CN115857241A - Electrochromic device containing transparent CdO layer - Google Patents
Electrochromic device containing transparent CdO layer Download PDFInfo
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- CN115857241A CN115857241A CN202211489606.7A CN202211489606A CN115857241A CN 115857241 A CN115857241 A CN 115857241A CN 202211489606 A CN202211489606 A CN 202211489606A CN 115857241 A CN115857241 A CN 115857241A
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Abstract
The invention provides an electrochromic device containing a transparent CdO layer, which comprises a first electrode, a gel electrolyte and a second electrode; the first electrode comprises a first FTO conductive glass, a first cadmium oxide layer disposed on the first FTO conductive glass layer, an electrochromic layer disposed on the first cadmium oxide layer; the second electrode includes: the first FTO conductive glass, a first cadmium oxide layer arranged on the first FTO conductive glass, and a counter electrode material layer arranged on the first cadmium oxide layer; the gel electrolyte is located between the electrochromic layer of the first electrode and the counter electrode material layer of the second electrode. The invention can effectively improve the performance of the electrochromic device by simultaneously adsorbing electrochromic molecules and counter electrode molecules by using the cadmium oxide film, so that the electrochromic device has the advantages of good color-changing uniformity, good memory effect, short reaction time and the like.
Description
Technical Field
The invention belongs to the technical field of electrochromic devices, and particularly relates to an electrochromic device containing a transparent CdO layer.
Background
Electrochromism refers to a phenomenon in which optical properties (reflectivity, transmittance, absorption, and the like) of a material undergo a stable and reversible color change under the action of an applied electric field, and is visually represented as a reversible change in color and transparency. And devices made with electrochromic materials are referred to as electrochromic devices. At present, electrochromic devices that have been industrialized mainly include: electrochromic intelligent dimming glass, electrochromic display and automatic anti-dazzling rearview mirror of automobile. The electrochromic intelligent glass has adjustability of light absorption and permeation under the action of an electric field, can selectively absorb or reflect external heat radiation and internal heat diffusion, simultaneously achieves the purposes of improving the natural illumination degree and preventing peeping, and is a development direction of energy-saving building materials.
The existing electrochromic device has the problems of poor color-changing uniformity, poor memory effect, slow reaction time and the like.
Disclosure of Invention
Based on the above, the invention aims to provide an electrochromic device containing a transparent CdO layer, which has the advantages of good color change uniformity, good memory effect, short reaction time and the like.
In order to achieve the purpose, the invention adopts the following technical scheme.
An electrochromic device comprising a first electrode, a gel electrolyte, and a second electrode;
the first electrode comprises a first FTO conductive glass, a first cadmium oxide layer disposed on the first FTO conductive glass layer, an electrochromic layer disposed on the first cadmium oxide layer;
the second electrode includes: the first FTO conductive glass, a first cadmium oxide layer arranged on the first FTO conductive glass, and a counter electrode material layer arranged on the first cadmium oxide layer;
the gel electrolyte is located between the electrochromic layer of the first electrode and the counter electrode material layer of the second electrode.
In some embodiments, the first cadmium oxide layer and/or the second cadmium oxide layer has a thickness from 5nm to 20nm.
In some embodiments, the electrochromic molecules in the electrochromic layer are selected from at least one of viologens, phenothiazines, and triphenylamines; preferably, the electrochromic molecule is selected from viologens.
In some embodiments, the counter electrode molecules in the counter electrode material layer are selected from at least one of ferrocene and benzoquinone small molecule compounds.
In some embodiments, the gel electrolyte comprises lithium perchlorate, polyvinyl butyral, and allyl carbonate; and the mass ratio of the lithium perchlorate to the polyvinyl butyral to the allyl carbonate is (0.5-2): (1-2): (15-30); and/or the solid content of the gel electrolyte is 5-25%.
The invention also provides a preparation method of the electrochromic device, which comprises the following steps: (1) preparing a first electrode: smearing cadmium oxide solution with the concentration of 0.1 mmol/L-5 mmol/L on the first FTO conductive glass, drying, then soaking in solution containing electrochromic molecules, taking out and drying to obtain the first electrode; (2) preparing a second electrode: smearing cadmium oxide solution with the concentration of 0.1 mmol/L-5 mmol/L on the second FTO conductive glass, drying, then soaking in solution containing counter electrode molecules, taking out and drying to obtain the second electrode; (3) And dropwise adding the gel electrolyte on the electrochromic layer of the first electrode, uniformly coating, covering the second electrode on the gel electrolyte in a staggered manner, leading out the electrodes, and carrying out UV (ultraviolet) curing and packaging to obtain the electrochromic device.
In some embodiments, the solvent of the cadmium oxide solution comprises glycerol, isopropanol and triethylamine, and the mass ratio of the glycerol to the isopropanol to the triethylamine is (0.05-0.15): (2-3.5): (0.1-0.4).
In some embodiments, the concentration of electrochromic molecules in the solution containing electrochromic molecules is
5 mmol/L-50 mmol/L; preferably, the concentration of the electrochromic molecules in the solution containing the electrochromic molecules is 10 mmol/L-45 mmol/L.
In some embodiments, the concentration of the counter electrode molecules in the solution containing the counter electrode molecules is 5mol/L to 100mol/L; preferably, the concentration of the counter electrode molecules in the solution containing the counter electrode molecules is 10mol/L to 80mol/L.
In some embodiments, the electrochromic molecule is selected from at least one of viologens, phenothiazines, and triphenylamines; and/or the counter electrode molecule is selected from at least one of ferrocene and benzoquinone small molecule compounds.
In some embodiments, the soaking time in step (1) and/or step (2) is 20-30 h.
The invention provides an electrochromic device, which has the following structure: the FTO glass, the cadmium oxide layer, the electrochromic layer, the electrolyte layer, the counter electrode material layer, the cadmium oxide layer and the FTO glass can effectively improve the performance of the electrochromic device by using the cadmium oxide film to adsorb electrochromic molecules and counter electrode molecules simultaneously, so that the electrochromic device has the advantages of good color change uniformity, better memory effect, short reaction time and the like, because the electrochromic molecules of the electrochromic device can be adsorbed on the cadmium oxide layer very uniformly, and the color change and color fading are very uniform; secondly, as the counter electrode molecules are adsorbed on the cadmium oxide particles, the migration-in and migration-out processes of ions are hindered, so that the electrochromic device has better memory effect and can realize color fading only by applying reverse voltage; finally, because the electrochromic molecules are adsorbed on the surface of the cadmium oxide layer, only the oxidation-reduction process of the surface is carried out, and the diffusion process is not carried out, so that the reaction time is short.
Drawings
FIG. 1 is a fade and stain plot for an electrochromic device of example 1.
Detailed Description
Experimental procedures according to the invention, in which no particular conditions are specified in the following examples, are generally carried out under conventional conditions, or under conditions recommended by the manufacturer. The various chemicals used in the examples are commercially available.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to only those steps or modules listed, but may alternatively include other steps not listed or inherent to such process, method, article, or device.
The "at least one" mentioned in the present invention means one or more than one. "and/or" describes the association relationship of the associated object, indicating that there may be three relationships, for example, a and/or B, which may indicate: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
The following description will be given with reference to specific examples.
Example 1
The present embodiment provides an electrochromic device comprising a first electrode, a gel electrolyte, and a second electrode; the first electrode comprises a first FTO conductive glass, a first cadmium oxide layer disposed on the first FTO conductive glass layer, an electrochromic layer disposed on the first cadmium oxide layer; the second electrode includes: the first FTO conductive glass, a first cadmium oxide layer arranged on the first FTO conductive glass, and a counter electrode material layer arranged on the first cadmium oxide layer;
the gel electrolyte is located between the electrochromic layer of the first electrode and the counter electrode material layer of the second electrode.
The gel electrolyte comprises lithium perchlorate, polyvinyl butyral, and allyl carbonate; and the mass ratio of the lithium perchlorate to the polyvinyl butyral to the allyl carbonate is 0.8:1:20; the solids content was 15%.
The electrochromic device is prepared by the following method:
(1) Preparing a first electrode: spin-coating a cadmium oxide solution (solvent comprising glycerol, isopropanol and triethylamine, and mass ratio of glycerol, isopropanol and triethylamine being 0.07): the rotating speed is 3000rpm/min, the annealing temperature is 100 ℃ (60 mins), then 200 ℃ (60 mins) is carried out, the first cadmium oxide layer with the dry film thickness of 15nm is obtained, then the first cadmium oxide layer is placed in a solution containing electrochromic molecules (the concentration of the electrochromic molecules is 30 mmol/L) to be soaked for 24 hours, and the first electrode is taken out and dried to obtain the first electrode;
(2) Preparing a second electrode: spin-coating a cadmium oxide solution (solvent comprising glycerol, isopropanol and triethylamine, and mass ratio of glycerol, isopropanol and triethylamine being 0.07): rotating at 3000rpm/min, annealing at 100 deg.C (60 mins), then 200 deg.C (60 mins) to obtain a second cadmium oxide layer with a dry film thickness of 15nm, soaking in a solution containing counter electrode molecules (the concentration of the counter electrode molecules is 50 mmol/L) for 24h, taking out and drying to obtain the second electrode;
(3) Dropping the gel electrolyte (containing 100 μm spacing balls) on the electrochromic layer of the first electrode, uniformly scraping with a scraper, then covering the second electrode on the gel electrolyte in a staggered manner, leading out the electrodes, and carrying out UV curing packaging to obtain the electrochromic device, wherein the fading and coloring graphs of which are shown in figure 1.
Example 2
The present embodiment provides an electrochromic device comprising a first electrode, a gel electrolyte, and a second electrode; the first electrode comprises a first FTO conductive glass, a first cadmium oxide layer disposed on the first FTO conductive glass layer, an electrochromic layer disposed on the first cadmium oxide layer; the second electrode includes: the first FTO conductive glass, a first cadmium oxide layer arranged on the first FTO conductive glass, and a counter electrode material layer arranged on the first cadmium oxide layer;
the gel electrolyte is located between the electrochromic layer of the first electrode and the counter electrode material layer of the second electrode.
The gel electrolyte comprises lithium perchlorate, polyvinyl butyral, and allyl carbonate; and the mass ratio of the lithium perchlorate to the polyvinyl butyral to the allyl carbonate is 1:1.5:25; the solids content was 20%.
The electrochromic device is prepared by the following method:
(1) Preparing a first electrode: spin-coating a cadmium oxide solution (solvent comprising glycerol, isopropanol and triethylamine, and mass ratio of glycerol, isopropanol and triethylamine being 0.1.3) with a concentration of 1.5mmol/L onto the first FTO conductive glass: the rotation speed is 5000rpm/min, the annealing temperature is 100 ℃ (60 mins), then 200 ℃ (60 mins), and a first cadmium oxide layer with the thickness of 10nm of a dry film is obtained; then placing the electrode in a solution containing electrochromic molecules (the concentration of the electrochromic molecules is 15 mmol/L) to be soaked for 26 hours, taking out and drying to obtain the first electrode;
(2) Preparing a second electrode: spin-coating a cadmium oxide solution (solvent comprising glycerol, isopropanol and triethylamine, and mass ratio of glycerol, isopropanol and triethylamine being 0.1.3) with a concentration of 1.5mmol/L onto the second FTO conductive glass: the rotation speed is 5000rpm/min, the annealing temperature is 100 ℃ (60 mins), then 200 ℃ (60 mins) is carried out, the second cadmium oxide layer with the dry film thickness of 10nm is obtained, then the second cadmium oxide layer is placed in a solution containing counter electrode molecules (the concentration of the counter electrode molecules is 70 mmol/L) to be soaked for 26 hours, and the second electrode is taken out and dried to obtain the second electrode;
(3) And dropwise adding the gel electrolyte (containing 100-micron spacing balls) on the electrochromic layer of the first electrode, uniformly blade-coating by using a scraper, covering the gel electrolyte with the second electrode in a staggered manner, leading out the electrodes, and carrying out UV curing and packaging to obtain the electrochromic device.
Example 3
The present embodiment provides an electrochromic device comprising a first electrode, a gel electrolyte, and a second electrode; the first electrode comprises a first FTO conductive glass, a first cadmium oxide layer disposed on the first FTO conductive glass layer, an electrochromic layer disposed on the first cadmium oxide layer; the second electrode includes: the first FTO conductive glass, a first cadmium oxide layer arranged on the first FTO conductive glass, and a counter electrode material layer arranged on the first cadmium oxide layer;
the gel electrolyte is located between the electrochromic layer of the first electrode and the counter electrode material layer of the second electrode.
The gel electrolyte comprises lithium perchlorate, polyvinyl butyral, and allyl carbonate; and the mass ratio of the lithium perchlorate to the polyvinyl butyral to the allyl carbonate is 1.5:2:28; the solids content was 10%.
The electrochromic device is prepared by the following method:
(1) Preparing a first electrode: spin-coating a cadmium oxide solution (solvent comprising glycerol, isopropanol and triethylamine, and mass ratio of glycerol, isopropanol and triethylamine being 0.07: the rotating speed is 2000rpm/min, the annealing temperature is 100 ℃ (60 mins), then 200 ℃ (60 mins) is carried out, the first cadmium oxide layer with the dry film thickness of 8nm is obtained, then the first cadmium oxide layer is placed in a solution containing electrochromic molecules (the concentration of the electrochromic molecules is 40 mmol/L) to be soaked for 20 hours, and the first electrode is taken out and dried to obtain the first electrode;
(2) Preparing a second electrode: spin-coating a cadmium oxide solution (solvent comprising glycerol, isopropanol and triethylamine, and mass ratio of glycerol, isopropanol and triethylamine being 0.07: the rotating speed is 2000rpm/min, the annealing temperature is 100 ℃ (60 mins), then 200 ℃ (60 mins) is carried out, the second cadmium oxide layer with the dry film thickness of 8nm is obtained, then the second cadmium oxide layer is placed in a solution containing counter electrode molecules (the concentration of the counter electrode molecules is 30 mol/L) to be soaked for 20 hours, and the second electrode is taken out and dried to obtain the second electrode;
(3) And dripping the gel electrolyte (containing 100-micron spacing balls) on the electrochromic layer of the first electrode, uniformly scraping and coating by using a scraper, covering the second electrode on the gel electrolyte in a staggered manner, leading out the electrodes, and carrying out UV (ultraviolet) curing and packaging to obtain the electrochromic device.
Example 4
This example provides an electrochromic device that is the same as example 1 except that the first and second cadmium oxide layers have a thickness of 3 nm.
Example 5
This example provides an electrochromic device that is the same as example 1 except that the first and second cadmium oxide layers have a thickness of 25 nm.
Comparative example 1
This comparative example provides an electrochromic device that is identical to example 1 except that it does not contain the first and second cadmium oxide layers, and both electrochromic molecules and counter electrode molecules are dissolved in the gel electrolyte to form a uniform all-in-one gel electrochromic device.
Comparative example 2
This comparative example provides an electrochromic device that is the same as example 1 except that the first and second cadmium oxide layers are replaced with first and second silver nanowire conductive layers.
The electrochromic devices in the above examples and comparative examples were examined for coloration time and fade time: an electrochemical workstation and an ultraviolet-visible spectrophotometer are adopted for combined test, and the test method is a chronopotentiometry.
The results are shown in table 1:
TABLE 1 test results
| Group of | Colouring time | Time of color fading | Optical contrast (607 nm) |
| Example 1 | 2.1s | 1.5s | 76.3％ |
| Example 2 | 1.9s | 1.4s | 72.3％ |
| Example 3 | 1.7s | 1.2s | 60.1％ |
| Example 4 | 1.3s | 1.0s | 41.9％ |
| Example 5 | 2.5s | 1.8s | 54.9％ |
| Comparative example 1 | 4.5s | 6.7s | 75.8％ |
| Comparative example 2 | - | - | - |
The above results indicate that the electrochromic device of the present invention (examples 1 to 3) has the advantages of good uniformity of color change, good memory effect, short reaction time, and the like, and both the coloring time and the fading time are short. In comparison with example 1, the thicknesses of the first cadmium oxide layer and the second cadmium oxide layer are smaller in example 4, and the thicknesses of the first cadmium oxide layer and the second cadmium oxide layer are larger in example 5. When the thickness of the cadmium oxide layer is too small (example 4), the number of adsorbed electrochromic molecules is small, which may affect the optical contrast of the device; when the thickness of the cadmium oxide layer is too large (example 5), the ion migration process may be greatly hindered, so that the reaction time may be increased, and the large thickness of the cadmium oxide may cause the cadmium oxide film to have color, which may also affect the optical contrast of the device.
Comparative example 1, which does not include the first cadmium oxide layer and the second cadmium oxide layer, results in a significant increase in both the coloration time and the discoloration time of the electrochromic device, as compared to example 1, because the discoloration and discoloration processes involve diffusion processes. Comparative example 2 replacing the first and second cadmium oxide layers with first and second silver nanowire layers failed to adsorb enough electrochromic molecules, resulting in failure to change color.
In conclusion, the invention can effectively improve the performance of the electrochromic device by simultaneously adsorbing electrochromic molecules and counter electrode molecules by using the cadmium oxide film, so that the electrochromic device has the advantages of good color change uniformity, good memory effect, short reaction time and the like.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, however, as long as there is no contradiction between the combinations of the technical features, the scope of the present description should be considered as being described in the present specification.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (10)
1. An electrochromic device, characterized in that it comprises a first electrode, a gel electrolyte and a second electrode;
the first electrode comprises a first FTO conductive glass, a first cadmium oxide layer disposed on the first FTO conductive glass layer, an electrochromic layer disposed on the first cadmium oxide layer;
the second electrode includes: the first FTO conductive glass, a first cadmium oxide layer arranged on the first FTO conductive glass, and a counter electrode material layer arranged on the first cadmium oxide layer;
the gel electrolyte is located between the electrochromic layer of the first electrode and the counter electrode material layer of the second electrode.
2. The electrochromic device of claim 1, wherein the first cadmium oxide layer and/or the second cadmium oxide layer has a thickness in the range of 5nm to 20nm.
3. The electrochromic device of claim 1, wherein the electrochromic molecules in the electrochromic layer are selected from at least one of viologens, phenothiazines, and triphenylamines.
4. The electrochromic device according to claim 1, wherein the counter electrode molecules in the counter electrode material layer are selected from at least one of ferrocene and benzoquinone small molecule compounds.
5. The electrochromic device of claim 1 wherein said gel electrolyte comprises lithium perchlorate, polyvinyl butyral, and allyl carbonate; and the mass ratio of the lithium perchlorate to the polyvinyl butyral to the allyl carbonate is (0.5-2): (1-2): (15-30); and/or the solid content of the gel electrolyte is 5-25%.
6. The method for producing an electrochromic device according to any one of claims 1 to 5, comprising the steps of: (1) preparing a first electrode: smearing cadmium oxide solution with the concentration of 0.1 mmol/L-5 mmol/L on the first FTO conductive glass, drying, then soaking in solution containing electrochromic molecules, taking out and drying to obtain the first electrode; (2) preparing a second electrode: smearing cadmium oxide solution with the concentration of 0.1 mmol/L-5 mmol/L on the second FTO conductive glass, drying, then soaking in solution containing counter electrode molecules, taking out and drying to obtain the second electrode; (3) And dripping the gel electrolyte on the electrochromic layer of the first electrode, uniformly coating, covering the second electrode on the gel electrolyte in a staggered manner, leading out the electrodes, and carrying out UV (ultraviolet) curing and packaging to obtain the electrochromic device.
7. The method according to claim 6, wherein the solvent of the cadmium oxide solution comprises glycerol, isopropanol and triethylamine, and the mass ratio of the glycerol to the isopropanol to the triethylamine is (0.05-0.15): (2-3.5): (0.1-0.4).
8. The method according to claim 6, wherein the concentration of the electrochromic molecule in the solution containing the electrochromic molecule is 5mmol/L to 50mmol/L; and/or the concentration of the counter electrode molecules in the solution containing the counter electrode molecules is 5 mol/L-100 mol/L.
9. The method according to claim 6, wherein the electrochromic molecule is at least one selected from viologens, phenothiazines, and triphenylamines; and/or the counter electrode molecule is selected from at least one of ferrocene and benzoquinone small molecule compounds.
10. The method according to claim 6, wherein the soaking time in step (1) and/or step (2) is 20 to 30 hours.
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| CN202211489606.7A CN115857241A (en) | 2022-11-25 | 2022-11-25 | Electrochromic device containing transparent CdO layer |
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| CN202211489606.7A CN115857241A (en) | 2022-11-25 | 2022-11-25 | Electrochromic device containing transparent CdO layer |
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