CN106479478B - A kind of electrochromic material and device based on metal nanoparticle - Google Patents
A kind of electrochromic material and device based on metal nanoparticle Download PDFInfo
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- CN106479478B CN106479478B CN201510524224.7A CN201510524224A CN106479478B CN 106479478 B CN106479478 B CN 106479478B CN 201510524224 A CN201510524224 A CN 201510524224A CN 106479478 B CN106479478 B CN 106479478B
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Abstract
The present invention relates to electrochromic material and devices fields, and in particular to a kind of electrochromic material and device based on metal nanoparticle.The composition of the electrochromic material based on metal nanoparticle of the present invention includes：The metal nanoparticle of 0.01wt%~1wt% and the ionic liquid electrolyte of 80wt%~99wt%；The metal nanoparticle is the nano-particle of 100wt% metal nanos silver or 10wt%~90wt% metallic silvers and other metal mixeds.Nano silver grain is mainly directly made in the present invention in ionic liquid; Nano silver grain surface obtained carries positive charge; wherein ionic liquid is both used as Nano silver grain protective agent simultaneously but also as electrolyte; the addition of other extra stabilizers and electrolyte is avoided in this way; both the preparation of entire electroluminescent color material had been enormously simplified; improve the stability of metallic silver; entire electrochromic property is also greatly improved simultaneously, so the present invention has prodigious innovative and potential commercial advantage.
Description
Technical field
The present invention relates to electrochromic material and devices fields, and in particular to a kind of electroluminescent change based on metal nanoparticle
Color material and device.
Background technology
Electrochromic research is derived from last century the mid-80, has attracted the sight of many researchers, research is most
Big target simplifies it, is commercialized.Electrochromic device generally requires bistable state, ignores blind angle, contrast height, system
The features such as at low cost, operating temperature range is wide, driving voltage is low, rich in color is made, electrochromic intelligent window, automobile are can be applied to
The fields such as automatic anti-glare rearview mirror, electrochromism glasses, goggles, smart card, intelligent label, instrument show, outdoor advertising.
Therefore the selection of electrochromic material is particularly important, if single electrochromic material can obtain the reversible light of multistable
State, that is that really have commercial exploitation.
Stable, reversible optical states variations occur under electric field action for electrochromic material.General electrochromism
The inorganic electrochromic material of device is divided into three classes, and the first kind is metal oxide, such as WO3、NiO、MoO3、V2O5Deng mainly
Pass through H+、Li+The extraction of plasma injects to reach stabilization and the change of optical states.Second class is that hydrogen lures in rare earth metal
Phase separation is led to change optical states.Third class is under extra electric field, and the generation of metal (such as Cu, Ni, Ag and Bi) ion can
It inverse sedimentation and is dissolved on transparent electrically-conductive backing plate, reversible optical states is stablized to obtain with this.Metal ion electro-deposition
Colourshifting process have the characteristics that quick response, rich in color, good reversibility, performance stablize.
Mainly by redox reaction receiving and losing electrons, the new oxidation state or reduction-state of generation exist general electrochromic material
Change with certain color in visible-range, but due to the electroluminescent change of common organic and inorganic or organic-inorganic hybrid material
Color material has limited oxidation state or reduction-state, so the color that same electrochromic material hardly results in very abundant becomes
Change, however metallic silver cationic electrodeposition can solve the single problem of common electrochromism color, metal silver ion passes through
It is electrodeposited on pole plate and forms silver nano-grain, silver nano-grain has the surface plasma effect being associated with size and pattern
It answers, different color changes is can get by the size of depositing nano particle, but directly electrodeposit metals silver ion has
Operational difficult, metal silver ion steady in a long-term in the form of an ion cannot be present in electrolyte, be needed to stablize silver ion
Complexity and the raising of cost that a large amount of stabilizer causes entire electrolyte are added, in order to solve problem above,
Silver nanoparticle or silver and the nano-particle of other metal mixeds are directly made in ionic liquid can greatly improve the steady of metallic silver
It is qualitative, and can different colours variation directly occur by powering up to deposit, it is not necessary that the crystal grain of nano silver is formed on pole plate in advance,
Ionic liquid is new generation of green solution, it has the advantages that many general electrolyte do not have, such as insignificant volatility, wide
Electrochemical window and good electric conductivity, so directly prepared in ionic liquid surface carry charge Nano silver grain, it is
A kind of completely new potential electrochromic material of richness.
Invention content
The first object of the present invention is to provide a kind of novel electrochromic functional material, the novel electrochromic functional material
It is to be mixed in proportion by metal nanoparticle, ionic liquid electrolyte and other additives.
The second object of the present invention is to provide a kind of electrochromic device based on above-mentioned novel electrochromic functional material
And preparation method thereof.
Specifically, the electrochromic material of the invention based on metal nanoparticle, composition include：0.01wt%~
The metal nanoparticle of 1wt% and the ionic liquid electrolyte of 89wt%~99wt%；The metal nanoparticle is 100wt%
The nanoparticle of metal nano silver (being individual pure nano silver) or 10wt%~90wt% metallic silvers and other metal mixeds
Son.
Other metal nanoparticles of the present invention are one kind or several in gold, iron, cobalt, nickel, ruthenium, rhodium, palladium, iridium and platinum
Kind.
The additive amount of the metal nanoparticle, preferably 0.1wt%~0.5wt%, further preferably 0.3wt%.
Multicomponent structures of metal nanoparticles can be uniform mixed structure, nucleocapsid and phase separation structure etc., excellent
Gold, silver are selected to be enriched in the nucleocapsid of nano-particle shell.The precursor salt of synthesis metal nanoparticle can be selected from corresponding metal
Compound, such as the precursor salt of Nano silver grain are optional to silver oxide, silver sulfide, silver nitrate, silver acetate and silver chlorate, preferably vinegar
Sour silver；Other metal nanoparticle precursors are oxide, sulfide, nitrate, acetate and the chlorate of other metals
In one kind.The combination of the combination structures of metal nanoparticles of the present invention most preferably silver and gold.
Electrochromic material according to the present invention, wherein the ionic liquid electrolyte is substituted imidazole, substituted pyridines
One kind in class, quaternary amines or pyrrolidines ionic liquid.Preferably, the ionic liquid electrolyte is 1- methyl -3-
(2- ethoxys) imidazoles bis-trifluoromethylsulfoandimide, 1- butyl -3- methylimidazoles hexafluorophosphoric acid, 1- butyl -3- methylimidazoles are double
One in trifluoro methylsulfonimide, tetrabutylammonium double trifluoromethanesulfonimide, N- ethyls and crassitude trifluoromethanesulfonic acids
Kind.The additive amount of the ionic liquid electrolyte, most preferably 98wt%.
Electrochromic material according to the present invention, the electrochromic material further include the addition of 0.1wt%~10wt%
Agent, preferably 3wt%.
Electrochromic material of the present invention can add a certain amount of additive to improve its performance.The additive
It is ultraviolet photoactive polymer, glass microsphere, metal salt, inorganic nano-particle, graphene, carbon nanotube and conduction for monomer
One kind in the functional materials such as graphite.
The monomer is ultraviolet photoactive polymer, and monomer forms polymer network skeleton under action of ultraviolet light,
Polymer network skeleton can enhance the extruded ability of device while enhance two interelectrode cohesive force of device.The polymerization
The monomer of object is bis- (4- (6 '-propenyloxy group hexyloxy) the benzoyloxy) -2- toluene (C6M) of 1,4- or 4- (6- acryloyls
Oxygroup) the hexyl methyl cinnamate base phenol ester of benzoic acid -4 ', preferably C6M.Institute's glass microsphere can control two electricity of broad area device
The gap of interpolar can also effectively improve the light scattering property of device coloured state, and the grain size of glass microsphere can be selected from 10-50 μm,
It is preferred that 20 μm.The metal salt can assistant metal nano-particle participate in electrochromic process, can be silver acetate, silver nitrate,
One or more of silver chlorate, silver bromide and silver iodide etc., preferably silver acetate；The inorganic nano-particle can effectively improve device
The light scattering property of part coloured state can be in zinc sulphide, copper oxide, copper chloride, barium carbonate, barium sulfate and cadmium sulfide etc.
One or more, preferably copper oxide.
The preparation method of above-mentioned electrochromic material provided by the invention, includes the following steps：
1) by the mixture of metal nano silver precursor or metal nano silver precursor and other metal nanoparticle precursors with
Organic solvent and ionic liquid electrolyte mixing, and the organic solvent being removed in vacuum under agitation in solution；Wherein, organic
The additive amount of solvent is 5-10 times of ionic liquid electrolyte volume；The organic solvent can select but be not limited to acetone,
One or more of acetonitrile, dichloromethane, ethyl acetate and ethyl alcohol.
2) it is removed into step 1) in the solution of organic solvent and is passed through hydrogen (H2), by metal nano silver precursor, Huo Zhejin
Belong to nano silver precursor and the mixture of other metal nanoparticle precursors is reduced to metal Nano silver grain or metallic silver and its
Electrochromic material is made in the nano-particle of its metal mixed.
When electrochromic material when containing additive of the present invention, can also be added after step 2) restores 0.1wt%~
Electrochromic material is made in the additive of 10wt%.
Further, when the additive added after step 2) reduction is ultraviolet photoactive polymer monomer, it is also necessary to
Photoinitiator is added to promote the polymerization crosslinking of polymer monomer to cure, the photoinitiator additive amount adds for polymer monomer
0.01wt%~0.05wt% of amount, the photoinitiator are preferably styrax diethyl ether (IGR 651).
Electrochromic device provided by the invention, including electrochromic material of the present invention.The electrochromism device
Part is made of the electrochromism functional layer of two transparent electrodes and folder between them, wherein the electrochromism functional layer
Material, that is, above-mentioned electrochromism functional material.Electrochromic device as shown in Figure 1, by two transparent electrodes 1 and intermediate electricity
Inducing off-coloring function layer 2 forms.
The present invention electrochromic device preparation method, including using electrochromic material injection by two transparent electrodes as
In the interlayer of pole plate, electrochromic device is made after sealing.
The transparent electrode is to be made of with the transparent conductive material for being plated in its surface transparent base；Wherein, described saturating
The one kind of bright base material in unorganic glass, organic glass and transparent membrane；The transparent conductive material is selected from the oxidation of doping
One kind in the zinc oxide of tin, the indium oxide of doping or doping.In electrochromic device the distance between two transparent electrodes by
The thickness of dottle pin controls, and separation pad is selected from nonconducting macromolecule membrane or glass microballoon, and nonconducting macromolecule is thin
Film is one kind in polytetrafluoroethylene (PTFE), polyethylene, polyvinyl chloride and polypropylene；The interval mat thickness is 10~50 μm, preferably
20μm。
Specifically, the mixing temperature that the present invention is related to when preparing electrochromic material can be selected from 10~80 DEG C, preferably 25
℃.The electrochromic device assembly program that step 2 is related to is：First separation pad is placed among two transparent electrodes, then uses ring
Oxygen resin glue carries out edge sealing processing to pole plate both sides, and the injection of electrochromic material can be used for after adhesive curing.By electroluminescent change
Color material solution is coated at the gap of component cases one end, and since capillary phenomenon acts on, thus electrochromic material locates inhalator
Part can will carry out the subsequent operation such as testing after the other both ends sealing of device.
Novel electrochromic material provided by the present invention is by metal nanoparticle, ionic liquid electrolyte and/or to add
Agent etc. is added to be mixed in a certain ratio.Electrochromic device according to the present invention is by conductive electrode, electrochromism function
The sandwich structure of layer, conductive electrode composition.By being sealed after electrochromic material is poured into device, electrochromism is just completed
The assembling of device.Under electric field action, such electrochromic device can realize three kinds of optical state transitions：Transparent state, coloured state
And minute surface state, wherein coloured state can still present the transformation of different colours, such as red, yellow and blue.The present invention's is electroluminescent
Electrochromic device is in same device by adjusting voltage, it can be achieved that phase co-conversion between three kinds of optical states, and with response
The advantages that time is short, good cycle, simple preparation process is expected to be applied to the fields such as electrochromic display device (ECD).
Nano silver grain is mainly directly made in the present invention in ionic liquid, and Nano silver grain surface obtained is with just
Charge, wherein ionic liquid were both used as Nano silver grain protective agent simultaneously but also as electrolyte, avoided so other more
The addition of remaining stabilizer and electrolyte had both enormously simplified the preparation of entire electroluminescent color material, and had improved the steady of metallic silver
It is qualitative, while entire electrochromic property (the getable color change of institute) is also greatly improved, so the present invention has
There is prodigious innovative and potential commercial advantage.
Description of the drawings
Fig. 1 is the structural schematic diagram of the electrochromic device of the present invention.
Fig. 2 is for electrochromic device in embodiment 1 to the transmitance schematic diagram of minute surface state from transparent state to coloured state.
Fig. 3 is for electrochromic device in embodiment 2 to the transmitance schematic diagram of minute surface state from transparent state to coloured state.
Fig. 4 is for electrochromic device in embodiment 3 to the transmitance schematic diagram of minute surface state from transparent state to coloured state.
Fig. 5 is for electrochromic device in embodiment 4 to the transmitance schematic diagram of minute surface state from transparent state to coloured state.
Fig. 6 is for electrochromic device in embodiment 5 to the transmitance schematic diagram of minute surface state from transparent state to coloured state.
Reference numeral
1, transparent electrode 2, electrochromism functional layer
Specific implementation mode
It is listed below a preferred embodiment of the present invention, be used only as explanation of the invention rather than is limited.
Embodiment 1
1wt% silver acetates, 5mL acetone and the double trifluoro methylsulphurs of 99wt% ionic liquid electrolyte 1- butyl -3- methylimidazoles
Acid imide, quickly stirring forms colourless mixed solution at room temperature.Under quick stirring, the acetone in solution is removed in vacuum,
Then it is passed through H under room temperature2Silver acetate is reduced to Nano silver grain as reducing agent.0.01g mixed solutions are injected into
By ITO as in the device of pole plate, tested after being sealed with fluid sealant.
Using two electrode systems, prepared electrochromic device transparent electrode both ends are added into two electrodes, between device
Every the DC voltage 5s, interval time 30s for applying 2V.Increase with conduction time, device is changed into Huang by initial transparent state
Color state, red color, ultraviolet state and minute surface state, referring to Fig. 2.Reversal procedure voltage is applied to device, device is changed by minute surface state
Purple state, red state, yellow state and transparent state.Forward and reverse programm voltage is applied to device cycle, device can be realized 200 times
Above cycle shows good stability.
Embodiment 2
0.01wt% silver acetates, 5mL acetone and 89.99wt% ionic liquid electrolytes (the double fluoroform sulphurs of tetrabutylammonium
Acid imide), quickly stirring forms colourless mixed solution at room temperature.Under quick stirring, the acetone in solution is removed in vacuum,
Then it is passed through H at ambient temperature2By silver nitrate and reducing palladium acetate it is gold and silver nano-particle as reducing agent.What is synthesized
9.99wt%C6M is added in gold and silver nano-particle ionic liquid and accounts for the photoinitiator styrax two of C6M additive amounts 0.01wt%
0.01g mixed solutions are injected by ITO as in the device of pole plate by ether (IGR 651), after being sealed with fluid sealant
365nm uviol lamp intensities are to be tested after polymerization 20min under 2mW/cm2.
The test method of device is the same as embodiment 1.Increase with conduction time, device is changed into yellow by initial transparent state
State, red state, ultraviolet state and minute surface state, referring to Fig. 3.Reversal procedure voltage is applied to device, device is changed into purple by minute surface state
Color state, red state, yellow state and transparent state.To device cycle apply forward and reverse programm voltage, device can realize 200 times with
On cycle, show good stability.
Embodiment 3
1wt% mixed metals precursor (90wt% silver acetates and 10wt% palladiums) 5mL acetone and 89.9wt% ionic liquids
1- methyl -3- (2- ethoxys) imidazoles bis-trifluoromethylsulfoandimide of body electrolyte, quickly stirring is formed without color contamination at room temperature
Close solution.Under quick stirring, the acetone in solution is removed in vacuum, is then passed through H under room temperature2As reducing agent by nitre
Sour silver and reducing palladium acetate are silver-colored Pd nano particle.A diameter of 20 are added in solution in the ionic liquid containing Nano silver grain
μm 10wt% glass microballoons be uniformly mixed.0.01g mixed solutions are injected by ITO as in the device of pole plate, with sealing
It is tested after glue sealing.
The test method of device is the same as embodiment 1.Increase with conduction time, device is changed into yellow by initial transparent state
State, red state, ultraviolet state and minute surface state, referring to Fig. 4.Reversal procedure voltage is applied to device, device is changed into purple by minute surface state
Color state, red state, yellow state and transparent state.To device cycle apply forward and reverse programm voltage, device can realize 200 times with
On cycle, show good stability.
Embodiment 4
1wt% metal mixeds precursor (50wt% silver acetates and 25wt% acetic acid gold and 25%wt palladiums) and 98wt% from
Sub- liquid electrolyte (1- butyl -3- methylimidazoles hexafluorophosphoric acid), quickly stirring forms colourless mixed solution at room temperature.Fast
Under the stirring of speed, the acetone in solution is removed in vacuum, is then passed through H under room temperature2As reducing agent by silver nitrate and acetic acid
Palladium is reduced to silver-colored Pd nano particle.(the oxidation of 1wt% additives is added in the solution in the ionic liquid containing Nano silver grain
Copper) it is uniformly mixed.0.01g mixed solutions are injected by ITO as in the device of pole plate, are surveyed after being sealed with fluid sealant
Examination.The test method of device is the same as embodiment 1.Referring to Fig. 5.Forward and reverse programm voltage is applied to device cycle, device can be real
Existing 200 times or more cycles, show good stability.
Embodiment 5
1wt% metal mixeds precursor (50wt% silver acetates and 25wt% ferric acetates and 25%wt nickel acetates) and 98wt% from
Sub- liquid electrolyte (1- butyl -3- methylimidazoles hexafluorophosphoric acid), quickly stirring forms colourless mixed solution at room temperature.Fast
Under the stirring of speed, the acetone in solution is removed in vacuum, is then passed through H under room temperature2As reducing agent by silver nitrate and acetic acid
Palladium is reduced to silver-colored Pd nano particle.(the oxidation of 1wt% additives is added in the solution in the ionic liquid containing Nano silver grain
Silver) it is uniformly mixed.0.01g mixed solutions are injected by ITO as in the device of pole plate, are surveyed after being sealed with fluid sealant
Examination.The test method of device is the same as embodiment 1.The test method of device is the same as embodiment 1.Referring to Fig. 6.Device cycle is applied positive
With reversal procedure voltage, device can realize 200 times or more cycles, show good stability.
Certainly, the present invention can also there are many embodiments, without deviating from the spirit and substance of the present invention, are familiar with
Those skilled in the art can disclosure according to the present invention make various corresponding changes and modification, but these it is corresponding change and
Deformation should all belong to the protection domain of appended claims of the invention.
Claims (9)
1. a kind of electrochromic material based on metal nanoparticle, which is characterized in that the composition packet of the electrochromic material
It includes：The metal nanoparticle of 0.01wt%~1wt% and the ionic liquid electrolyte of 80wt%~99wt%；The metal nano
Particle is the nano-particle of 100wt% metal nanos silver or 10wt%~90wt% metallic silvers and other metal mixeds；Its
In, other metals are one or more of gold, iron, cobalt, nickel, ruthenium, rhodium, palladium, iridium and platinum.
2. electrochromic material according to claim 1, which is characterized in that the ionic liquid electrolyte is 1- methyl-
3- (2- ethoxys) imidazoles bis-trifluoromethylsulfoandimide, 1- butyl -3- methylimidazoles hexafluorophosphoric acid, 1- butyl -3- methylimidazoles
In bis-trifluoromethylsulfoandimide, tetrabutylammonium double trifluoromethanesulfonimide, 1- ethyl-3-methylimidazole fluoroform sulphonates
It is a kind of.
3. electrochromic material according to claim 1, which is characterized in that the electrochromic material further includes
The additive of 0.1wt%~10wt%；The additive be monomer be ultraviolet photoactive polymer, glass microsphere, metal salt,
One kind in inorganic nano-particle, graphene, carbon nanotube and electrically conductive graphite；
Wherein, the monomer of the polymer be bis- (4- (6 '-propenyloxy group hexyloxy) the benzoyloxy) -2- toluene of Isosorbide-5-Nitrae-or
4- (6- acryloxies) hexyl methyl cinnamate base phenol ester of benzoic acid -4 '；The metal salt is silver acetate, silver nitrate, chlorine
Change one or more of silver, silver bromide and silver iodide；The inorganic nano-particle is zinc sulphide, copper oxide, copper chloride, carbonic acid
One or more of barium, barium sulfate and cadmium sulfide.
4. the preparation method of electrochromic material, includes the following steps described in a kind of claim 1：
1) by the mixture of metal nano silver precursor or metal nano silver precursor and other metal nanoparticle precursors with it is organic
Solvent and ionic liquid electrolyte mixing, and the organic solvent being removed in vacuum under agitation in solution；Wherein, organic solvent
Additive amount be 5-10 times of ionic liquid electrolyte volume；Wherein, the metal nano silver precursor be silver oxide, silver nitrate and
One kind in silver acetate, other metal nanoparticle precursors are in the oxide, nitrate and acetate of other metals
It is a kind of；
2) it is removed into step 1) in the ionic liquid of organic solvent and is passed through hydrogen, metal nano silver precursor or metal are received
The silver-colored precursor of rice and the mixture of other metal nanoparticle precursors are reduced to metal Nano silver grain or metallic silver and other gold
Belong to mixed nano-particle, electrochromic material is made.
5. preparation method according to claim 4, which is characterized in that the step 1) organic solvent is acetone, acetonitrile, two
One or more of chloromethanes, ethyl acetate and ethyl alcohol.
6. preparation method according to claim 4, which is characterized in that step 2) reduction after be additionally added 0.1wt%~
Electrochromic material is made in the additive of 10wt%；The additive is that monomer is that ultraviolet photoactive polymer, glass are micro-
One kind in ball, metal salt, inorganic nano-particle, graphene, carbon nanotube and electrically conductive graphite；
Wherein, the monomer of the polymer be bis- (4- (6 '-propenyloxy group hexyloxy) the benzoyloxy) -2- toluene of Isosorbide-5-Nitrae-or
4- (6- acryloxies) hexyl methyl cinnamate base phenol ester of benzoic acid -4 '；The metal salt is silver acetate, silver nitrate, chlorine
Change one or more of silver, silver bromide and silver iodide；The inorganic nano-particle is zinc sulphide, copper oxide, copper chloride, carbonic acid
One or more of barium, barium sulfate and cadmium sulfide.
7. a kind of electrochromic device, which is characterized in that the electrochromic device includes electrochromism described in claim 1
Material.
8. electrochromic device according to claim 7, which is characterized in that the electrochromic material further includes
The additive of 0.1wt%~10wt%；The additive be monomer be ultraviolet photoactive polymer, glass microsphere, metal salt,
One kind in inorganic nano-particle, graphene, carbon nanotube and electrically conductive graphite；
Wherein, the monomer of the polymer be bis- (4- (6 '-propenyloxy group hexyloxy) the benzoyloxy) -2- toluene of Isosorbide-5-Nitrae-or
4- (6- acryloxies) hexyl methyl cinnamate base phenol ester of benzoic acid -4 '；The metal salt is silver acetate, silver nitrate, chlorine
Change one or more of silver, silver bromide and silver iodide；The inorganic nano-particle is zinc sulphide, copper oxide, copper chloride, carbonic acid
One or more of barium, barium sulfate and cadmium sulfide.
9. the preparation method of the electrochromic device described in a kind of claim 7 or 8, including electrochromic material is injected by two
Electrochromic device is made as in the interlayer of pole plate in transparent electrode after sealing；
Wherein, the transparent electrode is to be made of with the transparent conductive material for being plated in its surface transparent base；The transparent base
The one kind of material in unorganic glass, organic glass and transparent membrane；The transparent conductive material is selected from the tin oxide of doping, mixes
One kind in the zinc oxide of miscellaneous indium oxide or doping；
The distance between two transparent electrodes are controlled by the thickness of separation pad in the electrochromic device, and separation pad is selected from and does not lead
Electricity macromolecule membrane or glass microballoon, nonconducting macromolecule membrane be polytetrafluoroethylene (PTFE), polyethylene, polyvinyl chloride and
One kind in polypropylene；The interval mat thickness is 10-50 μm.
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| A Localized Surface Plasmon Resonance-Based Multicolor Electrochromic Device with Electrochemically Size Controlled Silver Nanoparticles;Ayako Tsuboi等;《Adv. Mater.》;20131231;3197–3201 * |
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| CN106479478A (en) | 2017-03-08 |
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