CN115185134A - Method for recovering performance of electrochromic device - Google Patents
Method for recovering performance of electrochromic device Download PDFInfo
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- CN115185134A CN115185134A CN202210836491.8A CN202210836491A CN115185134A CN 115185134 A CN115185134 A CN 115185134A CN 202210836491 A CN202210836491 A CN 202210836491A CN 115185134 A CN115185134 A CN 115185134A
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 150000002500 ions Chemical class 0.000 claims description 23
- 239000003792 electrolyte Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 12
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 10
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical group O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 10
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 6
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 6
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 6
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 230000015556 catabolic process Effects 0.000 claims description 4
- 238000006731 degradation reaction Methods 0.000 claims description 4
- 239000011244 liquid electrolyte Substances 0.000 claims description 4
- 229920000767 polyaniline Polymers 0.000 claims description 4
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical group CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 230000001351 cycling effect Effects 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 3
- 238000007738 vacuum evaporation Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 230000002238 attenuated effect Effects 0.000 abstract description 25
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 230000001172 regenerating effect Effects 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000009831 deintercalation Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000004040 coloring Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/163—Operation of electrochromic cells, e.g. electrodeposition cells; Circuit arrangements therefor
Abstract
A method for recovering the performance of an electrochromic device relates to the field of electrochromic devices, in particular to a method for recovering the performance of an electrochromic device. The invention aims to solve the problems that the existing method for recovering the performance attenuation of the electrochromic film is not suitable for an electrochromic device, and the commercial application of the electrochromic device is limited after the performance of the electrochromic device is attenuated. One method of restoring the performance of electrochromic devices is to use heat treatment to restore the original performance of the electrochromic devices with degraded performance. The specific method comprises the following steps: and (3) carrying out heat treatment on the electrochromic device with the attenuated performance at the temperature of 40-800 ℃ to recover the initial performance of the electrochromic device with the attenuated performance. The invention provides a simple, convenient and novel method, the service life of the device can be obviously prolonged by regenerating the attenuated electrochromic device through heating, and the method has important value; the method for restoring the performance of the electrochromic device can restore the initial performance to 95-100 percent.
Description
Technical Field
The invention relates to the field of electrochromic devices, in particular to a method for recovering the performance of an electrochromic device.
Background
Electrochromism refers to a phenomenon that under the action of an external electric field, the material reversibly changes optical properties (transmittance, absorptivity, reflectivity and the like) through reversible intercalation and deintercalation of cations such as hydrogen ions and lithium ions. Electrochromic devices are typically composed of five thin films, including two transparent conductive layers, an electrochromic layer, an electrolyte layer, and an ion storage layer. The electrochromic device has great application potential in the fields of intelligent windows, anti-dazzling rearview mirrors, spacecraft thermal control systems, electronic tags and the like.
The optical properties of the electrochromic material change due to intercalation and deintercalation of small cations, however, the intercalating and deintercalating ions are not in equilibrium during cycling, as a fraction of the ions will be trapped. This can lead to degradation of the electrochromic material, limiting its commercial application. In recent years, efforts have been made to improve the cycle stability of the ECD, and to restore the performance of the attenuated electrochromic device due to the inevitable presence of ion trapping. It has been reported that the trapped ions can be released by applying a constant current or voltage to the electrochromic film. Therefore, the attenuation of the performance of the electrochromic film caused by the trapping can be eliminated, and the original performance can be recovered. However, this approach is not suitable for devices because when a constant current or voltage is applied to the electrochromic layer to release the trapped ions, the ions will be excessively embedded into the complementary layer.
Disclosure of Invention
The invention aims to solve the problems that the existing method for recovering the performance attenuation of the electrochromic film is not suitable for an electrochromic device, and the commercial application of the electrochromic device is limited after the performance attenuation of the electrochromic device, and provides a method for recovering the performance of the electrochromic device.
A method for restoring the performance of electrochromic devices is suitable for various types of electrochromic devices, including liquid electrolyte, gel electrolyte and solid electrolyte type devices. The electrochromic layer may be organic, such as: polyaniline, polythiophene, polypyrrole, etc., and can also be inorganic, such as: tungsten oxide, nickel oxide, vanadium oxide.
The performance of the electrochromic device is attenuated in the circulating process, and the optical modulation amplitude is reduced, the response speed is reduced, and the coloring efficiency is reduced.
One method of restoring the performance of electrochromic devices is to use heat treatment to restore the original performance of the electrochromic devices with degraded performance.
Further, the electrochromic device with the attenuated performance is subjected to heat treatment at the temperature of 40-800 ℃, so that the electrochromic device with the attenuated performance can recover the initial performance.
The invention has the advantages that:
1. after the method is used, the trapped ions can cross the energy barrier and be released again to restore the activity, so that the initial performance of the electrochromic device is restored;
2. the invention provides a simple, convenient and novel method, the service life of the device can be obviously prolonged by regenerating the attenuated electrochromic device through heating, the green sustainable development is realized, and the method has important value;
3. the method for restoring the performance of the electrochromic device can restore the initial performance to 95-100 percent.
Drawings
FIG. 1 is a diagram of a recovery mechanism for recovering the performance of an electrochromic device according to the present invention;
fig. 2 is a graph of transmittance control recovery performance for recovering the performance of an electrochromic device in example 1.
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 specific implementation way is as follows: in this embodiment, a method for recovering the performance of the electrochromic device is to recover the initial performance of the electrochromic device with degraded performance by using heat treatment.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: and (3) carrying out heat treatment on the electrochromic device with the attenuated performance at the temperature of 40-800 ℃ to recover the initial performance of the electrochromic device with the attenuated performance. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is: the time of the heat treatment is 20 min-300 min. The other steps are the same as those 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: the atmosphere of the heat treatment is air, argon or vacuum atmosphere. 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 (3) placing the electrochromic device with the attenuated performance into a tube furnace, a muffle furnace or an oven for heat treatment. 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 electrochromic device is an all-solid electrochromic device and is prepared on a glass substrate by adopting a magnetron sputtering method, the upper electrode and the lower electrode are indium tin oxide, the electrochromic layer is tungsten oxide, the electrolyte layer is lithium tantalate, the ion storage layer is nickel oxide, the performance of the prepared electrochromic device is attenuated after circulation, and the attenuated electrochromic device is subjected to heat treatment for 2 hours at 300 ℃. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and the first to sixth embodiments is: the electrochromic device is an all-solid electrochromic device and is prepared on a glass substrate by adopting a vacuum evaporation coating method, an upper electrode and a lower electrode are indium tin oxide, an electrochromic layer is tungsten oxide, an electrolyte layer is tantalum oxide, an ion storage layer is nickel oxide, and electrolyte ions are evaporated metal lithium. 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: the electrochromic device is an adhesive sandwiched electrochromic device, the electrochromic layer is tungsten oxide, the ion storage layer is nickel oxide, the substrate is ITO glass, the electrolyte layer is a mixture of lithium perchlorate dissolved in propylene carbonate and ultraviolet curing adhesive, the performance of the prepared electrochromic device is attenuated after circulation, and the attenuated electrochromic device is subjected to heat treatment for 50min at 50 ℃. 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: the electrochromic device is a liquid electrolyte electrochromic device, the electrochromic layer and the ion storage layer are both polyaniline, the substrate is a gold-plated porous membrane, the electrolyte layer is lithium perchlorate dissolved in propylene carbonate, the performance of the prepared electrochromic device is attenuated after circulation, and the attenuated electrochromic device is subjected to heat treatment at 50 ℃ for 30min.
The other steps are the same as those in the first to eighth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1: a method for restoring the performance of an electrochromic device is completed according to the following steps:
the electrochromic device is an all-solid electrochromic device and is prepared on a glass substrate by adopting a magnetron sputtering method, the upper electrode and the lower electrode are indium tin oxide, the electrochromic layer is tungsten oxide, the electrolyte layer is lithium tantalate, and the ion storage layer is nickel oxide.
Using the method of example 1, the decaying electrochromic device recovered 97% of the initial performance, as in fig. 2.
Fig. 2 is a graph of transmittance control recovery performance for recovering the performance of an electrochromic device in example 1.
As can be seen from fig. 2: in the initial state of the device, the 550nm transmittance modulation amplitude is 48.8%, and after circulation, the transmittance modulation amplitude is greatly reduced to 18.8%, the optical modulation range of the device at 550nm is recovered to 47.5%, the optical modulation range is only 1.3% lower than that in the initial state, and the recovery efficiency can reach 97%.
Example 2: a method for restoring the performance of an electrochromic device is completed according to the following steps:
the electrochromic device is an all-solid electrochromic device and is prepared on a glass substrate by adopting a vacuum evaporation coating method, an upper electrode and a lower electrode are indium tin oxide, an electrochromic layer is tungsten oxide, an electrolyte layer is tantalum oxide, an ion storage layer is nickel oxide, and electrolyte ions are evaporated metal lithium, the prepared electrochromic device has performance attenuation after circulation, and the attenuated electrochromic device is subjected to heat treatment for 2 hours at 350 ℃;
using the method of example 2, the decaying electrochromic device recovered 95% of the initial performance.
Example 3: a method for restoring the performance of an electrochromic device is completed according to the following steps:
the electrochromic device is an adhesive sandwiched electrochromic device, the electrochromic layer is tungsten oxide, the ion storage layer is nickel oxide, the substrate is ITO glass, the electrolyte layer is a mixture of lithium perchlorate dissolved in propylene carbonate and ultraviolet curing adhesive, the performance of the prepared electrochromic device is attenuated after circulation, and the attenuated electrochromic device is subjected to heat treatment for 50min at 50 ℃;
using the method of example 3, the attenuated electrochromic device recovered 100% of the original performance.
Example 4: a method for restoring the performance of an electrochromic device is completed according to the following steps:
the electrochromic device is a liquid electrolyte electrochromic device, the electrochromic layer and the ion storage layer are both polyaniline, the substrate is a gold-plated porous membrane, the electrolyte layer is lithium perchlorate dissolved in propylene carbonate, the performance of the prepared electrochromic device is attenuated after circulation, and the attenuated electrochromic device is subjected to heat treatment at 50 ℃ for 30min;
using the method of example 4, the attenuated electrochromic device recovered 98% of the original performance.
Claims (9)
1. A method for recovering the performance of an electrochromic device is characterized in that the method for recovering the performance of the electrochromic device is to recover the initial performance of the electrochromic device with the performance attenuation by adopting heat treatment.
2. The method of claim 1, wherein the deteriorated electrochromic device is heat-treated at 40 ℃ to 800 ℃ to restore the original performance of the deteriorated electrochromic device.
3. The method of claim 2, wherein the heat treatment time is 20min to 300min.
4. The method of claim 2, wherein the heat treatment is performed in an atmosphere of air, argon or vacuum.
5. The method for restoring the performance of the electrochromic device according to claim 2, wherein the electrochromic device with the degraded performance is put into a tube furnace, a muffle furnace or an oven for heat treatment.
6. The method of claim 2, wherein the electrochromic device is an all-solid electrochromic device and is prepared on a glass substrate by a magnetron sputtering method, the upper and lower electrodes are indium tin oxide, the electrochromic layer is tungsten oxide, the electrolyte layer is lithium tantalate, the ion storage layer is nickel oxide, the prepared electrochromic device shows performance degradation after cycling, and the degraded electrochromic device is subjected to heat treatment at 300 ℃ for 2h.
7. The method according to claim 2, wherein the electrochromic device is a full-solid electrochromic device and is prepared on a glass substrate by a vacuum evaporation coating method, the upper and lower electrodes are indium tin oxide, the electrochromic layer is tungsten oxide, the electrolyte layer is tantalum oxide, the ion storage layer is nickel oxide, and the electrolyte ions are evaporated metal lithium, the prepared electrochromic device shows performance degradation after cycling, and the degraded electrochromic device is subjected to heat treatment at 350 ℃ for 2 hours.
8. The method for recovering the performance of the electrochromic device according to claim 2, wherein the electrochromic device is a laminated electrochromic device, the electrochromic layer is tungsten oxide, the ion storage layer is nickel oxide, the substrate is ITO glass, the electrolyte layer is a mixture of lithium perchlorate dissolved in propylene carbonate and ultraviolet curing glue, the prepared electrochromic device has performance degradation after circulation, and the degraded electrochromic device is subjected to heat treatment at 50 ℃ for 50min.
9. The method for restoring the performance of the electrochromic device according to claim 2, wherein the electrochromic device is a liquid electrolyte electrochromic device, the electrochromic layer and the ion storage layer are both polyaniline, the substrate is a gold-plated porous membrane, the electrolyte layer is lithium perchlorate dissolved in propylene carbonate, the prepared electrochromic device shows performance decay after circulation, and the decayed electrochromic device is subjected to heat treatment at 50 ℃ for 30min.
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US20070097481A1 (en) * | 2005-10-11 | 2007-05-03 | Sage Electrochromics, Inc. | Electrochromic devices having improved ion conducting layers |
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US20150097944A1 (en) * | 2011-03-31 | 2015-04-09 | Sage Electrochromics, Inc. | System and method for detecting and repairing defects in an electrochromic device using thermal imaging |
CN107065372A (en) * | 2017-04-19 | 2017-08-18 | 无锡威迪变色玻璃有限公司 | A kind of electrochomeric glass self-repairing method and system |
CN113204146A (en) * | 2021-05-07 | 2021-08-03 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device taking water vapor as electrolyte and preparation method thereof |
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2022
- 2022-07-15 CN CN202210836491.8A patent/CN115185134A/en active Pending
Patent Citations (5)
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US20070097481A1 (en) * | 2005-10-11 | 2007-05-03 | Sage Electrochromics, Inc. | Electrochromic devices having improved ion conducting layers |
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