CN110543056B - Inorganic all-solid-state electrochromic device and preparation method thereof - Google Patents
Inorganic all-solid-state electrochromic device and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an inorganic all-solid-state electrochromic device and a preparation method thereof; belongs to the field of photoelectric devices. According to the invention, a nickel oxide ion storage layer is prepared at low temperature by using nickel oxide as a raw material through a solution method, then zirconium oxide is prepared as an ion conductive layer, and then hydrogen ions in electrolyte are injected into the ion storage layer through an external electric field, so that a laminated structure containing ions is obtained, and the original zirconium oxide without free mobile working ions can be used as the ion conductive layer. And then spin-coating a tungsten oxide electrochromic film and a transparent electrode on the substrate to form the inorganic all-solid-state electrochromic device.
Description
Technical Field
The invention belongs to the field of photoelectric devices, and particularly relates to an inorganic all-solid-state electrochromic device and a preparation method thereof.
Background
Electrochromic devices (ECDs) are widely used semiconductor devices, and the main purpose of the device is to control the intensity of visible light and solar radiation transmitted through the device by adjusting optical transmittance.
The intelligent window made of the traditional window and the electrochromic interlayer is widely applied to the field of buildings, and the window can be actively adjusted in light input by people, so that the room temperature is adjusted, and the energy consumption is reduced. The development of the intelligent window meets the environment-friendly requirement of green and low carbon, and the intelligent window is more popular and has a wide market along with the technical development.
The ion conducting layer of the traditional electrochromic device generally uses electrolyte or electrolyte gel which is formed by the electrolyte and organic gel, and has the defects of easy leakage, difficult packaging, no high temperature resistance, poor mechanical strength and the like.
If an inorganic material is used as the ion conductive layer, the above problems can be solved, and practical application of the electrochromic device is promoted.
In addition, the existing electrochromic devices are mainly used for electroplating and various vacuum methods (magnetron sputtering, laser pulse deposition and the like), but the methods have complex processes and higher cost and limit the industrial production and the popularization and application of the electrochromic devices to a certain extent.
Therefore, if a lower-cost electrochromic device and a preparation method can be developed, the production application of the electrochromic device can be further promoted.
Disclosure of Invention
The present invention aims to overcome the disadvantages and shortcomings of the prior art and to provide an inorganic all-solid electrochromic device and a method for manufacturing the same.
The invention has simple preparation process and low cost, and provides a positive technical basis for promoting the industrial production, popularization and application of the electrochromic device.
The invention is realized by the following technical scheme:
a preparation method of an inorganic all-solid-state electrochromic device comprises the following steps:
the method comprises the following steps: mixing nickel acetate (C)4H14NiO8) Dissolving ethylene glycol monomethyl ether (2-MOE), adding ethanolamine (C)2H7NO) as a stabilizer, heating, stirring, standing and aging to obtain a precursor A;
step two: spin-coating the precursor A obtained in the first step on a cleaned glass substrate with a transparent conductive electrode, and then annealing in an air atmosphere to obtain a nickel oxide film;
step three: zr (CH) (zirconium acetate)3COO)4Dissolving in ethylene glycol monomethyl ether (2-MOE), andadding ethanolamine (C)2H7NO) as a stabilizer, stirring, standing and aging to obtain a precursor solution B;
step four: spin-coating the precursor solution B obtained in the third step on the nickel oxide film obtained in the second step, and then annealing in an air atmosphere to obtain a laminated structure of zirconium oxide and nickel oxide;
step five: adding the laminated structure of the zirconium oxide and the nickel oxide obtained in the step four into a KOH electrolyte, fading under the condition of an external electric field, allowing hydrogen ions to enter and be stored in the laminated structure of the zirconium oxide and the nickel oxide, taking out and drying;
step six: mixing tungsten chloride (WCl)6) Dissolving in absolute ethyl alcohol (C)2H5OH), centrifugally stirring to obtain a precursor solution C;
step seven: spin-coating the precursor solution C obtained in the sixth step on the laminated structure of the zirconium oxide containing the hydrogen ions and the nickel oxide obtained in the fifth step, and annealing in the air atmosphere to obtain a nickel oxide/zirconium oxide/tungsten oxide laminated structure;
step eight: and (4) spinning and coating the silver nanowires on the laminated structure obtained in the step seven, and annealing in the air atmosphere to obtain the inorganic all-solid-state electrochromic device.
Heating in the first step, wherein the heating mode is oil bath or water bath, the temperature is 60 ℃, the stirring time is 2 hours, and the aging time is 24 hours;
in the first step, the concentration of nickel in the precursor A is 0.25-0.5 mol/L.
In the second step, the glass substrate with the transparent conductive electrode is ITO glass;
the spin coating in the second step is carried out under the following conditions: the method comprises the steps of firstly carrying out low-speed and then high-speed spinning, wherein the low-speed spinning speed is 700rpm, the high-speed spinning speed is 3000rpm, the spin-coating times are 3-5 times, the low-speed spin-coating time is 10s each time, the high-speed spin-coating time is 30-40 s, the annealing temperature between each spin-coating is 300 ℃, and the time is 3-5 min.
In the third step, the concentration of zirconium acetate in the precursor solution B is 0.3-0.6 mol/L, the stirring speed is 500rpm, and the aging time is 24 hours.
The spin coating in the fourth step is performed under the following spin coating conditions: the rotating speed is 4000-6000 rpm, the spin coating times are 3-5 times, the time of each spin coating is 30-40 s, the annealing temperature between each spin coating is 200 ℃, the time is 3-5 min, and the subsequent annealing temperature is 200 ℃.
The concentration of the KOH electrolyte in the fifth step is 0.1mol/L, the voltage of an external electric field is 1.5-2.5V, and the time for introducing hydrogen ions under the condition of the external electric field is 1-3 min;
and the drying in the fifth step is drying for 1-2 hours in a vacuum drying oven at the temperature of 70-100 ℃.
The centrifugal stirring time in the sixth step is 1-2 h, and the rotating speed is 3000 r/min;
and sixthly, the concentration of tungsten in the precursor solution in the step six is 0.25-0.5 mol/L.
The spin coating in the seventh step has the following process conditions: rotating at 3000rpm, performing spin coating for 1-2 times, and performing spin coating for 30-40 s each time;
the standing time in the seventh step is 30 min; the annealing temperature is 100-200 ℃, and the time is 1 h.
The spin coating in the step eight includes the following spin coating conditions: firstly low speed and then high speed, the low speed rotation speed is 700rpm, the high speed rotation speed is 3000rpm, the spin coating times are 2-4 times, the time of each low speed spin coating is 10s, the time of the high speed spin coating is 30-40 s, the annealing temperature between each spin coating is 100 ℃, the time is 3-5 min,
and in the step eight, the heat treatment temperature of the silver nanowires is 100-140 ℃, and the heat treatment time is 30 min-1 h.
An inorganic all-solid-state electrochromic device, the laminated structure of which comprises: the glass substrate layer, transparent conductive electrode layer, nickel oxide layer, zirconia layer, tungsten oxide layer, silver nanowire layer.
The action mechanism of the invention is as follows: the method comprises the steps of preparing a nickel oxide ion storage layer at a low temperature by using nickel oxide as a raw material through a solution method with simple process and low cost, then preparing zirconium oxide as an ion conductive layer, and then injecting hydrogen ions in electrolyte into the ion storage layer through an external electric field to obtain a laminated structure containing ions, so that the original zirconium oxide without free mobile working ions can be used as the ion conductive layer. And then spin-coating a tungsten oxide electrochromic film and a transparent electrode on the substrate to form the inorganic all-solid-state electrochromic device.
The preparation method and the obtained electrochromic device have the following advantages and beneficial effects:
the inorganic all-solid-state device is prepared by a solution method in an atmospheric environment, so that the problems of easy leakage, easy degradation and no high temperature resistance of a liquid electrolyte and an organic gel electrolyte are solved, and the practical application capability of the device is improved. Meanwhile, compared with the conventional vacuum method and electroplating, the method has the advantages that the process flow and the required equipment conditions are relatively simple, the production cost is greatly saved, and the method is favorable for large-scale industrial production.
The invention adopts the heat treatment temperature of 200 ℃ to anneal the zirconia film; the zirconia film obtained at the temperature has low density, loose structure and more ion conduction channels, and is beneficial to the ion conduction in the electrochromic process.
The invention adopts the drying temperature of 70-100 ℃, and hydrogen ions stored in the laminated structure of the zirconium oxide and the nickel oxide can not be separated due to overhigh temperature while the zirconium oxide and the nickel oxide are fully dried.
Annealing the tungsten oxide film by adopting a heat treatment temperature of 100-200 ℃; the tungsten oxide film obtained at the temperature is of an amorphous structure, and the structure is more favorable for ion injection in the electrochromic process when the tungsten oxide film is used as an electrochromic layer.
Drawings
Fig. 1 is a schematic view of a laminated structure of an inorganic all-solid electrochromic device according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) 1.224g of nickel acetate (C)4H14NiO8) Dissolving in 10ml ethylene glycol monomethyl ether (2-MOE), adding 0.5ml ethanolAmine (C)2H7NO) as a stabilizer, heating and stirring in an oil bath at 60 ℃ for 2h, standing and aging for 24h to obtain a precursor A;
(2) and ultrasonically cleaning the cut ITO conductive glass by using a detergent, deionized water and isopropanol successively, keeping for 15min each time, and drying in an oven after cleaning for later use.
(2) Spin-coating the precursor A obtained in the step (1) on a cleaned glass substrate with a transparent conductive electrode, firstly carrying out low-speed and then high-speed coating, wherein the low-speed rotation speed is 700rpm, the high-speed rotation speed is 3000rpm, the spin-coating times are 3 times, the low-speed spin-coating time is 10s and the high-speed spin-coating time is 30s, the annealing temperature between each spin-coating is 300 ℃, the annealing time is 3min, and then, the annealing is carried out for 1h at the temperature of 300 ℃ in the air atmosphere to obtain a nickel oxide;
(3) dissolving 1ml of zirconium acetate (liquid state, density of 1.279g/ml and Zr content of 15-16 wt%) in 2ml of ethylene glycol monomethyl ether (2-MOE), adding 12ul of ethanolamine, stirring at 500r/min, standing for 24h and aging to obtain 0.6mol/L precursor solution B;
(4) spin-coating the precursor solution B obtained in the step (3) on the nickel oxide film obtained in the step (2), wherein the spin-coating rotation speed is 6000rpm, the spin-coating time is 40s, the spin-coating times are 3 times, the annealing temperature between each spin-coating is 200 ℃, the annealing time is 3min, and then the annealing treatment is carried out for 1h at 200 ℃ to obtain a laminated structure of zirconium oxide and nickel oxide;
(5) adding the laminated structure of the zirconium oxide and the nickel oxide obtained in the step (4) into 0.1mo/LKOH electrolyte, adding a voltage of 2.5V for 1min for coloring, fading under the condition of an external electric field, allowing hydrogen ions to enter and store in the laminated structure of the zirconium oxide and the nickel oxide, taking out the film, and drying for 1h at 100 ℃ in a vacuum drying oven;
(6) 1g of WCl6(tungsten chloride) powder dissolved in 10ml of absolute ethanol (C)2H5OH), centrifugally stirring for 1h in a centrifugal machine at the speed of 3000r/min to obtain a precursor solution C;
(7) and (4) spin-coating the precursor solution C obtained in the step (6) on the laminated structure of the zirconium oxide and the nickel oxide containing the hydrogen ions obtained in the step (5), wherein the rotating speed is 3000r/min, and the spin-coating time is 40 s. Standing the wet film in air for 30min, and then annealing at 200 ℃ for 1h to obtain a nickel oxide/zirconium oxide/tungsten oxide laminated structure;
(8) and (3) spinning silver nanowires on the laminated structure obtained in the step (7), firstly spinning at low speed and then at high speed, wherein the low-speed rotation speed is 700rpm, the high-speed rotation speed is 3000rpm, the spinning times are 2 times, the time of each low-speed spinning is 10s, the time of the high-speed spinning is 30s, the annealing temperature between each spinning is 100 ℃, the time is 3min, and the annealing is carried out for 1h at 100 ℃ to obtain the inorganic all-solid-state electrochromic device.
Example 2
(1) 1.224g of nickel acetate (C)4H14NiO8) Dissolving in 20ml ethylene glycol monomethyl ether (2-MOE), adding 0.5ml ethanolamine (C)2H7NO) as a stabilizer, heating and stirring in an oil bath at 60 ℃ for 2h, standing and aging for 24h to obtain a precursor A;
(2) and ultrasonically cleaning the cut ITO conductive glass by using a detergent, deionized water and isopropanol successively, keeping for 15min each time, and drying in an oven after cleaning for later use.
(2) Spin-coating the precursor A obtained in the step (1) on a cleaned glass substrate with a transparent conductive electrode, firstly carrying out low-speed and then high-speed coating, wherein the low-speed rotation speed is 700rpm, the high-speed rotation speed is 3000rpm, the spin-coating times are 4 times, the low-speed spin-coating time is 10s and the high-speed spin-coating time is 30s, the annealing temperature between each spin-coating is 300 ℃, the annealing time is 3min, and then, the annealing is carried out for 1h at the temperature of 300 ℃ in the air atmosphere to obtain a nickel oxide;
(3) dissolving 1ml of zirconium acetate (liquid state, density of 1.279g/ml and Zr content of 15-16 wt%) in 4ml of ethylene glycol monomethyl ether (2-MOE), adding 12ul of ethanolamine, stirring at 500r/min, standing for 24h and aging to obtain 0.3mol/L precursor solution B;
(4) spin-coating the precursor solution B obtained in the step (3) on the nickel oxide film obtained in the step (2), wherein the spin-coating rotation speed is 6000rpm, the spin-coating time is 40s, the spin-coating times are 4 times, the annealing temperature between each spin-coating is 200 ℃, the annealing time is 3min, and then the annealing treatment is carried out for 1h at 200 ℃ to obtain a laminated structure of zirconium oxide and nickel oxide;
(5) adding the laminated structure of the zirconium oxide and the nickel oxide obtained in the step (4) into 0.1mo/LKOH electrolyte, adding a voltage of 2.5V for 1min for coloring, fading under the condition of an external electric field, allowing hydrogen ions to enter and store in the laminated structure of the zirconium oxide and the nickel oxide, taking out the film, and drying for 1h at 100 ℃ in a vacuum drying oven;
(6) 1g of WCl6(tungsten chloride) powder was dissolved in 20ml of absolute ethanol (C)2H5OH), centrifugally stirring for 1h in a centrifugal machine at the speed of 3000r/min to obtain a precursor solution C;
(7) and (4) spin-coating the precursor solution C obtained in the step (6) on the laminated structure of the zirconium oxide and the nickel oxide containing the hydrogen ions obtained in the step (5), wherein the rotating speed is 3000r/min, and the spin-coating time is 40 s. Standing the wet film in air for 30min, and then annealing at 100 ℃ for 1h to obtain a nickel oxide/zirconium oxide/tungsten oxide laminated structure;
(8) and (3) spinning silver nanowires on the laminated structure obtained in the step (7), firstly spinning at low speed and then at high speed, wherein the low-speed rotation speed is 700rpm, the high-speed rotation speed is 3000rpm, the spinning times are 2 times, the time of each low-speed spinning is 10s, the time of the high-speed spinning is 30s, the annealing temperature between each spinning is 100 ℃, the time is 3min, and the annealing is carried out for 1h at the temperature of 140 ℃ to obtain the inorganic all-solid-state electrochromic device.
As described above, the present invention can be preferably realized.
The embodiments of the present invention are not limited to the above-described 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 they are included in the scope of the present invention.
Claims (10)
1. A preparation method of an inorganic all-solid-state electrochromic device is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dissolving nickel acetate in ethylene glycol monomethyl ether, adding ethanolamine as a stabilizer, heating, stirring, standing and aging to obtain a precursor A;
step two: spin-coating the precursor A obtained in the first step on a cleaned glass substrate with a transparent conductive electrode, and then annealing in an air atmosphere to obtain a nickel oxide film;
step three: dissolving zirconium acetate in ethylene glycol monomethyl ether, adding ethanolamine as a stabilizer, stirring, standing and aging to obtain a precursor solution B;
step four: spin-coating the precursor solution B obtained in the third step on the nickel oxide film obtained in the second step, and then annealing in an air atmosphere to obtain a laminated structure of zirconium oxide and nickel oxide;
step five: adding the laminated structure of the zirconium oxide and the nickel oxide obtained in the step four into a KOH electrolyte, fading under the condition of an external electric field, allowing hydrogen ions to enter and be stored in the laminated structure of the zirconium oxide and the nickel oxide, taking out and drying;
step six: dissolving tungsten chloride in absolute ethyl alcohol, and centrifugally stirring to obtain a precursor solution C;
step seven: spin-coating the precursor solution C obtained in the sixth step on the laminated structure of the zirconium oxide containing the hydrogen ions and the nickel oxide obtained in the fifth step, and annealing in the air atmosphere to obtain a nickel oxide/zirconium oxide/tungsten oxide laminated structure;
step eight: and (4) spinning and coating the silver nanowires on the laminated structure obtained in the step seven, and annealing in the air atmosphere to obtain the inorganic all-solid-state electrochromic device.
2. The method for preparing the inorganic all-solid-state electrochromic device according to claim 1, wherein:
heating in the first step, wherein the heating mode is oil bath or water bath, the temperature is 60 ℃, the stirring time is 2 hours, and the aging time is 24 hours;
in the first step, the concentration of nickel in the precursor A is 0.25-0.5 mol/L.
3. The method for preparing the inorganic all-solid-state electrochromic device according to claim 2, wherein: in the second step, the glass substrate with the transparent conductive electrode is ITO glass;
and step two, spin coating, wherein the spin coating conditions are as follows: the method comprises the steps of firstly carrying out low-speed and then high-speed spinning, wherein the low-speed spinning speed is 700rpm, the high-speed spinning speed is 3000rpm, the spin-coating times are 3-5 times, the low-speed spin-coating time is 10s each time, the high-speed spin-coating time is 30-40 s, the annealing temperature between each spin-coating is 300 ℃, and the time is 3-5 min.
4. The method for preparing the inorganic all-solid-state electrochromic device according to claim 3, wherein: in the third step, the concentration of zirconium acetate in the precursor solution B is 0.3-0.6 mol/L, the stirring speed is 500rpm, and the aging time is 24 hours.
5. The method for preparing the inorganic all-solid-state electrochromic device according to claim 4, wherein: the spin coating in the fourth step is carried out under the following spin coating conditions: the rotating speed is 4000-6000 rpm, the spin coating times are 3-5 times, the time of each spin coating is 30-40 s, the annealing temperature between each spin coating is 200 ℃, the time is 3-5 min, and the subsequent annealing temperature is 200 ℃.
6. The method for preparing the inorganic all-solid-state electrochromic device according to claim 4, wherein: in the fifth step, the concentration of the KOH electrolyte is 0.1mol/L, the voltage of an external electric field is 1.5-2.5V, and the time for introducing hydrogen ions under the condition of the external electric field is 1-3 min;
and the drying in the step five is drying for 1-2 hours in a vacuum drying oven at the temperature of 70-100 ℃.
7. The method for preparing the inorganic all-solid-state electrochromic device according to claim 1, wherein: in the sixth step, the centrifugal stirring time is 1-2 h, and the rotating speed is 3000 r/min;
and sixthly, the concentration of tungsten in the precursor solution is 0.25-0.5 mol/L.
8. The method for preparing the inorganic all-solid-state electrochromic device according to claim 1, wherein:
the spin coating process conditions in the seventh step are as follows: rotating at 3000rpm, performing spin coating for 1-2 times, and performing spin coating for 30-40 s each time; then standing for 30 min; the annealing temperature is 100-200 ℃, and the annealing time is 1 h.
9. The method for preparing the inorganic all-solid-state electrochromic device according to claim 4, wherein:
and step eight, carrying out spin coating under the following spin coating conditions: firstly low speed and then high speed, the low speed rotation speed is 700rpm, the high speed rotation speed is 3000rpm, the spin coating times are 2-4 times, the time of each low speed spin coating is 10s, the time of the high speed spin coating is 30-40 s, the annealing temperature between each spin coating is 100 ℃, the time is 3-5 min,
and step eight, annealing the silver nanowires at the temperature of 100-140 ℃ for 30 min-1 h.
10. An inorganic all-solid-state electrochromic device obtained by the method for producing an inorganic all-solid-state electrochromic device according to any one of claims 1 to 9, the laminated structure of which comprises in order: the glass substrate layer, transparent conductive electrode layer, nickel oxide layer, zirconia layer, tungsten oxide layer, silver nanowire layer.
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| CN109581776A (en) * | 2019-01-02 | 2019-04-05 | 华南理工大学 | A kind of low cost electrochromic device and preparation method thereof |
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