CN113943928A - Preparation method of tungsten oxide electrochromic film with controllable ordered structure - Google Patents
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Abstract
A preparation method of a tungsten oxide electrochromic film with a controllable ordered structure relates to a preparation method of an electrochromic film. The invention aims to solve the technical problems that the existing tungsten oxide electrochromic material cannot simultaneously have large transmittance modulation, high response speed and high cycle stability. The electrochromic film takes a transparent conductive substrate as a substrate, adopts a magnetron sputtering technology, and precisely controls the sputtering power: namely, the power is continuously adjustable, and the power is gradually reduced to prepare the tungsten oxide electrochromic film with the controllable ordered structure; the method comprises the following steps: firstly, ultrasonically cleaning a transparent conductive substrate, and drying; and secondly, preparing the tungsten oxide film with the controllable ordered structure on the transparent conductive substrate by adopting a magnetron sputtering method and adopting a process for controlling sputtering power. The method is used for preparing the tungsten oxide electrochromic film with controllable ordered structure, high transmittance modulation amplitude, quick response and high cycle stability.
Description
Technical Field
The invention relates to a preparation method of an electrochromic film.
Background
Electrochromism is a phenomenon in which the optical properties (reflectivity, transmittance, absorption, etc.) of a material undergo a stable and reversible color change under the action of a small electric signal, and is visually represented by a reversible change in the color and transparency of the material, and a material having the electrochromism phenomenon is called an electrochromic material.
The electrochromic material can be divided into an inorganic electrochromic material and an organic electrochromic material according to the material types, wherein the inorganic electrochromic material also comprises transition metal oxides such as tungsten oxide, molybdenum oxide, vanadium oxide, titanium oxide, niobium oxide, nickel oxide and the like and a Prussian blue system, and the organic electrochromic material comprises materials such as polyaniline, polythiophene, viologen and the like. Electrochromic devices prepared from electrochromic materials have been widely applied in the fields of intelligent windows, displays, anti-glare rearview mirrors, aircraft portholes and the like, and have great application potential in the aspects of camouflage, spacecraft thermal control and the like.
At present, tungsten oxide is the most widely applied cathode electrochromic material in electrochromic materials, and has the characteristics of large optical modulation amplitude, low cost and high coloring efficiency. Over the years of research, researchers have found that the electrochromic properties of tungsten oxide are related to the ordered structure within itself. The tungsten oxide film with a highly disordered structure is synthesized by the Wenzeltao et al, and tests show that although the tungsten oxide film has larger optical modulation, the relatively loose structure of the tungsten oxide film has a trapping effect on the inserted lithium ions, so that the cycling stability of the film is poor.
Jian Zhen Ou et al prepared a tungsten oxide film having a highly ordered structure, and studies showed that the film had stable cycle stability but had a slow coloring/discoloring response speed. In addition, by searching the prior art, chinese patent 201210402383.6 applies for a preparation method of a vertically aligned tungsten oxide nanostructure electrochromic film by using a hydrothermal reaction, and although the tungsten oxide nanostructure film synthesized by using the method has electrochromic properties such as a fast discoloration speed, a high discoloration efficiency, a high cycling stability and the like, and the properties of the tungsten oxide electrochromic film are improved to a certain extent, the synthesis process is too complex, and the controllability of the preparation conditions is poor. In summary, how to synthesize the tungsten oxide electrochromic material having the advantages of highly disordered tungsten oxide and highly ordered tungsten oxide by using a relatively simple preparation process capable of large-scale preparation becomes a big problem in practical application of the material, and no related report exists on preparing tungsten oxide electrochromic material with controllable ordered structure by controlling sputtering power (power is continuously adjustable and gradually reduced) by using a simple magnetron sputtering technology so as to obtain large transmittance modulation, high response speed and good cycle stability.
Disclosure of Invention
The invention aims to solve the technical problems that the existing tungsten oxide electrochromic material cannot simultaneously have large transmittance modulation, high response speed and high cycle stability, and provides a preparation method of a tungsten oxide electrochromic film with a controllable ordered structure.
A preparation method of a tungsten oxide electrochromic film with a controllable ordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
secondly, preparing a tungsten oxide electrochromic film with a controllable ordered structure on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 0.5 Pa-4.0 Pa, the sputtering power is changed during deposition, and the method specifically comprises the following steps:
depositing for 3-5 min under the highest sputtering power AW, then regulating the highest sputtering power AW to the lowest sputtering power BW at a constant speed for deposition, wherein the regulating speed is 0.5-5W/min, and stopping deposition when the lowest sputtering power BW is regulated;
the maximum sputtering power AW is any value of 50W-300W, the minimum sputtering power BW is any value of 30W-250W, and the maximum sputtering power is at least higher than the minimum sputtering power of 20W;
the ion diffusion coefficient of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 5.0 multiplied by 10-11～3.0×10-9。
The invention has the advantages that:
firstly, a transparent conductive substrate is used as a substrate, and a tungsten oxide electrochromic film with a controllable ordered structure is prepared on the transparent conductive substrate by controlling sputtering power (the power is continuously adjustable and gradually reduced); the tungsten oxide electrochromic film with the controllable ordered structure, which is prepared by the invention, integrates the tungsten oxide film with the highly disordered structure, has the advantages of high response speed, large modulation amplitude of transmittance and good cycle stability of the highly ordered tungsten oxide film in the electrochromic process, has good electrochromic performance, and can ensure that the electrochromic film has the characteristics of good cycle stability and quick response while keeping large optical modulation amplitude;
the method is used for preparing the tungsten oxide electrochromic film with controllable ordered structure, high transmittance modulation amplitude, quick response and high cycle stability.
Drawings
FIG. 1 is a plan view of an electron microscope of an electrochromic tungsten oxide film with controllable ordered structure prepared in the first embodiment;
FIG. 2 is a schematic structural diagram of a controllable ordered structure tungsten oxide electrochromic film prepared in the first embodiment;
FIG. 3 is a graph showing the transmittance spectra of an electrochromic film of tungsten oxide with controllable ordered structure in the colored state and the bleached state, in which 1 is bleached and 2 is colored, prepared in the first example;
FIG. 4 is a graph showing the transmittance spectra of an electrochromic film of tungsten oxide having a controllable ordered structure in a colored state and a discolored state, in which 1 is discolored and 2 is colored, prepared in example II;
FIG. 5 is a transmission spectrum of a tungsten oxide electrochromic film with controllable ordered structure prepared in example three, wherein 1 is discoloration and 2 is coloration.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
The first embodiment is as follows: the embodiment provides a preparation method of a tungsten oxide electrochromic film with a controllable ordered structure, which is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
secondly, preparing a tungsten oxide electrochromic film with a controllable ordered structure on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 0.5 Pa-4.0 Pa, the sputtering power is changed during deposition, and the method specifically comprises the following steps:
depositing for 3-5 min under the highest sputtering power AW, then regulating the highest sputtering power AW to the lowest sputtering power BW at a constant speed for deposition, wherein the regulating speed is 0.5-5W/min, and stopping deposition when the lowest sputtering power BW is regulated;
the maximum sputtering power AW is any value of 50W-300W, the minimum sputtering power BW is any value of 30W-250W, and the maximum sputtering power is at least higher than the minimum sputtering power of 20W;
the ion diffusion coefficient of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 5.0 multiplied by 10-11～3.0×10-9。
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the volume ratio of oxygen to argon in the working pressure in the second step is (0.5-50): 50-99.5. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the volume ratio of oxygen to argon in the working pressure in the second step is 0.5: 99.5. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: and the volume ratio of oxygen to argon in the working pressure in the second step is 50: 50. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and the volume ratio of the oxygen to the argon in the working pressure in the second step is 30: 70. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 20 nm-800 nm. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 300 nm. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: and step two, firstly depositing for 5min under the highest sputtering power of 300W, then uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W for deposition, wherein the adjustment rate is 0.5W/min, and stopping deposition when the lowest sputtering power of 30W is adjusted. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and step two, firstly depositing for 5min at the highest sputtering power of 300W, then uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W for deposition, wherein the adjustment rate is 1W/min, and stopping deposition when the lowest sputtering power of 30W is adjusted. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: and step two, firstly depositing for 5min at the highest sputtering power of 300W, then uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W for deposition, wherein the adjustment rate is 2W/min, and stopping deposition when the lowest sputtering power of 30W is adjusted. The other steps are the same as those in the first to ninth embodiments.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The first embodiment is as follows: a preparation method of a tungsten oxide electrochromic film with a controllable ordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
the transparent conductive substrate in the first step is ITO;
secondly, preparing a tungsten oxide electrochromic film with a controllable ordered structure on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 0.5Pa, the sputtering power is changed during deposition, and the method specifically comprises the following steps:
firstly, depositing for 5min under the highest sputtering power of 300W, then uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W for deposition, wherein the adjusting rate is 0.5W/min, and stopping deposition when the lowest sputtering power of 30W is adjusted;
the volume ratio of oxygen to argon in the working pressure in the second step is 50: 50;
the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 800nm, and the ion diffusion coefficient is 3.0 multiplied by 10-9；
The transmittance of the tungsten oxide electrochromic film with the controllable ordered structure prepared in the first embodiment at 550nm is modulated to be 82.9%, the coloring/fading time is respectively 5.3s and 4.8s, and the transmittance modulation retention rate after 1000 cycles of stability is 96%.
FIG. 1 is a plan view of an electron microscope of an electrochromic tungsten oxide film with a controllable ordered structure prepared in the first embodiment;
as can be seen from fig. 1, the surface of the tungsten oxide electrochromic film with controllable ordered structure prepared in the first example is granular and has some small cracks.
FIG. 2 is a schematic structural diagram of a tungsten oxide electrochromic film with controllable ordered structure prepared in the first embodiment;
as can be seen from FIG. 2, the ordered structure of the thin film gradually changes from high to low as the sputtering power changes from high to low.
FIG. 3 is a graph showing the transmittance spectra of the electrochromic film of tungsten oxide with controllable ordered structure in the colored state and the bleached state, in which 1 is bleached and 2 is colored;
as can be seen from fig. 3, the electrochromic tungsten oxide film with controllable ordered structure prepared in the first example has a large transmittance modulation (82.9% at 550 nm).
Example two: a preparation method of a tungsten oxide electrochromic film with a controllable ordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
the transparent conductive substrate in the first step is ITO;
secondly, preparing a tungsten oxide electrochromic film with a controllable ordered structure on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 4.0Pa, the sputtering power is changed during deposition, and the method specifically comprises the following steps:
depositing for 5min under the condition that the highest sputtering power is 54W, then uniformly adjusting the highest sputtering power from 54W to the lowest sputtering power of 30W for deposition, wherein the adjusting rate is 1W/min, and stopping deposition when the lowest sputtering power is 30W;
the volume ratio of oxygen to argon in the working pressure in the second step is 0.5: 99.5;
the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 20nm, and the ion diffusion coefficient is 5.0 multiplied by 10-11；
The transmittance of the tungsten oxide electrochromic film with the controllable ordered structure prepared in the second embodiment at 550nm is adjusted to 16.4%, the coloring/fading time is 1.9s and 1.4s respectively, and the transmittance adjustment retention rate after 1000 cycles of stability is 98%.
FIG. 4 is a graph showing transmittance spectra in a colored state and a discolored state of the tungsten oxide electrochromic film with controllable ordered structure prepared in example two, in which 1 is discoloring and 2 is coloring;
as can be seen from fig. 4, the tungsten oxide electrochromic film with controllable ordered structure prepared in example two has a small transmittance modulation (16.4% at 550 nm).
Example three: a preparation method of a tungsten oxide electrochromic film with a controllable ordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
the transparent conductive substrate in the first step is ITO;
secondly, preparing a tungsten oxide electrochromic film with a controllable ordered structure on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 4.0Pa, the sputtering power is changed during deposition, and the method specifically comprises the following steps:
firstly, depositing for 5min under the highest sputtering power of 200W, then uniformly adjusting the highest sputtering power of 200W to the lowest sputtering power of 40W for deposition, wherein the adjusting rate is 2W/min, and stopping deposition when the lowest sputtering power of 40W is adjusted;
the volume ratio of oxygen to argon in the working pressure in the second step is 30: 70;
step two, the ordered structure controllable tungsten oxide is electrically inducedThe thickness of the color-changing film is 300nm, and the ion diffusion coefficient is 7.0 multiplied by 10-10；
The transmittance of the tungsten oxide electrochromic film with the controllable ordered structure prepared in the third embodiment at 550nm is adjusted to 51.0%, the coloring/fading time is 2.8s and 2.1s respectively, and the transmittance adjustment retention after 1000 cycles of stability is 97%.
FIG. 5 is a transmission spectrum of the electrochromic film of tungsten oxide with controllable ordered structure prepared in example three, wherein 1 is discoloration and 2 is coloration.
As can be seen from fig. 5, the tungsten oxide electrochromic film with controllable ordered structure prepared in example three has a large transmittance modulation (51.0% at 550 nm).
Comparative example one: a preparation method of a tungsten oxide electrochromic film with a highly ordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
secondly, preparing a tungsten oxide electrochromic film on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 1.0Pa, the sputtering power is 250W, and the deposition time is 100 min;
the volume ratio of oxygen to argon in the working pressure in the second step is 40: 60;
the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 380nm, and the ion diffusion coefficient is 4.0 multiplied by 10-11；
The transmittance of the tungsten oxide electrochromic film prepared in the first comparative example at 550nm was adjusted to 25.0%, the coloring/fading times were 18.9s and 17.5s, respectively, and the transmittance adjustment retention after 1000 cycles of stability was 99%.
Comparative example two: a preparation method of a tungsten oxide electrochromic film with a highly disordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
secondly, preparing a tungsten oxide electrochromic film on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 1.5Pa, the sputtering power is 50W, and the deposition time is 180 min;
the volume ratio of oxygen to argon in the working pressure in the second step is 50: 50;
the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 420nm, and the ion diffusion coefficient is 2.0 multiplied by 10-9；
The transmittance of the tungsten oxide electrochromic film prepared in the second comparative example at 550nm was adjusted to 86.0%, the coloring/fading times were 1.8s and 1.3s, respectively, and the transmittance adjustment retention after 1000 cycles of stability was 36%.
Claims (10)
1. A preparation method of a tungsten oxide electrochromic film with a controllable ordered structure is characterized in that the preparation method of the tungsten oxide electrochromic film with the controllable ordered structure is completed according to the following steps:
firstly, ultrasonically cleaning a transparent conductive substrate by sequentially adopting acetone, ethanol and ultrapure water, and drying;
secondly, preparing a tungsten oxide electrochromic film with a controllable ordered structure on the transparent conductive substrate obtained in the first step by adopting a magnetron sputtering process;
the process conditions of the magnetron sputtering process in the step two are as follows: the target material is a tungsten target, the working pressure is mixed gas of oxygen and argon, the working pressure is 0.5 Pa-4.0 Pa, the sputtering power is changed during deposition, and the method specifically comprises the following steps:
depositing for 3-5 min under the highest sputtering power AW, then regulating the highest sputtering power AW to the lowest sputtering power BW at a constant speed for deposition, wherein the regulating speed is 0.5-5W/min, and stopping deposition when the lowest sputtering power BW is regulated;
the maximum sputtering power AW is any value of 50W-300W, the minimum sputtering power BW is any value of 30W-250W, and the maximum sputtering power is at least higher than the minimum sputtering power of 20W;
the ion diffusion coefficient of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 5.0 multiplied by 10-11～3.0×10-9。
2. The method according to claim 1, wherein the transparent conductive substrate in step two is an ITO, FTO, AZO, Ag nanowire or Ag nano-frame layer.
3. The method for preparing an electrochromic film of tungsten oxide with controllable ordered structure as claimed in claim 1, wherein the volume ratio of oxygen to argon in the working pressure in step two is (0.5-50): (50-99.5).
4. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 2, wherein the volume ratio of oxygen to argon in the working gas pressure in the second step is 0.5: 99.5.
5. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 2, wherein the volume ratio of oxygen to argon in the working gas pressure in the second step is 50: 50.
6. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 2, wherein the volume ratio of oxygen to argon in the working gas pressure in the second step is 30: 70.
7. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 1, wherein the thickness of the tungsten oxide electrochromic film with the controllable ordered structure in the step two is 20nm to 800 nm.
8. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 1, wherein in the second step, the deposition is performed for 5min under the highest sputtering power of 300W, and then the deposition is performed by uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W, wherein the adjustment rate is 0.5W/min, and the deposition is stopped when the lowest sputtering power of 30W is adjusted.
9. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 1, wherein in the second step, the deposition is performed for 5min under the highest sputtering power of 300W, and then the deposition is performed by uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W, wherein the adjustment rate is 1W/min, and the deposition is stopped when the lowest sputtering power of 30W is adjusted.
10. The method for preparing the tungsten oxide electrochromic film with the controllable ordered structure according to claim 1, wherein in the second step, the deposition is performed for 5min under the highest sputtering power of 300W, and then the deposition is performed by uniformly adjusting the highest sputtering power of 300W to the lowest sputtering power of 30W, wherein the adjustment rate is 2W/min, and the deposition is stopped when the lowest sputtering power of 30W is adjusted.
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