CN117939971A - Film, preparation method thereof, photoelectric device and display device - Google Patents
Film, preparation method thereof, photoelectric device and display device Download PDFInfo
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- CN117939971A CN117939971A CN202211261950.0A CN202211261950A CN117939971A CN 117939971 A CN117939971 A CN 117939971A CN 202211261950 A CN202211261950 A CN 202211261950A CN 117939971 A CN117939971 A CN 117939971A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000012298 atmosphere Substances 0.000 claims abstract description 120
- 239000002904 solvent Substances 0.000 claims abstract description 94
- 239000010954 inorganic particle Substances 0.000 claims abstract description 79
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000001301 oxygen Substances 0.000 claims abstract description 30
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 30
- 239000010410 layer Substances 0.000 claims description 160
- 239000000463 material Substances 0.000 claims description 55
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 52
- 238000001035 drying Methods 0.000 claims description 45
- 239000002096 quantum dot Substances 0.000 claims description 41
- 230000005693 optoelectronics Effects 0.000 claims description 38
- 239000002346 layers by function Substances 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 32
- 239000000758 substrate Substances 0.000 claims description 27
- 239000011787 zinc oxide Substances 0.000 claims description 26
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 24
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
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- JSGVZVOGOQILFM-UHFFFAOYSA-N 3-methoxy-1-butanol Chemical compound COC(C)CCO JSGVZVOGOQILFM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 239000011258 core-shell material Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910004613 CdTe Inorganic materials 0.000 claims description 6
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- -1 biaryl anthracene derivative Chemical class 0.000 claims description 5
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 4
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 claims description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 3
- FWXNJWAXBVMBGL-UHFFFAOYSA-N 9-n,9-n,10-n,10-n-tetrakis(4-methylphenyl)anthracene-9,10-diamine Chemical compound C1=CC(C)=CC=C1N(C=1C2=CC=CC=C2C(N(C=2C=CC(C)=CC=2)C=2C=CC(C)=CC=2)=C2C=CC=CC2=1)C1=CC=C(C)C=C1 FWXNJWAXBVMBGL-UHFFFAOYSA-N 0.000 claims description 3
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- 229910005540 GaP Inorganic materials 0.000 claims description 3
- PJANXHGTPQOBST-VAWYXSNFSA-N Stilbene Natural products C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 claims description 3
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- 239000005083 Zinc sulfide Substances 0.000 claims description 3
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 3
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- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 3
- 150000002220 fluorenes Chemical class 0.000 claims description 3
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 3
- HZXMRANICFIONG-UHFFFAOYSA-N gallium phosphide Chemical compound [Ga]#P HZXMRANICFIONG-UHFFFAOYSA-N 0.000 claims description 3
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- 238000002156 mixing Methods 0.000 claims description 3
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- GGROONUBGIWGGS-UHFFFAOYSA-N oxygen(2-);zirconium(4+);hydrate Chemical compound O.[O-2].[O-2].[Zr+4] GGROONUBGIWGGS-UHFFFAOYSA-N 0.000 claims description 3
- 150000003220 pyrenes Chemical class 0.000 claims description 3
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- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 claims description 3
- 235000021286 stilbenes Nutrition 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims 1
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- Electroluminescent Light Sources (AREA)
Abstract
The application discloses a film, a preparation method thereof, a photoelectric device and a display device. According to the preparation method of the film, the first film layer is treated by using the first atmosphere, and oxygen (O 2), water vapor (H 2 O) and alcohol vapor contained in the first atmosphere interact with the surfaces of the inorganic particles to block chemical connection between the first solvent and the surfaces of the inorganic particles, so that the first solvent is prevented from affecting the surface state of the inorganic particles and the performance of the inorganic particles, the first solvent is prevented from blocking the injection and transmission of electrons, the first solvent is prevented from negatively affecting the electron transmission performance of the film, and the removal of the first solvent in the first film layer is promoted, so that the residual of the solvent in the film is reduced.
Description
Technical Field
The application relates to the technical field of display, in particular to a film, a preparation method thereof, a photoelectric device and a display device.
Background
Optoelectronic devices such as organic electroluminescent devices (OLEDs) and quantum dot electroluminescent devices (QLEDs) are becoming increasingly popular for use and interest. The OLED, QLED and other structures mainly comprise an anode, a hole functional layer, a light emitting layer, an electron functional layer and a cathode. The material of the electronic functional layer is usually an inorganic nano material, such as zinc oxide nano particles, which has the advantages of more matching with the material energy level structure of the light-emitting layer, easy design and control of material synthesis, high electron transmission property and the like.
The solution film formation is widely used for preparing film layers such as electronic functional layers due to the advantages of easy patterning, easy operation, mass production, compatibility with flexibility, panel display and the like. In the case of film formation using the solution method, the nanoparticles are dispersed using a solvent, and then the solvent is removed to form a film. However, some solvents may be difficult to completely remove, such as solvents of ink used in inkjet printing, may partially remain in the electronic functional layer, affect injection and transmission of electrons, negatively affect electron transmission performance of the electronic functional layer, and reduce light emitting efficiency and service life of the optoelectronic device.
Disclosure of Invention
In view of the above, the present application provides a thin film, a method for preparing the same, an optoelectronic device and a display device, and aims to improve solvent residue in an electronic functional layer.
The embodiment of the application is realized in such a way that a preparation method of a film is provided, which comprises the following steps: providing a first film layer, wherein the first film layer comprises inorganic particles and a first solvent combined on the surfaces of the inorganic particles; treating the first film layer by using a first atmosphere to obtain a film; wherein the first atmosphere comprises oxygen, water vapor and alcohol vapor.
Optionally, in some embodiments of the present application, the alcohol vapor is selected from at least one of ethanol vapor, n-propanol vapor, isopropanol vapor, n-butanol vapor, tert-butanol vapor; and/or in the first atmosphere, the humidity range is 20% -60%; and/or the ratio of the vapor pressure of water to the vapor pressure of alcohol in the first atmosphere is 1:6-1:2; and/or the partial pressure of oxygen in the first atmosphere is 20% or more.
Optionally, in some embodiments of the present application, the time for treating the first film layer with the first atmosphere is 5 to 30 minutes; and/or the temperature of the first film layer treated by the first atmosphere is 40-80 ℃.
Optionally, in some embodiments of the application, the inorganic particles are selected from doped inorganic oxide particles or undoped inorganic nano-oxide particles selected from one or more of zinc oxide, titanium dioxide, tin dioxide, aluminum oxide, calcium oxide, silicon dioxide, gallium oxide, zirconium oxide, nickel oxide, zirconium trioxide, zinc sulfide, zinc selenide, cadmium sulfide, indium phosphide, gallium phosphide; the doped inorganic nano-oxide particles comprise the undoped inorganic nano-oxide particles and a doping element, wherein the doping element is selected from one or more of Mg, ca, li, ga, al, co, mn, in; and/or the inorganic particles are nano particles with a core-shell structure; and/or the first solvent is selected from one or more of ethylene glycol, diethylene glycol, polyethylene glycol, ethylene glycol monobutyl ether, methoxybutanol, dipropylene glycol and glycerol.
Optionally, in some embodiments of the present application, after the treating the first film layer with the first atmosphere, the method further includes: drying, wherein the pressure of the drying is less than or equal to 0.01Pa; and/or the drying temperature is 40-80 ℃; and/or said treating said first film layer with a first atmosphere and said drying thereafter is repeated at least twice.
Optionally, in some embodiments of the present application, after the treating the first film layer with the first atmosphere, the method further includes: treating the first film layer by using a second atmosphere to obtain the film; wherein the second atmosphere comprises oxygen and alcohol vapor.
Optionally, in some embodiments of the application, in the second atmosphere, the vapor pressure of the alcohol vapor is less than or equal to 8KPa; and/or the partial pressure of oxygen in the second atmosphere is 20% or more.
Optionally, in some embodiments of the present application, after the treating the first film layer with the second atmosphere, the method further includes: drying, wherein the pressure of the drying is less than or equal to 0.01Pa; and/or the drying temperature is 40-80 ℃; and/or said treating said first film layer with a second atmosphere and said drying thereafter is repeated at least twice.
Optionally, in some embodiments of the present application, the providing a first film layer includes: providing inorganic particles and a second solvent, and mixing to obtain an inorganic particle solution; providing a substrate, arranging the inorganic particle solution on the substrate, and drying to form the first film layer, wherein the second solvent comprises the first solvent.
Optionally, in some embodiments of the present application, the second solvent is selected from one or more of ethylene glycol, diethylene glycol, polyethylene glycol, ethylene glycol monobutyl ether, methoxybutanol, dipropylene glycol, glycerol; and/or the concentration of the inorganic particle solution is 10-80 mg/mL; and/or the average particle diameter of the inorganic particles is 2-8 nm; and/or the drying pressure is 0.001 to 10Pa.
Correspondingly, the embodiment of the application also provides a film, which is prepared by the preparation method of the film.
Correspondingly, the embodiment of the application also provides an optoelectronic device, which comprises a laminated anode, a luminescent layer, an electronic functional layer and a cathode; the electronic functional layer is prepared by the preparation method of the film, or the electronic functional layer is the film.
Alternatively, in some embodiments of the application, the anode and the cathode are independently selected from a metal electrode, a carbon electrode, a doped or undoped metal oxide electrode, and a composite electrode; wherein the material of the metal electrode is at least one selected from Al, ag, cu, mo, au, ba, ca and Mg; the material of the carbon electrode is at least one selected from graphite, carbon nano tube, graphene and carbon fiber; the material of the doped or undoped metal oxide electrode is at least one selected from ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO; the material of the composite electrode is at least one selected from AZO/Ag/AZO、AZO/Al/AZO、ITO/Ag/ITO、ITO/Al/ITO、ZnO/Ag/ZnO、ZnO/Al/ZnO、TiO2/Ag/TiO2、TiO2/Al/TiO2、ZnS/Ag/ZnS and ZnS/Al/ZnS; and/or the material of the light emitting layer is an organic light emitting material or a quantum dot light emitting material, the organic light emitting material is selected from at least one of a biaryl anthracene derivative, a stilbene aromatic derivative, a pyrene derivative or a fluorene derivative, a blue light emitting TBPe fluorescent material, a green light emitting TTPA fluorescent material, an orange light emitting TBRb fluorescent material and a red light emitting DBP fluorescent material, the quantum dot light emitting material is selected from at least one of a single structure quantum dot and a core-shell structure quantum dot, the single structure quantum dot is selected from at least one of a group II-VI compound, a group III-V compound, a group IV-VI compound and a group I-III-VI compound, the group II-VI compound is selected from at least one of CdSe、CdS、CdTe、ZnSe、ZnS、CdTe、ZnTe、CdZnS、CdZnSe、CdZnTe、ZnSeS、ZnSeTe、ZnTeS、ZnSeSTe、CdSeS、CdSeTe、CdTeS、CdZnSeS、CdZnSeTe、CdSeSTe、CdZnSeSTe and CdZnSTe, the group III-VI compound is selected from at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, the group IV-VI compound is selected from at least one of PbS, pbSe, pbTe, pbSeS, pbSeTe, pbSTe, the group I-III-VI compound is selected from at least one of a group of a cums 3 and an AgInS 56, the core-35, the quantum dot is selected from at least one of a group of a quantum dot and a quantum dot is selected from a group of 35.
Correspondingly, the embodiment of the application also provides a display device which comprises the photoelectric device.
According to the preparation method of the film, the first film layer is treated by using the first atmosphere, and oxygen, water vapor and alcohol vapor contained in the first atmosphere interact with the surfaces of the inorganic particles to block chemical connection between the first solvent and the surfaces of the inorganic particles, so that the first solvent is prevented from affecting the surface state and performance of the inorganic particles, the first solvent is prevented from blocking electron injection and electron transmission, and the first solvent is prevented from negatively affecting the electron transmission performance of the film. In addition, active oxygen and a hydroxyl ligand are introduced to the surface of the inorganic particles through the treatment of the first atmosphere, so that the surface defects of the inorganic particles are passivated, the electron transmission performance of the film is enhanced, and the luminous efficiency of the photoelectric device is improved. And the treatment of the first atmosphere can promote the removal of the first solvent in the first film layer, thereby reducing the residual solvent in the film and prolonging the service life of the device.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of an embodiment of a method for preparing a thin film according to the present application;
FIG. 2 is a schematic structural diagram of an embodiment of an optoelectronic device according to the present application;
FIG. 3 is a J-V plot of the electrical properties of a Quantum dot light emitting diode device;
fig. 4 is a c.e. -L curve of the corresponding electrical properties of the qd led.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application based on the embodiments of the present application. Furthermore, it should be understood that the detailed description is presented herein for purposes of illustration and description only, and is not intended to limit the application. In the present application, unless otherwise specified, terms such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present application, the term "comprising" means "including but not limited to". Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1to 6 has specifically disclosed sub-ranges, such as from 1to 3, from 1to 4, from 1to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1,2,3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
The solvent used in the solvent method may be a solvent having a relatively high boiling point (150 ℃ C. Or higher). For example, the boiling point of the solvent used in ink-jet printing cannot be too low, otherwise ink-jet abnormality and patterning abnormality can be caused by blockage of the nozzle due to the easy volatilization of the solvent. However, the solvent with a higher boiling point is difficult to completely remove through common physical low-pressure treatment, annealing temperature treatment and the like, part of the solvent can remain in the electronic functional layer, and chemical connection, such as coordination connection, can be formed between the surface of the inorganic nano material such as zinc oxide nano particles and the surface of the inorganic nano material, so that the surface state and performance of the inorganic nano material such as the zinc oxide nano particles are influenced, the injection and transmission of electrons are hindered, and the electron transmission performance of the electronic functional layer is negatively influenced, so that the performance of the photoelectric device is influenced. In addition, the injection of electrons is reduced, which leads to excessive injection of holes, and thus, the material of the light emitting layer (such as a quantum dot material) is oxidized, and thus, the light emitting performance is drastically reduced. And when the material of the hole functional layer is an organic material, excessive holes can cause oxidation and denaturation of the organic material, so that the hole injection and transmission performances of the hole functional layer are affected, and the performances of the photoelectric device are also affected.
Based on the above, the application provides a film, a preparation method thereof, an optoelectronic device and a display device, so as to solve the problem that solvent residues have negative effects on electron injection and electron transmission. In particular as follows.
Referring to fig. 1, fig. 1 is a schematic flow chart of an embodiment of a method for preparing a thin film according to the present application, where the method includes the following steps:
Step S11: providing a first film layer, wherein the first film layer comprises inorganic particles and a first solvent combined on the surfaces of the inorganic particles;
Step S12: treating the first film layer by using a first atmosphere to obtain a film; wherein the first atmosphere comprises oxygen, water vapor and alcohol vapor.
In the preparation of the first film layer, after the solvent is removed by drying or the like, some solvent may exist between the inorganic particles or chemical bonds (e.g., chemical bond bonds, coordinate bond bonds, van der Waals bond, etc.) may exist on the surfaces of the inorganic particles, which cannot be removed by physical means such as drying, and remain in the first film layer. According to the application, the first film layer is treated by using the first atmosphere, and oxygen, water vapor and alcohol vapor contained in the first atmosphere interact with the surfaces of the inorganic particles to block chemical connection between the first solvent and the surfaces of the inorganic particles, so that the first solvent is prevented from affecting the surface state of the inorganic particles and the performance of the inorganic particles, the first solvent is prevented from blocking electron injection and electron transmission, and the first solvent is prevented from negatively affecting the electron transmission performance of the film. In addition, active oxygen and a hydroxyl ligand are introduced to the surface of the inorganic particles through the treatment of the first atmosphere, so that the surface defects of the inorganic particles are passivated, and the electron transport performance of the film is enhanced. And the treatment of the first atmosphere can promote the removal of the first solvent in the first film layer, thereby reducing the residual solvent in the film.
In the step S11:
The inorganic particles are selected from doped or undoped inorganic particles, and the undoped inorganic particles are selected from one or more of zinc oxide, titanium dioxide, tin dioxide, aluminum oxide, calcium oxide, silicon dioxide, gallium oxide, zirconium oxide, nickel oxide, zirconium trioxide, zinc sulfide, zinc selenide, cadmium sulfide, indium phosphide and gallium phosphide; the doped inorganic particles include the undoped inorganic particles and a doping element selected from one or more of Mg, ca, li, ga, al, co, mn, in.
In one embodiment, the inorganic particles may also be core-shell structures.
The average particle diameter of the inorganic particles is 2 to 8nm, specifically, the average particle diameter of the inorganic particles may be 2～7nm、2～6nm、2～5nm、2～4nm、2～3nm、3～8nm、3～7nm、3～6nm、3～5nm、3～4nm、4～8nm、4～7nm、4～6nm、4～5nm、5～8nm、5～7nm、5～6nm、6～8nm、6～7nm、7～8nm or the like.
The first solvent is selected from solvents with boiling points of 150 ℃ or higher. Further, the first solvent is selected from solvents having a boiling point of 150-250 ℃. Specifically, the first solvent may be one or more selected from ethylene glycol, diethylene glycol, polyethylene glycol, ethylene glycol monobutyl ether, methoxybutanol, dipropylene glycol, and glycerol. The boiling point of the first solvent is higher, and the first solvent still remains in the first film layer and is easily combined on the surfaces of the inorganic particles, so that the surface state of the inorganic particles and the performance of the inorganic particles are affected. According to the application, the first film layer is treated by using the first atmosphere, and oxygen, water vapor and alcohol vapor contained in the first atmosphere interact with the surfaces of the inorganic particles to block chemical connection between the first solvent with a higher boiling point and the surfaces of the inorganic particles, so that the residue of the first solvent is reduced, and the electron injection and transmission performance of the film is improved.
It is understood that the first film layer is a solid film, and may be a solid film layer, which is formed by drying a liquid film or removing a solvent, and is mainly made of the inorganic particles, with respect to the liquid film or the liquid film.
In the step S12:
The alcohol vapor is at least one selected from ethanol vapor, n-propanol vapor, isopropanol vapor, n-butanol vapor and tert-butanol vapor.
In the first atmosphere, the humidity range is 20% -60%. It will be appreciated that the humidity here is the relative humidity, in particular the ratio of the actual water vapour pressure in the first atmosphere to the saturated water vapour pressure at the prevailing air temperature, expressed as a percentage. This humidity range may provide sufficient water vapor to act on the first film layer along with oxygen and alcohol vapors in the first atmosphere.
In the first atmosphere, the ratio of the vapor pressure of water to the vapor pressure of alcohol is any ratio of 1:6 to 1:2, specifically, the ratio of the vapor pressure of water to the vapor pressure of alcohol may be any ratio of 1:6 to 1:3, 1:5 to 1:4, 1:3 to 1:2, 1:5 to 1:2. The range of the ratio of the vapor pressure to the alcohol vapor pressure can provide enough vapor and alcohol vapor to interact with the surfaces of the inorganic particles to block the chemical connection between the first solvent and the surfaces of the inorganic particles, thereby avoiding the first solvent from affecting the surface state of the inorganic particles and the performance of the inorganic particles and avoiding the first solvent from obstructing the injection and transmission of electrons.
The partial pressure of oxygen in the first atmosphere is 20% or more, specifically, the partial pressure of oxygen may be 20 to 30%, 30 to 40%, 40 to 50%, or the like.
In one embodiment, the first atmosphere contains only oxygen, water vapor and alcohol vapor. In other embodiments, the first atmosphere may further include an inert gas such as nitrogen or helium. In one embodiment, the first atmosphere may be obtained by controlling humidity and alcohol vapor in air, wherein the air contains about 78% (volume fraction) nitrogen and about 21% (volume fraction) oxygen.
In an embodiment, the processing the first film layer with the first atmosphere may specifically be: and placing the first film layer in the first atmosphere for treatment. Specifically, the method comprises the following steps: placing the first film layer in an inert environment or a vacuum environment, injecting oxygen, water vapor and alcohol vapor into the inert environment or the vacuum environment to form the first atmosphere, and treating the first film layer by using the first atmosphere. The oxygen gas, the water vapor, and the alcohol vapor may be injected separately or may be mixed and then injected, and are not limited thereto.
The first film layer is treated with the first atmosphere for 5 to 30 minutes, such as 5 to 10 minutes, 5 to 25 minutes, 10 to 20 minutes, 15 to 25 minutes, 20 to 30 minutes, 25 to 30 minutes, and the like.
Further, in an embodiment, the temperature of the first film layer treated with the first atmosphere is 40 to 80 ℃. Specifically, the temperature may be 40 to 70 ℃, 40 to 50 ℃, 40 to 60 ℃, 40 to 70 ℃, 50 to 60 ℃, 50 to 80 ℃,60 to 80 ℃, 70 to 80 ℃, or the like. The temperature range can improve the reactivity and the treatment effect of oxygen, water vapor and alcohol vapor in the first atmosphere on the first film layer. Accordingly, in the subsequent step S13, the first film layer may be dried while maintaining the temperature range. In other words, the temperature range of the drying treatment in step S13 may be 40 to 80 ℃.
After the first film layer is treated by using the first atmosphere, the method further comprises: and (5) drying.
The drying may be performed at a low pressure, and the pressure range of the low pressure drying may be 0.01Pa or less, specifically 0.005 to 0.01Pa, 0.001 to 0.005Pa, or the like. The drying time is 10min or more, specifically 10-30 min, 30-60 min, etc. Specifically, the low-pressure drying may be performed at room temperature or at a temperature of 40 to 80 ℃. The low-pressure drying is carried out at the temperature of 40-80 ℃, so that the solvent removal can be quickened, and the residual solvent can be removed more thoroughly.
In one embodiment, the treating the first film layer with the first atmosphere and the drying may be repeated a plurality of times. I.e. after said drying, the first film layer is then subjected to a treatment in a first atmosphere and said drying is performed again, and so on. And (3) performing treatment on the first film layer by using the first atmosphere, and performing repeated treatment and drying as a repeated unit for two times or more, and performing deeper activation on the first film layer to perform more complete and thorough treatment on the first film layer so as to obtain the film.
In a specific embodiment, the treatment and the drying of the first film layer with the first atmosphere may be repeated 3-8 times, so that the first film layer may be sufficiently treated, and the difficulty of preparation and processing may be increased while avoiding excessive repetition.
In an embodiment, after the first film layer is treated with the first atmosphere, the method further includes treating the first film layer with a second atmosphere to obtain the film.
The second atmosphere is a dry air atmosphere, and the second atmosphere comprises dry air and alcohol vapor. The dry air does not contain water vapor and contains oxygen. Therefore, the second atmosphere contains oxygen and alcohol vapor, and does not contain water vapor.
In a specific embodiment, the second atmosphere may be obtained by drying the first atmosphere to remove moisture and water vapor. In other embodiments, the second atmosphere may be formed directly from dry air and the alcohol vapor.
In a specific embodiment, in the second atmosphere, the vapor pressure of the alcohol is less than or equal to 8KPa. At this time, the vapor pressure of ethanol is the vapor pressure corresponding to one atmosphere (101.3 KPa) at 26 ℃.
The partial pressure of oxygen in the second atmosphere is 20% or more, specifically, the partial pressure of oxygen may be 20 to 30%, 30 to 40%, 40 to 50%, or the like.
In this embodiment, after the first film layer is treated by using the first atmosphere, the first film layer is treated by using the second atmosphere without water vapor, so as to avoid that the water vapor is treated for multiple times, and the energy level of the zinc oxide particles is affected, so that the electrical properties of the zinc oxide particles are affected, and thus the electrical properties of the thin film formed by the preparation are affected.
After the first film layer is treated with the first atmosphere containing water vapor in step S12, that is, after the first atmosphere blocks chemical connection between the first solvent and the surface of the inorganic particles and removes the first solvent, the first film layer is treated with the second atmosphere without water vapor in this step, so that the residue of the first solvent in the thin film is reduced as much as possible, and the water vapor is prevented from being treated for multiple times, which affects the energy level, the electrical property, and the like of the inorganic particles, thereby affecting the electrical property, and the like of the thin film formed by the preparation. In addition, the first film layer is treated through the second atmosphere, so that excessive water molecules in the film are avoided. When the film is used as a functional layer of the photoelectric device, corrosion of other film layers in the photoelectric device caused by water molecules contained in the film, such as corrosion of electrodes when the photoelectric device is electrified, is avoided, and performance of the photoelectric device is attenuated.
Further, in an embodiment, the drying is further included after the treating the first film layer with the second atmosphere.
The drying may be performed at a low pressure, and the pressure range of the low pressure drying may be 0.01Pa or less, specifically 0.005 to 0.01Pa, 0.001 to 0.005Pa, or the like. The drying time is 10min or more, specifically 10-30 min, 30-60 min, etc. Specifically, the low-pressure drying may be performed at room temperature or at a temperature of 40 to 80 ℃.
Further, the treatment of the first film layer using the second atmosphere and the subsequent drying may be repeated a plurality of times, specifically, 2 to 3 times, 3 to 8 times, or the like. The first film layer is treated by the second atmosphere and then dried as a repeating unit for two times or more, so that the first film layer is more fully and thoroughly treated, and the difficulty of preparation and processing can be avoided from being increased by too much repetition.
In one embodiment, the providing a first film layer specifically includes the following steps:
step S21: providing inorganic particles and a second solvent, and mixing to obtain an inorganic particle solution;
Step S22: providing a substrate, arranging the inorganic particle solution on the substrate, and drying to form the first film layer, wherein the second solvent at least comprises the first solvent.
It is understood that the first solvent is a solvent that remains in the first film layer after the inorganic particle solution is dried and the solvent is removed. Thus, the source of the first solvent is the second solvent. The second solvent contains at least the first solvent, in other words, the second solvent may also contain other solvents than the first solvent.
It is understood that the first solvent may be a single solvent or a mixed solvent of a plurality of solvents, and the second solvent may be a single solvent or a mixed solvent of a plurality of solvents.
In an embodiment, the second solvent is selected from one or more of ethylene glycol, diethylene glycol, polyethylene glycol, ethylene glycol monobutyl ether, methoxybutanol, dipropylene glycol, glycerol. For example, the second solvent is a mixed solvent of ethylene glycol monobutyl ether and methoxybutanol.
The inorganic particle solution may be a dispersion of the inorganic particles or a colloidal solution of the inorganic particles. The concentration of the inorganic particle solution is 10-80 mg/mL, specifically 10-70 mg/mL, 20-60 mg/mL, 30-50 mg/mL, 40-50 mg/mL, etc. This concentration can uniformly disperse the zinc oxide particles and can uniformly spread out on the substrate.
In the step S22:
The inorganic particle solution is disposed on the substrate, and may be disposed specifically by a solution method. The solution method may be spin coating, printing, inkjet printing, knife coating, printing, dip-coating, dipping, spraying, roll coating, casting, slit coating, bar coating, or the like.
In a specific embodiment, the inorganic particle solution is a zinc oxide particle solution, and the zinc oxide particle solution is used as ink, and the ink is printed on the substrate by an inkjet printing method. The second solvent in the zinc oxide particle solution has a higher boiling point, so that zinc oxide particles can be fully dispersed, and the phenomenon that ink jet abnormality and patterning abnormality (namely printed pattern abnormality) are caused by blockage of a spray head of the ink jet printing equipment due to volatilization of the solvent is avoided.
The drying pressure is in the range of 0.001-10 Pa for 10-30 min to remove the second solvent in the inorganic particle solution as much as possible.
The application provides a film, which is prepared by the preparation method of the film.
Referring to fig. 2, fig. 2 is a schematic structural diagram of an embodiment of an optoelectronic device according to the present application. The application also provides an optoelectronic device 100, which comprises a laminated anode 10, a luminescent layer 20, an electronic functional layer 30 and a cathode 40, wherein the electronic functional layer 30 is the thin film or is prepared by the preparation method of the thin film.
After the electronic functional layer 30 in the optoelectronic device 100 is treated in the first atmosphere, active oxygen and a hydroxyl ligand are introduced to the surface of the inorganic particles, so that the surface defects of the inorganic particles are passivated, the electron transmission performance of the electronic functional layer 30 is enhanced, and a forward aging passivation reaction can occur with the cathode 40, so that the performance of the optoelectronic device 100 is further improved.
Wherein, in one embodiment, the anode 10 and the cathode 40 are independently selected from a metal electrode, a carbon electrode, a doped or undoped metal oxide electrode, and a composite electrode; wherein the material of the metal electrode is at least one selected from Al, ag, cu, mo, au, ba, ca and Mg; the material of the carbon electrode is at least one selected from graphite, carbon nano tube, graphene and carbon fiber; the material of the doped or undoped metal oxide electrode is at least one selected from ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO; the material of the composite electrode is at least one selected from AZO/Ag/AZO、AZO/Al/AZO、ITO/Ag/ITO、ITO/Al/ITO、ZnO/Ag/ZnO、ZnO/Al/ZnO、TiO2/Ag/TiO2、TiO2/Al/TiO2、ZnS/Ag/ZnS and ZnS/Al/ZnS. Wherein "/" represents a laminated structure, for example, the composite electrode AZO/Ag/AZO represents an electrode of a composite structure in which AZO layers, ag layers, and AZO layers are laminated in three layers.
In an embodiment, the material of the light-emitting layer 20 is an organic light-emitting material or a quantum dot light-emitting material, the organic light-emitting material is at least one selected from a biaryl anthracene derivative, a stilbene aromatic derivative, a pyrene derivative or a fluorene derivative, a blue light-emitting TBPe fluorescent material, a green light-emitting TTPA fluorescent material, an orange light-emitting TBRb fluorescent material and a red light-emitting DBP fluorescent material, the quantum dot light-emitting material is at least one selected from a single-structure quantum dot and a core-shell structure quantum dot, the single-structure quantum dot is at least one selected from a II-VI compound, a III-V compound, a IV-VI compound and a I-III-VI compound, the II-VI compound is at least one selected from CdSe、CdS、CdTe、ZnSe、ZnS、CdTe、ZnTe、CdZnS、CdZnSe、CdZnTe、ZnSeS、ZnSeTe、ZnTeS、ZnSeSTe、CdSeS、CdSeTe、CdTeS、CdZnSeS、CdZnSeTe、CdSeSTe、CdZnSeSTe and CdZnSTe, the III-V compound is at least one selected from InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, the IV-VI compound is at least one selected from PbS, pbSe, pbTe, pbSeS, pbSeTe, pbSTe, the I-III-VI compound is at least one selected from a cus core and a cus core-858 3, the quantum dot is at least one selected from a quantum-shell structure quantum dot is at least one selected from a quantum-35.
It will be appreciated that when the material of the light emitting layer 20 is an organic light emitting material, the optoelectronic device 100 is an organic electroluminescent device. When the material of the light emitting layer 20 is a quantum dot light emitting material, the optoelectronic device 100 is a quantum dot electroluminescent device.
In an embodiment, the optoelectronic device 100 further comprises a hole-function layer 50, wherein the hole-function layer 50 is disposed between the anode 10 and the light-emitting layer 20. When the hole function layer 50 includes two layers, a hole injection layer and a hole transport layer, the hole injection layer is disposed near the anode 10 side, and the hole transport layer is disposed near the light emitting layer 20 side.
The hole transport layer is made of a material selected from the group consisting of poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (TFB), polyvinylcarbazole (PVK), poly (N, N '-bis (4-butylphenyl) -N, N' -bis (phenyl) benzidine) (poly-TPD), poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-Phenylenediamine) (PFB), 4',4 "-tris (carbazole-9-yl) triphenylamine (TCATA), 4' -bis (9-Carbazole) Biphenyl (CBP), N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine (TPD), N '-diphenyl-N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine (NPB), poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) (PEDOT); PSS), spiro-NPB, spiro-TPD, doped or undoped NiO, moO 3、WO3、V2O5, P-gallium nitride, crO 3、CuO、MoS2、MoSe2、WS3、WSe3, cuS, cuSCN.
The hole injection layer is made of a material with hole injection capability and is selected from one or more of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS), 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanoquinone-dimethane (F4-TCNQ), 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-Hexaazabenzophenanthrene (HATCN), copper phthalocyanine (CuPc), transition metal oxide and transition metal chalcogenide; wherein the transition metal oxide comprises one or more of NiO, moO 2、WO3 and CuO; the metal chalcogenide comprises one or more of MoS 2、MoSe2、WS3、WSe3 and CuS.
It will be appreciated that in addition to the above functional layers, functional layers conventionally used in optoelectronic devices, such as an electron blocking layer, an electron injection layer, a hole blocking layer, and/or an interface modification layer, may be added to the optoelectronic device 100.
It will be appreciated that the materials and thicknesses of the various layers of the optoelectronic device 100 may be correspondingly configured and adjusted depending on the lighting requirements of the optoelectronic device 100.
The optoelectronic device 100 further comprises a substrate (not shown). The substrate may be a rigid substrate or a flexible substrate. The rigid substrate can be ceramic material or various glass materials and the like. The flexible substrate may be a substrate formed of a material such as a polyimide film (PI) and its derivatives, polyethylene naphthalate (PEN), phosphoenolpyruvic acid (PEP), or diphenylene ether resin.
It is understood that the optoelectronic device 100 may be a front-up optoelectronic device or an inverted optoelectronic device. When the optoelectronic device 100 is a front-side optoelectronic device, the substrate is bonded to the side of the anode 10 remote from the light-emitting layer 20. When the optoelectronic device 100 is an inverted optoelectronic device, the substrate is bonded to the side of the cathode 40 remote from the light emitting layer 20.
It will be appreciated that in addition to the above functional layers, functional layers conventionally used in optoelectronic devices, such as an electron blocking layer, an electron injection layer, a hole blocking layer, and/or an interface modification layer, may be added to the optoelectronic device 100.
It will be appreciated that the materials and thicknesses of the various layers of the optoelectronic device 100 may be correspondingly configured and adjusted depending on the lighting requirements of the optoelectronic device 100.
The application also provides a preparation method of the photoelectric device. In one embodiment, a method of fabricating an optoelectronic device includes the steps of:
step S31: providing a cathode;
Step S32: forming an electron function layer on the cathode;
step S33: and forming a stacked light emitting layer and anode on the electronic functional layer.
The photovoltaic device prepared in this embodiment is an inverted photovoltaic device.
In another embodiment, a method of fabricating an optoelectronic device includes the steps of:
Step S41: providing a laminated anode and a light-emitting layer;
Step S42: forming an electron functional layer on the light emitting layer;
Step S43: a cathode is formed on the electronically functional layer.
The photovoltaic device prepared in this embodiment is a front-mounted photovoltaic device.
The electronic function layer is formed by the preparation method of the film.
It can be understood that, when the optoelectronic device further includes a hole function layer, the step S33 is: and forming a stacked light emitting layer, hole function layer and anode on the electron function layer. The step S41 is as follows: a laminated anode, an electron functional layer and a light-emitting layer are provided.
In the preparation method of the photoelectric device provided by the application, the preparation methods of the anode, the hole functional layer, the light-emitting layer and the cathode can be realized by adopting conventional technologies in the field, such as a chemical method or a physical method. Wherein, the chemical method comprises chemical vapor deposition, continuous ion layer adsorption and reaction, anodic oxidation, electrolytic deposition and coprecipitation. Physical methods include physical plating methods and solution methods, wherein the physical plating methods include: thermal evaporation plating, electron beam evaporation plating, magnetron sputtering, multi-arc ion plating, physical vapor deposition, atomic layer deposition, pulsed laser deposition, etc.; the solution method may be spin coating, printing, ink jet printing, knife coating, printing, dip-coating, dipping, spray coating, roll coating, casting, slit coating, bar coating, or the like.
It will be appreciated that where the optoelectronic device further comprises an electron injection layer, an electron blocking layer, a hole blocking layer, and/or an interface modification layer, both of the above-described methods of preparation further comprise the step of forming the corresponding layers described above using the chemical or physical methods described above.
The application also relates to a display device comprising the photoelectric device provided by the application. The display device may be any electronic product with a display function, including but not limited to a smart phone, a tablet computer, a notebook computer, a digital camera, a digital video camera, a smart wearable device, a smart weighing electronic scale, a vehicle-mounted display, a television set or an electronic book reader, wherein the smart wearable device may be, for example, a smart bracelet, a smart watch, a Virtual Reality (VR) helmet, etc.
The present application will now be described in more detail by way of the following examples, which are intended to be illustrative of the application and not limiting thereof.
Example 1
Step 1: the substrate plated with ITO was ultrasonically washed with acetone and ethanol for 15min, then washed with deionized water and then blow-dried, then dried on a heating plate at 150 ℃ for 10min, and then irradiated with Ultraviolet (UV) light for 20min to increase the work function of ITO.
Step 2: spin coating PEDOT: PSS (mass fraction 2.8%), spin-coating at 4000rpm for 30s, followed by heating on a hot plate at 150℃for 20min, yielded a hole injection layer with a thickness of 30 nm.
Step 3: TFB (concentration of 8 mg/mL) was spin-coated on the hole injection layer in an inert atmosphere at 3000rpm for 30s, followed by heating with a hot plate at 120℃for 20min to obtain a hole transport layer having a thickness of 20 nm.
Step 4: and spin-coating CdZnSe/ZnSe/ZnS/CdZnS/ZnS quantum dot solution (concentration of 20 mg/mL) on the hole-transporting layer, rotating at 3000rpm for 30s, and heating on a heating plate at 80 ℃ for 5min to obtain a luminescent layer with a thickness of 40 nm.
Step 5: spin-coating ZnO solution (the concentration is 30mg/mL, the solvent is ethylene glycol monobutyl ether and methoxybutanol mixed in a volume ratio of 7:3) on the luminescent layer, rotating at 4000rpm for 30s, and then pumping for 20min at a low pressure of 0.01Pa to remove the solvent to obtain a first film layer;
Placing the substrate containing the first film layer in a first atmosphere for exposure treatment for 10min, and then pumping air for 15min under 0.0005Pa to obtain an electron transport layer with the thickness of 40 nm; wherein the first atmosphere is an air atmosphere, the humidity is 40%, and the ratio of the vapor pressure of water to the vapor pressure of ethanol is 1:4.
Step 6: al is evaporated on the electron-functional layer by thermal evaporation at a vacuum of not higher than 3X 10 -4 Pa at a rate of 1 angstrom/sec for 200s to obtain a cathode having a thickness of 20 nm.
Example 2
This embodiment is substantially the same as embodiment 1 except that: in step 5, the substrate containing the first film layer is placed in a first atmosphere for treatment and the air extraction process are carried out at 50 ℃.
Example 3
This embodiment is substantially the same as embodiment 1 except that: in step 5, the ratio of the vapor pressure of water to the vapor pressure of ethanol is 1:6.
Example 4
This embodiment is substantially the same as embodiment 1 except that: in step 5, the ratio of the vapor pressure of water to the vapor pressure of ethanol is 1:2.
Example 5
This embodiment is substantially the same as embodiment 1 except that: in step 5, the ratio of the vapor pressure of water to the vapor pressure of ethanol is 1:10.
Example 6
This embodiment is substantially the same as embodiment 1 except that: in step 5, the ratio of the vapor pressure of water to the vapor pressure of ethanol is 1:1.
Example 7
This embodiment is substantially the same as embodiment 1 except that: in step 5, the humidity in the first atmosphere was 60%, the exposure time was 5min, and then the air was evacuated at 0.005Pa for 10min.
Example 8
This embodiment is substantially the same as embodiment 1 except that: in the step 5, the humidity in the first atmosphere is 20%, and the exposure time is 10min; the substrate containing the first film layer was subjected to a first atmosphere treatment and a pumping process, both at 80 ℃.
Example 9
This embodiment is substantially the same as embodiment 2 except that: in step 5, the substrate containing the first film layer is placed in a first atmosphere to carry out exposure treatment and air extraction, and the steps are repeated for 6 times, so as to obtain the electron transport layer.
Example 10
This embodiment is substantially the same as embodiment 1 except that: in the step 5, after the substrate containing the first film layer is placed in a first atmosphere to be exposed and subjected to the air extraction step, the substrate containing the first film layer is placed in a second atmosphere to be exposed, wherein the second atmosphere contains oxygen and ethanol vapor, and the exposure time is 10min; then pumping air for 15min under the pressure of 0.0005 Pa; wherein the second atmosphere is obtained by drying the first atmosphere.
Example 11
This embodiment is substantially the same as embodiment 2 except that: in the step 5, after the step of exposing and exhausting the substrate containing the first film layer in the first atmosphere, the step of exposing and exhausting the substrate containing the first film layer in the second atmosphere is repeated for 5 times; wherein the second atmosphere contains oxygen and ethanol vapor, the exposure time is 10min, and the temperature is 50 ℃; the air extraction is 0.0005Pa and 15min at 50 ℃.
Example 12
This embodiment is substantially the same as embodiment 11 except that: in step 5, the n-butanol vapor contained in the first atmosphere is not ethanol vapor.
Example 13
This embodiment is substantially the same as embodiment 11 except that: in step 5, the mixed vapor of n-butanol vapor and ethanol vapor contained in the first atmosphere is in a ratio of 1:1.
Comparative example 1
This embodiment is substantially the same as embodiment 1 except that: in step 5, the first film layer is obtained without subsequent exposure treatment and air extraction treatment, and is directly used as an electron transport layer.
Experimental example 1
JVL data were obtained from the quantum dot light emitting diode test of examples 1, 2, 9, 11 and comparative example 1, and the electrical properties of the devices were determined as shown in fig. 3 and 4. Fig. 3 is a J-V curve (i.e., current density versus voltage curve) of the electrical properties of the qd led, and fig. 4 is a c.e. -L curve (i.e., current efficiency versus brightness curve) of the electrical properties of the qd led.
As can be seen from fig. 3, as the voltage increases, the current density of the qd-led of examples 1,2, 9, and 11 is greater than that of the qd-led of comparative example 1, indicating that the carrier injection and transport properties of the qd-led of examples 1,2, 9, and 11 are greater than that of comparative example 1. As can be seen from fig. 4, the quantum dot light emitting devices of examples 1,2, 9, and 11 all have higher current efficiency than that of comparative example 1, and it is shown that the quantum dot light emitting devices of examples 1,2, 9, and 11 have better light emitting efficiency and other properties than those of comparative example 1. As can be seen from fig. 3 and fig. 4, the electronic functional layer formed by the first atmosphere treatment of the present application can improve the carrier injection and transmission performance of the optoelectronic device, and improve the light emitting efficiency of the optoelectronic device.
Experimental example 2
The working life test was performed on the quantum dot light emitting diodes of examples 1 to 13 and comparative example 1, and the working life of each quantum dot light emitting diode piece was determined using constant current driving of 2mA, and the test results are referred to in table 1 below. Wherein L (cd/m 2) represents the highest luminance of the device; at a T95_1K (h) of 1000nit, the brightness was attenuated to 95% for the required time.
TABLE 1
As can be seen from table 1, the maximum brightness L and lifetime t95_1k of the qd leds of examples 1 to 13 are much greater than those of the qd led of comparative example 1. The electronic functional layer formed by the first atmosphere treatment can improve the carrier injection and transmission performance of the photoelectric device, and improve the luminous efficiency, the service life and other performances of the photoelectric device.
Compared with embodiment 1, the treatment in the first atmosphere and the air extraction process in the first film layer in embodiments 2 and 8 can be more favorable for removing the first solvent with a higher boiling point in a slightly heated environment (at 40-80 ℃), so that the carrier injection and transmission performance is further improved, and the performances such as the luminous efficiency and the service life of the photoelectric device are further improved.
Embodiments 1 to 6 can show that the ratio of the vapor pressure of water to the vapor pressure of ethanol in the first atmosphere is in the range of 1:6 to 1:2, and the formed quantum dot light emitting diode has better luminescence property and service life, and can provide enough vapor and alcohol vapor to interact with the surface of the inorganic particles together with oxygen, so that the chemical connection between the first solvent and the surface of the inorganic particles is blocked, the surface state of the inorganic particles and the performance of the inorganic particles are prevented from being influenced by the first solvent, the injection and transmission of electrons are prevented from being blocked by the first solvent, and the properties such as luminescence efficiency, service life and the like of the photoelectric device are improved.
Example 7 has a higher humidity, a relatively shorter exposure time, and a different pumping pressure than example 1, and has improved luminous performance and life.
Compared with embodiment 2, in embodiment 9, the first film layer is subjected to repeated first atmosphere and air extraction treatment, so that the light emitting performance and the service life of the quantum dot light emitting diode are improved to a certain extent, and the repeated first atmosphere and air extraction treatment is indicated, so that the first film layer can be activated more deeply, the first film layer can be treated more fully and thoroughly, and the first solvent is removed more thoroughly.
Compared with example 1, the first film layer of example 10 is added with a second atmosphere (without water vapor) and air extraction, so that the luminescence performance and lifetime of the quantum dot light-emitting diode are improved to some extent, and in this description, after the first film layer is treated with the first atmosphere containing water vapor, that is, after the first atmosphere blocks the chemical connection between the first solvent and the surface of the inorganic particles and removes the first solvent, the first film layer is treated with the second atmosphere without water vapor, so that the residue of the first solvent in the electron transport layer can be reduced as much as possible. And the first film layer is treated through the second atmosphere, so that excessive water molecules in the electron transmission layer are avoided, and the phenomenon that the water molecules in the electron transmission layer erode other film layers in the quantum dot light emitting diode to cause the attenuation of the performance of the quantum dot light emitting diode is avoided.
Compared with example 10, the second atmosphere treatment and the subsequent pumping treatment are repeated for 5 times in example 11, and the light emitting performance and the service life of the quantum dot light emitting diode are significantly improved, which means that the second atmosphere treatment and the subsequent pumping treatment are repeated to further reduce or even completely remove the residue of the first solvent in the electron transport layer.
The preparation method, the film, the photoelectric device and the display device of the thin film provided by the embodiment of the application are described in detail, and specific examples are applied to the description of the principle and the implementation mode of the application, and the description of the above examples is only used for helping to understand the method and the core idea of the application; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, the present description should not be construed as limiting the present application.
Claims (13)
1. A method of producing a film comprising:
Providing a first film layer, wherein the first film layer comprises inorganic particles and a first solvent combined on the surfaces of the inorganic particles;
Treating the first film layer by using a first atmosphere to obtain a film;
Wherein the first atmosphere comprises oxygen, water vapor and alcohol vapor.
2. The method of claim 1, wherein,
The alcohol vapor comprises at least one of ethanol vapor, n-propanol vapor, isopropanol vapor, n-butanol vapor and tert-butanol vapor; and/or
In the first atmosphere, the humidity range is 20% -60%; and/or
In the first atmosphere, the ratio of the vapor pressure of water to the vapor pressure of alcohols is 1:6-1:2; and/or
The partial pressure of oxygen in the first atmosphere is more than or equal to 20%; and/or
The first film layer is treated by using a first atmosphere for 5-30 min; and/or
The temperature of the first film layer treated by the first atmosphere is 40-80 ℃.
3. The method of claim 1, wherein,
The inorganic particles are selected from doped or undoped inorganic particles, and the undoped inorganic particles are selected from one or more of zinc oxide, titanium dioxide, tin dioxide, aluminum oxide, calcium oxide, silicon dioxide, gallium oxide, zirconium oxide, nickel oxide, zirconium trioxide, zinc sulfide, zinc selenide, cadmium sulfide, indium phosphide and gallium phosphide; the doped inorganic particles comprise the undoped inorganic particles and a doping element, wherein the doping element is selected from one or more of Mg, ca, li, ga, al, co, mn, in; and/or
The inorganic particles are of a core-shell structure; and/or
The first solvent is selected from one or more of ethylene glycol, diethylene glycol, polyethylene glycol, ethylene glycol monobutyl ether, methoxybutanol, dipropylene glycol and glycerol.
4. The method of manufacturing of claim 1, wherein after the treating the first film layer with the first atmosphere, further comprises: drying;
wherein the drying pressure is less than or equal to 0.01Pa; and/or
The drying temperature is 40-80 ℃; and/or
The treating the first film layer with a first atmosphere and the drying thereafter is repeated at least twice.
5. The method of manufacturing of claim 1, wherein after the treating the first film layer with the first atmosphere, further comprises:
Treating the first film layer by using a second atmosphere to obtain the film;
wherein the second atmosphere comprises oxygen and alcohol vapor.
6. The method according to claim 5, wherein,
In the second atmosphere, the vapor pressure of the alcohol vapor is less than or equal to 8KPa; and/or
And the oxygen partial pressure in the second atmosphere is more than or equal to 20 percent.
7. The method according to claim 5, wherein,
After the first film layer is treated by using the second atmosphere, the method further comprises: drying;
wherein the drying pressure is less than or equal to 0.01Pa; and/or
The drying temperature is 40-80 ℃; and/or
The treating the first film layer with a second atmosphere and the drying thereafter is repeated at least twice.
8. The method of manufacturing of claim 1, wherein providing the first film layer comprises:
providing inorganic particles and a second solvent, and mixing to obtain an inorganic particle solution;
Providing a substrate, arranging the inorganic particle solution on the substrate, and drying to form the first film layer.
9. The method of claim 8, wherein the second solvent is selected from one or more of ethylene glycol, diethylene glycol, polyethylene glycol, ethylene glycol monobutyl ether, methoxybutanol, dipropylene glycol, glycerol; and/or
The concentration of the inorganic particle solution is 10-80 mg/mL; and/or
The average particle diameter of the inorganic particles is 2-8 nm; and/or
The drying pressure is 0.001-10 Pa.
10. A film prepared by the method of any one of claims 1-9.
11. An optoelectronic device comprising a stacked anode, a light emitting layer, an electronic functional layer, and a cathode; wherein the electronic functional layer is prepared by the preparation method of the film according to any one of claims 1 to 9, or the electronic functional layer is the film according to claim 10.
12. The optoelectronic device of claim 11, wherein,
The anode and the cathode are independently selected from a metal electrode, a carbon electrode, a doped or undoped metal oxide electrode, and a composite electrode; wherein the material of the metal electrode is at least one selected from Al, ag, cu, mo, au, ba, ca and Mg; the material of the carbon electrode is at least one selected from graphite, carbon nano tube, graphene and carbon fiber; the material of the doped or undoped metal oxide electrode is at least one selected from ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO; the material of the composite electrode is at least one selected from AZO/Ag/AZO、AZO/Al/AZO、ITO/Ag/ITO、ITO/Al/ITO、ZnO/Ag/ZnO、ZnO/Al/ZnO、TiO2/Ag/TiO2、TiO2/Al/TiO2、ZnS/Ag/ZnS and ZnS/Al/ZnS; and/or
The material of the light emitting layer is an organic light emitting material or a quantum dot light emitting material, the organic light emitting material is selected from at least one of a biaryl anthracene derivative, a stilbene aromatic derivative, a pyrene derivative or a fluorene derivative, a blue light emitting TBPe fluorescent material, a green light emitting TTPA fluorescent material, an orange light emitting TBRb fluorescent material and a red light emitting DBP fluorescent material, the quantum dot light emitting material is selected from at least one of a single-structure quantum dot and a core-shell structure quantum dot, the single-structure quantum dot is selected from at least one of a II-VI compound, a III-V compound, a IV-VI compound and an I-III-VI compound, the II-VI compound is selected from at least one of CdSe、CdS、CdTe、ZnSe、ZnS、CdTe、ZnTe、CdZnS、CdZnSe、CdZnTe、ZnSeS、ZnSeTe、ZnTeS、ZnSeSTe、CdSeS、CdSeTe、CdTeS、CdZnSeS、CdZnSeTe、CdSeSTe、CdZnSeSTe and CdZnSTe, the III-V compound is selected from at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, the IV-VI compound is selected from at least one of PbS, pbSe, pbTe, pbSeS, pbSeTe, pbSTe, the I-III-VI compound is selected from at least one of an InS 2、CuInSe2 and an InS 2 core-shell structure quantum dot is selected from at least one of a quantum dot, and a quantum dot is selected from at least one of a quantum dot of a quantum-shell structure of a InS 3435.
13. A display device, characterized in that it comprises an optoelectronic device according to any one of claims 11-12.
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