doping the reaction gas with the inert gas to perform reactive sputtering on a second target material, and forming an ion storage layer on the ion conduction layer;
forming a second conductive layer on the ion storage layer;
the reaction gas is oxygen.
Further, the plasma etching is to ionize the inert gas, and bombard the first electrochromic layer with the inert gas, which is guided by an electric field to ionize.
Further, the ion storage layer includes a first ion storage layer and a second ion storage layer; when the second target is doped with the reactive gas by the inert gas for reactive sputtering, the method further includes:
doping the second target with the reaction gas by the inert gas for reactive sputtering to form the first ion storage layer on the ion conducting layer;
forming a second transition layer on the first ion storage layer;
carrying out plasma etching on the second transition layer by using the inert gas;
and doping the second target with the inert gas into the reaction gas for reactive sputtering, and forming the second ion storage layer on the second transition layer.
Further, the plasma etching is to ionize the inert gas and bombard the second transition layer with the inert gas ionized by electric field guidance.
Further, the first transition layer and the second transition layer are formed by reactive sputtering of a third target material with the inert gas, wherein the third target material comprises one or more of silver, aluminum, copper and nichrome.
Further, when the first electrochromic layer is subjected to plasma etching, the inert gas subjected to plasma etching breaks down the first electrochromic layer and the first transition layer to partially expose the covered first conductive layer.
Further, when the second transition layer is subjected to plasma etching, the plasmatized inert gas breaks down the second transition layer to partially expose the first ion storage layer covered by the second transition layer.
Further, the first target comprises a material selected from the group consisting of: tungsten, molybdenum, niobium, titanium, tantalum.
Further, the second target comprises a material selected from the group consisting of: nickel, iridium, cobalt, manganese, tungsten.
The invention has the technical effects that: by adding the transition layer, the conductivity of the electrode is increased. And the electron and ion mobility of the film can be adjusted by adjusting the coverage rate of the transition layer on the functional layer of the electrochromic device, so that the improvement of the coloring and fading uniformity is realized. In addition, the electrochromic glass can have wider infrared regulation and control capability.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments made with reference to the following drawings:
fig. 1 is a schematic structural diagram according to an embodiment of the present invention.
Description of reference numerals: 100-a substrate; 105-a first conductive layer; 110; a transition layer; 1101-a first transition layer; 1102 — a second transition layer; 115-an electrochromic layer; 120-ion conducting layer; 125-an ion storage layer; 1251 — a first ion storage layer; 1252 — a second ion storage layer; 130-second conductive layer.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
In the drawings, structurally identical elements are represented by like reference numerals, and structurally or functionally similar elements are represented by like reference numerals throughout the several views. The size and thickness of each component shown in the drawings are arbitrarily illustrated, and the present invention is not limited to the size and thickness of each component. The thickness of the components may be exaggerated where appropriate in the figures to improve clarity.
As shown in fig. 1, the present invention discloses an all-solid-state fast response electrochromic device, which includes a substrate 100, and a first conductive layer 105, an electrochromic layer 115, an ion conducting layer 120, an ion storage layer 125, and a second conductive layer 130 sequentially disposed on the substrate 100; further comprising: a transition layer 110; the transition layer 110 is at least one of located between the electrochromic layer 115 and the first conductive layer 105 or located in the ion storage layer 125, and the transition layer 110 is a rugged conductive film layer.
For convenience of expression, the transition layer 110 between the electrochromic layer 115 and the first conductive layer 105 is defined herein as a first transition layer 1101. The transition layer 110 located within the ion storage layer 125 is a second transition layer 1102. The ion storage layer 125 is divided into two parts, a first ion storage layer 1251 and a second ion storage layer 1252, by a second transition layer 1102. In other words, the second transition layer 1102 is located between the first ion storage layer 1251 and the second ion storage layer 1252.
The first conductive layer 105 and the second conductive layer 130 are conventional conductive layers, and the material includes one or more of Indium Tin Oxide (ITO), aluminum-doped zinc oxide (AZO), boron-doped zinc oxide (BZO), and fluorine-doped tin oxide (FTO). Electrochromic layer 115, ion conducting layer 110, ion storage layer 125, and second electrically conductive layer 130 are stacked in order starting with first electrically conductive layer 105.
In particular, a first transition layer 1101 is present between the first conductive layer 105 and the electrochromic layer 115, the first transition layer 1101 being a flat or rugged conductive film layer having a thickness of about 5 to 50nm, further 10 to 40nm, further 15 to 30nm, further 20 nm. The conductive film layer is generally a pure metal layer, preferably silver, aluminum, copper, and nichrome. This is because the metal has excellent ductility and flexibility in addition to excellent conductive properties, and is convenient for processing a flat or uneven conductive film layer. Preferably, the rugged conductive film layer has a regular plurality of recess regions thereon, and thus, each layer will be formed as the rugged electrochromic layer 115, the ion conductive layer 120, the ion storage layer 125, and the like, during the electrochromic device continues to be stacked. Through forming unevenness's structure on electrochromic device, when light shines, light can be in the depressed area to the not equidirectional free reflection, forms the diffuse reflection, and the electrochromic effect that from this represents in the people's naked eye can be more even, and colour purity is higher, and the colour difference is littleer. Preferably, the coverage of first transition layer 1101 on first conductive layer 105 is about 15% to 80%. Further, the rugged transition layer 1101 increases its contact area with the electrochromic layer 115, and the adhesion between the layers is better.
An electrochromic layer 115 is stacked on the first transition layer 1101, having a thickness of 150 to 650nm, and a material selected from tungsten oxide (WO)x) Molybdenum oxide (MoO)x) Niobium oxide (NbO)x) Titanium oxide (TiO)x) Tantalum oxide (TaO)x) One or more of (a).
Further, in the above materials, tooNitrogen may be further added to form an oxynitride, such as tungsten oxynitride (WO)xNy) Molybdenum oxynitride (MoO)xNy) Niobium oxynitride (NbO)xNy) Titanium oxynitride (TiO)xNy) Tantalum oxynitride (TaO)xNy) And the like. Depending on the nitrogen content, the x and y parameters vary accordingly. The molar number of nitrogen atoms in the electrochromic layer 115 may be generally 0.05% to 20%, or 0.5% to 5%, or 0.5% to 10% of the total atomic molar number. Thereby causing crystal distortion in the electrochromic layer 115, further increasing the ion transport speed of the electrochromic layer.
An ion conducting layer 120 is deposited on the electrochromic layer 115 to a film thickness of 3 to 300 nm. The material is selected from the following materials or their mixtures: lithium silicon oxide (LiSi)zOx) Lithium tantalum oxide (LiTa)zOx) Lithium niobium oxide (LiNb)zOx) Lithium cobalt oxide (LiCo)zOx) Lithium aluminum oxide (LiAl)zOx) Lithium phosphorus oxide (LiP)zOx) Lithium boron oxide (LiB)zOx). Ion conducting layer 120 is used to transport lithium ions from electrochromic layer 115 or ion storage layer 125 to each other when first electrically conductive layer 105 is energized with second electrically conductive layer 130. Similarly, when the current is reversed, lithium ions flow in the opposite direction, cycling the electrochromic device between colored and faded.
An ion storage layer 125 is deposited on the ion conducting layer 120, the ion storage layer 125 comprising a first ion storage layer 1251 and a second ion storage layer 1252, a second transition layer 1102 being located between the first ion storage layer 1251 and the second ion storage layer 1252. A second conductive layer 130 is located over the second ion storage layer 1252. The thickness of the first ion storage layer 1251 is 150 to 650nm, and the thickness of the second ion storage layer 1252 is 50 to 100 nm. The second transition layer 1102 has a thickness of 5 to 50nm, similar to the first transition layer 1101. Second transition layer 1102 is also a rugged conductive film layer, preferably using a ductile, more workable metal such as silver, aluminum, copper, nichrome, consistent with first transition layer 1101. When the electrochromic device is powered on, one pole of the power supply is connected to the first conductive layer 105, and the other pole is connected to the second conductive layer 130 and the second transition layer 1102 simultaneously, so that current can be conducted from the second conductive layer 130 and the second transition layer 1102 simultaneously. At this time, the ions in the first ion storage layer 1251 and the second ion storage layer 1252 move towards the electrochromic layer 115 at the same time, and since the distance between the first ion storage layer 1251 and the electrochromic layer 115 is closer, the speed of the ions reaching the electrochromic layer 115 is faster, so that the response speed of the electrochromic device is increased, and when the ions leave quickly, the first ion storage layer 1251 firstly enters a gray state, so that when the ions react in the user experience, the color change feedback of the electrochromic glass is faster and more timely, and the user experience is enhanced. The second ion storage layer 1252 is arranged to maintain the ion content of the conventional ion storage layer in the prior art, so that after the ions in the first ion storage layer 1251 and the second ion storage layer 1252 sequentially reach the electrochromic layer 115, the electrochromic device can maintain the light transmittance after coloring before the improvement, and avoid the reduction of the ion content due to the thinning of the ion storage layer 125, thereby having a negative effect on the light transmittance of the electrochromic device after coloring. The coverage of the second transition layer 1102 in the first ion storage layer 1251 is preferably 3 to 60%. Generally, the coverage is lower, e.g., 3% higher conductivity, and the response speed is faster. And under the condition of higher coverage rate, the transmittance of the electrochromic device in a bleaching state is better, and the color change process is more uniform. Therefore, the adjustment of the coverage rate needs to find a balance point between the response speed of the device and the transmittance of the device in a bleaching state according to actual requirements.
The material of the ion storage layer 125 may be selected from conventional materials in the art, such as nickel oxide (NiO)x) Iridium oxide (IrO)x) Manganese oxide (MnO)x) Cobalt oxide (CoO)x). In addition, nitrogen element can be further introduced, and the mole number of the introduced nitrogen atoms can be about 0.05-15% of the whole atom mole number. The conventional nickel oxide and iridium oxide material is converted into a nickel oxynitride, iridium oxynitride or cobalt oxynitride material, so that the stability of the device in the process of fading can be improved, because the nitride is relative to the oxideHas higher binding energy. In addition, tungsten can be introduced into the ion storage layer 120, so that the ion transmission performance of the electrochromic device can be further enhanced, and the fading performance of the device can be slightly influenced.
Alternatively, the electrochromic materials in the electrochromic layer 115 and the ion storage layer 125 are a cathodic coloring material and an anodic coloring material, respectively. For example, the electrochromic layer 115 may employ a cathode coloring material such as tungsten oxynitride; the ion storage layer 125 may employ an anodic coloring material, such as nickel oxynitride. That is, after lithium ions are removed from the ion storage layer 125, the ion storage layer also enters a colored state. Thus, the electrochromic layer 115 and the ion storage layer 125 combine and collectively reduce the light transmittance transmitted through the overall electrochromic device.
Further, the substrate 100 may also be a curved substrate. The high ductility of the metal in the transition layer 110 is utilized, so that the defect that each functional layer in the deposited electrochromic device is easy to break in the state that the substrate 100 is a curved surface can be overcome, and the electrochromic device can keep good conductivity and color-changing performance when applied to the curved surface substrate.
Further, the first transition layer 1101 is a mesh conductive film layer, and a contact interface is included between the electrochromic layer 115 and the first conductive layer 105. Therefore, the electrochromic layer 115 is simultaneously contacted with the first conductive layer 105 and the first transition layer 1101, so that the speed of conducting electrons of the electrochromic device after being electrified is higher, the electrons can be simultaneously transmitted through the first conductive layer 105 and the first transition layer 1101, the response of the device is higher, and the response speed of the electrochromic device can be further improved by 15% -25% compared with that of the electrochromic device. The mesh-shaped conductive film layers are positioned among the same film layers, so that the resistance is smaller and uniform. After the electrochromic device is electrified, the electron transmission can be carried out in a large area in the layer, and the electrochromic device is stable and reliable.
Further, the second transition layer 1102 is a mesh-shaped conductive film layer, and a contact interface is included between the first ion storage layer 1251 and the second ion storage layer 1252. Therefore, the surface resistance of the ion storage layer 125 is further reduced, the electron transmission speed of the electrochromic device after being electrified is increased, and the color changing efficiency of the electrochromic device is improved.
The invention also provides a preparation method of the all-solid-state quick response electrochromic device, which comprises the following steps:
step S20: forming a first transition layer 1101 on first conductive layer 105 with isolation from the outside air;
the first conductive layer 105 may be deposited directly on the substrate 100 using vacuum coating, evaporation coating, sol-gel, or the like. The deposition process of the second conductive layer 130 is the same. The first transition layer 1101 may be formed by depositing a third target on the first conductive layer 105 by reactive sputtering using the inert gas, or may be formed by vacuum deposition, evaporation deposition, or the like. The film thickness is generally 5 to 50 nm. The third target material comprises one or more of silver, aluminum, copper and nickel-chromium alloy.
Step S21: performing reactive sputtering on the first target by doping an inert gas into a reaction gas to form a first electrochromic layer on the first transition layer 1101; carrying out plasma etching on the first electrochromic layer by using the inert gas; doping the first target material with the reaction gas by using the inert gas for reactive sputtering, and forming a second electrochromic layer on the first electrochromic layer;
the electrochromic layer 115 includes a first electrochromic layer and a second electrochromic layer, and in order to deposit the uneven electrochromic layer 115, it is first necessary to deposit the first electrochromic layer on the first transition layer 1101, and the film thickness is about 50 to 150 nm. Specifically, the first target is bombarded with an inert gas, preferably argon, and doped with a reactive gas to form a mixed gas in a plasma state and perform reactive sputtering to form a corresponding compound on the first transition layer 1101. The reaction gas may be oxygen, and the first target may be one or more of tungsten, molybdenum, niobium, titanium, and tantalum, or an oxide of the corresponding metal. During sputtering, the metal on the target is ionized and deposited on the substrate under the magnetic field created by the N and S magnets fixed around the target. In order to effectively control the oxidation valence state, the mixed gas in the plasma state and the metal ions can be pumped away by using the pumping channel, and at the moment, the metal deposited on the substrate cannot be kept in the oxygen-containing atmosphere, so that secondary oxidation cannot be caused. Meanwhile, the power of the pumping channel should be adjusted accordingly, so that the mixed gas in the plasma state and the metal ions can stay on the periphery of the substrate for a sufficient time, and the metal ions can be deposited on the substrate.
And after the inert gas is plasmatized by a plasma etcher, the plasmatized inert gas is guided by an electric field to bombard the first electrochromic layer, so that the first electrochromic layer forms an uneven shape. The inert gas is preferably argon and the electric field is preferably generated by the motor windings. Further, the plasmatized inert gas may also bombard the first transition layer 1101 during bombardment of the first electrochromic layer, thereby allowing the later deposited second electrochromic layer to bond more tightly to the first electrochromic layer and the first transition layer 1101. And during the bombardment, a part of the first electrochromic layer may be peeled off, thereby regulating the coverage rate and specific shape of the first electrochromic layer and the first transition layer 1101 on the first conductive layer 105. Specifically, the energy density during deposition sputtering and the density of a film layer after sputtering can be used for regulation, and the higher the film layer density is, the lower the coverage rate is. A second electrochromic layer is then deposited on the first electrochromic layer, in the same way as when the first electrochromic layer was deposited, complementing the thickness of the electrochromic layer 115 to 150 to 650 nm. At this time, the layered structure of the second electrochromic layer is the same as that of the first electrochromic layer, and is in an uneven shape. Each of the functional layers deposited thereafter will be covered in turn with the same layered structure as the electrochromic layer 115.
Step S22: forming an ion conducting layer 120 on the second electrochromic layer;
the fourth target is reactively sputtered by vacuum plating, magnetron sputtering, or the like to form the ion conductive layer 120 on the electrochromic layer 115. The fourth target may be selected from conventional targets known in the art, such as lithium, silicon, cobalt, boron, phosphorus, or mixtures thereof.
Step S23: performing reactive sputtering on the second target material by doping the reactive gas with the inert gas to form an ion storage layer 125 on the ion conducting layer 120;
the ion storage layer 120 may use metal nickel, iridium, tungsten, cobalt, manganese, etc. as a second target material, and uses inert gas as a carrier gas to dope the first reaction gas for reactive sputtering, which is similar to the electrochromic layer 115, and the details are not repeated here. In addition, because the pure metal nickel and the metal cobalt have magnetism and interfere the arrangement process of particles in the magnetron sputtering process, the tungsten-containing alloy with the metal can be used to achieve the purpose of demagnetizing the target material.
Step S24: forming a second conductive layer 130 on the ion storage layer 125;
the second conductive layer 130 is formed in the same manner as the first conductive layer 105, and is not described herein again.
Further, the ion storage layer 125 includes a first ion storage layer 1251 and a second ion storage layer 1252, and when the reactive sputtering is performed by doping the reactive gas with the inert gas as the second target, the method further includes:
step S231: performing reactive sputtering on the second target material by doping the reactive gas with the inert gas to form a first ion storage layer 1251 on the ion conduction layer 120;
step S232: forming a second transition layer 1102 on the first ion storage layer 1251, and performing plasma etching on the second transition layer 1102 with an inert gas;
step S233: performing reactive sputtering on the second target by doping the reactive gas with the inert gas, and forming a second ion storage layer 1251 on the second transition layer 1102;
the material of the second transition layer 1102 is the same as the first transition layer 1101, and the deposition method is the same, which is not described herein again.
Further, when the first electrochromic layer is plasma etched, the plasmatized inert gas bombards the first electrochromic layer and the first transition layer 1101, partially exposing the covered first conductive layer 105. It should be noted that the energy density parameter during the plasma etching needs to be carefully adjusted, so that the first conductive layer 105 cannot be damaged and the substrate 100 can be exposed while the first conductive layer 105 is partially exposed.
At this time, the first electrochromic layer and the first transition layer 1101 are bombarded to form a mesh structure, partially exposing the first conductive layer 105. Therefore, when the second electrochromic layer is subsequently deposited, the electrochromic layer 115 can pass through the first transition layer 1101 and directly contact the first conductive layer 105, so that electrons can be simultaneously transmitted to the electrochromic layer 115 through the first transition layer 1101 and the first conductive layer 105 when the electrochromic device is powered on, the electron transmission speed is further increased, and the color change response speed is improved.
Further, when the second transition layer 1102 is plasma etched, the inert gas that is plasmatized bombards the second transition layer to partially expose the first ion storage layer 1251 covered by the second transition layer 1102.
At this time, the second transition layer 1102 forms a mesh-like structure, and the first ion storage layer 1251 and the second ion storage layer 1252 are in contact with each other through the mesh-like structure formed by the second transition layer 1102, so that the area resistance of the ion storage layer 125 is further reduced, the electron transmission speed of the electrochromic device after being electrified is increased, and the color change efficiency of the electrochromic device is improved.
Further, nitrogen-containing gas may be added to the reaction gas. The nitrogen-containing gas may include: nitrogen (N)2) Ammonia (NH)3) Nitrogen monoxide (NO), nitrogen dioxide (NO)2) Dinitrogen oxide (N)2O), Nitrogen Fluoride (NF)3) And other mixed gases containing the aforementioned gases, and the mole ratio of nitrogen element in the mixed gas is required to achieve the objective of the invention. Specifically, when performing the deposition of the electrochromic layer 115 or the deposition of the ion conducting layer 120 and the ion storage layer 125, all the gases, regardless of the means of entering the reactor, should include an inert gas as a carrier gas, and oxygen and nitrogen-containing gases as reaction gases. For example, the electrochromic layer 115 may be formed by mixing the nitrogen-containing gas in the reaction gas in a proportion sufficient to make the deposited electrochromic layer 115 contain nitrogenThe whole atomic mole number is about 0.05% to 20%. Taking nitrogen as a preferred embodiment, the mixing ratio of the nitrogen and the oxygen in the reaction gas is (0.1-10): 1.
in addition, when other nitrogen-containing gases are used, such as ammonia gas, nitrogen fluoride, etc., the impurity elements therein cannot form stable compounds with the metal, and are pumped out by the pumping channel during the sputtering deposition process.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (20)
1. An all-solid-state fast response electrochromic device is characterized by comprising a substrate, and a first conducting layer, an electrochromic layer, an ion conducting layer, an ion storage layer and a second conducting layer which are sequentially arranged on the substrate; wherein a stack of the electrochromic layer up to a face of the ion storage layer is rugged.
2. The all-solid-state fast response electrochromic device according to claim 1, further comprising: a first transition layer; the first transition layer is located between the electrochromic layer and the first conducting layer, and the first transition layer is a smooth or uneven conducting film layer.
3. The all-solid-state fast response electrochromic device according to claim 1, further comprising: and the second transition layer is positioned in the ion storage layer and is an uneven conductive film layer.
4. The all-solid-state fast response electrochromic device of claim 3, wherein said first transition layer and said second transition layer are selected from one or more of the following materials: silver, aluminum, copper, nichrome.
5. The all-solid-state fast response electrochromic device according to claim 2, wherein the first transition layer is a mesh conductive film layer, and a contact interface is included between the electrochromic layer and the first conductive layer.
6. The all-solid-state fast response electrochromic device according to claim 5, wherein a coverage of the transition layer between the electrochromic layer and the first conductive layer on the first conductive layer is 15 to 80%.
7. The all-solid-state fast response electrochromic device according to claim 3, wherein said second transition layer is a reticulated conductive film layer, said ion storage layer comprising a first ion storage layer and a second ion storage layer, said first ion storage layer and said second ion storage layer including a contact interface therebetween.
8. The all-solid-state fast response electrochromic device according to claim 7, wherein a coverage of the second transition layer on the first ion storage layer is 3 to 60%.
9. The all-solid-state fast response electrochromic device according to claim 1, wherein said electrochromic layer includes a cathodic coloring material therein and said ion storage layer includes an anodic coloring material therein.
10. The all-solid-state fast response electrochromic device according to claim 9, wherein said cathodic coloring material is selected from at least one of the following materials: tungsten oxynitride, molybdenum oxynitride, niobium oxynitride, titanium oxynitride, tantalum oxynitride; the anodic coloring material is selected from at least one of the following materials: nickel oxynitride, iridium oxynitride, manganese oxynitride, cobalt oxynitride, tungsten nickel oxynitride, tungsten iridium oxynitride, tungsten manganese oxynitride, tungsten cobalt oxynitride.
11. The all-solid-state fast response electrochromic device according to claim 1, wherein said substrate is a curved substrate.
12. A preparation method of an all-solid-state quick response electrochromic device is characterized by comprising the following steps:
forming a first transition layer on the first conductive layer under the condition of isolating the outside air;
carrying out reactive sputtering on a first target material by doping an inert gas into a reaction gas, forming a first electrochromic layer on the first transition layer, and carrying out plasma etching on the first electrochromic layer by using the inert gas; doping the first target material with the reaction gas by using the inert gas for reactive sputtering, and forming a second electrochromic layer on the first electrochromic layer;
forming an ion conducting layer on the second electrochromic layer;
doping the reaction gas with the inert gas to perform reactive sputtering on a second target material, and forming an ion storage layer on the ion conduction layer;
forming a second conductive layer on the ion storage layer;
the reaction gas is oxygen.
13. The method of claim 12, wherein the plasma etching is to plasmatize the inert gas and bombard the first electrochromic layer with the inert gas that is plasmatized by electric field guidance.
14. The method for manufacturing an all-solid-state fast response electrochromic device according to claim 12, wherein the ion storage layer includes a first ion storage layer and a second ion storage layer; when the second target is doped with the reactive gas by the inert gas for reactive sputtering, the method further includes:
doping the second target with the reaction gas by the inert gas for reactive sputtering to form the first ion storage layer on the ion conducting layer;
forming a second transition layer on the first ion storage layer;
carrying out plasma etching on the second transition layer by using the inert gas;
and doping the second target with the inert gas into the reaction gas for reactive sputtering, and forming the second ion storage layer on the second transition layer.
15. The method of claim 14, wherein the plasma etching is performed by plasmatizing the inert gas and bombarding the second transition layer with the electric field to guide the plasmatized inert gas.
16. The method of claim 14, wherein the first transition layer and the second transition layer are formed by reactive sputtering a third target with the inert gas, the third target comprising one or more of silver, aluminum, copper, and nichrome.
17. The method of preparing an all-solid-state fast response electrochromic device according to claim 13, wherein when the first electrochromic layer is plasma etched, the inert gas plasmatized breaks down the first electrochromic layer and the first transition layer to partially expose the covered first conductive layer.
18. The method of preparing an all-solid-state fast response electrochromic device according to claim 15, wherein when the second transition layer is plasma etched, the inert gas plasmatized breaks down the second transition layer to partially expose the first ion storage layer covered by the second transition layer.
19. The method of claim 12, wherein the first target material comprises a material selected from the group consisting of: tungsten, molybdenum, niobium, titanium, tantalum.
20. The method of claim 12, wherein the second target material comprises a material selected from the group consisting of: nickel, iridium, cobalt, manganese, tungsten.
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| CN113755805A (en) * | 2021-09-09 | 2021-12-07 | 宁波伯宇科技有限公司 | Curved surface coating process for electrochromic lens |
| CN113759624A (en) * | 2021-09-09 | 2021-12-07 | 宁波伯宇科技有限公司 | Process for manufacturing curved surface electrochromic lens |
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