CN109709737B - Method for manufacturing electrochromic film - Google Patents
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Abstract
The invention belongs to an electrochromic inorganic film technology, and relates to a manufacturing method of an electrochromic film, which comprises the following steps: the cleaned transparent conductive material is placed in a magnetron sputtering chamber, the parameters of the sputtering chamber are well controlled, and the opening angle between a molecular pump and a vacuum sputtering chamber is well controlled; carrying out pre-sputtering treatment on the metal target material with the first layer of film growing, opening a substrate baffle plate to carry out sputtering growing treatment on the first layer of film, and controlling sputtering power and time to enable the first layer of film to expand to a proper thickness; and growing a second layer of film on the basis of the first layer of inorganic electrochromic film, carrying out pre-sputtering treatment on the metal target sputtered by the second layer of film, and controlling to enable the second layer of film to expand to a proper thickness. The invention utilizes the magnetron sputtering method to increase a protective film with electrochromic performance or a protective film with good ion conductivity on the basis of the first layer of electrochromic film so as to obtain the electrochromic film with a novel structure, thereby effectively improving the electrochromic performance of the single-film electrochromic film.
Description
Technical Field
The invention relates to a preparation technology of an electrochromic inorganic thin film material, in particular to a manufacturing method of a novel electrochromic thin film.
Background
In recent years, the fields of sustainable development, energy conservation, environmental protection and other new energy science and technologies have become the most important topic worth of research in the modern times. However, at present, the mode of life and production of human beings mainly uses non-renewable energy such as petroleum, coal, natural gas and the like, and when various new energy sources are not popularized and used, it is particularly important to take various measures to reduce the energy consumption. The energy consumption of buildings is increased year by year, and the energy loss caused by building appliances such as doors, windows and the like is particularly important to be reduced by adopting an effective method, so that the energy loss of the windows is improved, the heat insulation performance of the windows is improved, and the light shielding performance gradually becomes a new focus of people.
Meanwhile, the appearance of energy-saving glass and intelligent windows enables people to see a new hope of energy conservation and emission reduction. The electrochromic smart window can realize the adjustment of optical properties such as transmission and absorption of light irradiated from the outdoor to solve the problem of energy loss caused by the influence of external environment on the indoor. Besides being used on glass of buildings, the electrochromic materials can also be applied to anti-chord rearview mirrors of automobiles to reduce the accidents of traffic accidents, and windshields and window glasses of automobiles to reduce the loss of heat insulation performance in automobiles caused by external irradiation light. Electrochromic materials can also be applied to various types of displays, personal objects such as clothing.
Electrochromism means that the optical properties (reflectivity, transmittance, absorption rate and the like) of a material are stably and reversibly changed continuously under the action of an external electric field, and the electrochromism can be expressed in the appearance that the color and the transparency of the material are reversibly changed continuously. Most of the inorganic electrochromic materials are transition metal oxides or derivatives thereof. Since the change of light absorption of the inorganic electrochromic material is caused by the double injection or extraction of ions and electrons, in the inorganic electrochromic material (e.g., WO)3、MoO3) The electrochromic film has high coloring efficiency, good stability and invisibilityBlind corners and the like, and is widely researched and used. However, the existing inorganic electrochromic material has the problems of long response time and deviation after cyclic voltammetry is carried out for many times.
At present, the techniques for preparing electrochromic films mainly comprise the following types:
1. chemical vapor deposition
Although the chemical vapor deposition method has the advantages of high growth speed of the film, good film forming quality and easy control of doping, the chemical vapor deposition method has the defects of more complex equipment, higher temperature requirement, inapplicability to the film prepared at low temperature, poor binding force of the film and easy falling.
2. Sol-gel process
The method does not need vacuum equipment, has simple process, can obtain a film with ideal thickness and components, and the sol usually contains water and alcohol substances, and the elimination of the water and alcohol substances needs drying and heat treatment; the cracking of the film during the heat treatment is a problem that must be solved. In addition, the adhesion between the film layer and the substrate is poor, the thickness uniformity of the film is difficult to control, and the compactness is poor.
3. Vacuum vapor deposition
Vacuum deposition has a long history and is well studied in the laboratory, resulting in many mature processes. The method has the advantages of high deposition rate, large deposition area, high production efficiency and simpler equipment and operation, and is a main technical means for preparing the film in laboratories and industrial production. However, the disadvantages of the vacuum evaporation method are also very significant, and the films prepared by this method have the following disadvantages:
the aggregate density is small, and the refractive index is lower than the value of a bulk.
Secondly, residual gas and water vapor are easy to adsorb, the optical absorption is large, and the timeliness is poor.
And the surface and the interface are uneven, and the internal scattering and the surface scattering are large.
High stress and anisotropy.
Low hardness, small adhesion and poor firmness.
4. The pulse excimer laser valve shot deposition (PLD) is a new type ingot steaming technology developed in recent years, and has the advantage of high film forming speed, but the bonding force between the film layer and the substrate is poor, the defects are many, the film is easy to be polluted, and the quality of the film is poor.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for manufacturing a novel electrochromic film, which comprises the steps of growing an inorganic electrochromic film with proper thickness on a substrate by a doping or non-doping method by utilizing a magnetron sputtering method on a transparent conductive material substrate and controlling the temperature, pressure, oxygen doping amount and sputtering variable in a cavity; then changing the material system of the swelling film, and swelling a layer of TaO with good ion conduction capability on the basis of the first layer of electrochromic film2Film or TiO with electrochromic properties2The electrochromic film with the novel structure is obtained, and the electrochromic performance of the single-film electrochromic film is effectively improved.
In order to achieve the above purpose, the invention provides the following technical scheme: a manufacturing method of a novel electrochromic film comprises the following steps:
step 1: the cleaned transparent conductive material is placed in a magnetron sputtering chamber, the pipeline is vacuumized, and the total flow of gas and the proportional content of oxygen and argon in the sputtering chamber are controlled;
step 2: regulating the temperature of the sputtering chamber within a required range, well controlling the opening angle between the molecular pump and the vacuum sputtering chamber, and controlling the gas pressure in the sputtering chamber within the required range;
and step 3: carrying out pre-sputtering treatment on a metal target material needing to be subjected to first layer film growth, removing impurities on the surface of the original target material, then opening a substrate baffle plate to carry out sputtering growth treatment on the first layer film, and controlling sputtering power and sputtering time to enable the first layer film to be expanded to a proper thickness;
and 4, step 4: placing the substrate of the second layer film to be grown at the same position as the substrate of the first layer film, and growing the second layer film on the basis of the inorganic electrochromic film grown on the first layer;
and 5: controlling the total flow of gas and the proportional content of oxygen and argon in the second sputtering chamber, adjusting the temperature of the chamber, and controlling the gas pressure in the chamber;
step 6: carrying out pre-sputtering treatment on the metal target material needing to be subjected to second-layer film sputtering, removing impurities on the surface of the original target material, then opening a substrate baffle plate to carry out sputtering growth treatment on the second-layer film, and controlling the sputtering time to ensure that the second-layer film is expanded to a proper thickness;
the second film is a protective film having electrochromic properties or a protective film having good ion conductivity.
Preferably, step 3 is to perform a pre-sputtering treatment on the metallic tungsten target material grown on the first layer of film, or perform a pre-sputtering treatment of co-sputtering the metallic tungsten target material grown on the first layer of film and the metallic titanium target material. When the step 3 is used for carrying out pre-sputtering treatment on the metal tungsten target material with the grown first layer of film, the sputtering power is controlled to be between 50w and 200w, the sputtering time is between 10min and 1h, and the WO to be grown is subjected to pre-sputtering treatment3The film thickness is controlled between 100nm and 400 nm. When the pre-sputtering treatment of co-sputtering is carried out on the metal tungsten target and the metal titanium target which grow on the first layer of film in the step 3, the sputtering power of the metal tungsten target is controlled to be 150w, the sputtering power of the metal titanium target is controlled to be 50w, the sputtering time is 17min, and the WO to be grown is treated3Doped TiO 22The film thickness of the thin film (2) was controlled to 360 nm.
And 6, sputtering the second layer of film to obtain the metal target which is a metal titanium target or a metal tantalum target. In the step 6, the sputtering growth treatment of the second layer film is carried out, the power of the metallic titanium target material is controlled to be 150w, the sputtering time is 11min, and TiO to be grown is treated2The film thickness of (2) is controlled at 100 nm; controlling the power of the tantalum target material at 130w, sputtering for 30min, and growing TaO2The film thickness of (2) was controlled to 100 nm.
Preferably, the line vacuum in step 1 is pulled to 1.0x10-4pa～1.0x10-5pa, controlling the total gas flow at 40 sccm-100 sccm, and controlling the proportional content of oxygen and argon at 20% -40%; the temperature range of the chamber in the step 2 is controlled to be 30-150 ℃, and the gas pressure intensity range in the sputtering chamber is controlled to be 0.5-3 pa; step 5 gasThe total flow is controlled to be 40 sccm-100 sccm, the proportional content of oxygen and argon is controlled to be 20% -40%, the temperature of the chamber is controlled to be 30-150 ℃, and the gas pressure in the chamber is controlled to be 0.5 pa-3 pa.
Compared with the prior art, the invention has the following beneficial effects:
1. the substrate of the electrochromic film manufactured by the invention is transparent conductive ITO glass or FTO glass. By utilizing a magnetron sputtering method on a transparent conductive material substrate, by controlling the temperature, the pressure, the oxygen doping amount and the sputtering variable in a cavity, firstly growing an inorganic electrochromic film with a proper thickness (such as 100-350nm) on the substrate by a doping or non-doping method; then changing the material system of the swelling membrane, and swelling a layer of TaO with good ion conduction capability on the basis of the first layer of electrochromic film2Film or TiO with weak electrochromic characteristics2The electrochromic film with the novel structure is obtained, and the electrochromic performance of the single-film electrochromic film is effectively improved.
2. Based on the inorganic electrochromic film, a layer of film with stable performance and related electrochromic material system of the original electrochromic film performance or a protective film with good ion conduction capability is superposed on the original electrochromic film, the electrochromic performance of the original single inorganic electrochromic film is improved by utilizing different characteristics of different inorganic electrochromic materials or materials with ion conduction capability, the process is simple and convenient to manufacture, and the required requirements can be met in the same chamber.
Drawings
FIG. 1 is a schematic view of an electrochromic film structure fabricated by the method of the present invention;
FIG. 2 is a schematic view of another electrochromic film structure fabricated by the method of the present invention;
FIG. 3 is a schematic structural view of an electrochromic film fabricated in example 1;
FIG. 4 is a schematic structural view of an electrochromic film fabricated in example 2;
FIG. 5 is a schematic view of the electrochromic film structure fabricated in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited to these examples.
The invention takes transparent conductive material ITO glass or FTO glass as the substrate of the electrochromic film, utilizes the magnetron sputtering method, and controls the parameters of temperature, pressure intensity, oxygen doping amount, sputtering variable and the like in the magnetron sputtering chamber, firstly grows a layer of inorganic electrochromic film on the transparent conductive material substrate by the doping or non-doping method, and then grows a layer of TaO with good ion conduction capability on the basis of the first layer of electrochromic film2Film or TiO with electrochromic properties2And (3) a film to finally finish the preparation of the electrochromic film with the novel structure, as shown in figure 1. The following will illustrate the implementation of the present invention in detail with different inorganic electrochromic film materials.
Example 1
Step 1: putting the cleaned ITO glass or FTO glass into a magnetron sputtering chamber, and vacuumizing a pipeline to 1.0x10- 4pa～1.0x10-5pa, controlling the parameters in the sputtering chamber, and controlling the total amount of the gas in the sputtering chamber to be between 40sccm and 100sccm, for example, controlling the total amount of the gas to be 80sccm, and controlling the content of the oxygen and the argon to be between 20% and 40%, in this embodiment, controlling the ratio of the oxygen and the argon to be 24sccm:56 sccm.
Step 2: opening a temperature device in the chamber, and controlling the temperature range of the sputtering chamber to be 30-150 ℃, for example, adjusting the temperature of the chamber to be 50 ℃; the opening angle between the molecular pump and the vacuum sputtering chamber is well controlled, and the angle is controlled to be 18 degrees in the embodiment, so that the pressure in the sputtering chamber reaches 0.5pa to 3 pa. This embodiment can control the pressure in the chamber to be 2 pa.
And step 3: turning on a direct-current power supply, carrying out pre-sputtering treatment on the metal tungsten target material needing to be subjected to the first layer film growth, wherein the treatment time is 10-15 min, the impurities on the surface of the original target material are removed, and then opening a substrate baffle plate to feedThe sputtering power can be controlled between 50 w-200 w, for example, 150w, the sputtering time can be set between 10 min-1 h, the sputtering time can be set to 17min, and the WO to be grown is treated3The thickness of the film is controlled between 100nm and 400nm, and finally the WO is generated3The film thickness may be 360 nm.
And 4, step 4: the substrate on which the second layer is to be grown is placed at the same position as the substrate on which the first layer is to be grown, and WO is grown on the first layer3Performing a second layer TiO film by a direct current sputtering Ti target material mode on the basis of the electrochromic film2By sputter growth of a second layer of TiO2Covering the first layer of film WO3As shown in fig. 2.
And 5: the total amount of gas and the proportional content of oxygen and argon in the second sputtering chamber are controlled to be 24sccm:56sccm, and then the temperature device is turned on to adjust the temperature range of the chamber within a suitable temperature range, for example, 50 ℃.
And 6, controlling the opening angle between the molecular pump and the vacuum chamber, wherein the opening angle is controlled to be 18 degrees in the embodiment, so that the pressure in the chamber reaches 2 pa. Then turning on a direct current power supply, carrying out pre-sputtering treatment on the metallic titanium target material needing to be subjected to the second layer film growth for 10-15 min to remove impurities on the surface of the original target material, then turning on a substrate baffle plate to carry out sputtering growth treatment on the second layer film, controlling the power at 150w and the sputtering time at 11min, and subjecting TiO to be grown to sputtering growth treatment2The film thickness of (2) is controlled to be 100 nm.
It should be noted that, in the second sputtering growth in this embodiment, the numerical ranges of the parameters such as the total amount of gas in the chamber, the proportional content of oxygen and argon, the chamber temperature range, the chamber pressure, the pre-sputtering treatment time, the sputtering power, and the like are substantially the same as those in the first sputtering growth, but the growth thickness of the thin film is different.
Example 2
The sputtering principle and the selected value range of the process parameters of this embodiment are substantially the same as those of embodiment 1, and the difference is mainly the metal target.
Step 1: putting the cleaned ITO glass or FTO glass into a magnetron sputtering chamber, and vacuumizing a pipeline to 1.0x10- 4pa～1.0x10-5pa, controlling the parameters in the sputtering chamber, and controlling the total amount of gas in the chamber to be 80sccm, wherein the ratio of oxygen to argon is controlled to be 24sccm:56 sccm.
Step 2: and opening a temperature device in the sputtering chamber, adjusting the temperature of the chamber to 50 ℃, and controlling the opening angle between the molecular pump and the vacuum sputtering chamber, wherein the opening angle is also controlled to be 18 degrees in the embodiment, so that the pressure in the chamber reaches 2 pa.
And step 3: turning on a direct current power supply, carrying out pre-sputtering treatment on the metal tungsten target material needing to be subjected to the first layer film growth for 10-15 min to remove impurities on the surface of the original target material, then turning on a substrate baffle to carry out sputtering growth treatment on the first layer film, controlling the power at 150w and the sputtering time at 17min, and carrying out pre-sputtering treatment on the WO to be grown3The film thickness was controlled at a value of 360 nm.
And 4, step 4: the substrate on which the second layer is to be grown is placed at the same position as the substrate on which the first layer is to be grown, and WO is grown on the first layer3Performing second-layer film TaO by a direct current sputtering Ta target material mode on the basis of the electrochromic film2By sputter growth of the second layer of film TaO2Covering the first layer of film WO3Of (2) is provided.
And 5: the total amount of gas and the proportional content of oxygen and argon in the second sputtering chamber are controlled at 24sccm:56sccm, and then the temperature device is turned on to adjust the temperature of the chamber within a suitable temperature range, for example, 50 ℃.
And 6, controlling the opening angle between the molecular pump and the vacuum sputtering chamber to be 18 degrees, so that the pressure in the sputtering chamber reaches 2 pa. And then, turning on a direct-current power supply, and carrying out pre-sputtering treatment on the metal tantalum Ta target material needing to be subjected to second-layer film growth, wherein the treatment time is 10-15 min for removingRemoving impurities on the surface of the original target material, opening a substrate baffle plate to perform sputtering growth treatment of a second layer of film, controlling the power at 130w, sputtering for 30min, and growing TaO to be grown2The film thickness of (2) is controlled to be 100 nm.
Example 3:
the sputtering principle and the selected value range of the process parameters of this embodiment are substantially the same as those of embodiment 1, and the difference is mainly the metal target.
Step 1: putting the cleaned ITO glass or FTO glass into a magnetron sputtering chamber, and vacuumizing a pipeline to 1.0x10- 4pa～1.0x10-5pa, controlling the parameters in the sputtering chamber, and controlling the total amount of gas in the chamber to be 80sccm, wherein the ratio of oxygen to argon is controlled to be 24sccm:56 sccm.
Step 2: and opening the temperature device in the cavity, adjusting the temperature of the cavity to 50 ℃, controlling the opening angle between the molecular pump and the vacuum cavity to be 18 degrees, and enabling the pressure in the cavity to reach 2 pa.
And step 3: opening a direct current power supply, carrying out co-sputtering pre-sputtering treatment on a metal tungsten target and a metal titanium target which need to be subjected to first layer film growth, wherein the treatment time is 10-15 min, the treatment time is used for removing impurities on the surface of the original target, then opening a substrate baffle plate to carry out sputtering growth treatment on the first layer film, the sputtering power of the metal tungsten target is controlled at 150w, the sputtering power of the metal titanium target is controlled at 50w, the sputtering time is 17min, and the WO to be grown is subjected to sputtering growth treatment3Doped TiO 22The film thickness of the thin film (2) was controlled to a value of 360 nm.
And 4, step 4: the substrate on which the second layer is to be grown is placed at the same position as the substrate on which the first layer is to be grown, and WO is grown on the first layer3Doped TiO 22Performing second-layer film TaO by a direct current sputtering Ta target material mode on the basis of the electrochromic film2By sputter growth of the second layer of film TaO2Covered with a first layer of WO3Doped TiO 22The surface of the film.
And 5: the total amount of gas and the proportional content of oxygen and argon in the second sputtering chamber are controlled at 24sccm:56sccm, and then the temperature device is turned on to adjust the temperature of the chamber within a suitable temperature range, for example, 50 ℃.
And 6, controlling the opening angle between the molecular pump and the vacuum chamber to be 18 degrees, so that the pressure in the chamber reaches 2 pa. Then opening a direct current power supply, carrying out pre-sputtering treatment on the metal tantalum Ta target material needing to be subjected to the second-layer film growth for 10-15 min to remove impurities on the surface of the original target material, then opening a substrate baffle plate to carry out sputtering growth treatment on the second-layer film, controlling the power at 130w, carrying out sputtering for 30min, and carrying out pre-sputtering treatment on TaO to be grown2The film thickness of (2) is controlled to be 100 nm.
As can be seen from the above examples, the present invention adopts the magnetron sputtering method to perform the film coating, so that the film has excellent adhesion with the substrate. In addition, the film has high growth rate and easily controlled technological parameters, can be used for preparing refractory material films, can realize large-area film preparation, and has the advantages of good stability and convenient preparation. Compared with a single-film pure electrochromic film, the single-film pure electrochromic film has room for improvement of electrochromic properties such as cyclic voltammetry stability, and the like, so that the stability of the single-film electrochromic material can be improved and the electrochromic property can be improved by the preparation of the composite electrochromic film.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The manufacturing method of the novel electrochromic film is characterized by comprising the following steps of:
step 1: the cleaned transparent conductive material is placed in a magnetron sputtering chamber, the pipeline is vacuumized, and the total flow of gas and the proportional content of oxygen and argon in the sputtering chamber are controlled;
step 2: regulating the temperature of the sputtering chamber within a required range, well controlling the opening angle between the molecular pump and the vacuum sputtering chamber, and controlling the gas pressure in the sputtering chamber within the required range;
and step 3: carrying out pre-sputtering treatment on a metal target material needing to be subjected to first layer film growth, removing impurities on the surface of the original target material, then opening a substrate baffle plate to carry out sputtering growth treatment on the first layer film, and controlling sputtering power and sputtering time to enable the first layer film to be expanded to a proper thickness;
and 4, step 4: the substrate of the second layer film to be grown is arranged at the same position as the substrate of the first layer film to be grown, and the second layer film is grown on the basis of the inorganic electrochromic film grown on the first layer;
and 5: controlling the total flow of gas and the proportional content of oxygen and argon in the second sputtering chamber, adjusting the temperature of the chamber, and controlling the gas pressure in the chamber;
step 6: carrying out pre-sputtering treatment on the metal target material needing to be subjected to second-layer film sputtering, removing impurities on the surface of the original target material, then opening a substrate baffle plate to carry out sputtering growth treatment on the second-layer film, and controlling the sputtering time to ensure that the second-layer film is expanded to a proper thickness;
the second film is a protective film with electrochromic performance or a protective film with good ion conductivity;
step 3, carrying out pre-sputtering treatment on the metal tungsten target material with the first layer of film growth, or carrying out co-sputtering pre-sputtering treatment on the metal tungsten target material with the first layer of film growth and a metal titanium target material;
the first film is WO3Film, the second film being TiO2A film; alternatively, the first film is WO3Film, the second film is TaO2A film; alternatively, the first film is WO3Doped TiO 22The second film is TaO2And (3) a membrane.
2. The method for preparing the novel electrochromic film according to claim 1, wherein the pre-sputtering treatment time is 10-15 min.
3. The method for preparing the novel electrochromic film as claimed in claim 1, wherein when the step 3 is performed to pre-sputter the metal tungsten target material grown on the first film, the sputtering power is controlled to be between 50w and 200w, the sputtering time is controlled to be between 10min and 1h, and the WO to be grown is treated3The film thickness is controlled between 100nm and 400 nm.
4. The method for preparing a novel electrochromic film according to claim 1, wherein when the pre-sputtering treatment of co-sputtering the metal tungsten target and the metal titanium target for the first film growth is performed in step 3, the sputtering power of the metal tungsten target is controlled to be 150w, the sputtering power of the metal titanium target is controlled to be 50w, the sputtering time is 17min, and the WO to be grown is treated3Doped TiO 22The film thickness of the thin film (2) was controlled to 360 nm.
5. The method for preparing a novel electrochromic film according to claim 1, wherein the metal target sputtered by the second film in step 6 is a metal titanium target or a metal tantalum target.
6. The method of claim 5, wherein the second film is sputter grown in step 6 by controlling the power of the titanium metal target at 150w for 11min, and growing TiO on the target2The film thickness of (2) is controlled at 100 nm; controlling the power of the tantalum target material at 130w, sputtering for 30min, and growing TaO2The film thickness of (2) was controlled to 100 nm.
7. The method for preparing the novel electrochromic film as claimed in claim 1, wherein the vacuum pumping of the pipeline in step 1 is up to 1.0x10-4pa～1.0x10-5pa, controlling the total gas flow at 40 sccm-100 sccm, and controlling the proportional content of oxygen and argon at 20% -40%; the temperature range of the chamber in the step 2 is controlled to be 30-150 ℃, and the gas pressure intensity range in the sputtering chamber is controlled to be0.5pa to 3 pa; in the step 5, the total flow of the gas is controlled to be 40 sccm-100 sccm, the proportional content of the oxygen and the argon is controlled to be 20% -40%, the temperature of the chamber is controlled to be 30-150 ℃, and the pressure of the gas in the chamber is controlled to be 0.5 pa-3 pa.
8. The method for forming a novel electrochromic film according to claim 7, wherein the ratio of oxygen to argon in step 1 is controlled to 24sccm to 56 sccm.
9. The method of claim 1, wherein in step 2, the opening angle between the molecular pump and the vacuum chamber is controlled to be 18 °.
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| CN102168247B (en) * | 2011-04-15 | 2012-10-03 | 河南大学 | Preparation method and application of TiO2/WO3 composite film |
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