CN107740059B - Ionization method of electrochromic device, preparation method and product - Google Patents
Ionization method of electrochromic device, preparation method and product Download PDFInfo
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- CN107740059B CN107740059B CN201710978658.3A CN201710978658A CN107740059B CN 107740059 B CN107740059 B CN 107740059B CN 201710978658 A CN201710978658 A CN 201710978658A CN 107740059 B CN107740059 B CN 107740059B
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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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Abstract
The invention discloses an ionization method of an electrochromic device, the electrochromic device comprises an anode electrochromic layer, and the method for ionizing the anode electrochromic layer comprises the following steps: the ion layer is directly deposited on the static anode electrochromic layer by utilizing the magnetron sputtering of the rotary target, the target material outside the rotary target is kept to rotate at a constant speed in the deposition process, the magnetic rod inside the rotary target directly swings at a constant speed in a reciprocating mode over against the anode electrochromic layer, and the deposition process is controlled by detecting the transmittance of the anode electrochromic layer in the deposition process. The invention has the beneficial effects that: when the electrochromic device is prepared, the lithium target is uniformly deposited in a dynamic and static mixed coating mode, the deposition amount of an ion source playing a key role in the electrochromic device can be conveniently controlled when the color change reaction of the anode color change layer is detected on line, so that the preparation of the electrochromic device becomes simple and effective, and the industrialization of electrochromic glass is facilitated.
Description
Technical Field
The invention belongs to the technical field of electrochromic device preparation, and particularly relates to an electrochromic device ionization method, a preparation method and a product.
Background
Electrochromism refers to reversible oxidation or reduction reaction of a material under the action of change of polarity and strength of an applied electric field, so that the color of the material is reversibly and stably changed. The electrochromic glass prepared by utilizing the performance can intelligently adjust light and heat of sunlight penetrating through the glass, and reduce energy consumption (refrigeration or heating, illumination and the like) of buildings needed for improving indoor comfort, is the most advanced building energy-saving glass at present, and has huge application market today emphasizing green and ecological development.
A typical electrochromic glass consists of a bottom conductive layer, an electrochromic layer, an ion conducting layer, an ion storage layer, and a top conductive layer. Under the action of an electric field, ions in the ion storage layer enter the electrochromic layer through the ion conducting layer to realize a color changing effect; applying a reverse electric field, ions leave the electrochromic layer via the ion conducting layer back to the ion storage layer to achieve color fading. In order to improve the color changing effect, the ion storage layer can use a color changing material (if the electrochromic layer is a cathode color changing material, the ion storage layer uses an anode color changing material, or vice versa) which is opposite to the oxidation reduction reaction of the electrochromic layer to achieve the color changing superposition effect, and the color changing performance of the electrochromic glass is obviously improved.
At present, the preparation of electrochromic glass generally adopts a physical vapor deposition or evaporation method, a transparent conducting layer and an electrochromic layer respectively grow on two glass substrates, and the front surfaces of the two pieces of glass are heated and bonded by lithium glue to prepare the laminated electrochromic glass. In the preparation of the device, the transparent conducting layer and the electrochromic layer are both subjected to magnetron sputtering, the preparation process is mature and simple, the deposition rate is low, the thickness can be easily controlled by adjusting process parameters such as power, deposition time and the like, the control is relatively convenient, and the ion source control of the electrochromic device playing a key role is very difficult. The ion source usually selects pure lithium metal, and is generally stored in a vacuum environment for preventing pollution, but in actual production, even if the humidity of the environment with an open cavity is less than 5%, the material is influenced by the open cavity and is easily subjected to chemical reaction with water and gas in the routine maintenance and cleaning process of the vacuum cavity, and an oxide layer is formed on the surface. In the preparation process of the device, the surface of the target material with oxidized surface is gradually cleaned to expose the metallic elemental lithium along with continuous sputtering, but the deposition rates of the same process parameters are greatly different, and the deposition rate of the oxidized state is higher than that of the metallic state. Different from other functional film layers, the difference of 1nm of lithium (or lithium oxide) deposition thickness can cause great difference of device appearance and performance, and cannot be controlled by simple film thickness online detection equipment.
A commonly used method comprises the steps of burning a target by using 100% working gas, sputtering to remove a surface oxide layer, and finally carrying out magnetron sputtering on a stable metal lithium simple substance, wherein the whole process needs about 60KW & H, is time-consuming, consumes materials, and is easy to cause secondary pollution of a cavity. The method is a common method, simultaneously uses working gas and reaction gas, sputters the oxide on the surface of the target material, and simultaneously slightly poisons and oxidizes the target material, maintains the dynamic balance of the oxidation degree of the surface of the target material, and ensures the consistency of the deposition rate, but the dynamic balance point is not easy to find in the actual production, lithium is extremely sensitive to the reaction gas, the poisoning of the target material is aggravated by introducing the reaction gas less than 3sccm, and the dynamic balance of the oxidation state and the metal state is broken. Too few ion sources are deposited, so that the electrochromic modulation range is small, and the resistance of the top transparent conductive layer is influenced and remarkably increased when the electrochromic modulation range is serious, and the color change effect cannot be achieved. Too many ion sources can greatly influence the initial color and the color change speed of the electrochromic device, and the ionization technology is a key technology for restricting the industrialized popularization of the electrochromic glass due to the ion sources to the cavity.
Disclosure of Invention
In order to solve the technical problem of ion source control playing a key role in an electrochromic device, the invention provides an ionization method of the electrochromic device.
The invention also provides a manufacturing method of the electrochromic device and the prepared electrochromic device.
An ionization method of an electrochromic device, which comprises an anode electrochromic layer, is characterized in that the ionization method of the anode electrochromic layer is as follows: the ion layer is directly deposited on the static anode electrochromic layer by utilizing the magnetron sputtering of the rotary target, the target material outside the rotary target is kept to rotate at a constant speed in the deposition process, the magnetic rod inside the rotary target directly swings at a constant speed in a reciprocating mode over against the anode electrochromic layer, and the deposition process is controlled by detecting the transmittance of the anode electrochromic layer in the deposition process.
The invention adopts a dynamic and static mixed coating method, namely, the substrate is static (convenient for detection); the target material magnetic field rotates in a small range, so that the deposited film is more uniform; the method is characterized in that an alkali metal material is directly deposited after an anode electrochromic layer is deposited and grown, ions are injected into the film layer to enable the anode electrochromic film layer to generate a color change reaction (the process can also be called ionization), the ion source is controlled by a method of stopping depositing the alkali metal without changing through detecting the transmittance after the color change reaction on line, and the ionization technology conveniently solves the key technical problem of restricting the industrialized popularization of the electrochromic glass.
Preferably, the rotating speed of the target material is 5-20 revolutions per minute; more preferably 8 to 15 rpm.
Preferably, the swinging angle of the magnetic rod is 100-150 degrees; further preferably 110 to 140 degrees. In the invention, the magnetic bar swings to the middle position (60 degrees and alive at-60 degrees) at a constant speed in a reciprocating manner and directly faces the substrate or the anode electrochromic film layer.
Preferably, the swinging speed of the magnetic rod is 5-20 degrees/min.
By adopting the magnetron sputtering parameters, the precise control of the ion layer and the ionization degree is more facilitated.
Preferably, the on-line detection system preferably uses an optical detection device, and may be a transmission type or a reflection type detection system.
Preferably, the light source of the transmittance detection device is a halogen lamp, the halogen lamp is transmitted into the cavity of the magnetron sputtering through a high-temperature resistant optical fiber, the visible light spectrometer is transmitted out of the cavity behind the anode electrochromic layer through the high-temperature resistant optical fiber, and the read transmittance data is used for synchronously controlling the operation of the magnetron sputtering.
Preferably, the ion source adopted by the ion layer is one or more of lithium, lithium oxide or lithium peroxide.
Preferably, the deposition of the ionic layer is stopped when the transmittance of the anodic electrochromic layer no longer increases.
The invention also provides a preparation method of the electrochromic device, which comprises the step of depositing and growing a bottom transparent conducting layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an ion source and a top transparent conducting layer on the transparent substrate in sequence, or depositing and growing a bottom transparent conducting layer, an anode electrochromic layer, an ion source, an ion conducting layer, a cathode electrochromic layer and a top transparent conducting layer on the transparent substrate in sequence.
preferably, the thickness of the bottom transparent conductive layer is 100-500nm, the thickness of the cathode electrochromic layer is 300-800nm, the thickness of the ion conductive layer is 1-50nm, the thickness of the anode electrochromic layer is 100-500nm, and the thickness of the top transparent conductive layer is 100-500 nm.
The invention also provides an electrochromic device which is prepared by the preparation method of the electrochromic device in any technical scheme.
The invention can conveniently and accurately control the core material ion source of the electrochromic device, has simple process and is beneficial to large-area industrialized manufacture of the electrochromic glass.
The invention adopts a dynamic and static mixed coating mode, the substrate is static, the ion source uses a rotating cathode and a magnetic bar in the rotating cathode uniformly swings to control the uniformity; ions of the ion layer are deposited and injected into the anode electrochromic layer at the same time, so that the anode electrochromic layer generates color change reaction (ionization), and the deposition amount of the ion layer can be conveniently controlled by detecting the color change reaction of the anode electrochromic layer on line. The anode color changing layer after complete color changing (ionization) has the function of an ion storage layer (storing ions required by cathode color changing), and when a forward or reverse direct current voltage is applied, the anode color changing layer and the cathode electrochromic layer change color/fade in a complementary manner, so that the electrochromic glass realizes better color changing/fading performance. Here, it is also possible to deposit an anodic electrochromic layer and an ionic layer on the lowermost transparent substrate, and then to produce an ion conducting layer, a cathodic electrochromic layer, the two electrochromic layers being produced without a distinction, except that the ionic layer must be deposited next to the anodic electrochromic layer.
Preferably, the amount of the ionic layer deposited onto the anodic electrochromic layer is such that the anodic electrochromic layer no longer changes. In actual detection, the ionization end point of the anode electrochromic layer, namely the color change end point of the anode electrochromic layer, is determined based on the fact that the light transmittance of the anode electrochromic layer is not increased.
Preferably, the magnetron sputtering process adopts a mixed atmosphere of argon containing oxygen, wherein the atomic percentage content of the oxygen is 0.5%. The ionization preparation method has the advantages that the uniformity of the longitudinal film is mainly ensured by the uniformity of the magnetic field and the gas distribution, the transverse uniformity is ensured by the rotation angle and the speed of the magnetic bar, and the integral deposition amount is ensured by the closed-loop control of an optical feedback system.
The invention has the beneficial effects that: when the electrochromic device is prepared, the lithium target is uniformly deposited in a dynamic and static mixed coating mode, the deposition amount of an ion source playing a key role in the electrochromic device can be conveniently controlled when the color change reaction of the anode color change layer is detected on line, so that the preparation of the electrochromic device becomes simple and effective, and the industrialization of electrochromic glass is facilitated.
Drawings
FIG. 1 is a schematic cross-sectional view of a device of the present invention;
FIG. 2 is a flow chart for device fabrication according to the present invention;
FIG. 3 is a schematic illustration of an ion source deposition and control film of the present invention.
in the figure: 1. transparent base, 2, bottom transparent conducting layer, 3, cathode electrochromic layer, 4, ion conducting layer, 5, anode electrochromic layer, 6, ion source, 7, top transparent conducting layer, 100, electrochromic device.
Fig. 4 shows the magnetic field strength at the surface of the lithium target.
Fig. 5 is a graph of the change between target voltage and power.
Fig. 6 is a graph of the change between color difference and power.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
Example (b): an all-solid-state electrochromic glass (see figure 1) has five layers as a whole, wherein the lowest layer is a transparent substrate 1, and five layers of electrochromic devices, namely a bottom transparent conducting layer 2, a cathode electrochromic layer 3, an ion conducting layer 4, an anode electrochromic layer 5 and a top transparent conducting layer 7, are sequentially deposited and grown on the transparent substrate; the anodic electrochromic layer is a structural layer on which the ion source 6 is deposited and which is fully ionized. The number of ion sources deposited onto the anodic electrochromic layer is based on fully ionizing the anodic electrochromic layer.
The all-solid-state electrochromic glass can also adopt a structure of a five-layer electrochromic device, wherein the bottom layer is a transparent substrate 1, and a bottom transparent conducting layer 2, an anode electrochromic layer 5, an ion conducting layer 4, a cathode electrochromic layer 3 and a top transparent conducting layer 7 are sequentially deposited and grown on the transparent substrate. I.e. the positions of the anode electrochromic layer 5 and the cathode electrochromic layer 3, can be interchanged, but the ionization must be performed on the anode electrochromic layer 5, i.e. the anode electrochromic layers are all structural layers on which the ion source 6 is deposited and which are completely ionized.
3 0.23 1.8 3.6The size of the glass substrate is 370 × 470 × 1.1mm, the thickness of the bottom transparent conducting layer is 10-1000nm, the thickness of the cathode electrochromic layer is 200-800nm, the thickness of the ion conducting layer is 1-50nm, the thickness of the anode electrochromic layer is 100-350nm, and the thickness of the top transparent conducting layer is 10-1000 nm.
The preparation method of the all-solid-state electrochromic glass (see attached figure 2) comprises the steps of growing a bottom transparent conductive layer 2 on a transparent substrate 1 by a physical vapor deposition method, depositing and growing a cathode electrochromic layer 3 on the bottom transparent conductive layer, depositing an ion conductive layer 5 on the cathode electrochromic layer, depositing and growing an anode electrochromic layer 5, depositing an ion source 6 on the anode electrochromic layer in a manner of directly diffusing into the anode electrochromic layer, depositing and growing a top transparent conductive layer 7 on the anode electrochromic layer, and carrying out vacuum annealing at 300 ℃ for 0.5h under the vacuum degree of 10 -6 Torr after film coating.
The invention ionizes the anode electrochromic layer, namely, the deposition of the ion layer on the anode electrochromic layer adopts a dynamic and static mixed coating mode, the substrate is static, the measurement by a detector is convenient, the rotating speed of the rotating cathode is 10 r/min, the rotating angle range of the magnetic rod is 120 degrees, and the swinging speed is 10 degrees/min. The light source of the used transmittance detection device is a halogen lamp and is transmitted into the cavity through the high-temperature-resistant optical fiber, the data of the visible light spectrometer transmitted out of the cavity behind the substrate through the high-temperature-resistant optical fiber are synchronously controlled into the PLC module of the coating device, the correction is completed in the pre-sputtering process, and the stability function during the pre-sputtering detection is also realized.
The magnetic field uniformity data on the surface of the lithium target used by the invention is shown in fig. 4, any two (marked as 1# and 2#) target materials in fig. 3 are vertically arranged in the center of the cavity, the long edge of the glass substrate is parallel to the vertical target materials and is arranged in the effective sputtering area in the middle of the target materials, and the magnetic field uniformity data on the surface of the lithium target is shown in fig. 4.
The effect of the atmosphere on the effectiveness of the ionization method of the present invention is further investigated as follows:
Firstly, by adopting the existing method, argon with the purity of 99.999% is used for sputtering a metallic lithium target, and we find that an oxide layer on the surface of the target is gradually stripped along with the duration of sputtering time, so that the sputtering voltage and current of the target jump, the target voltage rises from 188V to 318V, and the target voltage has a further rising trend. The sputtering voltage and current of the target material have a close relationship with the number of deposited lithium atoms, and the color consistency of the electrochromic glass finished product can be influenced by adopting the existing method. In order to further find out more optimal ionization conditions, the inventor carries out sputtering reaction by sputtering to 110-125 KWH through 5sccm of oxygen, the target voltage is maintained at about 260V, argon with the purity of 99.999% is continuously introduced to sputter the metal lithium target after 125 KWH, and the target voltage continuously and rapidly rises. The graph of the change between target voltage and power using the above method is shown in fig. 5. As can be seen from FIG. 5, the sputtering voltage of the lithium target was maintained in a relatively stable range when oxygen gas of 5sccm was introduced into the argon atmosphere.
To further verify the conclusion of the present invention, an electrochromic glass having an apparent yellow-green color was prepared by co-sputtering in a mixed atmosphere of argon/oxygen (oxygen atomic ratio of 0.5%) at a target voltage of 195V, using as a test standard the Lab values of the CIE standard as shown in the following table:
Meanwhile, by adopting the existing method, the relationship between the color difference and the power of the electrochromic glass prepared by different target voltages is tested, and the great difference of the color difference value along with the increase of the sputtering time is found, as shown in fig. 6. From this, it can be further demonstrated that there is a close correlation between the target voltage and the color difference of the electrochromic glass.
Finally, by adopting the method of the invention, through adjusting sputtering gas, argon oxygen mixed gas (0.5 At% O 2, namely argon containing 0.5% of oxygen (atomic percentage content)) is used for sputtering, the sputtering voltage of the lithium target is maintained At 195V-198V, compared with a test standard sample, the color difference Delta E of the prepared sample is all less than 1.0, the average transmittance of a visible light wave band (380-760 nm) is stabilized At 62.0% +/-0.2%, and by adopting the existing method, the color difference of an electrochromic device is gradually deteriorated to more than 50, the initial state transmittance is increased to 65.8% from 61.0%, but the color change adjusting range is greatly reduced.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (5)
1. An ionization method of an electrochromic device, which comprises an anode electrochromic layer, is characterized in that the ionization method of the anode electrochromic layer is as follows: directly depositing an ion layer on a static anode electrochromic layer by utilizing magnetron sputtering of a rotating target, wherein in the deposition process, a target material outside the rotating target is kept to rotate at a constant speed, a magnetic rod inside the rotating target directly reciprocates to swing at a constant speed against the anode electrochromic layer, and the deposition process is controlled by detecting the transmittance of the anode electrochromic layer in the deposition process; the ion source adopted by the ion layer is one or more of lithium, lithium oxide or lithium peroxide; the rotating speed of the target material is 5-20 revolutions per minute; the swinging angle of the magnetic rod is 100-150 degrees; the swinging speed of the magnetic bar is 5-20 degrees/min;
In the magnetron sputtering process, a mixed atmosphere of argon containing oxygen is adopted, wherein the atomic percentage content of the oxygen is 0.5%.
2. The ionization method of electrochromic device according to claim 1, wherein the light source of the transmittance detection device is a halogen lamp, and is transmitted into the cavity of the magnetron sputtering through the high temperature resistant optical fiber, and is transmitted to the visible light spectrometer outside the cavity through the high temperature resistant optical fiber behind the anode electrochromic layer, and the read transmittance data is used for synchronously controlling the operation of the magnetron sputtering.
3. The method of claim 1, wherein the deposition of the ionic layer is stopped when the transmittance of the anodic electrochromic layer no longer increases.
4. A preparation method of an electrochromic device comprises the steps of depositing and growing a bottom transparent conducting layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an ion source and a top transparent conducting layer on a transparent substrate in sequence; or sequentially depositing and growing a bottom transparent conducting layer, an anode electrochromic layer, an ion source, an ion conducting layer, a cathode electrochromic layer and a top transparent conducting layer on a transparent substrate, wherein the method for depositing the ion source on the anode electrochromic layer adopts the ionization method of the electrochromic device as claimed in any one of claims 1 to 3.
5. An electrochromic device, characterized by being prepared by the method for preparing an electrochromic device according to claim 4.
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| CN109402565A (en) * | 2018-10-11 | 2019-03-01 | 暨南大学 | A kind of growing method of nickel oxide film, nickel oxide film and its photoelectric device |
| CN111584540A (en) * | 2019-02-19 | 2020-08-25 | 陕西坤同半导体科技有限公司 | Controllable transparent display device |
| CN111338149B (en) * | 2020-03-24 | 2023-07-28 | 江苏繁华应材科技股份有限公司 | Nitrogen-containing electrochromic device and preparation method thereof |
| CN113981400B (en) * | 2021-09-10 | 2023-10-20 | 浙江上方电子装备有限公司 | Electrochromic device capable of displaying pattern and coating method thereof |
| CN114089466B (en) * | 2021-11-24 | 2023-08-25 | 长春理工大学 | Electrochromic sensing optical fiber |
| CN115616938B (en) * | 2022-08-26 | 2024-01-05 | 广州汽车集团股份有限公司 | Control method and device of electrochromic device, electronic equipment and storage medium |
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