CN109962150B - Packaging film, preparation method thereof and photoelectric device - Google Patents
Packaging film, preparation method thereof and photoelectric device Download PDFInfo
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- CN109962150B CN109962150B CN201711339298.9A CN201711339298A CN109962150B CN 109962150 B CN109962150 B CN 109962150B CN 201711339298 A CN201711339298 A CN 201711339298A CN 109962150 B CN109962150 B CN 109962150B
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- 229920006280 packaging film Polymers 0.000 title claims description 38
- 239000012785 packaging film Substances 0.000 title claims description 38
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000010408 film Substances 0.000 claims abstract description 238
- 239000000919 ceramic Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 36
- 238000005538 encapsulation Methods 0.000 claims abstract description 36
- 229920000642 polymer Polymers 0.000 claims abstract description 33
- 239000010409 thin film Substances 0.000 claims abstract description 22
- 239000012528 membrane Substances 0.000 claims abstract description 16
- 230000005693 optoelectronics Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 39
- 238000002156 mixing Methods 0.000 claims description 34
- 239000004626 polylactic acid Substances 0.000 claims description 32
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 17
- -1 polytetrafluoroethylene Polymers 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 15
- 239000000178 monomer Substances 0.000 claims description 15
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011787 zinc oxide Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 239000004310 lactic acid Substances 0.000 claims description 7
- 235000014655 lactic acid Nutrition 0.000 claims description 7
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 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
- 229920001155 polypropylene Polymers 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 3
- 230000004888 barrier function Effects 0.000 abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
- 239000001301 oxygen Substances 0.000 abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 17
- 230000035699 permeability Effects 0.000 abstract description 4
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 description 19
- 238000005266 casting Methods 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 12
- 229920006381 polylactic acid film Polymers 0.000 description 12
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 9
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 239000007795 chemical reaction product Substances 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 235000013842 nitrous oxide Nutrition 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 229920000144 PEDOT:PSS Polymers 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- FFXSNCCQTHARBR-UHFFFAOYSA-N dioxosilane ethanol Chemical compound C(C)O.[Si](=O)=O FFXSNCCQTHARBR-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002096 quantum dot Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- GSWAOPJLTADLTN-UHFFFAOYSA-N oxidanimine Chemical compound [O-][NH3+] GSWAOPJLTADLTN-UHFFFAOYSA-N 0.000 description 2
- 238000012536 packaging technology Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- INNSZZHSFSFSGS-UHFFFAOYSA-N acetic acid;titanium Chemical compound [Ti].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O INNSZZHSFSFSGS-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 229920006281 multilayer packaging film Polymers 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/80—Constructional details
- H10H20/85—Packages
- H10H20/852—Encapsulations
- H10H20/854—Encapsulations characterised by their material, e.g. epoxy or silicone resins
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/01—Manufacture or treatment
- H10H20/036—Manufacture or treatment of packages
- H10H20/0362—Manufacture or treatment of packages of encapsulations
Landscapes
- Wrappers (AREA)
- Laminated Bodies (AREA)
Abstract
本发明公开一种封装薄膜及其制备方法、光电器件，其中，所述封装薄膜包括层叠设置的第一有机薄膜、由聚合物和陶瓷材料组成的第一共混膜、由陶瓷材料组成的1‑4层陶瓷膜、由聚合物和陶瓷材料组成的第二共混膜、第二有机薄膜。本发明将第一有机薄膜和第二有机薄膜作为水汽阻隔层，将1‑4层致密的陶瓷膜作为氧气阻隔层，同时在所述陶瓷膜和有机薄膜之间设置由聚合物和陶瓷材料组成的共混层，所述共混层能有效提升有机薄膜和陶瓷膜之间的结合力，从而增强封装薄膜的水氧阻隔性能，进而满足光电器件对水汽渗透率的要求，提高光电器件的使用寿命。
The invention discloses an encapsulation film, a preparation method thereof, and an optoelectronic device, wherein the encapsulation film comprises a first organic thin film arranged in layers, a first blended film composed of a polymer and a ceramic material, and a first organic film composed of a ceramic material. ‑4 layers of ceramic membrane, second blend membrane composed of polymer and ceramic material, second organic thin film. In the present invention, the first organic film and the second organic film are used as the water vapor barrier layer, and 1-4 layers of dense ceramic films are used as the oxygen barrier layer. The blended layer can effectively improve the bonding force between the organic film and the ceramic film, thereby enhancing the water and oxygen barrier properties of the encapsulated film, thereby meeting the requirements for water vapor permeability of optoelectronic devices and improving the use of optoelectronic devices. life.
Description
Technical Field
The invention relates to the field of photoelectric devices, in particular to a packaging film, a preparation method thereof and a photoelectric device.
Background
The service life of the photoelectric device is a very important parameter, and in order to improve the service life of the photoelectric device and enable the photoelectric device to reach a commercial level, packaging is a crucial link. For photoelectric devices, the package is not only a physical protection against scratches, but also an important protection against the permeation of moisture and oxygen in the external environment, which can accelerate the aging of the device when the moisture or oxygen in the environment permeates into the device. Therefore, the packaging structure of the photoelectric device must have good water and oxygen permeation barrier function.
Currently, the packaging technology of commercial photoelectric devices is being developed from the conventional cover plate type packaging to the novel thin film integrated packaging. Compared with the traditional cover plate packaging, the thin film packaging can obviously reduce the thickness and the quality of the device, about 50% of potential packaging cost is saved, and meanwhile, the thin film packaging can be suitable for the flexible device. Thin film packaging technology will be a necessary trend for development.
The prior art generally adopts an organic thin film with transparent hydrophobic property as an encapsulation film of a photoelectric device, however, the existing organic thin film generally has better water vapor barrier property, but the poor gas barrier property limits the wide application of the organic thin film as an encapsulation thin film material in the photoelectric device.
In order to improve the gas barrier property of the organic packaging film material, the most commonly adopted means is to introduce a layer of inorganic ceramic film in the middle of the organic film to form a multilayer film packaging structure. However, the incompatibility between the pure inorganic ceramic film and the organic film leads to poor performance of the composite material, thereby affecting the water and oxygen barrier performance of the packaging film material.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned deficiencies of the prior art, the present invention aims to provide a packaging film, a method for preparing the same, and a photovoltaic device, and aims to solve the problem of poor water oxygen barrier performance of the conventional packaging film.
The technical scheme of the invention is as follows:
a packaging film comprises a first organic film, a first blended film composed of polymer and ceramic material, 1-4 layers of ceramic film composed of ceramic material, a second blended film composed of polymer and ceramic material, and a second organic film which are sequentially stacked.
The packaging film is characterized in that the ceramic material is one or more of silicon oxide, aluminum oxide, zinc oxide, titanium oxide and tungsten oxide.
The packaging film is characterized in that the first organic film material, the second organic film material, the polymer in the first blended film and the polymer in the second blended film are independently selected from one or more of polylactic acid, polytetrafluoroethylene, polymethylsiloxane and polypropylene.
The encapsulation film, wherein the thickness of the first organic film is 1-3 μm; and/or the thickness of the second organic thin film is 1-3 μm.
The packaging film, wherein the thickness of the first blended film is 0.8-1.2 μm; and/or the thickness of the second blend film is 0.8 to 1.2 μm.
The packaging film is characterized in that the thickness of the ceramic film is 0.1-1 μm.
A preparation method of an encapsulation film comprises the following steps:
providing a device to be packaged, and depositing a first organic film on the surface of the device;
depositing a first blended film on the first organic thin film, the first blended film consisting of a polymer and a ceramic material;
depositing N ceramic films which are arranged in a laminated manner on the first blending film, wherein N is more than or equal to 1 and less than or equal to 4;
depositing a second blended membrane on the Nth ceramic membrane, wherein the second blended membrane consists of a polymer and a ceramic material;
depositing a second organic thin film on the second blended film.
The preparation method of the packaging film comprises the following steps of:
under the alkaline condition, carrying out a first reaction on an inorganic precursor and an organic monomer according to a preset weight ratio under an inert atmosphere;
adding a catalyst, and carrying out a second reaction under a vacuum condition to obtain a blending material;
drying the blending material and dispersing the dried blending material into a tetrahydrofuran solvent to obtain a blending liquid consisting of a polymer and a ceramic material;
depositing a blend liquid consisting of polymer and ceramic material on the first organic film to obtain a first blend film.
The preparation method of the packaging film comprises the following step of preparing an inorganic precursor, wherein the inorganic precursor is tetraethoxysilane, aluminum nitrate, zinc acetate, sodium tungstate or tetrabutyl titanate.
The preparation method of the packaging film comprises the step of preparing the packaging film by using the organic monomer, wherein the organic monomer is one or more of lactic acid, tetrafluoroethylene, methyl siloxane and propylene.
The preparation method of the packaging film comprises the step of preparing a packaging film, wherein the catalyst is one or more of stannous octoate, stannous acetate and hydrochloric acid.
The preparation method of the packaging film comprises the step of carrying out primary reaction at the temperature of 50-100 ℃ and/or at the heating rate of 0.5-1 ℃/min.
The preparation method of the packaging film comprises the step of carrying out a second reaction at a temperature of 150-200 ℃.
An optoelectronic device comprises a first electrode, a light emitting layer and a second electrode, wherein an encapsulation film is arranged on the second electrode, and the encapsulation film is the encapsulation film or the encapsulation film prepared by the method.
Has the advantages that: the packaging film provided by the invention comprises a first organic film, a first blended film, 1-4 layers of ceramic films, a second blended film and a second organic film, wherein the first organic film, the first blended film, the first ceramic film, the second blended film and the second organic film are stacked. According to the invention, the first organic film and the second organic film are used as water vapor barrier layers, 1-4 layers of compact ceramic films are used as oxygen barrier layers, and the blending layer composed of polymers and ceramic materials is arranged between the ceramic films, so that the binding force between the organic films and the ceramic films can be effectively improved by the blending layer, the water oxygen barrier property of the packaging film is enhanced, the requirement of a photoelectric device on the water vapor permeability is further met, and the service life of the photoelectric device is prolonged.
Drawings
FIG. 1 is a schematic structural diagram of a preferred embodiment of an encapsulation film according to the present invention;
FIG. 2 is a flowchart illustrating a method for manufacturing a packaging film according to a preferred embodiment of the present invention.
Detailed Description
The invention provides a packaging film, a preparation method thereof and a photoelectric device, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear and definite. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a preferred embodiment of an encapsulation film according to the present invention, and as shown in the figure, the encapsulation film includes a first organic film 10, a first blend film 20 composed of polymer and ceramic material, 1-4 ceramic films 30 composed of ceramic material, a second blend film 40 composed of polymer and ceramic material, and a second organic film 50, which are stacked.
Specifically, in the embodiment, the first organic film and the second organic film are used as water vapor barrier layers, the dense ceramic film is used as an oxygen barrier layer, and the blend film composed of the polymer and the ceramic material is added between the ceramic film and the organic film, so that the compatibility between the ceramic film and the organic film can be enhanced, the defects between the film layers can be reduced, and the water oxygen barrier performance and the optical performance of the packaging film can be enhanced.
Preferably, the first organic film material, the second organic film material, the polymer in the first blended film and the polymer in the second blended film are all transparent hydrophobic materials, and specifically may be one or more of polylactic acid, polytetrafluoroethylene, polymethylsiloxane and polypropylene. By way of example, polylactic acid (PLA) is preferred in this embodiment to prepare organic films and blend films because it not only has strong water vapor barrier property, but also is a new renewable and degradable environment-friendly material, and many properties of PLA can be controlled by preparation process and modification means.
Preferably, in the present embodiment, in order to ensure that the encapsulation film has better water vapor barrier property, the first organic film is set to be 1-3 μm.
More preferably, the thickness of the second organic thin film is also set to 1 to 3 μm.
In order to make up for the defect of poor gas barrier property of the organic film, 1 to 4 layers of compact ceramic films made of ceramic materials are arranged between the first organic film and the second organic film.
In one embodiment, the ceramic material is one or more of silicon oxide, aluminum oxide, zinc oxide, titanium oxide, and tungsten oxide, but is not limited thereto. The silicon oxide is preferably used as the ceramic film material, because the silicon oxide film has high transparency and high density, and has stronger bonding force with the organic film and optimal oxygen resistance.
More preferably, in this embodiment, in order to ensure that the encapsulation film has better oxygen barrier performance, the ceramic film is provided with 2-3 layers, and the thickness of the ceramic film is set to be 0.1-1 μm.
Furthermore, in the embodiment, a layer of blended film composed of polymer and ceramic material is arranged between the ceramic film and the organic film, and the blended film can not only enhance the compatibility between the ceramic film and the organic film, but also reduce the defects between the film layers, thereby enhancing the water-oxygen barrier property and the optical property of the packaging film.
Preferably, in the present embodiment, in order to enhance the bonding force between the ceramic membrane and the organic thin film, the thickness of the first blend membrane is set to 0.8 to 1.2 μm.
More preferably, the thickness of the second blend film is also set to 0.8 to 1.2 μm.
The multilayer packaging film provided by the embodiment can form a good covering step, can effectively isolate the permeation of water vapor and oxygen by utilizing the combined action of multiple layers of films, and can meet the requirement of a photoelectric device on the water vapor permeability, thereby prolonging the service life of the photoelectric device; meanwhile, the packaging film belongs to a transparent film and can be used for packaging structures of top light-emitting devices and screens.
Further, the present invention also provides a method for preparing an encapsulation film, wherein, as shown in fig. 2, the method comprises the steps of:
s1, providing a device to be packaged, and depositing a first organic film on the surface of the device;
s2, depositing a first blended film on the first organic thin film, wherein the first blended film is composed of a polymer and a ceramic material;
s3, depositing N ceramic films which are arranged in a laminated mode on the first blending film, wherein N is more than or equal to 1 and less than or equal to 4;
s4, depositing a second blended membrane on the Nth ceramic membrane, wherein the second blended membrane is composed of a polymer and a ceramic material;
and S5, depositing a second organic thin film on the second blended film.
Further, the preparation of the first mixed film deposited on the first organic thin film includes the steps of:
under the alkaline condition, carrying out a first reaction on an inorganic precursor and an organic monomer according to a preset weight ratio under an inert atmosphere;
adding a catalyst, and carrying out a second reaction under a vacuum condition to obtain a blending material;
drying the blending material and dispersing the dried blending material into a tetrahydrofuran solvent to obtain a blending liquid consisting of a polymer and a ceramic material;
depositing a blend liquid consisting of polymer and ceramic material on the first organic film to obtain a first blend film.
Preferably, the inorganic precursor is tetraethoxysilane, aluminum nitrate, zinc acetate, sodium tungstate or tetrabutyl titanate, but is not limited thereto.
Preferably, the organic monomer is one or more of lactic acid, tetrafluoroethylene, methyl siloxane and propylene, but is not limited thereto.
More preferably, the inorganic precursor and the organic monomer are first reacted in a weight ratio of 1:1 under an inert atmosphere.
Preferably, the catalyst is one or more of stannous octoate, stannous acetate and hydrochloric acid, but is not limited thereto.
Preferably, the temperature of the first reaction is 50-100 ℃ and/or the heating rate is 0.5-1 ℃/min.
Preferably, the temperature of the second reaction is 150-200 ℃.
Preferably, the inert atmosphere is one or more of nitrogen, helium, neon and argon, but is not limited thereto.
In a specific embodiment of preparing the polylactic acid-silicon dioxide blending liquid, 30% strong ammonium oxide is added into ethanol as a catalyst, then the mixture is stirred at the temperature of 50-80 ℃, 10-20ml of Tetraethoxysilane (TEOS) is added while the mixture is stirred, and the mixture is continuously stirred for 15-25 hours to obtain a silicon dioxide ethanol solution;
under the alkaline condition, reacting a 10% silicon dioxide ethanol solution with lactic acid according to the weight ratio of 1:1 in a nitrogen atmosphere at the reaction temperature of 80 ℃, the heating rate of 0.8 ℃/min and the reaction time of 1.5h, then adding 0.05g of stannous octoate as a catalyst, and continuing the reaction in vacuum for 5h at the reaction temperature of 180 ℃; wherein, the reaction equation is as follows:
SiO2-OH+OH-CO(CH3)CH-OH=SiO2-O-CO(CH3)CH-OH
SiO2-O-CO(CH3)CH-OH+OH-CO(CH3)CH-OH=SiO2-O-（CO(CH3)CH-O）nH
and drying the product obtained by the reaction, and dispersing the product in a tetrahydrofuran solvent to obtain the polylactic acid-silicon dioxide blending liquid.
In a specific embodiment of preparing the polymethylsiloxane-silicon dioxide blending liquid, 30% strong ammonium oxide is added into ethanol as a catalyst, then the mixture is stirred at the temperature of 50-80 ℃, 10-20ml of Tetraethoxysilane (TEOS) is added while the mixture is stirred, and the mixture is continuously stirred for 15-25 h to obtain a silicon dioxide ethanol solution;
reacting 15% silicon dioxide ethanol solution and methyltrimethoxysilane at a weight ratio of 1:1 in a nitrogen atmosphere, stirring at 50-60 ℃ for 10-20 min, adjusting the pH value to 2-3 by hydrochloric acid, hydrolyzing a precursor compound to form a semi-interpenetrating network under the catalytic action of hydrochloric acid, and simultaneously performing hydrolysis and monomer polymerization to obtain the silicon dioxide-polymethylsiloxane blended material;
and drying the silicon dioxide-polymethylsiloxane blending material, and then dispersing the silicon dioxide-polymethylsiloxane blending material in a tetrahydrofuran solvent to prepare the polymethylsiloxane-silicon dioxide blending liquid.
In a specific embodiment of preparing the polytetrafluoroethylene-titanium dioxide blended solution, under the alkaline condition, tetrabutyl titanate alcohol solution and tetrafluoroethylene are reacted for 0.5 to 1 hour according to a certain proportion under the inert atmosphere, 0.01 to 1g of hydrochloric acid is added, the pH value is adjusted to be between 2 and 3 through the hydrochloric acid, and the polytetrafluoroethylene-titanium dioxide blended solution is formed under the catalytic action of the hydrochloric acid.
The polymer-ceramic material blending liquid prepared by the method has good bonding force of the blending membrane, and the inorganic ceramic material is hybridized in a polymer network, so that the stability of the blending membrane is improved to a certain extent.
Preferably, in the present embodiment, the organic thin film and the blend film may be prepared by casting, spin coating or printing.
The ceramic membrane is preferably prepared by a PECVD method: preparation of SiO by PECVD (plasma enhanced chemical vapor deposition)2For example, a device to be packaged is placed on a substrate of a PECVD apparatus, and Silane (SiH) is introduced4) And laughing gas (N)2O) reacting in a plasma state, wherein the process temperature is lower than 150 ℃, and the reaction equation is as follows:
SiH4+2N2O=SiO2+2N2+H2
the specific process parameter of the coating is SiH4Is 10-45 sccm, N2O is 100-2300-; wherein, nitrogen is used as a diluent gas and mainly has the function of influencing the partial pressure condition of reaction gas in the reaction chamber; the power of the PECVD device is preferably between 30W and 200W, wherein the smaller the power, the smaller the deposition rate, and the better the film uniformity, but the deposition rate and the film uniformity need to be considered, so the power is selected between 30W and 200W. The film deposition rate is kept between 20 nm and 50 nm.
Further, the invention also provides a photoelectric device, which comprises a first electrode, a light emitting layer and a second electrode, wherein an encapsulation film is arranged on the second electrode, and the encapsulation film is the encapsulation film described in any one of the above, or the encapsulation film prepared by any one of the above methods. The packaging film can effectively isolate the permeation of water vapor and oxygen on the basis of ensuring the luminous efficiency and the luminous brightness of the device, thereby prolonging the service life of the device.
The photoelectric device and the packaging method thereof of the present invention are explained in detail by the following embodiments:
example 1
1. The photoelectric device has the following structure: ITO substrate/PEDOT: PSS (50 nm)/poly-TPD (30 nm)/quantum dot luminescent layer (20 nm)/ZnO (30 nm)/silver (70 nm)/packaging film (4100 nm),wherein the packaging film is made of PLA/SiO2-PLA blend film/SiO2/ SiO2-PLA blend film/PLA composite film, the SiO2The thickness of the film is 100 nm, the thickness of the two PLA films is 1000nm, and the two SiO films are2The thickness of the PLA blend film is 1000 nm.
2. The packaging method of the photoelectric device comprises the following steps:
1) casting 10 mg/ml of PLA chloroform solution on the top surface of a silver electrode of a photoelectric device by adopting a casting method to form a film, and then carrying out vacuum drying for 30 min at 0.8 Pa at the temperature of 120 ℃ to prepare a PLA film;
2) under the alkaline condition, SiO with the mass fraction of 5 wt percent2Alcohol solution and lactic acid were mixed according to 1:1 in the nitrogen atmosphere, the reaction temperature is 100 ℃, the reaction time is 1h, after the reaction is finished, 0.01g of stannous octoate serving as a catalyst is added into the reaction system to continue the reaction for 5h in vacuum, and the reaction temperature is 150 ℃. Dissolving the reaction product in tetrahydrofuran solution with the concentration of 10 mg/ml, casting the reaction product on the surface of the PLA film to form a film, and then drying the film in vacuum at the temperature of 120 ℃ under the pressure of 0.8 Pa for 30 min to prepare SiO2-a PLA blend film;
3) then using PECVD method, using Silane (SiH)4) 16 sccm and laughing gas (N)2O) is 120 sccm, the reaction is carried out in a plasma state, the process temperature is 150 ℃, the power is 40W, the nitrogen flow is 300sccm, and the coating rate is 25 nm/min to prepare the silicon dioxide film;
4) preparing a layer of SiO on the surface of the silicon dioxide film by adopting the method in the step 2)2-a PLA blend film;
5) the method of step 1) is adopted, and the SiO is obtained in step 4)2Preparing a PLA film on the surface of the PLA blended film, and then carrying out vacuum drying for 30 min at the temperature of 120 ℃ under 0.8 Pa to realize packaging of the optoelectronic device.
Example 2
1. The photoelectric device has the following structure: ITO substrate/PEDOT: PSS (50 nm)/poly-TPD (30 nm)/quantum dot luminescent layer (20 nm)/ZnO (30 nm)/silver(70 nm)/packaging film (9000 nm), wherein the packaging film is made of PLA/SiO2-PLA blend film/SiO2/ SiO2-PLA blend film/PLA composite film, the SiO2The thickness of the film is 1000nm, the thickness of the two PLA films is 3000 nm, and the two SiO films2The thickness of the PLA blend film is 1000 nm.
2. The packaging method of the photoelectric device comprises the following steps:
1) casting 10 mg/ml of PLA chloroform solution on the top surface of a silver electrode of a photoelectric device by adopting a casting method to form a film, and then carrying out vacuum drying for 30 min at 0.8 Pa at the temperature of 120 ℃ to prepare a PLA film;
2) under the alkaline condition, SiO with the mass fraction of 20 wt percent2Alcohol solution and lactic acid were mixed according to 1:1 in the nitrogen atmosphere, the reaction temperature is 100 ℃, the reaction time is 1h, after the reaction is finished, 0.01g of stannous octoate serving as a catalyst is added into the reaction system to continue the reaction for 5h in vacuum, and the reaction temperature is 150 ℃. Dissolving the reaction product in tetrahydrofuran solution with the concentration of 10 mg/ml, casting the reaction product on the surface of the PLA film to form a film, and then drying the film in vacuum at the temperature of 120 ℃ under the pressure of 0.8 Pa for 30 min to prepare SiO2-a PLA blend film;
3) then using PECVD method, using Silane (SiH)4) 40 sccm and laughing gas (N)2O) is 300sccm, the reaction is carried out in a plasma state, the process temperature is 150 ℃, the power is 190W, the nitrogen flow is 600 sccm, and the coating rate is 40 nm/min to prepare the silicon dioxide film;
4) preparing a layer of SiO on the surface of the silicon dioxide film by adopting the method in the step 2)2-a PLA blend film;
5) the method of step 1) is adopted, and the SiO is obtained in step 4)2Preparing a PLA film on the surface of the PLA blended film, and then carrying out vacuum drying for 30 min at the temperature of 120 ℃ under 0.8 Pa to realize packaging of the optoelectronic device.
Example 3
1. The photoelectric device has the following structure: ITO substrate/PEDOT: PSS (50 nm)/poly-TPD (30 nm)/quantum dot light emitting layer (20 nm)/ZnO (30 nm)/silver (70 nm)/packaging film (4100 nm), wherein the packaging film is made of PLA/ZnO-PLA blended film/ZnO/ZnO-PLA blended film/PLA composite film, the thickness of the ZnO film is 100 nm, the thicknesses of the two PLA films are both 1000nm, and the thicknesses of the two ZnO-PLA blended films are both 1000 nm.
2. The packaging method of the photoelectric device comprises the following steps:
1) casting 10 mg/ml of PLA chloroform solution on the top surface of a silver electrode of a photoelectric device by adopting a casting method to form a film, and then carrying out vacuum drying for 30 min at 0.8 Pa at the temperature of 120 ℃ to prepare a PLA film;
2) under the alkaline condition, mixing ZnO alcohol solution with the mass fraction of 10 wt% and lactic acid according to the weight ratio of 1:1 in the nitrogen atmosphere, the reaction temperature is 100 ℃, the reaction time is 1h, after the reaction is finished, 0.01g of stannous octoate serving as a catalyst is added into the reaction system to continue the reaction for 5h in vacuum, and the reaction temperature is 150 ℃. Dissolving the reaction product in tetrahydrofuran solution, wherein the concentration of the solution is 10 mg/ml, casting the reaction product on the surface of the PLA film to form a film, and then performing vacuum drying on the film for 30 min at the temperature of 120 ℃ under 0.8 Pa to prepare a ZnO-PLA blended film;
3) followed by PECVD using zinc acetate (DEZn) of 50 sccm and laughing gas (N)2O) is 100 sccm, and the reaction is carried out in a plasma state, wherein the process temperature is 100 ℃, the power is 150W, the nitrogen flow is 600 sccm, and the coating rate is 40 nm/min to prepare the zinc oxide film;
4) preparing a ZnO-PLA blended film on the surface of the zinc oxide film by adopting the method in the step 2);
5) preparing a PLA film on the surface of the ZnO-PLA blended film in the step 4) by adopting the method in the step 1), and then carrying out vacuum drying for 30 min at 0.8 Pa at the temperature of 120 ℃ to realize packaging of the optoelectronic device.
Example 4
1. The photoelectric device has the following structure: ITO substrate/PEDOT: PSS (50 nm)/poly-TPD (30 nm)/quantum dot light emitting layer (20 nm)/ZnO (30 nm)/silver (70 nm)/packaging film (4100 nm), wherein the packaging film is made of PTFE/TiO2-PTFE blend film/TiO 2/TiO 2-PTFE blend film/PTFE film, the thickness of the TiO2 film is 100 nm, the thicknesses of two layers of Polytetrafluoroethylene (PTFE) films are both 1000nm, and the thicknesses of two layers of TiO2-PTFE blend film are both 1000 nm.
2. The packaging method of the photoelectric device comprises the following steps:
1) casting 10 mg/ml PTFE chloroform solution on the top surface of a silver electrode of a photoelectric device by adopting a casting method to form a film, and then carrying out vacuum drying for 30 min at 0.8 Pa at the temperature of 120 ℃ to prepare a PTFE film;
2) under the alkaline condition, mixing a TiO2 alcohol solution with the mass fraction of 10 wt% and tetrafluoroethylene according to the weight ratio of 1:1 under the nitrogen atmosphere, the reaction temperature is 100 ℃, the reaction time is 1h, 0.01g of hydrochloric acid is added into the reaction system after the reaction is finished and is used as a catalyst to continue the reaction for 5h in vacuum, and the reaction temperature is 150 ℃. Dissolving the reaction product in tetrahydrofuran solution, wherein the concentration of the solution is 10 mg/ml, casting the reaction product on the surface of the PTFE film to form a film, and then drying the film in vacuum at the temperature of 120 ℃ under 0.8 Pa for 30 min to prepare a TiO2-PTFE blend film;
3) then PECVD using titanium acetate (DETi) of 50 sccm and laughing gas (N)2O) is 100 sccm, the reaction is carried out in a plasma state, the process temperature is 100 ℃, the power is 150W, the nitrogen flow is 600 sccm, and the coating rate is 40 nm/min to prepare the titanium dioxide film;
4) preparing a TiO2-PTFE blended film on the surface of the titanium dioxide film by adopting the method in the step 2);
5) preparing a PTFE film on the surface of the TiO2-PTFE blended film in the step 4) by adopting the method in the step 1), and then drying the film for 30 min in vacuum at 0.8 Pa at the temperature of 120 ℃ to realize the packaging of the optoelectronic device.
In summary, the encapsulation film provided by the present invention includes a first organic film, a first blend film composed of a polymer and a ceramic material, a ceramic film composed of a ceramic material, a second blend film composed of a polymer and a ceramic material, and a second organic film, which are stacked. According to the invention, the first organic film and the second organic film are used as water vapor barrier layers, 1-4 layers of compact ceramic films are used as oxygen barrier layers, and the blending layer composed of polymers and ceramic materials is arranged between the ceramic films, so that the binding force between the organic films and the ceramic films can be effectively improved by the blending layer, the water oxygen barrier property of the packaging film is enhanced, the requirement of a photoelectric device on the water vapor permeability is further met, and the service life of the photoelectric device is prolonged.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (14)
1. A packaging film is characterized by comprising a first organic film, a first blended film, 1-4 ceramic films, a second blended film and a second organic film, wherein the first organic film, the first blended film, the 1-4 ceramic films, the second blended film and the second organic film are stacked; under the alkaline condition, the ceramic material and the organic monomer are subjected to a first reaction according to a preset weight ratio; adding a catalyst, and carrying out a second reaction under a vacuum condition to obtain a blending material for forming the first blending film, wherein the organic monomer is a monomer for forming the polymer.
2. The encapsulation film according to claim 1, wherein the ceramic material is one or more of silicon oxide, aluminum oxide, zinc oxide, titanium oxide, and tungsten oxide.
3. The encapsulation film according to claim 1, wherein the first organic film material, the second organic film material, the polymer in the first blended film, and the polymer in the second blended film are independently selected from one or more of polylactic acid, polytetrafluoroethylene, polymethylsiloxane, and polypropylene.
4. The encapsulation film according to claim 1, wherein the first organic film has a thickness of 1 to 3 μm; and/or the second organic thin film has a thickness of 1 to 3 μm.
5. The encapsulation film according to claim 1, wherein the first blended film has a thickness of 0.8 to 1.2 μm; and/or the second blended film has a thickness of 0.8 to 1.2 μm.
6. The encapsulation film according to claim 1, wherein the ceramic film has a thickness of 0.1 to 1 μm.
7. A method for preparing an encapsulation film is characterized by comprising the following steps:
providing a device to be packaged, and depositing a first organic film on the surface of the device;
depositing a first blended film on a first organic thin film, wherein the first blended film is composed of a polymer and a ceramic material, and the ceramic material and an organic monomer are subjected to a first reaction according to a preset weight ratio under an alkaline condition; adding a catalyst, and carrying out a second reaction under a vacuum condition to obtain a blending material for forming a first blending film, wherein the organic monomer is a monomer for forming the polymer;
depositing N ceramic films which are arranged in a laminated manner on the first blending film, wherein N is more than or equal to 1 and less than or equal to 4;
depositing a second blended membrane on the Nth ceramic membrane, wherein the second blended membrane consists of a polymer and a ceramic material;
depositing a second organic thin film on the second blended film.
8. The method for preparing an encapsulation film according to claim 7, wherein the preparing for depositing the first mixed film on the first organic film comprises the steps of:
under the alkaline condition, carrying out a first reaction on an inorganic precursor and an organic monomer according to a preset weight ratio under an inert atmosphere;
adding a catalyst, and carrying out a second reaction under a vacuum condition to obtain a blending material;
drying the blending material and dispersing the dried blending material into a tetrahydrofuran solvent to obtain a blending liquid consisting of a polymer and a ceramic material;
depositing a blend liquid consisting of polymer and ceramic material on the first organic film to obtain a first blend film.
9. The method of preparing an encapsulation film according to claim 8, wherein the inorganic precursor is ethyl orthosilicate, aluminum nitrate, zinc acetate, sodium tungstate or tetrabutyl titanate.
10. The method of manufacturing an encapsulation film according to claim 8, wherein the organic monomer is one or more of lactic acid, tetrafluoroethylene, methyl siloxane and propylene.
11. The method for preparing the encapsulation film according to claim 8, wherein the catalyst is one or more of stannous octoate, stannous acetate and hydrochloric acid.
12. The method of manufacturing an encapsulation film according to claim 8, wherein the temperature of the first reaction is 50 to 100 ℃ and/or the temperature increase rate is 0.5 to 1 ℃/min.
13. The method as claimed in claim 8, wherein the temperature of the second reaction is 150-200 ℃.
14. An optoelectronic device comprising a first electrode, a light-emitting layer and a second electrode, wherein an encapsulation film is disposed on the second electrode, wherein the encapsulation film is the encapsulation film according to any one of claims 1 to 6, or the encapsulation film is prepared by the method according to any one of claims 7 to 13.
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| CN104167506A (en) * | 2013-05-20 | 2014-11-26 | 海洋王照明科技股份有限公司 | Organic light emitting device and preparation method thereof |
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