CN116939903A - Electroluminescent device based on waterborne polyurethane-silver nanowire and preparation method thereof - Google Patents
Electroluminescent device based on waterborne polyurethane-silver nanowire and preparation method thereof Download PDFInfo
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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000004814 polyurethane Substances 0.000 claims abstract description 29
- 239000011268 mixed slurry Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 20
- 238000004528 spin coating Methods 0.000 claims description 18
- 229910002113 barium titanate Inorganic materials 0.000 claims description 16
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical group [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 15
- 229920002635 polyurethane Polymers 0.000 claims description 14
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 12
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 12
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 12
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 12
- -1 polyethylene terephthalate Polymers 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 10
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 9
- 238000007650 screen-printing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 238000007639 printing Methods 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 claims description 3
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 83
- 239000003989 dielectric material Substances 0.000 description 14
- 239000004205 dimethyl polysiloxane Substances 0.000 description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002033 PVDF binder Substances 0.000 description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 229920001748 polybutylene Polymers 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 229910052963 cobaltite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
- H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source
- H05B33/145—Arrangements of the electroluminescent material
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention belongs to the field of chemical industry, and particularly relates to an electroluminescent device based on waterborne polyurethane-silver nanowires and a preparation method thereof. The preparation method of the invention comprises the following steps: a transparent electrode layer is arranged on the surface of the substrate by utilizing silver nanowire conductive ink, and a mask is utilized to cover a local transparent electrode layer; a dielectric layer is arranged on the surface of the transparent electrode layer by utilizing aqueous Polyurethane (PU); mixing aqueous Polyurethane (PU), luminescent powder and filler to prepare luminescent layer mixed slurry, and arranging a luminescent layer on the surface of a dielectric layer by using the luminescent layer mixed slurry; a back electrode layer is arranged on the surface of the light-emitting layer by silver paste; and then removing the mask to obtain the electroluminescent device based on the aqueous polyurethane-silver nanowire. The invention has simple process, and the obtained electroluminescent device has high stability and uniformity.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to an electroluminescent device based on waterborne polyurethane-silver nanowires and a preparation method thereof.
Background
The silver nanowire-based flexible alternating current electroluminescent device has great application potential in new application scenes such as display, wearable electronic fields and the like. In the whole device structure, the electrode layer, the dielectric layer and the light-emitting layer are mainly divided. The silver nanowire transparent conductive film is used as a top transparent electrode layer, an electric field is applied by utilizing high conductivity of the silver nanowire transparent conductive film, meanwhile, the loss of light emitted by a light-emitting layer is reduced by high transmittance of the silver nanowire transparent conductive film, and the silver nanowire transparent conductive film has the flexibility of a device, so that the silver nanowire transparent conductive film is the most potential transparent electrode material for replacing ITO glass. In addition, when the device is actually constructed, the dielectric layer is often used as a dispersion matrix of the light-emitting layer powder. For the material selection of the dielectric layer, the luminous intensity, luminous uniformity, process flow, matching with the electrode layer, etc. are mainly considered.
Currently, the materials of the common dielectric layers used for constructing the silver nanowire-based flexible alternating current electroluminescent device mainly comprise polyvinylidene fluoride (PVDF), polybutylene (PB), polydimethylsiloxane (PDMS), hydroxypropyl methylcellulose (HPMC) and the like.
The alternating current electroluminescent device prepared by taking PVDF and PB as dielectric materials has higher luminous intensity, but PVDF and PB are difficult to dissolve in conventional solvents, and are required to be dissolved in solvents with large toxicity such as acetone, NMP, DMF and the like, so that the alternating current electroluminescent device has large requirements on production management and production equipment and is not beneficial to large-scale production. Patent CN114784202a describes a wearable flexible low temperature resistant self-driven electroluminescent system and a method for constructing the same, which uses polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) as a dielectric material and a luminescent layer matrix, the dielectric material needs to be dissolved in acetone, and thus an electroluminescent device is constructed. Acetone is toxic and is not suitable for mass production of enterprises. CN113629201a describes a triboelectric induced electroluminescent device construction method that can identify fingerprints and has better brightness than commercial LEDs, and also uses PVDF-HFP as the dielectric material, and N, N-Dimethylformamide (DMF) as the solvent. DMF is strong in solvent toxicity and high in toxicity, and meanwhile, when a silver nanowire-based electroluminescent device is constructed, the electrode of the silver nanowire transparent conductive film is damaged, so that the construction of an electric field is affected, and the luminous performance of the device is affected.
PDMS and HPMC are used as dielectric materials, and can be dissolved by adopting a conventional solvent, but the luminous intensity of an alternating current electroluminescent device prepared by using the PDMS and HPMC as dielectric materials is lower. CN109634020a describes an electroluminescent device based on nanocellulose-silver nanowires and its application, with Polydimethylsiloxane (PDMS) as a matrix for the dielectric layer and the light-emitting layer. PDMS has good optical property, stretchability, easy molding and biocompatibility, but the dielectric constant is only 2.7 (100 KHz), and the luminous intensity of the prepared alternating current electroluminescent device is too low.
At present, no excellent dielectric material for alternating current electroluminescence exists in the market, and the dielectric material can simultaneously meet the conditions of easy dissolution, high dielectric constant, no damage to a transparent electrode of a silver nanowire and the like, thereby preventing the large-scale preparation of a silver nanowire-based alternating current electroluminescent device.
Disclosure of Invention
The invention aims to provide an electroluminescent device based on aqueous polyurethane-silver nanowires and a preparation method thereof, and the device has good luminous effect.
In order to solve the technical problems, the invention provides a preparation method of an electroluminescent device based on aqueous polyurethane-silver nanowires, which comprises the following steps:
1) Preparation of transparent electrode layer:
uniformly mixing silver nanowire dispersion liquid, hydroxypropyl methylcellulose, fluorocarbon FSO-100 and deionized water (stirring for 30+/-10 min at room temperature) to obtain silver nanowire conductive ink;
a transparent electrode layer is arranged on the surface of the substrate by utilizing silver nanowire conductive ink, and a mask is utilized to cover a local transparent electrode layer;
in the silver nanowire conductive ink, the solid content of the silver nanowire is 0.15-0.17 wt%, the solid content of the hydroxypropyl methylcellulose is 0.25-0.26 wt%, and the solid content of the fluorocarbon FSO-100 is 0.0015-0.0025 wt% (preferably 0.002 wt%);
description: fluorocarbon FSO-100 as a surfactant;
2) Preparation of dielectric layer:
a dielectric layer is arranged on the surface of the transparent electrode layer by utilizing aqueous Polyurethane (PU);
the solid content of the aqueous polyurethane is 30% -40%, and the cloth viscosity is less than 200cps;
3) Preparation of a light-emitting layer:
mixing aqueous Polyurethane (PU), luminescent powder and filler to prepare luminescent layer mixed slurry, and arranging a luminescent layer on the surface of a dielectric layer by using the luminescent layer mixed slurry;
aqueous polyurethane: luminescent powder = 2: (1+/-0.1) mass ratio of filler: aqueous polyurethane=0 to 25 mass percent (preferably 1 to 15%, more preferably 5 to 15%);
4) Preparation of the back electrode layer:
a back electrode layer is arranged on the surface of the light-emitting layer by silver paste;
and then taking down the mask set in the step 1) to obtain the electroluminescent device based on the waterborne polyurethane-silver nanowire.
Description: the aqueous Polyurethane (PU) in the step 2) and the aqueous Polyurethane (PU) in the step 3) are the same material.
As an improvement of the preparation method of the electroluminescent device based on the aqueous polyurethane-silver nanowire, the invention:
the thickness of the transparent electrode layer in the step 1) is 20-30 mu m;
the thickness of the dielectric layer in the step 2) is 50-80 mu m;
the thickness of the luminescent layer in the step 3) is 30-50 mu m;
the thickness of the back electrode layer in the step 4) is 30-50 mu m.
As an improvement of the method for preparing an electroluminescent device based on aqueous polyurethane-silver nanowires according to the invention, in the step 3):
the filler is barium titanate, ceramic filler or carbon filler;
the ceramic filler is lead zirconate titanate,
the carbon-based filler is carbon black.
As a further improvement of the preparation method of the electroluminescent device based on the aqueous polyurethane-silver nanowire: the substrate in the step 1) is a polyethylene terephthalate (PET) film; for example, a polyethylene terephthalate (PET) film of 10cm by 10 cm.
As a further improvement of the method for the preparation of an electroluminescent device based on aqueous polyurethane-silver nanowires according to the invention, the step 1) is:
printing a film on the surface of a polyethylene terephthalate (PET) film by a slit coating method, and drying to form a transparent electrode layer;
the step 2) is as follows:
dripping aqueous Polyurethane (PU) on the surface of the transparent electrode layer, spin-coating to form a film, and drying to form a dielectric layer;
the step 3) is as follows:
dripping the mixed slurry of the luminescent layer on the surface of the dielectric layer, spin-coating to form a film, and drying to form the luminescent layer;
the step 4) is as follows:
and 3) placing the product obtained in the step 3) on a screen printing sample stage, printing silver paste electrodes on the light-emitting layer in a screen printing mode, and drying to form a back electrode layer.
As a further improvement of the method for the preparation of an electroluminescent device based on aqueous polyurethane-silver nanowires according to the invention,
in step 1):
the solvent of the silver nanowire dispersion is at least one (i.e., one or more) of water, ethanol, isopropanol;
a slit coating method, wherein the ink injection speed is 1.5mL/min, the coating speed is 5mm/s, the drying (substrate heating) temperature is 45 ℃, and the time is 10+/-2 min;
in step 2):
spin coating rotation speed is 1000rpm, spin coating time is 20s;
the drying temperature is 60 ℃ and the drying time is 30min;
in step 3):
spin coating rotation speed is 1000rpm, spin coating time is 20s;
the drying temperature is 60 ℃ and the drying time is 30min;
in step 4):
the screen plate used for screen printing is 100-400 meshes.
The beneficial effects of the invention are as follows:
the invention prepares the silver nanowire-based electroluminescent device, uses aqueous Polyurethane (PU) to replace traditional substances such as polyvinylidene fluoride, polydimethylsiloxane and the like as dielectric layer materials and luminescent layer matrix materials, has good hydrophilicity, can be dissolved in conventional solvent water, is easy to spread on the surface of a silver nanowire film, has no damage to a transparent electrode layer, has higher dielectric constant, further increases the dielectric constant of the luminescent layer by adding barium titanate, and simply obtains the non-toxic dielectric layer and the luminescent layer with high dielectric constant, and the electroluminescent device constructed has high luminous intensity and uniform luminescence (figure 2). The silver nanowire transparent film electrode is prepared through screen printing, and has excellent photoelectric performance and good flexibility and bending performance (figure 3).
In conclusion, the process is simple, and the obtained electroluminescent device is high in stability and uniformity.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of an electroluminescent device based on aqueous polyurethane-silver nanowires
FIG. 2 is a diagram showing light-emitting materials of the devices constructed in examples 2 to 3 and comparative examples 1 to 3.
Fig. 3 is a graph showing the change in luminous intensity after multiple bending in example 1.
Detailed Description
The invention will be further described with reference to the following specific examples, but the scope of the invention is not limited thereto:
the ingredients used in the present invention can all be obtained in conventional commercially available forms.
The silver nanowire dispersion liquid is silver nanowire deionized water dispersion liquid, the concentration of the silver nanowire is 0.01-1 mg/ml, the diameter of the silver nanowire is 20-90 nm, and the length of the silver nanowire is 10-30 mu m. For example, xwaynano-AgNW-20 silver nanowire dispersion (concentration of silver nanowire is 1mg/ml, diameter of silver nanowire is 45nm, length of silver nanowire is 30 μm) manufactured by Zhejiang Xishi nanotechnology Co.
The solid content of the aqueous Polyurethane (PU) is 30-40%, the cloth viscosity is less than 200cps, for example, PU-3407 (the solid content of the aqueous polyurethane is 30-40%, and the cloth viscosity is less than 200 cps) produced by Shundesansheng trade company can be selected.
The luminescent powder is green D512CT luminescent powder produced by Shanghai Cork.
The silver paste with the solid content of 71.3 percent can be selected from MGT-SR-G70 silver paste of Sichuan Chong Chinese electronic technology Co.
Example 1: an electroluminescent device based on aqueous polyurethane-silver nanowires, comprising the steps of:
1) Preparation of transparent electrode layer
Stirring silver nanowire dispersion liquid, hydroxypropyl methylcellulose, fluorocarbon FSO-100 (surfactant) and deionized water at room temperature for 30min for uniform mixing to obtain silver nanowire conductive ink; the solid content of silver nanowires in the silver nanowire conductive ink is 0.16 wt%, the solid content of hydroxypropyl methyl cellulose is 0.256 wt%, the solid content of FSO-100 is 0.002 wt%, the silver nanowire conductive ink is printed on the surface of a polyethylene terephthalate (PET) film (with the thickness of 125 mu m) of 10cm multiplied by 10cm to form a film by a slit coating method, the ink injection speed is 1.5mL/min during slit coating, and the coating speed is 5mm/s; drying (10 minutes at 45 ℃) to form a transparent electrode layer (coating layer) having a thickness of 25 μm;
cutting into 5cm×5cm, and covering a mask of 0.5cm×5cm on either edge of the transparent electrode layer, so that the transparent electrode layer of 0.5cm×5cm size is covered by the mask; the result was named silver nanowire transparent electrode.
2) Preparation of dielectric layers
Placing the silver nanowire transparent electrode obtained in the step 1) on a sucker of a spin coating device, measuring 3mL of aqueous polyurethane by using an injector, dripping the aqueous polyurethane on the surface of a transparent electrode layer, setting the spin coating rotating speed to 1000rpm for 20s, transferring the transparent electrode layer into a 60 ℃ oven for heating for 30min after spin coating to form a dielectric layer positioned on the transparent electrode layer; the dielectric layer thickness was 50 μm.
3) Preparation of light-emitting layer
Stirring 6g of aqueous Polyurethane (PU), 0.9g of barium titanate and 3g of luminous powder for 30min to obtain luminous layer mixed slurry; placing the film obtained in the step 2) on a sucker of a spin coating device, measuring 3mL of luminescent layer mixed slurry by using an injector, dripping the slurry on the surface of a dielectric layer, setting the spin coating rotating speed to 1000rpm for 20s, transferring the film to a 60 ℃ oven for heating for 30min after spin coating to form a luminescent layer positioned on the dielectric layer; the thickness of the light-emitting layer was 50. Mu.m.
4) Preparation of the back electrode layer
Placing the film obtained in the step 3) on a screen printing sample table, selecting a 200-mesh screen, utilizing silver paste with the solid content of 71.3% to screen print a silver paste electrode on the light-emitting layer, and drying in an oven at 80 ℃ for 30min to form a back electrode layer positioned on the light-emitting layer, wherein the thickness of the back electrode layer is 50 mu m.
And then the mask arranged in the step 1) is taken down, so that the transparent electrode layer originally covered by the mask is exposed, and the electroluminescent device based on the aqueous polyurethane-silver nanowire can be obtained.
Example 2-1: an electroluminescent device based on aqueous polyurethane-silver nanowires, the amount of barium titanate in the luminescent layer mixed slurry of step 3) of example 1 is changed from 0.9g to 0, and the rest is the same as that of example 1.
Example 2-2: an electroluminescent device based on aqueous polyurethane-silver nanowires, the amount of barium titanate in the luminescent layer mixed slurry of step 3) of example 1 is changed from 0.9g to 0.06g, and the rest is the same as example 1.
Examples 2-3: an electroluminescent device based on aqueous polyurethane-silver nanowires, the amount of barium titanate in the luminescent layer mixed slurry of step 3) of example 1 is changed from 0.9g to 0.3g, and the rest is the same as example 1.
Example 3 an electroluminescent device based on aqueous polyurethane-silver nanowires, the barium titanate in the luminescent layer mixed slurry of step 3) of example 1 was changed to lead zirconate titanate, the amount remained unchanged at 0.9g, and the rest was identical to example 1.
Example 4 an electroluminescent device based on aqueous polyurethane-silver nanowires, the barium titanate in the luminescent layer mixed slurry in example 1 was changed to carbon black, the amount remained unchanged at 0.9g, and the rest was identical to example 1.
Comparative example 1: the procedure of example 1, step 2) and step 3) was repeated except that the aqueous Polyurethane (PU) as a dielectric material was changed to Polydimethylsiloxane (PDMS) and the amount of barium titanate in the mixed slurry of the light-emitting layer was changed to 0.
Comparative example 2: the procedure of example 1, step 2) and step 3) was followed except that the aqueous Polyurethane (PU) as a dielectric material was changed to hydroxypropyl methylcellulose (HPMC) in an amount constant, and the amount of barium titanate in the luminescent layer mixed slurry was changed to 0.
Comparative example 3: the procedure of example 1 was followed except that the aqueous Polyurethane (PU) as a dielectric material in both step 2) and step 3) of example 1 was changed to Polybutene (PB) in an amount constant, and the amount of barium titanate in the mixed slurry of the light-emitting layer was changed to 0.
Comparative example 4: the procedure of example 1 was followed except that the aqueous Polyurethane (PU) used as the dielectric material in both step 2) and step 3) of example 1 was polyvinylidene fluoride (PVDF) and the amount of barium titanate in the mixed slurry of the light-emitting layer was changed to 0.
All the above examples and comparative examples were tested for performance, wherein the brightness test was performed at an ac voltage of 100V,100Hz, in the following manner: A100V, 100Hz alternating voltage is applied between the back electrode layer and the transparent electrode layer by a copper flat nozzle clamp, and then the luminous wavelength and luminous intensity of the device are detected.
The results are shown in Table 1 below:
TABLE 1
As can be seen from Table 1, the dielectric constant of the aqueous Polyurethane (PU) used as the dielectric material and the luminescent layer matrix was higher, and the luminescent brightness of the device was higher. The dielectric constant of the PU system after barium titanate is added is the same as PB, but the brightness of the device is higher.
The luminous patterns of the devices constructed in example 2 and comparative examples 1 to 3 are shown in fig. 2, in which the light emission of the device constructed by the dielectric material and the light-emitting layer matrix of PU is more uniform.
Comparative example 5 an electroluminescent device based on aqueous polyurethane-silver nanowires, the amount of barium titanate in the mixed slurry of the luminescent layer in example 1 was changed to calcium titanate, and was maintained at 0.9g, and the rest was identical to example 1. The properties obtained are shown in Table 1.
Comparative example 6 an electroluminescent device based on aqueous polyurethane-silver nanowires was prepared by changing barium titanate in the mixed slurry of the luminescent layer in example 1 to lanthanum cobaltite, the amount remained unchanged at 0.9g, and the rest was identical to example 1. The properties obtained are shown in Table 1.
Finally, it should also be noted that the above list is merely a few specific embodiments of the present invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (10)
1. The preparation method of the electroluminescent device based on the aqueous polyurethane-silver nanowire is characterized by comprising the following steps:
1) Preparation of transparent electrode layer:
uniformly mixing silver nanowire dispersion liquid, hydroxypropyl methylcellulose, fluorocarbon FSO-100 and deionized water to obtain silver nanowire conductive ink;
a transparent electrode layer is arranged on the surface of the substrate by utilizing silver nanowire conductive ink, and a mask is utilized to cover a local transparent electrode layer;
in the silver nanowire conductive ink, the solid content of the silver nanowire is 0.15-0.17 wt%, the solid content of the hydroxypropyl methylcellulose is 0.25-0.26 wt%, and the solid content of the fluorocarbon FSO-100 is 0.0015-0.0025 wt%;
2) Preparation of dielectric layer:
a dielectric layer is arranged on the surface of the transparent electrode layer by utilizing waterborne polyurethane;
3) Preparation of a light-emitting layer:
mixing waterborne polyurethane, luminescent powder and filler to prepare luminescent layer mixed slurry, and arranging a luminescent layer on the surface of the dielectric layer by using the luminescent layer mixed slurry;
aqueous polyurethane: luminescent powder = 2: (1+/-0.1) mass ratio of filler: aqueous polyurethane=0 to 25% mass ratio;
4) Preparation of the back electrode layer:
a back electrode layer is arranged on the surface of the light-emitting layer by silver paste;
and then taking down the mask set in the step 1) to obtain the electroluminescent device based on the waterborne polyurethane-silver nanowire.
2. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 1, characterized in that:
the thickness of the transparent electrode layer in the step 1) is 20-30 mu m;
the thickness of the dielectric layer in the step 2) is 50-80 mu m;
the thickness of the luminescent layer in the step 3) is 30-50 mu m;
the thickness of the back electrode layer in the step 4) is 30-50 mu m.
3. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 2, characterized in that in said step 3):
the filler is barium titanate, ceramic filler or carbon filler;
the ceramic filler is lead zirconate titanate,
the carbon-based filler is carbon black.
4. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 3, characterized in that the substrate in step 1) is a polyethylene terephthalate film.
5. The method for preparing an electroluminescent device based on aqueous polyurethane-silver nanowires according to any one of claims 1 to 4, characterized in that:
the step 1) is as follows:
printing a film on the surface of the polyethylene terephthalate film by a slit coating method, and drying to form a transparent electrode layer;
the step 2) is as follows:
dripping aqueous polyurethane on the surface of the transparent electrode layer, spin-coating to form a film, and drying to form a dielectric layer;
the step 3) is as follows:
dripping the mixed slurry of the luminescent layer on the surface of the dielectric layer, spin-coating to form a film, and drying to form the luminescent layer;
the step 4) is as follows:
and 3) placing the product obtained in the step 3) on a screen printing sample stage, printing silver paste electrodes on the light-emitting layer in a screen printing mode, and drying to form a back electrode layer.
6. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 5, characterized in that in step 1):
the solvent of the silver nanowire dispersion liquid is at least one of water, ethanol and isopropanol;
the slit coating method has the ink injection speed of 1.5mL/min, the coating speed of 5mm/s, the drying temperature of 45 ℃ and the time of 10+/-2 min.
7. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 5, characterized in that in step 2):
spin coating rotation speed is 1000rpm, spin coating time is 20s;
the drying temperature is 60 ℃ and the drying time is 30min.
8. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 5, characterized in that in the step 3):
spin coating rotation speed is 1000rpm, spin coating time is 20s;
the drying temperature is 60 ℃ and the drying time is 30min.
9. The method for manufacturing an electroluminescent device based on aqueous polyurethane-silver nanowires according to claim 5, characterized in that:
in the step 4): the screen plate adopted in the screen printing is 100-400 meshes;
the solid content of the aqueous polyurethane is 30% -40%, and the cloth viscosity is less than 200cps.
10. An electroluminescent device based on aqueous polyurethane-silver nanowires prepared by the method according to any one of claims 1 to 9.
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| CN119754046A (en) * | 2024-12-12 | 2025-04-04 | 苏州大学 | Polyurethane synthetic leather capable of electroluminescent display and preparation method thereof |
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