CN111505880B - Thermally responsive electrolyte material and preparation method and application thereof - Google Patents
Thermally responsive electrolyte material and preparation method and application thereof Download PDFInfo
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- CN111505880B CN111505880B CN202010446160.4A CN202010446160A CN111505880B CN 111505880 B CN111505880 B CN 111505880B CN 202010446160 A CN202010446160 A CN 202010446160A CN 111505880 B CN111505880 B CN 111505880B
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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
- G02F1/1514—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 characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—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 characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
- G02F1/1525—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 characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material characterised by a particular ion transporting layer, e.g. electrolyte
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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
- G02F1/163—Operation of electrochromic cells, e.g. electrodeposition cells; Circuit arrangements therefor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a thermally responsive electrolyte material, a preparation method and application thereof, (1) a thermally responsive pigment and filler is prepared: putting the pigment into a solvent, adding a coupling agent for ultrasonic treatment to modify or coat the surface of the pigment, centrifugally drying, dispersing into the solvent, adding a thermal response material in an ultrasonic state, and finally centrifugally drying to obtain the thermal response pigment; (2) preparing a thermally responsive electrolyte material: mixing an organic polymer, a plasticizer, a solvent, lithium salt and the like, and then adding the thermally responsive pigment obtained in the step (1) into the mixture to prepare a thermally responsive electrolyte material; the color of the electrochromic device is controlled by the thermally responsive electrolyte. The invention changes the state of the thermal response phase change material under different temperature conditions, so that the electrolyte shows different color changes, and further the electrochromic device shows different colors.
Description
Technical Field
The invention relates to an electrolyte material and a preparation method and application thereof, in particular to a thermally responsive electrolyte material and a preparation method and application thereof, belonging to the field of electronic materials.
Background
Electrochromic is a phenomenon in which optical properties (reflectance, transmittance, absorptivity, etc.) of a material change in color stably and reversibly under the action of an applied electric field, and is expressed as a reversible change in color, transparency, etc. in appearance. Materials having electrochromic properties are referred to as electrochromic materials, and devices made from electrochromic materials are referred to as electrochromic devices.
The electrochromic intelligent glass has light absorption and transmission adjustability under the action of an electric field, can selectively absorb or reflect external heat radiation and internal heat diffusion, reduces a large amount of energy which is required to be consumed when an office building and a residential building keep cool in summer and warm in winter, plays roles in improving natural illumination degree and peeping prevention, solves the problem of urban light pollution which is continuously deteriorated in modern times, and is a development direction of energy-saving building materials; the electrochromic material has bistable property, and the electrochromic display device made of the electrochromic material does not need a backlight, and after displaying a static image, the display content is unchanged, so that power is not consumed, the energy-saving effect is obvious, and the device has the advantages of no blind angle, high contrast ratio and the like; the automatic anti-glare rearview mirror prepared by the electrochromic material can adjust the intensity of reflected light according to the intensity of external light through an electronic induction system, so as to achieve the anti-glare effect and ensure safer driving; electrochromic devices are absorption-type devices and have infrared-change emissivity properties, and can be used as intelligent optical camouflage or temperature regulation materials in military and aerospace fields.
In electrochromic devices, the electrolyte provides a channel for ion transport in electrochromic, and the performance and state of the electrolyte have a greater impact on the color changing performance and color state of the device. The invention provides a preparation method of an electrolyte with thermal response characteristics, and the electrolyte can be used for regulating and controlling the color of an electrochromic device.
Disclosure of Invention
The invention aims to provide a thermally responsive electrolyte material capable of realizing switching regulation and control of various colors, and a preparation method and application thereof.
The purpose of the invention is realized in the following way:
a thermally responsive electrolyte material is prepared by the following steps:
(1) Preparing a thermally responsive pigment filler: and (3) placing the pigment into a solvent, adding a coupling agent for ultrasonic treatment to modify or coat the surface of the pigment, centrifugally drying, dispersing into the solvent, adding a thermal response material in an ultrasonic state, and finally centrifugally drying to obtain the thermal response pigment.
(2) Preparing a thermally responsive electrolyte material: mixing an organic polymer, a plasticizer, a solvent, a lithium salt, and the like, and then adding the thermally responsive pigment obtained in the step (1) to the above-mentioned mixed species to prepare a thermally responsive electrolyte material.
The pigment is one or more of chromate, sulfate, azo pigment, phthalocyanine pigment, anthraquinone, indigo group, quinacridone, dioxazine and arylmethane pigment; the coupling agent is one or more of organic chromium complex, silane, titanate, aluminate compound and the like; the thermal response material is one or more of polyacrylic acid-b-poly N-isopropyl acrylamide, polymethacrylic acid-b-poly N-isopropyl acrylamide, polymethyl allyl alcohol-b-poly N-isopropyl acrylamide triarylmethane phthalides, fluoran and triphenylmethane; the organic polymer is one or more of polyethylene glycol, polymethyl methacrylate, polymethyl acrylate, polybutyl methacrylate and polyacrylonitrile;
a method of preparing a thermally responsive electrolyte material comprising the steps of:
(1) Preparing a thermally responsive pigment filler: and (3) placing the pigment into a solvent, adding a coupling agent for ultrasonic treatment to modify or coat the surface of the pigment, centrifugally drying, dispersing into the solvent, adding a thermal response material in an ultrasonic state, and finally centrifugally drying to obtain the thermal response pigment.
(2) Preparing a thermally responsive electrolyte material: mixing an organic polymer, a plasticizer, a solvent, a lithium salt, and the like, and then adding the thermally responsive pigment obtained in the step (1) to the above-mentioned mixed species to prepare a thermally responsive electrolyte material.
The pigment is one or more of chromate, sulfate, azo pigment, phthalocyanine pigment, anthraquinone, indigo group, quinacridone, dioxazine and arylmethane pigment;
the coupling agent is one or more of organic chromium complex, silane, titanate, aluminate compound and the like;
the thermal response material is one or more of polyacrylic acid-b-poly N-isopropyl acrylamide, polymethacrylic acid-b-poly N-isopropyl acrylamide, polymethyl allyl alcohol-b-poly N-isopropyl acrylamide triarylmethane phthalides, fluoran and triphenylmethane;
the organic polymer is one or more of polyethylene glycol, polymethyl methacrylate, polymethyl acrylate, polybutyl methacrylate and polyacrylonitrile;
a method for color modulation in a electrochromic device responsive to a color-changing electrolyte material, comprising the steps of:
firstly, spraying an electrochromic material polythiophene onto a first conductive layer ITO glass;
secondly, scraping the prepared thermally responsive electrolyte material on the surface of the color-changing thiophene layer;
thirdly, spraying polypyrrole as an ion storage layer on the surface of ITO glass of the second conductive layer; and finally, attaching the ITO glass coated with the electrolyte and the color-changing layer with the ITO glass coated with the polypyrrole to prepare the electrochromic device.
Fourth, the voltage regulating device changes color, and simultaneously, the temperature regulating thermal response color changing electrolyte is controlled to realize the regulation of different colors.
The regulation voltage range is-5V; the temperature regulation and control range is 15-80 ℃; the color-changing layer and the ion storage layer can be one or more of polyaniline and derivatives thereof, polythiophene and derivatives thereof, transition metal oxide and polypyrrole respectively; the color change range is one or more of red color system, yellow color system, green color system and blue color system.
Compared with the prior art, the invention has the beneficial effects that:
the electrolyte material is simple to prepare, the color regulation and control in the color-changing device are simple, the switching regulation and control of various colors can be realized, and the electrolyte material has very important civil and military values;
the invention changes the state of the thermal response phase change material under different temperature conditions, so that the electrolyte shows different color changes, and further the electrochromic device shows different colors.
Detailed Description
The invention is described in more detail below by way of example, with reference to embodiments and specific operating procedures:
the preparation of a response color-changing electrolyte material and the application technology of the response color-changing electrolyte material in electrochromic are as follows:
(1) Preparation of thermally responsive pigment and filler
And (3) placing the pigment into a solvent, adding a coupling agent for ultrasonic treatment to modify or coat the surface of the pigment, centrifugally drying, dispersing into the solvent, adding a thermal response material in an ultrasonic state, and finally centrifugally drying to obtain the thermal response pigment.
(2) Preparation of thermally responsive electrolyte material
The thermally responsive electrolyte material is prepared by mixing an organic polymer, a plasticizer, a solvent, a lithium salt, etc., and then adding the thermally responsive pigment obtained in (1) to the above-mentioned mixed species.
(3) Preparation of multi-color electrochromic device
The multi-color electrochromic device comprises a first conductive layer, a color-changing layer, a thermally-responsive electrolyte, an ion storage layer and a second conductive layer, wherein the voltage regulating device changes color, and simultaneously, the temperature is controlled to regulate the thermally-responsive color-changing electrolyte to realize regulation of different colors.
The pigment in the step (1) can be one or more of inorganic pigments or organic pigments such as chromates, sulfates, azo pigments, phthalocyanine pigments, anthraquinone, indigo, quinacridone, dioxazine, arylmethane pigments and the like;
the coupling agent in the step (1) can be one or more of organic chromium complexes, silanes, titanates, aluminate compounds and the like;
the thermal response material in the step (1) may be one or more of high molecular polymers (polyacrylic acid-b-poly-N-isopropyl acrylamide, polymethacrylic acid-b-poly-N-isopropyl acrylamide, polymethylallyl alcohol-b-poly-N-isopropyl acrylamide), thermochromic dyes (triarylmethane phthalides, fluorans, triphenylmethane compounds, etc.);
the plasticizer in the step (1) comprises one or more of phthalate, aliphatic dibasic acid ester, fatty acid ester, benzene polyacid ester, polyol ester, epoxy hydrocarbon, alkyl sulfonate and the like;
the organic polymer in the step (2) comprises one or more of polyethylene glycol, polymethyl methacrylate, polymethyl acrylate, polybutyl methacrylate, polyacrylonitrile and the like;
the solvent in the step (2) comprises one or more of acetonitrile, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and the like;
the lithium salt in the step (2) comprises one or more of lithium perchlorate (LiClO 4), lithium hexafluorophosphate (LiPF 6), lithium tetrafluoroborate (LiBF 4) and the like;
thermally responsive electric as described in step (2)Ionic conductivity range of electrolyte material 10 -2 ～10 -5 S/cm；
The first conductive layer and the second conductive layer in the step (3) may be one or more of indium tin oxide conductive material, aluminum foil, copper foil, nano metal wire conductive material, etc., respectively;
the regulation voltage range in the step (3) is-5V;
the color-changing layer and the ion storage layer in the step (3) can be one or more of polyaniline and derivatives thereof, polythiophene and derivatives thereof, transition metal oxide, polypyrrole and the like respectively;
the temperature regulation and control range of the step (3) is 15-80 ℃;
and (3) one or more of red, yellow, green and blue color in the color change range.
Example 1
Step one: putting 5g of chrome yellow pigment into 100ml of toluene, adding a silane coupling agent 5gKH for ultrasonic treatment for 30min, modifying the chrome yellow surface, centrifuging, drying the precipitate, dispersing the precipitate into xylene, adding a thermally responsive material polyacrylic acid-b-poly N-isopropyl acrylamide under the ultrasonic condition, centrifuging after ultrasonic treatment for 10min, and drying to obtain the thermally responsive pigment.
Step two: and 5g of polymethyl methacrylate, 5ml of plasticizer phthalate, 10ml of acetonitrile, 20g of lithium perchlorate and the like are stirred and mixed uniformly, and then the thermally responsive pigment obtained in the step one is added into the mixture to prepare the thermally responsive electrolyte material.
Step three: firstly, spraying an electrochromic material polythiophene onto a first conductive layer ITO glass; secondly, scraping the thermally responsive electrolyte material prepared in the second step on the surface of the color-changing thiophene layer; thirdly, spraying polypyrrole as an ion storage layer on the surface of ITO glass of the second conductive layer; and finally, attaching the ITO glass coated with the electrolyte and the color-changing layer with the ITO glass coated with the polypyrrole to prepare the electrochromic device.
Step four: adding the electrochromic device prepared in the step three into a 2V voltage device at 25 ℃ to change the blue color into light yellow, increasing the ambient temperature to 40 ℃, changing the device into dark yellow, and changing the device into blue when the voltage is changed into-1V.
Example 2
Step one: 3g of chrome green pigment is put into 100ml of tetrahydrofuran, then silane coupling agent 5gKH is added for ultrasound for 30min, the chrome yellow surface is modified, then centrifugation is carried out, the precipitate is dried and then dispersed into dimethylbenzene, and a thermochromic material triphenylmethane is added under the ultrasound condition, centrifugation is carried out after ultrasound for 30min, and drying is carried out, thus obtaining the thermal response pigment.
Step two: and 5g of polyacrylonitrile, 3ml of plasticizer phthalate, 3ml of acetonitrile, 15g of lithium hexafluorophosphate and the like are stirred and mixed uniformly, and then the thermally responsive pigment obtained in the step one is added into the mixture to prepare the thermally responsive electrolyte material.
Step three: firstly, spraying an electrochromic material yellow polythiophene derivative onto a first conductive layer nano silver wire film; secondly, scraping the thermally responsive electrolyte material prepared in the second step on the surface of the yellow polythiophene derivative coating; thirdly, coating the nano nickel oxide of the ion storage layer on the surface of the aluminum foil of the second conductive layer; and finally, attaching the nano silver wire film coated with the electrolyte and the color-changing layer and the aluminum foil coated with the nano nickel oxide to prepare the electrochromic device.
Step four: and (3) adding the electrochromic device prepared in the step (III) into a 3V voltage device at 25 ℃ to change yellow into dark green, increasing the ambient temperature to 50 ℃, changing the device into light green, and changing the device into dark yellow when the voltage is changed to-1.5V.
Example 3
Step one: 5g of phthalocyanine blue pigment is put into 100ml of tetrahydrofuran, then 5g of titanate linking agent is added for ultrasonic treatment for 30min, the surface of phthalocyanine blue is modified, then centrifugation is carried out, the precipitate is dried and then dispersed into dimethylbenzene, the thermochromic material fluoran is added under the ultrasonic condition, and after ultrasonic treatment for 30min, centrifugation and drying are carried out, thus obtaining the thermal response pigment.
Step two: and (3) stirring and mixing 4g of polyacrylonitrile, 5ml of plasticizer aliphatic dibasic acid ester, 2ml of acetonitrile, 15g of lithium tetrafluoroborate and the like, and adding the thermally responsive pigment obtained in the step (I) into the mixture after uniformly mixing to prepare the thermally responsive electrolyte material.
Step three: firstly, spraying an electrochromic material blue polythiophene derivative onto a first conductive layer nano silver wire film; secondly, scraping the thermally responsive electrolyte material prepared in the second step onto the surface of the blue polythiophene derivative coating; thirdly, coating the nano nickel oxide of the ion storage layer on the surface of the aluminum foil of the second conductive layer; and finally, attaching the nano silver wire film coated with the electrolyte and the color-changing layer and the aluminum foil coated with the nano nickel oxide to prepare the electrochromic device.
Step four: adding the electrochromic device prepared in the step three into a 3V voltage device at 25 ℃ to change yellow into emerald, increasing the ambient temperature to 50 ℃, changing the device into blue, and changing the device into dark yellow when the voltage is changed to-1.5V.
The above examples merely represent basic embodiments of the invention, which are described in more detail and are not to be construed as limiting the scope of the claims. It should be noted that, for those skilled in the art, several technical variations and modifications can be made without departing from the method of the present principles, which falls within the protection scope of the present patent application.
To sum up: the invention provides a preparation method of a response color-changing electrolyte material and a color regulating method in an electrochromic device, which are characterized in that the color of the electrochromic device is regulated and controlled by a thermal response electrolyte. The main components of the thermal response color matching electrolyte comprise a thermal response phase change material, pigment and filler, an organic polymer, an organic solvent, acid or lithium salt and the like, and the state of the thermal response phase change material is changed under different temperature conditions, so that the electrolyte shows different color changes, and further the electrochromic device shows different colors.
Claims (9)
1. The thermally responsive electrolyte material is characterized by comprising the following steps:
(1) Preparing a thermally responsive pigment: putting the pigment into a solvent, adding a coupling agent for ultrasonic treatment to modify or coat the surface of the pigment, centrifugally drying, dispersing into the solvent, adding a thermal response material in an ultrasonic state, and finally centrifugally drying to obtain the thermal response pigment;
(2) Preparing a thermally responsive electrolyte material: mixing an organic polymer, a plasticizer, a solvent and a lithium salt, and then adding the thermally responsive pigment obtained in the step (1) to the mixture to prepare a thermally responsive electrolyte material.
2. The thermally responsive electrolyte material of claim 1 wherein said pigment is one or more of chromate, sulfate, azo pigment, phthalocyanine pigment, anthraquinone, indigo, quinacridone, dioxazine and arylmethane based pigment; the coupling agent is one or more of organic chromium complex, silane, titanate and aluminate compounds; the thermal response material is one or more of polyacrylic acid-b-poly N-isopropyl acrylamide, polymethacrylic acid-b-poly N-isopropyl acrylamide, polymethyl allyl alcohol-b-poly N-isopropyl acrylamide triarylmethane phthalides, fluoran and triphenylmethane; the organic polymer is one or more of polyethylene glycol, polymethyl methacrylate, polymethyl acrylate, polybutyl methacrylate and polyacrylonitrile.
3. The preparation method of the thermally responsive electrolyte material is characterized by comprising the following steps:
(1) Preparing a thermally responsive pigment: putting the pigment into a solvent, adding a coupling agent for ultrasonic treatment to modify or coat the surface of the pigment, centrifugally drying, dispersing into the solvent, adding a thermal response material in an ultrasonic state, and finally centrifugally drying to obtain the thermal response pigment;
(2) Preparing a thermally responsive electrolyte material: mixing an organic polymer, a plasticizer, a solvent and a lithium salt, and then adding the thermally responsive pigment obtained in the step (1) to the mixture to prepare a thermally responsive electrolyte material.
4. The method for producing a thermally responsive electrolyte material as claimed in claim 3, wherein the pigment is one or more of chromate, sulfate, azo pigment, phthalocyanine pigment, anthraquinone, indigo, quinacridone, dioxazine and arylmethane based pigment.
5. The method for producing a thermally responsive electrolyte material as claimed in claim 3, wherein the coupling agent is one or more of organochromium complex, silane, titanate and aluminate compounds.
6. The method for producing a thermally responsive electrolyte material as claimed in claim 3, wherein the thermally responsive material is one or more of polyacrylic acid-b-poly-N-isopropylacrylamide, polymethacrylic acid-b-poly-N-isopropylacrylamide, polymethylpropenol-b-poly-N-isopropylacrylamide triarylmethane phthalides, fluorans and triphenylmethanes.
7. The method for producing a thermally responsive electrolyte material as claimed in claim 3, wherein the organic polymer is one or more of polyethylene glycol, polymethyl methacrylate, polymethyl acrylate, polybutyl methacrylate, and polyacrylonitrile.
8. A method of color modulation in an electrochromic device of a thermally responsive electrolyte material as claimed in any one of claims 1-2, comprising the steps of:
firstly, spraying an electrochromic material polythiophene onto a first conductive layer ITO glass;
secondly, scraping the prepared thermally responsive electrolyte material on the surface of the color-changing thiophene layer;
thirdly, spraying polypyrrole as an ion storage layer on the surface of ITO glass of the second conductive layer; finally, the ITO glass coated with the electrolyte and the color-changing layer is attached to the ITO glass coated with the polypyrrole to prepare an electrochromic device;
fourth, the voltage regulating device changes color, and simultaneously, the temperature regulating thermal response color changing electrolyte is controlled to realize the regulation of different colors.
9. The method for color modulation of a thermally responsive electrolyte material in an electrochromic device of claim 8 wherein the modulation voltage range is-5V to 5V; the temperature is regulated and controlled to be 15-80 ℃; the color change is one or more of red color system, yellow color system, green color system and blue color system.
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