CN111273497A - Packaging method of electro-deposition electrochromic device - Google Patents
Packaging method of electro-deposition electrochromic device Download PDFInfo
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- CN111273497A CN111273497A CN202010090340.3A CN202010090340A CN111273497A CN 111273497 A CN111273497 A CN 111273497A CN 202010090340 A CN202010090340 A CN 202010090340A CN 111273497 A CN111273497 A CN 111273497A
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- 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
- G02F1/153—Constructional details
- G02F1/161—Gaskets; Spacers; Sealing of cells; Filling or closing of cells
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- 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
- G02F1/1506—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
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Abstract
The invention discloses a packaging method of an electro-deposition electrochromic device, which is applied to the field of electrochromic materials and devices. The problem that the performance of an encapsulated electrochromic device is sharply reduced due to liquid leakage caused by the fact that the ultraviolet glue can be corroded by electrolyte when the existing encapsulated electrolyte is directly used for injecting a hole is solved; according to the invention, Polydimethylsiloxane (PDMS) serving as an insulating material is introduced into the electrolyte and the sealing material, so that a barrier effect is achieved in an electrolyte injection hole, the corrosion phenomenon caused by direct contact of the electrolyte and the sealing material is avoided, the packaging effect is improved, the service life is prolonged, and the device performance is obviously improved.
Description
Technical Field
The invention belongs to the field of electrochromic materials and devices, and particularly relates to a packaging technology of an electro-deposition electrochromic device.
Background
Electrochromism refers to a phenomenon that optical properties (reflectivity, transmittance, absorptivity and the like) of a material are changed stably and reversibly by color under the action of an external electric field or current, and a device prepared by using the electrochromism material is called an electrochromism device.
The electro-deposition type electrochromic device refers to that under the action of an external electric field or current, electrochemical oxidation-reduction reaction occurs inside the device. The packaging method directly influences the performance of the device in the preparation process of the device, the packaging material and the electrolyte are ensured not to react in the aspect of packaging material selection, and bubbles are prevented from being generated in an electrolyte layer during packaging. In the prior electro-deposition electrochromic device packaging, ultraviolet glue is directly used for sealing the injection hole, the packaging mode has poor sealing performance, and the ultraviolet glue is easily corroded by electrolyte, so that the performance of the electrochromic device is rapidly reduced.
Disclosure of Invention
In order to solve the technical problem, the invention provides a packaging method of an electrodeposition electrochromic device, wherein an isolation material-polydimethylsiloxane which does not react with an electrolyte is used in the packaging process of the electrodeposition electrochromic device, so that the direct contact between the electrolyte and a sealing material is avoided.
The technical scheme adopted by the invention is as follows: an encapsulation method of an electro-deposition electrochromic device comprises the following steps:
s1, preprocessing two conductive substrates used by a device to obtain a conductive substrate (1) and a conductive substrate (2);
s2, cutting the bonding material into a specific shape to obtain a composite bonding layer (3) and a composite bonding layer (4);
placing a conductive substrate (1), a composite bonding layer (3), a composite bonding layer (4) and a conductive substrate (2) in sequence, and bonding under certain conditions to form an electrolyte box;
s3, the electrolyte box further comprises an injection hole (5) and an injection hole (6), the prepared electrolyte is injected into the electrolyte box through the injection hole (5) and the injection hole (6), and the electrolyte injection hole (5) and the injection hole (6) are processed;
s4, preparing polydimethylsiloxane according to a certain proportion, and pretreating the prepared polydimethylsiloxane;
s5, treating the electrolyte injection hole (5) and the electrolyte injection hole (6), then injecting the polydimethylsiloxane obtained in the step S4 into the electrolyte injection hole (5) and the electrolyte injection hole (6), finishing primary sealing, and cleaning the end face of the opening;
s6, standing the device obtained in the step S5 for a period of time, sealing the injection holes (5) and (6) by using ultraviolet curing glue, and curing for a period of time under an ultraviolet lamp.
The preparation process of the box containing the electrolyte in the step S2 is as follows:
a1, cutting the adhesive material into a specific shape to obtain a composite adhesive layer (3) and a composite adhesive layer (4); placing the composite bonding layer (3) and the composite bonding layer (4) between the conductive substrate (1) and the conductive substrate (2) to form a square shape integrally, wherein the conductive surfaces of the conductive substrate (1) and the conductive substrate (2) are inward, and an electrolyte injection hole (5) and an injection hole (6) are reserved;
a2, bonding the conductive substrate (1) and the conductive substrate (2) by using the composite adhesive layer (3) and the composite adhesive layer (4) at high temperature and pressure to form the electrolyte box.
The sizes of the composite bonding layer (3) and the composite bonding layer (4) in the step A1 are matched, the composite bonding layer (3) and the composite bonding layer (4) form a square structure, injection holes (5) and injection holes (6) are reserved in the square structure, the injection holes (5) and the injection holes (6) are trapezoidal, the short bottom of the trapezoid faces inwards, and the long bottom of the trapezoid faces outwards.
The composite bonding layer (3) and the composite bonding layer (4) are of a sandwich structure formed by sequentially overlapping a bonding material, an insulating gasket and a bonding material.
And A2, keeping the temperature at 100-50 ℃ for 5-120 minutes, and applying 2000-3000 Pa pressure to a box containing the electrolyte.
The electrolyte in step S3 includes two systems:
the first system is prepared by the following steps: dissolving 0.3-2 mmol of silver nitrate, 0.1-2 mmol of copper chloride and 0.5-4 mmol of tetrabutylammonium bromide in 1.0-4 g of polyvinyl butyral and 10-20 g of dimethyl sulfoxide, and stirring at room temperature for 0.5-3 hours to obtain a first mixed solution; dissolving 0.3-2 mmol of silver nitrate and 0.1-2 mmol of copper chloride in 5-20 wt% of dimethyl sulfoxide and 20-65mmol of 1-butyl-3 ethyl imidazole bromide, stirring at room temperature for 0.5-2 h to obtain a second mixed solution, and mixing the first mixed solution and the second mixed solution to prepare an electrolyte;
the second electrolyte system is prepared by the following steps: dissolving 0.3-2 mmol of silver nitrate, 0.1-2 mmol of copper chloride and 0.5-4 mmol of tetrabutylammonium bromide in 1.0-4 g of polyvinyl butyral and 10-20 g of dimethyl sulfoxide, and stirring at room temperature for 0.5-3 hours to obtain a first mixed solution; dissolving 0.3-2 mmol of silver nitrate and 0.1-2 mmol of copper chloride in 5-20 wt% of dimethyl sulfoxide, stirring at room temperature for 0.5-2 h to obtain a second mixed solution, and mixing the first mixed solution and the second mixed solution to prepare an electrolyte.
And step S4, mixing the polydimethylsiloxane serving as the main agent and the curing agent according to the mass ratio of 20: 1-5: 1, stirring at the speed of 100-500 r/min, and stirring for 5-20 minutes. The pretreatment comprises the following steps: and (3) placing the prepared polydimethylsiloxane in a vacuum environment with the pressure less than 5Pa for 10-40 minutes, and then keeping the polydimethylsiloxane in an environment with the temperature of 50-70 ℃ for 1-20 minutes.
The process of the injection hole (5) and the injection hole (6) described in step S5 is:
cleaning the inside and outside of the injection holes (5) and (6) by using filter paper, absolute ethyl alcohol and dust-free cloth, and having no residual electrolyte;
defining the angle formed by the long bottom and the inclined waist of the trapezoid as α, and slowly injecting polydimethylsiloxane from the side of the injection hole (5) and the injection hole (6) close to the angle α while sealing the injection hole (5) and the injection hole (6);
after finishing the preliminary sealing, the end face of the opening is wiped and cleaned by using absolute ethyl alcohol and dust-free cloth.
Step S6, the device obtained in the step S5 is kept still for 1-24 hours; coating ultraviolet curing glue on the peripheries of the injection holes (5) and (6) for curing for 2-10 minutes, taking out the device and standing for 5-10 minutes, and repeating the standing process after coating the ultraviolet glue and coating the ultraviolet glue for 1-3 times.
Step S2, one of the conductive substrate (1) and the conductive substrate (2) has an island-shaped nanoparticle rough layer, and the side of the conductive substrate having the island-shaped nanoparticle rough layer faces the electrolyte box.
The invention has the beneficial effects that: an insulating material which does not react with the electrolyte, namely polydimethylsiloxane, is used in an injection hole to play a role in blocking in the organic electrolyte packaging process of the electro-deposition electrochromic device. The packaging mode provided by the invention avoids the direct contact of the electrolyte and the sealing material, thereby avoiding the corrosion of the electrolyte to the sealing material, greatly improving the packaging effect, obviously improving the performance of the device and prolonging the service life.
Drawings
Fig. 1 is a plan view of the device package of the present invention.
Description of reference numerals: 1 and 2 are the treated ITO conductive glass; 3 and 4 an adhesive layer comprising a sarin film and an insulating spacer; 5 and 6 are electrolyte injection holes; 7 is an electrolyte cartridge; and 8 is the opening diameter.
Detailed Description
In order to facilitate the understanding of the technical contents of the present invention by those skilled in the art, the present invention will be further explained with reference to the accompanying drawings.
As shown in fig. 1, the device package plane structure of the present invention has the following technical solutions: a packaging method of an electrodeposition type electrochromic device protected by an insulating material comprises the following steps:
s1, preprocessing a device by using a substrate; in the step S1, the common substrate of the device is commercial ITO transparent conductive glass, the thickness of the ITO film is 160-240nm, and the sheet resistance is 5-10 Ω/cm2. Pretreatment of the substrate for the device includes ultrasonic cleaning in acetone, ethanol and deionized water, or pretreatment of the substrate using other methods as mentioned by way of example.
S2, cutting the heat-sealing material, namely the Shalin film and the insulating gasket, into a specific shape, and placing the special shape at a proper position to bond the substrates 1 and 2 to form a box for containing the electrolyte.
S3, injecting a proper amount of prepared electrolyte into the electrolyte box to enable the liquid level to reach the position of the diameter 8 of the opening;
s4, preparing polydimethylsiloxane from the main agent and the curing agent according to a certain ratio, and removing bubbles and drying the prepared polydimethylsiloxane for a period of time;
s5, cleaning the residual electrolyte in the electrolyte injection holes 5 and 6, then injecting polydimethylsiloxane into the holes 5 and 6, and cleaning the residual polydimethylsiloxane on the end faces of the holes;
s6, standing for a period of time, sealing the injection holes 5 and 6 by using ultraviolet curing glue, and curing for a period of time under an ultraviolet lamp
Example one:
this example introduces a method of packaging a bistable electrochromic device, comprising the steps of:
s1, preprocessing a device by using substrates 1 and 2: placing the ITO transparent conductive glass in acetone, ethanol and ultrapure water in sequence, and ultrasonically cleaning for 5 minutes to remove dust and grease on the surface of the ITO transparent conductive glass; treating for 5 minutes in an environment with power of 8W by using a plasma cleaning machine; the substrate 1 was immersed in (3-Mercaptopropyl) trimethoxysilane (3-Mercaptopropyl) methylidynesilane (MPTMS) for 2 hours at room temperature, and then washed with ethanol to remove impurities, and placed in an oven to be dried. By radio frequency magnetron sputtering, a tungsten target (the diameter is 100mm, the purity is 99.999 percent) and a silver sheet (the diameter is 5mm multiplied by 8mm, the purity is 99.999 percent) are used for forming W, Ag and O mixed nano islands which are uniformly distributed and have the diameter of about 280nm on the surface of the substrate 2; and (3) placing the substrate 6 in dilute nitric acid with the mass concentration of 1.6M for 45s, washing and soaking the substrate for 100s by using deionized water, and blowing away the deionized water by using a high-purity nitrogen gun to obtain the island-shaped rough nano particle layer with the final diameter of about 185 nm.
S2, cutting the heat-sealing material, namely the Shalin film and the insulating gasket, into a specific shape, placing the specific shape at a proper position, and bonding the substrates 1 and 2 to form a box for containing the electrolyte. The method specifically comprises the following steps:
firstly, two films of bonding material sarin and one insulating gasket are cut, and the shapes of the composite bonding layer (3) and the composite bonding layer (4) are formed. The material of the composite adhesive layer (3) and the composite adhesive layer (4) is a heat sealing film including but not limited to a sarin film, and the insulating gasket includes but not limited to a polyethylene terephthalate (PET) insulating film. The number of the sand forest mold layers is 1-4, and the number of the corresponding insulating gasket layers is 0-3.
The composite adhesive layers (3) and (4) are specifically: the cut material is in a sandwich structure of 'Shalin film/insulating gasket/Shalin film'.
The shape of the composite bonding layer (3) is similar to a concave shape, the difference is that two opposite bonding edges of the composite bonding layer (3) are in a right trapezoid-like shape, the short bottom edges of the two trapezoid-shaped bonding edges are positioned in the concave shape, the angle formed by the long bottom edge and the oblique waist is α and ranges from 90 degrees to 45 degrees, the composite bonding layer (4) is in an isosceles trapezoid shape, the angle formed between the long bottom edge and the waist edge of the trapezoid is β and ranges from 90 degrees to 30 degrees, the sealing effect of a finished product is poor due to the fact that the angles are α and β are too small, the sealing effect of injection holes (5) and (6) is poor due to too large angle, the sizes of the composite bonding layers (3) and (4) are matched with the substrates (1) and (2), the composite bonding layer is in a shape of a square after being placed, the long bottom edges of the composite bonding layer (4) are positioned in the square shape of the square, the shapes of the reserved holes (5) and the trapezoid (6) after being placed in the composite bonding layer (3) and (4) are in a shape of a trapezoid, and.
Placing composite bonding layers (3) and (4) on the rough surface of the substrate 2 to form a semi-closed space shaped like a Chinese character 'kou', and reserving injection holes (5) and (6) with the opening diameter of 2 mm; the substrate 1 is pressed onto the substrate 2 with the composite adhesive layer placed, with the two substrate conductive surfaces facing each other, leaving an electrode of about 1cm on one side edge at the same time.
The thickness of the film of the sarin used for packaging is 60 mu m, the thickness of the insulating gasket is 100 mu m, and the conductive surfaces of the two layers of ITO transparent conductive glass face to one side of the electrolyte layer in the packaging process. The sealed electrolyte containing box is heated on a constant temperature heating table at a constant temperature of 120 ℃ for 60 minutes, and a pressure of 2500 Pa is applied to ensure tight adhesion, and the space height of the electrolyte containing box obtained after the treatment is about 150 mu m.
S3, injecting a proper amount of prepared electrolyte into the electrolyte box to enable the liquid level to reach the position with the diameter of the opening being 8, repeatedly cleaning the electrolyte injection holes 5 and 6 by using absolute ethyl alcohol, filter paper and dust-free cloth, and cleaning the residual electrolyte;
the electrolyte formulation procedure used in this example was: : dissolving 0.5mmol of silver nitrate, 0.1mmol of copper chloride, 2.5mmol of tetrabutylammonium bromide and 136mg of polyvinyl butyral in 10ml of dimethyl sulfoxide, and stirring at room temperature for 2 hours; 10mL of 1-butyl-3-ethylimidazole bromide was added to the mixture, and the mixture was stirred at room temperature for 1 hour to prepare an electrolyte solution. The prepared electrolyte was injected through the electrolyte injection hole 5 by a syringe, and the injection was completed when the electrolyte surface reached the opening 8 of the injection hole 6.
S4, preparing polydimethylsiloxane from the main agent and the curing agent according to the mass ratio of 10:1, and then stirring for 10 minutes at the rotating speed of 200r/min in magnetic stirring; the reaction solution was kept in an atmosphere of 5Pa for 30 minutes, and then kept in a drying oven at 60 ℃ for 8 minutes. The insulation material Polydimethylsiloxane (PDMS) is commercially available as dow corning SYLGARD 184.
S5, injecting polydimethylsiloxane into the holes 5 and 6, wiping the end faces of the holes with absolute ethyl alcohol and dust-free cloth, and removing the residual polydimethylsiloxane on the end faces;
s6, standing in the air for 5 hours, and coating the ultraviolet curing glue on the outer parts of the injection holes 5 and 6. Irradiating under ultraviolet lamp for 3 min, taking out, standing for 5 min, and repeating the process for 3 times. The sealing material used was a UV curable adhesive sold under the LOCTITE brand name, model AA 352.
Example two:
this example introduces a method for packaging a tristate electrochromic device, comprising the steps of:
s1, preprocessing a device by using substrates 1 and 2: placing the ITO transparent conductive glass in acetone, ethanol and ultrapure water in sequence, and ultrasonically cleaning for 5 minutes to remove dust and grease on the surface of the ITO transparent conductive glass; treating for 5 minutes in an environment with power of 8W by using a plasma cleaning machine; the substrate 1 was immersed in (3-Mercaptopropyl) trimethoxysilane (3-Mercaptopropyl) methylidynesilane (MPTMS) for 2 hours at room temperature, and then washed with ethanol to remove impurities, and placed in an oven to be dried. By radio frequency magnetron sputtering, a tungsten target (the diameter is 100mm, the purity is 99.999 percent) and a silver sheet (the diameter is 5mm multiplied by 8mm, the purity is 99.999 percent) are used for forming W, Ag and O mixed nano islands which are uniformly distributed and have the diameter of about 280nm on the surface of the substrate 2; and (3) placing the substrate 6 in dilute nitric acid with the mass concentration of 1.6M for 45s, washing and soaking the substrate for 100s by using deionized water, and blowing away the deionized water by using a high-purity nitrogen gun to obtain the island-shaped rough nano particle layer with the final diameter of about 185 nm.
S2, cutting the heat-sealing material, namely the Shalin film and the insulating gasket, into a specific shape, and placing the special shape at a proper position to bond the substrates 1 and 2 to form a box for containing the electrolyte. The method specifically comprises the following steps:
firstly, two films of bonding material sarin are cut, and the shapes of the composite bonding layer (3) and the composite bonding layer (4) are formed. And (3) combining the cut and formed materials into composite adhesive layers (3) and (4) according to a structure of a 'Shalin film/Shalin film' type. Placing composite bonding layers (3) and (4) on the rough surface of the substrate 2 to form a semi-closed space shaped like a Chinese character 'kou', and reserving injection holes (5) and (6) with the opening diameter of 2 mm; the substrate 1 is pressed onto the substrate 2 with the composite adhesive layer placed, with the two substrate conductive surfaces facing each other, leaving an electrode of about 1cm on one side edge at the same time.
The thickness of the film of the obtained sarin for packaging is 60 mu m, and the conductive surfaces of the two layers of ITO transparent conductive glass face to one side of the electrolyte layer in the packaging process. The sealed electrolyte containing box is heated on a constant temperature heating table at a constant temperature of 120 ℃ for 60 minutes, and a pressure of 2500 Pa is applied to ensure tight adhesion, and the space height of the electrolyte containing box obtained after the treatment is about 60 mu m.
S3, injecting a proper amount of prepared electrolyte into the electrolyte box to enable the liquid level to reach the position with the diameter of the opening being 8, repeatedly cleaning the electrolyte injection holes 5 and 6 by using absolute ethyl alcohol, filter paper and dust-free cloth, and cleaning the residual electrolyte;
the electrolyte formulation procedure used in this example was: dissolving 0.5mmol of silver nitrate, 0.1mmol of copper chloride, 2.5mmol of tetrabutylammonium bromide and 136mg of polyvinyl butyral in 10ml of dimethyl sulfoxide, and stirring at room temperature for 2 hours;
s4, preparing polydimethylsiloxane from the main agent and the curing agent according to the mass ratio of 10:1, and then stirring for 10 minutes at the rotating speed of 200r/min in magnetic stirring; the reaction solution was kept in an atmosphere of 5Pa for 30 minutes, and then kept in a drying oven at 60 ℃ for 8 minutes. The insulation material Polydimethylsiloxane (PDMS) is commercially available as dow corning SYLGARD 184.
S5, injecting polydimethylsiloxane into the holes 5 and 6, wiping the end faces of the holes with absolute ethyl alcohol and dust-free cloth, and removing the residual polydimethylsiloxane on the end faces;
s6, standing in the air for 1 hour, and coating the ultraviolet curing glue outside the injection holes 5 and 6. Irradiating under ultraviolet lamp for 3 min, taking out, standing for 5 min, and repeating the process for 3 times. The sealing material used was a UV curable adhesive sold under the LOCTITE brand name, model AA 352.
In the invention, the sealing performance of the device is poor due to the overlarge diameter 8 of the opening, and the time consumed for packaging is prolonged; the too small diameter of the drilled hole reduces the injection efficiency of the electrolyte. The opening diameter 8 in this embodiment is 2-10mm in size.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. An encapsulation method of an electro-deposition electrochromic device is characterized by comprising the following steps:
s1, preprocessing two conductive substrates used by a device to obtain a conductive substrate (1) and a conductive substrate (2);
s2, cutting the bonding material into a specific shape to obtain a composite bonding layer (3) and a composite bonding layer (4);
placing a conductive substrate (1), a composite bonding layer (3), a composite bonding layer (4) and a conductive substrate (2) in sequence, and bonding under certain conditions to form an electrolyte box;
s3, the electrolyte box further comprises an injection hole (5) and an injection hole (6), the prepared electrolyte is injected into the electrolyte box through the injection hole (5) and the injection hole (6), and the electrolyte injection hole (5) and the injection hole (6) are processed;
s4, preparing polydimethylsiloxane according to a certain proportion, and pretreating the prepared polydimethylsiloxane;
s5, treating the electrolyte injection hole (5) and the electrolyte injection hole (6), then injecting the polydimethylsiloxane obtained in the step S4 into the electrolyte injection hole (5) and the electrolyte injection hole (6), finishing primary sealing, and cleaning the end face of the opening;
s6, standing the device obtained in the step S5 for a period of time, sealing the injection holes (5) and (6) by using ultraviolet curing glue, and curing for a period of time under an ultraviolet lamp.
2. The method for encapsulating an electrodeposition electrochromic device according to claim 1, wherein the case containing the electrolyte solution of step S2 is prepared by:
a1, cutting the adhesive material into a specific shape to obtain a composite adhesive layer (3) and a composite adhesive layer (4); placing the composite bonding layer (3) and the composite bonding layer (4) between the conductive substrate (1) and the conductive substrate (2) to form a square shape integrally, wherein the conductive surfaces of the conductive substrate (1) and the conductive substrate (2) are inward, and an electrolyte injection hole (5) and an injection hole (6) are reserved;
a2, bonding the conductive substrate (1) and the conductive substrate (2) by using the composite adhesive layer (3) and the composite adhesive layer (4) at high temperature and pressure to form the electrolyte box.
3. The packaging method of the electrodeposition electrochromic device according to claim 2, wherein the size of the composite adhesive layer (3) and the size of the composite adhesive layer (4) in the step a1 are matched, the composite adhesive layer (3) and the composite adhesive layer (4) form a square structure, an injection hole (5) and an injection hole (6) are reserved on the square structure, the injection hole (5) and the injection hole (6) are trapezoidal, the short bottom of the trapezoid faces inwards, and the long bottom of the trapezoid faces outwards.
4. The method for encapsulating the electro-deposition electrochromic device according to claim 3, wherein the composite adhesive layer (3) and the composite adhesive layer (4) are of a sandwich structure formed by sequentially overlapping an adhesive material, an insulating gasket and an adhesive material.
5. The method for encapsulating an electrodeposited electrochromic device according to claim 4, wherein the high temperature of step A2 is 100-50 ℃, the constant temperature time is 5-120 minutes, and the pressure of 2000-3000 Pa is applied to a box containing the electrolyte.
6. The method for encapsulating an electrodeposited electrochromic device according to claim 5, wherein the electrolyte solution in the step S3 comprises two systems:
the first system is prepared by the following steps: dissolving 0.3-2 mmol of silver nitrate, 0.1-2 mmol of copper chloride and 0.5-4 mmol of tetrabutylammonium bromide in 1.0-4 g of polyvinyl butyral and 10-20 g of dimethyl sulfoxide, and stirring at room temperature for 0.5-3 hours to obtain a first mixed solution; dissolving 0.3-2 mmol of silver nitrate and 0.1-2 mmol of copper chloride in 5-20 wt% of dimethyl sulfoxide and 20-65mmol of 1-butyl-3 ethyl imidazole bromide, stirring at room temperature for 0.5-2 h to obtain a second mixed solution, and mixing the first mixed solution and the second mixed solution to prepare an electrolyte;
the second electrolyte system is prepared by the following steps: dissolving 0.3-2 mmol of silver nitrate, 0.1-2 mmol of copper chloride and 0.5-4 mmol of tetrabutylammonium bromide in 1.0-4 g of polyvinyl butyral and 10-20 g of dimethyl sulfoxide, and stirring at room temperature for 0.5-3 hours to obtain a first mixed solution; dissolving 0.3-2 mmol of silver nitrate and 0.1-2 mmol of copper chloride in 5-20 wt% of dimethyl sulfoxide, stirring at room temperature for 0.5-2 h to obtain a second mixed solution, and mixing the first mixed solution and the second mixed solution to prepare an electrolyte.
7. The method for packaging an electrodeposition electrochromic device as in claim 1, wherein the polydimethylsiloxane serving as the main agent and the curing agent in the step S4 are mixed at a mass ratio of 20:1 to 5:1, a stirring speed of 100 to 500r/min, and a stirring time of 5 to 20 minutes. The pretreatment comprises the following steps: and (3) placing the prepared polydimethylsiloxane in a vacuum environment with the pressure less than 5Pa for 10-40 minutes, and then keeping the polydimethylsiloxane in an environment with the temperature of 50-70 ℃ for 1-20 minutes.
8. The method for encapsulating an electrodeposition electrochromic device according to claim 1, wherein the treatment of the injection hole (5) and the injection hole (6) in step S5 is:
cleaning the inside and outside of the injection holes (5) and (6) by using filter paper, absolute ethyl alcohol and dust-free cloth, and having no residual electrolyte;
defining the angle formed by the long bottom and the inclined waist of the trapezoid as α, and slowly injecting polydimethylsiloxane from the side of the injection hole (5) and the injection hole (6) close to the angle α while sealing the injection hole (5) and the injection hole (6);
after finishing the preliminary sealing, the end face of the opening is wiped and cleaned by using absolute ethyl alcohol and dust-free cloth.
9. The method for encapsulating an electrodeposition electrochromic device according to claim 1, wherein the device obtained in S5 is left for 1 to 24 hours in step S6; coating ultraviolet curing glue on the peripheries of the injection holes (5) and (6) for curing for 2-10 minutes, taking out the device and standing for 5-10 minutes, and repeating the standing process after coating the ultraviolet glue and coating the ultraviolet glue for 1-3 times.
10. The packaging method of an electrodeposited electrochromic device according to claim 1, wherein one of the conductive substrate (1) and the conductive substrate (2) is provided with the island-shaped nanoparticle rough layer in step S2, and the side of the conductive substrate provided with the island-shaped nanoparticle rough layer faces the electrolyte box.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010090340.3A CN111273497A (en) | 2020-02-13 | 2020-02-13 | Packaging method of electro-deposition electrochromic device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010090340.3A CN111273497A (en) | 2020-02-13 | 2020-02-13 | Packaging method of electro-deposition electrochromic device |
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