CN103594649A - Organic electroluminescent device and preparation method thereof - Google Patents
Organic electroluminescent device and preparation method thereof Download PDFInfo
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- CN103594649A CN103594649A CN201210290605.XA CN201210290605A CN103594649A CN 103594649 A CN103594649 A CN 103594649A CN 201210290605 A CN201210290605 A CN 201210290605A CN 103594649 A CN103594649 A CN 103594649A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000010410 layer Substances 0.000 claims abstract description 525
- 239000000758 substrate Substances 0.000 claims abstract description 113
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 76
- 230000004888 barrier function Effects 0.000 claims abstract description 72
- 239000011241 protective layer Substances 0.000 claims abstract description 58
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 27
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims abstract description 13
- 239000000113 methacrylic resin Substances 0.000 claims abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 188
- 238000007738 vacuum evaporation Methods 0.000 claims description 96
- 238000001704 evaporation Methods 0.000 claims description 92
- 230000008020 evaporation Effects 0.000 claims description 92
- 238000005401 electroluminescence Methods 0.000 claims description 52
- 238000000034 method Methods 0.000 claims description 48
- 239000005083 Zinc sulfide Substances 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 239000004411 aluminium Substances 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 229910052709 silver Inorganic materials 0.000 claims description 14
- 239000004332 silver Substances 0.000 claims description 14
- 239000010931 gold Substances 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 11
- 238000004544 sputter deposition Methods 0.000 claims description 11
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical group [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 8
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 claims description 8
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical group [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract 2
- 230000017525 heat dissipation Effects 0.000 abstract 2
- 229910004504 HfF4 Inorganic materials 0.000 abstract 1
- 229910007998 ZrF4 Inorganic materials 0.000 abstract 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 abstract 1
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 description 49
- 239000002346 layers by function Substances 0.000 description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 36
- 230000005540 biological transmission Effects 0.000 description 36
- 238000002347 injection Methods 0.000 description 35
- 239000007924 injection Substances 0.000 description 35
- 230000027756 respiratory electron transport chain Effects 0.000 description 35
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 30
- 239000000203 mixture Substances 0.000 description 30
- GEQBRULPNIVQPP-UHFFFAOYSA-N 2-[3,5-bis(1-phenylbenzimidazol-2-yl)phenyl]-1-phenylbenzimidazole Chemical compound C1=CC=CC=C1N1C2=CC=CC=C2N=C1C1=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=C1 GEQBRULPNIVQPP-UHFFFAOYSA-N 0.000 description 18
- VQGHOUODWALEFC-UHFFFAOYSA-N 2-phenylpyridine Chemical compound C1=CC=CC=C1C1=CC=CC=N1 VQGHOUODWALEFC-UHFFFAOYSA-N 0.000 description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 15
- 229910052760 oxygen Inorganic materials 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000011521 glass Substances 0.000 description 11
- GULMSHUCHQYPKF-UHFFFAOYSA-N 2,3,4-tri(carbazol-9-yl)-n,n-diphenylaniline Chemical class C1=CC=CC=C1N(C=1C(=C(C(=CC=1)N1C2=CC=CC=C2C2=CC=CC=C21)N1C2=CC=CC=C2C2=CC=CC=C21)N1C2=CC=CC=C2C2=CC=CC=C21)C1=CC=CC=C1 GULMSHUCHQYPKF-UHFFFAOYSA-N 0.000 description 10
- 150000005360 2-phenylpyridines Chemical class 0.000 description 10
- DHDHJYNTEFLIHY-UHFFFAOYSA-N 4,7-diphenyl-1,10-phenanthroline Chemical group C1=CC=CC=C1C1=CC=NC2=C1C=CC1=C(C=3C=CC=CC=3)C=CN=C21 DHDHJYNTEFLIHY-UHFFFAOYSA-N 0.000 description 10
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical compound [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 description 10
- 229910052792 caesium Inorganic materials 0.000 description 10
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 10
- 238000005538 encapsulation Methods 0.000 description 10
- 229910052741 iridium Inorganic materials 0.000 description 10
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 10
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 10
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 10
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/842—Containers
- H10K50/8423—Metallic sealing arrangements
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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Abstract
The invention relates to an organic electroluminescent device, comprising an anode conductive substrate, a luminescent layer, a cathode, a protective layer, a fluoride layer, an organic barrier layer, a moisture absorption layer and a heat dissipation layer which are sequentially laminated, wherein the fluoride layer is made of at least one of AlF3, HfF4, ZrF4, LiF, CeF2 and YF3; and the organic barrier layer is made of at least one of polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin. The organic electroluminescent device further comprises a package cover, wherein the package cover packages the luminescent layer, the cathode, the protective layer, the fluoride layer, the organic barrier layer, the moisture absorption layer and the heat dissipation layer on the anode conductive substrate. The organic electroluminescent device is long in service life. The invention further provides a preparation method of the organic electroluminescent device.
Description
Technical field
The present invention relates to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is that the luminous organic material of making one deck tens nanometer thickness on ito glass is made luminescent layer, and there is the metal electrode of one deck low work function luminescent layer top.While being added with voltage on electrode, luminescent layer just produces light radiation.
OLED device have active illuminating, luminous efficiency high, low in energy consumption, light, thin, without advantages such as angle limitations, by insider, thought to be most likely at the device of new generation that occupies dominance on following illumination and display device market.As a brand-new illumination and Display Technique, the ten years development in the past of OLED technology is swift and violent, has obtained huge achievement.Because the whole world is increasing, throw light on and show that producer drops into research and development one after another, having promoted greatly the industrialization process of OLED, making the growth rate of OLED industry surprising, having arrived the eve of scale of mass production at present.
Yet organic electroluminescence device is subject to after moisture and moisture erosion, can cause that the material of organic electroluminescence device inner member occurs aging and then lost efficacy, thereby the life-span of described organic electroluminescence device is shorter.
Summary of the invention
Based on this, be necessary to provide longer organic electroluminescence device of a kind of life-span and preparation method thereof.
, comprise the anode conducting substrate, luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and the heat dissipating layer that stack gradually; Wherein,
The material of described fluoride layer is AlF
3, HfF
4, ZrF
4, LiF, CeF
2and YF
3in at least one;
The material on described organic barrier layer is at least one in polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin;
Described organic electroluminescence device also comprises cap, and described cap is packaged in described luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer in described anode conducting substrate.
In a preferred embodiment, the material of described protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS.
In a preferred embodiment, the material of described moisture absorbed layer is at least one in CaO, BaO, SrO and MgO.
In a preferred embodiment, the material of described heat dissipating layer is at least one in aluminium, silver and copper.
In a preferred embodiment, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, and the material of described dielectric layer is zinc sulphide, tin indium oxide or zinc oxide aluminum, and the material of described metal level is at least one in aluminium, silver and gold.
A preparation method for organic electroluminescence device, comprises the steps:
In anode conducting substrate, form luminescent layer;
On described luminescent layer, form negative electrode;
On described negative electrode, form protective layer;
Adopt the method for vacuum evaporation to form fluoride layer on described protective layer, the material of wherein said fluoride layer is AlF
3, HfF
4, ZrF
4, LiF, CeF
2and YF
3in at least one, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100nm ~ 200nm;
On described fluoride layer, form organic barrier layer, comprise: under inert atmosphere, first at least one in polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin is spin-coated on described fluoride layer, thickness is 1 μ m ~ 1.5 μ m, then adopting wavelength is that the ultraviolet light of 200nm ~ 400nm is cured, and light intensity is 10 ~ 15mW/cm
2, time for exposure 200 ~ 300s;
On described organic barrier layer, form moisture absorbed layer;
On described moisture absorbed layer, form heat dissipating layer; And
Use cap that described luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
In a preferred embodiment, adopt the method for vacuum evaporation to form protective layer, the material of wherein said protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 300nm.
In a preferred embodiment, the method that forms described moisture absorbed layer comprises: with CaO, BaO, SrO,
Accompanying drawing explanation
By the more specifically explanation of the preferred embodiments of the present invention shown in accompanying drawing, above-mentioned and other object of the present invention, that Characteristics and advantages will become will be more clear.In whole accompanying drawings, identical Reference numeral is indicated identical part, and deliberately by actual size equal proportion convergent-divergent, draws accompanying drawing, focuses on illustrating purport of the present invention.
Fig. 1 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 2 is preparation method's the flow chart of the organic electroluminescent of an execution mode.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement to be much different from alternate manner described here, and those skilled in the art can do similar improvement without prejudice to intension of the present invention in the situation that, so the present invention is not subject to the restriction of following public concrete enforcement.
Refer to Fig. 1, the organic electroluminescence device 100 of an execution mode comprises that in the anode conducting MgO stacking gradually, any one is target, adopts the preparation of vacuum sputtering method to form, and base vacuum degree is 2 * 10
-4pa, sputter thickness is 100nm ~ 200nm.
In a preferred embodiment, the method that forms described heat dissipating layer comprises: adopt the method for vacuum evaporation, by least one evaporation in aluminium, silver and copper, to described moisture absorbed layer, vacuum degree is 8 * 10
-5pa～3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 500nm
In a preferred embodiment, adopt vapour deposition method to form described negative electrode, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, the material of described dielectric layer is zinc sulphide, tin indium oxide or zinc oxide aluminum, and the material of described metal level is at least one in aluminium, silver and gold.
Above-mentioned organic electroluminescence device adopts the method for evaporation to prepare protective layer, avoids negative electrode to be damaged; Organic barrier layer can cooperatively interact with fluoride layer, effectively the corrosion of block water oxygen; Moisture absorbed layer can absorbing moisture, reduces the destruction of moisture to device; Cap can further improve waterproof oxygen ability, thereby makes the life-span of organic electroluminescence device longer.
Anode conducting substrate 10 is glass conductive substrates or organic PETG (PET) film substrate that conducts electricity.The ITO layer in anode conducting substrate 10 with the anode pattern of being prepared with.The thickness of ITO layer is 100nm ~ 150nm.
Functional layer 20 is formed at anode conducting substrate 10 surfaces.Functional layer 20 comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer stacking gradually.Be appreciated that hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, now functional layer 20 only comprises luminescent layer.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.
The material of hole transmission layer is 4,4', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3).CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.
Preferably, the number of plies on fluoride layer 50 and organic barrier layer 60 is multilayer, for example, be more than or equal to 3 layers, and these two layers of alternative arrangements, with the 60/ organic barrier layer 60 of fluoride layer 50/, the organic barrier layer of fluoride layer 50/ ... this structural arrangement.
Moisture absorbed layer 70 is formed at the surface on organic barrier layer 60.The material of moisture absorbed layer 70 is at least one in CaO, BaO, SrO and MgO.The thickness of moisture absorbed layer 70 is 100nm ~ 200nm.Moisture absorbed layer 70 can absorbing moisture, reduces the destruction of moisture to device.
The mode that above-mentioned organic electroluminescence device 100 adopts organic barrier layer 60 to match with fluoride layer 50, the corrosion of block water oxygen effectively.
Refer to Fig. 2, the preparation method of above-mentioned organic electroluminescence device 100 comprises the steps:
Step S110, in anode conducting substrate 10, form functional layer 20.
Anode conducting substrate 10 can be glass conductive substrates or organic PETG (PET) film substrate that conducts electricity.Anode conducting substrate 10 has the ITO layer of the anode pattern of being prepared with.The thickness of ITO layer is 100nm ~ 150nm.
Preliminary treatment was first carried out to remove the pollutant on anode conducting substrate 10 surfaces in anode conducting substrate 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase anode conducting substrate 10 surfaces is to improve the work function on anode conducting substrate 10 surfaces.Be specially, anode conducting substrate 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
Functional layer 20 comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer stacking gradually.
In present embodiment, the material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.Hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, and now functional layer 20 only comprises luminescent layer.
Step S120, on functional layer 20 surface, form negative electrodes 30.
When negative electrode 30 is single layer structure, the thickness of negative electrode 30 is 100nm, and the material of negative electrode 30 is aluminium (Al), silver (Ag) or gold (Au), and negative electrode 30 is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
When negative electrode 30 is sandwich construction, negative electrode 30 comprises two layer medium layer and is located at the metal level between two layer medium layer.The thickness of dielectric layer is 30nm, and the thickness of metal level is 10nm.The material of dielectric layer is zinc sulphide (ZnS), tin indium oxide (ITO) or zinc oxide aluminum (AZO), and the material of metal level is silver (Ag).Wherein, tin indium oxide (ITO) or zinc oxide aluminum (AZO) are made by sputter, base vacuum degree 2 * 10
-4pa; ZnS or Ag are formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
The method of step S130, employing vacuum evaporation forms protective layer 40 on negative electrode 30.
The material of protective layer 40 is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS.During vacuum evaporation, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 300nm.
The method of step S140, employing vacuum evaporation forms fluoride layer 50 on protective layer 40.
The material of fluoride layer 50 is AlF
3, HfF
4, ZrF
4, LiF, CeF
2and YF
3in at least one.While using the method making of vacuum evaporation, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate
thickness 100nm ~ 200nm.
Step S150, on fluoride layer 50, form organic barrier layer 60.
The concrete formation step on organic barrier layer 60 is as follows: under inert atmosphere, first at least one in polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin is spin-coated on described fluoride layer, thickness is 1 μ m ~ 1.5 μ m, then adopting wavelength is that the ultraviolet light of 200nm ~ 400nm is cured, and light intensity is 10 ~ 15mW/cm
2, time for exposure 200 ~ 300s.
Preferably, replace repeating step S140, S150 at least three times.
Step S160, on organic barrier layer 60, form moisture absorbed layer 70.
Concrete, take in CaO, BaO, SrO, MgO that any one is target, adopt the preparation of vacuum sputtering method to form moisture absorbed layer 70.Base vacuum degree is 2 * 10
-4pa, sputter thickness is 100nm ~ 200nm.
Step S170, on moisture absorbed layer 70, form heat dissipating layer 80.
Concrete, the method for employing vacuum evaporation forms heat dissipating layer 80 by least one evaporation in aluminium, silver and copper to moisture absorbed layer 70, and vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 500nm.
Step S180, use cap 90 are encapsulated in functional layer 20, negative electrode 30, protective layer 40, fluoride layer 50, organic barrier layer 60, moisture absorbed layer 70 and heat dissipating layer 80 in anode conducting substrate 10.
The material of cap 90 is tinsel.In cap 90, be formed with host cavity.Thereby cap 90 is covered on heat dissipating layer, 80 surfaces are contained in host cavity by functional layer 20, negative electrode 30, protective layer 40, fluoride layer 50, organic barrier layer 60, moisture absorbed layer 70 and heat dissipating layer 80.
The edge of cap 90 is fixed on anode conducting substrate 10.Edge-coating packaging plastic at cap 90 is tightly connected cap 90 and anode conducting substrate 10, thereby functional layer 20, negative electrode 30, protective layer 40, fluoride layer 50, organic barrier layer 60, moisture absorbed layer 70 and heat dissipating layer 80 are encapsulated in anode conducting substrate 10.In present embodiment, packaging plastic is epoxy encapsulation glue, and the thickness of packaging plastic is 15 μ m ~ 20 μ m, with UV light (λ=365nm), is cured, and light intensity is 10 ~ 15mW/cm
2, the time for exposure is 300 ~ 400s.
The preparation method of above-mentioned organic electroluminescence device, preparation technology is simple, easily preparation in enormous quantities; Adopt the method for evaporation to prepare protective layer 40, avoid negative electrode to be damaged; Thereby fluoride layer 50 improves with the stacked compactness that makes in organic barrier layer 60, and the two cooperation is the corrosion of block water oxygen effectively; Cap 90 adopts tinsel can effectively improve waterproof oxygen ability, extends the useful life of organic electroluminescence device 100.
Below in conjunction with specific embodiment, organic electroluminescence device provided by the invention and preparation method thereof is elaborated.
Embodiment 1
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/CuPc/ (AlF
3/ polytetrafluoroethylene)
3the organic electroluminescence device of/CaO/Cu/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck CuPc, vacuum degree 3 * 10
-5pa, evaporation rate
thickness 200nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is AlF
3.Adopt the method for vacuum evaporation to make, vacuum degree is 5 * 10
-5pa, evaporation rate is
thickness is 100nm.
5, on fluoride layer, form organic barrier layer.
The material on organic barrier layer is polytetrafluoroethylene, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1 μ m, is then cured light intensity 10mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
Replace repeating step 4,5 three three layers of fluoride layer and organic barrier layers with formation alternative arrangement.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts CaO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 100nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is metallic aluminium.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 200nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 350s.
Embodiment 2
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/NPB/ (HfF
4/ methacrylic resin)
3the organic electroluminescence device of/BaO/Ag/ cap.
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is ZnS/Al/ZnS.The thickness of negative electrode is 110nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck NPB, vacuum degree 3 * 10
-5pa, evaporation rate
thickness 300nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is HfF
4.Adopt the method for vacuum evaporation to make, vacuum degree is 6 * 10
-5pa, evaporation rate
thickness is 150nm.
5, on fluoride layer, form organic barrier layer.
The material on organic barrier layer is methacrylic resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.5 μ m, are then cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
Replace repeating step 4,5 three three layers of fluoride layer and organic barrier layers with formation alternative arrangement.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts BaO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 200nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is argent.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 500nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 10mW/cm with UV light (λ=365nm)
2, time for exposure 400s.
Embodiment 3
Preparation structure is: ITO/NPB:MoO3/TCTA/TPBI:Ir (ppy) 3/Bphen/Bphen:CsN3/Al/Alq3/ (ZrF
4/ cycloaliphatic epoxy resin)
3the organic electroluminescence device of/SrO/Cu/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is ITO/Ag/ITO.The thickness of negative electrode is 120nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck Alq3, vacuum degree 3 * 10
-5pa, evaporation rate
thickness 250nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is ZrF
4.Adopt the method for vacuum evaporation to make, vacuum degree is 4 * 10
-5pa, evaporation rate
thickness is 200nm.
5, on fluoride layer, form organic barrier layer.
The material on organic barrier layer is cycloaliphatic epoxy resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.2 μ m, are then cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 230s.
Replace repeating step 4,5 three three layers of fluoride layer and organic barrier layers with formation alternative arrangement.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts SrO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 150nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is metallic copper.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 300nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 300s.
Embodiment 4
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/SiO/ (LiF/ polytetrafluoroethylene)
3the organic electroluminescence device of/MgO/Cu-Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is AZO/Au/AZO.The thickness of negative electrode is 110nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck SiO, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 200nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is LiF.Adopt the method for vacuum evaporation to make, vacuum degree is 7 * 10
-5pa, evaporation rate
thickness is 100nm.
5, on fluoride layer, form organic barrier layer.
The material on organic barrier layer is polytetrafluoroethylene, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1 μ m, is then cured light intensity 10mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
Replace repeating step 4,5 three three layers of fluoride layer and organic barrier layers with formation alternative arrangement.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts MgO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 100nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is albronze, and copper aluminium mass ratio is 3:1.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 500nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 350s.
Embodiment 5
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/MgF
2/ (CeF
2/ methacrylic resin)
3the organic electroluminescence device of/CaO/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is AZO/Al/AZO.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck MgF
2, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 300nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is CeF
2.Adopt the method for vacuum evaporation to make, vacuum degree is 3 * 10
-5pa, evaporation rate
thickness is 200nm.
5, on fluoride layer, form organic barrier layer.
The material on organic barrier layer is methacrylic resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.5 μ m, are then cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 200s.
Replace repeating step 4,5 three three layers of fluoride layer and organic barrier layers with formation alternative arrangement.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts CaO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 200nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is metallic aluminium.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 300nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 15mW/cm with UV light (λ=365nm)
2, time for exposure 400s.
Embodiment 6
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/ZnS/ (YF
3/ cycloaliphatic epoxy resin)
3the organic electroluminescence device of/BaO/Ag/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is ZnS/Au/ZnS.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck ZnS, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 250nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is YF3.Adopt the method for vacuum evaporation to make, vacuum degree is 8 * 10
-5pa, evaporation rate
thickness is 150nm.
5, on fluoride layer, form organic barrier layer.
The material on organic barrier layer is cycloaliphatic epoxy resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.2 μ m, are then cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 230s.
Replace repeating step 4,5 three three layers of fluoride layer and organic barrier layers with formation alternative arrangement.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts BaO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 150nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is argent.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 300nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 350s.
Comparative example 1
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/SiO/ (LiF)
3the organic electroluminescence device of //MgO/Cu-Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is AZO/Au/AZO.The thickness of negative electrode is 110nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck SiO, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 200nm.
4, adopt the method for vacuum evaporation to form fluoride layer on described protective layer.
The material of fluoride layer is LiF.Adopt the method for vacuum evaporation to make, vacuum degree is 7 * 10
-5pa, evaporation rate
thickness is 100nm.
Repeating step 4 three times.
5, on 4, form moisture absorbed layer.
The material of moisture absorbed layer adopts MgO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 100nm.
6, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is albronze, and copper aluminium mass ratio is 3:1.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 500nm.
7, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 350s.
Comparative example 2
Preparation structure is: ITO/NPB:MoO
3/ TCTA/TPBI:Ir (ppy)
3/ Bphen/Bphen:CsN
3/ Al/ZnS/ (cycloaliphatic epoxy resin)
3the organic electroluminescence device of/BaO/Ag/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, in conductive substrates, form functional layer.
Preliminary treatment was first carried out to remove the pollutant on substrate 10 surfaces in conductive substrates 10 surfaces before forming functional layer 20, and the oxygen content of carrying out surface active increase conductive substrates 10 surfaces is to improve the work function on conductive substrates 10 surfaces.Be specially, conductive substrates 10 is adopted successively and removes each Ultrasonic Cleaning of acetone, ethanol, ionized water and ethanol 5min, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-bis-(1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and be entrained in the molybdenum oxide (MoO in NPB
3).MoO
3quality percentage composition be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 " tri-(carbazole-9-yl) triphenylamines (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy)
3).The quality percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen
3), CsN
3quality percentage composition be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 * 10
-5pa, evaporation rate is
2, on functional layer surface, form negative electrode.
The material of negative electrode is ZnS/Au/ZnS.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 * 10
-5pa, evaporation rate is
3, at cathode surface, form protective layer.
Adopt the mode of vacuum evaporation on negative electrode, to prepare one deck ZnS, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 250nm.
4, on 3, form organic barrier layer.
The material on organic barrier layer is cycloaliphatic epoxy resin, adopts the technique of first spin coating post-exposure to make, and under inert atmosphere, makes, and gluing thickness 1.2 μ m, are then cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 230s.
Repeating step 4 three times.
6, on organic barrier layer, form moisture absorbed layer.
The material of moisture absorbed layer adopts BaO, uses sputtering method to make, base vacuum degree 2 * 10
-4pa, sputter thickness 150nm.
7, on moisture absorbed layer, form heat dissipating layer.
The material of heat dissipating layer is argent.Adopt the method for vacuum evaporation to make, vacuum degree 5 * 10
-5pa, evaporation rate
thickness 300nm.
8, use cap that luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
Edge-coating epoxy encapsulation glue (thickness 15 μ m) at tinsel, is cured light intensity 11mW/cm with UV light (λ=365nm)
2, time for exposure 350s.
The preparation used of the embodiment of the present invention and comparative example and tester are: high vacuum coating equipment (scientific instrument development center, Shenyang Co., Ltd, pressure <1 * 10
-32400), chroma-luminance meter (Konica Minolta, model: CS-100A), IEI point gum machine system, DYMAX photocuring system Pa), electric current one voltage tester (U.S. Keithly company, model:.
Refer to table 1, table 1 is depicted as the test result of aqueous vapor penetrance (Water Vapor Transmission Rate) of the organic electroluminescence device of embodiment 1～embodiment 6 and comparative example 1～2 preparation.The aqueous vapor penetrance of the organic electroluminescence device of embodiment 1～embodiment 6 preparations is all less than 9.3 * 1O as can be seen from Table 1
-5g/m
2/ day, the aqueous vapor penetrance (5.4 * 1O of the organic electroluminescence device of preparing much smaller than comparative example
-2) waterproof effect is better, can effectively reduce the erosion of outside aqueous vapor to organic electroluminescence device, thereby improve the life-span of organic electroluminescence device.
Table 1
| WVTR(g/m 2/day) | |
| Embodiment 1 | 3.5×10 -5 |
| Embodiment 2 | 3.8×10 -5 |
| Embodiment 3 | 1.9×10 -5 |
| Embodiment 4 | 1.1×10 -5 |
| Embodiment 5 | 2.7×10 -5 |
| Embodiment 6 | 3.4×10 -5 |
| Comparative example 1 | 3.2×10 -4 |
| Comparative example 2 | 5.4×10 -2 |
Refer to table 2, it is 1000cd/m at original intensity that table 2 is depicted as organic electroluminescence device prepared by embodiment 1 ~ embodiment 6 and comparative example
2condition under life-span.
Table 2
As can be seen from Table 2, the initial brightness of the organic electroluminescence device of embodiment 1 ~ embodiment 6 preparations is 1000cd/m
2time, the life-span reaches more than 13000 hours, and the life-span is longer.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an organic electroluminescence device, is characterized in that, comprises the anode conducting substrate, luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and the heat dissipating layer that stack gradually; Wherein,
The material of described fluoride layer is AlF
3, HfF
4, ZrF
4, LiF, CeF
2and YF
3in at least one;
The material on described organic barrier layer is at least one in polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin;
Described organic electroluminescence device also comprises cap, and described cap is packaged in described luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer in described anode conducting substrate.
2. organic electroluminescence device according to claim 1, is characterized in that: the material of described protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS.
3. organic electroluminescence device according to claim 1, is characterized in that: the material of described moisture absorbed layer is at least one in CaO, BaO, SrO and MgO.
4. organic electroluminescence device according to claim 1, is characterized in that, the material of described heat dissipating layer is at least one in aluminium, silver and copper.
5. organic electroluminescence device according to claim 1, it is characterized in that: described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, the material of described dielectric layer is zinc sulphide, tin indium oxide or zinc oxide aluminum, and the material of described metal level is at least one in aluminium, silver and gold.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the steps:
In anode conducting substrate, form luminescent layer;
On described luminescent layer, form negative electrode;
On described negative electrode, form protective layer;
Adopt the method for vacuum evaporation to form fluoride layer on described protective layer, the material of wherein said fluoride layer is AlF
3, HfF
4, ZrF
4, LiF, CeF
2and YF
3in at least one, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 100nm ~ 200nm;
On described fluoride layer, form organic barrier layer, comprise: under inert atmosphere, first at least one in polytetrafluoroethylene, methacrylic resin and cycloaliphatic epoxy resin is spin-coated on described fluoride layer, thickness is 1 μ m ~ 1.5 μ m, then adopting wavelength is that the ultraviolet light of 200nm ~ 400nm is cured, and light intensity is 10 ~ 15mW/cm
2, time for exposure 200 ~ 300s;
On described organic barrier layer, form moisture absorbed layer;
On described moisture absorbed layer, form heat dissipating layer; And
Use cap that described luminescent layer, negative electrode, protective layer, fluoride layer, organic barrier layer, moisture absorbed layer and heat dissipating layer are packaged in described anode conducting substrate.
7. the preparation method of organic electroluminescence device according to claim 1, is characterized in that: adopt the method for vacuum evaporation to form protective layer, the material of wherein said protective layer is CuPc, NPB, Alq3, SiO, MgF
2and at least one in ZnS, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 300nm.
8. the preparation method of organic electroluminescence device according to claim 1, it is characterized in that: the method that forms described moisture absorbed layer comprises: take in CaO, BaO, SrO, MgO that any one is target, adopt the preparation of vacuum sputtering method to form, base vacuum degree is 2 * 10
-4pa, sputter thickness is 100nm ~ 200nm.
9. the preparation method of organic electroluminescence device according to claim 1, it is characterized in that: the method that forms described heat dissipating layer comprises: the method that adopts vacuum evaporation, by at least one evaporation in aluminium, silver and copper, to described moisture absorbed layer, vacuum degree is 8 * 10
-5pa ~ 3 * 10
-5pa, evaporation rate is
thickness is 200nm ~ 500nm.
10. the preparation method of organic electroluminescence device according to claim 1, it is characterized in that: adopt vapour deposition method to form described negative electrode, described negative electrode comprises two layer medium layer and is located at the metal level between described two layer medium layer, the material of described dielectric layer is zinc sulphide, tin indium oxide or zinc oxide aluminum, and the material of described metal level is at least one in aluminium, silver and gold.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108376747A (en) * | 2018-01-31 | 2018-08-07 | 云谷（固安）科技有限公司 | Organic light-emitting display device and preparation method thereof |
| CN109686860A (en) * | 2018-12-26 | 2019-04-26 | 上海晶合光电科技有限公司 | A kind of multi-functional encapsulation cover plate and preparation method thereof |
| CN111599934A (en) * | 2020-05-07 | 2020-08-28 | Tcl华星光电技术有限公司 | Display panel and preparation method thereof |
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2012
- 2012-08-15 CN CN201210290605.XA patent/CN103594649A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108376747A (en) * | 2018-01-31 | 2018-08-07 | 云谷（固安）科技有限公司 | Organic light-emitting display device and preparation method thereof |
| CN109686860A (en) * | 2018-12-26 | 2019-04-26 | 上海晶合光电科技有限公司 | A kind of multi-functional encapsulation cover plate and preparation method thereof |
| CN111599934A (en) * | 2020-05-07 | 2020-08-28 | Tcl华星光电技术有限公司 | Display panel and preparation method thereof |
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