CN104124359A - Organic light-emitting device and preparation method thereof - Google Patents
Organic light-emitting device and preparation method thereof Download PDFInfo
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- CN104124359A CN104124359A CN201310143913.4A CN201310143913A CN104124359A CN 104124359 A CN104124359 A CN 104124359A CN 201310143913 A CN201310143913 A CN 201310143913A CN 104124359 A CN104124359 A CN 104124359A
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- organic electroluminescence
- electroluminescence device
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 67
- 239000011521 glass Substances 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 238000002347 injection Methods 0.000 claims abstract description 33
- 239000007924 injection Substances 0.000 claims abstract description 33
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 24
- 150000003752 zinc compounds Chemical class 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 238000005401 electroluminescence Methods 0.000 claims description 39
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 31
- 230000005540 biological transmission Effects 0.000 claims description 29
- 238000001704 evaporation Methods 0.000 claims description 28
- 230000008020 evaporation Effects 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 22
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 22
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 claims description 20
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- 238000005566 electron beam evaporation Methods 0.000 claims description 11
- 238000007747 plating Methods 0.000 claims description 11
- 239000004411 aluminium Substances 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 claims description 9
- 239000005083 Zinc sulfide Substances 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 8
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- SNTWKPAKVQFCCF-UHFFFAOYSA-N 2,3-dihydro-1h-triazole Chemical class N1NC=CN1 SNTWKPAKVQFCCF-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- VIZUPBYFLORCRA-UHFFFAOYSA-N 9,10-dinaphthalen-2-ylanthracene Chemical compound C12=CC=CC=C2C(C2=CC3=CC=CC=C3C=C2)=C(C=CC=C2)C2=C1C1=CC=C(C=CC=C2)C2=C1 VIZUPBYFLORCRA-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 claims description 4
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 claims description 4
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 4
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 4
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000075 oxide glass Substances 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 4
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 claims description 4
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 4
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 claims description 4
- 150000002736 metal compounds Chemical class 0.000 claims description 3
- 239000004305 biphenyl Substances 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 142
- ZVFQEOPUXVPSLB-UHFFFAOYSA-N 3-(4-tert-butylphenyl)-4-phenyl-5-(4-phenylphenyl)-1,2,4-triazole Chemical group C1=CC(C(C)(C)C)=CC=C1C(N1C=2C=CC=CC=2)=NN=C1C1=CC=C(C=2C=CC=CC=2)C=C1 ZVFQEOPUXVPSLB-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000003599 detergent Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical group [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 description 6
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- HXWWMGJBPGRWRS-CMDGGOBGSA-N 4- -2-tert-butyl-6- -4h-pyran Chemical compound O1C(C(C)(C)C)=CC(=C(C#N)C#N)C=C1\C=C\C1=CC(C(CCN2CCC3(C)C)(C)C)=C2C3=C1 HXWWMGJBPGRWRS-CMDGGOBGSA-N 0.000 description 5
- AWXGSYPUMWKTBR-UHFFFAOYSA-N 4-carbazol-9-yl-n,n-bis(4-carbazol-9-ylphenyl)aniline Chemical compound C12=CC=CC=C2C2=CC=CC=C2N1C1=CC=C(N(C=2C=CC(=CC=2)N2C3=CC=CC=C3C3=CC=CC=C32)C=2C=CC(=CC=2)N2C3=CC=CC=C3C3=CC=CC=C32)C=C1 AWXGSYPUMWKTBR-UHFFFAOYSA-N 0.000 description 5
- ZOKIJILZFXPFTO-UHFFFAOYSA-N 4-methyl-n-[4-[1-[4-(4-methyl-n-(4-methylphenyl)anilino)phenyl]cyclohexyl]phenyl]-n-(4-methylphenyl)aniline Chemical compound C1=CC(C)=CC=C1N(C=1C=CC(=CC=1)C1(CCCCC1)C=1C=CC(=CC=1)N(C=1C=CC(C)=CC=1)C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 ZOKIJILZFXPFTO-UHFFFAOYSA-N 0.000 description 5
- 101000837344 Homo sapiens T-cell leukemia translocation-altered gene protein Proteins 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 102100028692 T-cell leukemia translocation-altered gene protein Human genes 0.000 description 5
- 238000001771 vacuum deposition Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical class C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002772 conduction electron Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
-
- 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
- H10K50/805—Electrodes
- H10K50/82—Cathodes
-
- 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
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
-
- 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
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/856—Arrangements for extracting light from the devices comprising reflective means
Landscapes
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention provides an organic light-emitting device and a preparation method thereof. According to the organic light-emitting device, the cathode is made from a mixing material formed by mixing of a zinc compound, a metal with the work function of -4.0eV to -5.5eV, and a silicon compound based on a mass ratio of 1: (0.5-2) : (1-5). Therefore, the electron injection capability and stability of the device are improved and the light can reach the conductive anode glass substrate effectively, thereby improving the luminous efficiency of the device. The preparation method is simple and is easy to control and operation; and the raw material is easy to access.
Description
Technical field
The invention belongs to organic electroluminescent field, be specifically related to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind ofly to take organic material as luminescent material, the energy conversion device that can be luminous energy the electric energy conversion applying.It has the outstanding properties such as ultra-thin, self-luminous, response are fast, low-power consumption, in fields such as demonstration, illuminations, has application prospect very widely.
The structure of organic electroluminescence device is sandwich structure, accompanies one or more layers organic film between negative electrode and conductive anode.In containing the device of sandwich construction, inner side, the two poles of the earth mainly comprises luminescent layer, implanted layer and transport layer.Organic electroluminescence device is carrier injection type luminescent device, at anode and negative electrode, add after operating voltage, hole is from anode, electronics is injected into respectively the organic material layer of device work from negative electrode, it is luminous that two kinds of charge carriers form hole-duplet in luminous organic material, and then light sends from electrode.
In traditional luminescent device, general is all to using the metal of low work function or alloy as negative electrode, in this structure, the metallochemistry character of low work function is active, in air, be easy to oxidation, make the less stable of device, and the electronic injection ability of negative electrode is not good, cause device luminous efficiency, to go out optical property lower.
Summary of the invention
In order to address the above problem, the present invention aims to provide a kind of organic electroluminescence device compared with high light-emitting efficiency and preparation method thereof that has.
First aspect, the invention provides a kind of organic electroluminescence device, comprise the conductive anode substrate of glass stacking gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, the material of described negative electrode is zinc compound, the metal that work function is-4.0eV～-5.5eV and silicon compound are according to mass ratio 1:(0.5～2): the composite material that (1～5) is mixed to form, wherein, described zinc compound is zinc oxide, zinc sulphide, a kind of in zinc selenide and zinc chloride, the metal that described work function is-4.0eV～-5.5eV is aluminium, silver, a kind of in platinum and gold, described silicon compound is silicon monoxide, a kind of in silicon dioxide and sodium metasilicate.
Preferably, conductive anode substrate of glass is a kind of in indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) and indium-zinc oxide glass (IZO).More preferably, conductive anode substrate of glass is ITO.
Preferably, the material of hole injection layer is molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) in a kind of.More preferably, the material of hole injection layer is WO
3.
Preferably, the thickness of hole injection layer is 20～80nm.More preferably, the thickness of hole injection layer is 30nm.
Preferably, the material of hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, a kind of in 4'-diamines (NPB).More preferably, the material of hole transmission layer is NPB.
Preferably, the thickness of hole transmission layer is 20～60nm.More preferably, the thickness of hole transmission layer is 40nm.
Preferably, the material of luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis-(betanaphthyl) anthracene (ADN), 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1,1 '-biphenyl (BCzVBi) and oxine aluminium (Alq
3) in a kind of.More preferably, the material of luminescent layer is Alq
3.
Preferably, the thickness of luminescent layer is 5～40nm.More preferably, the thickness of luminescent layer is 20nm.
The material of electron transfer layer is to have higher electron mobility, effectively the organic molecule material of conduction electron.
Preferably, the material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2, a kind of in 4-triazole derivative and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).More preferably, the material of electron transfer layer is Bphen.
Preferably, the thickness of electron transfer layer is 40～200nm.More preferably, the thickness of electron transfer layer is 100nm.
Preferably, the material of electron injecting layer is cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) and lithium fluoride (LiF) in a kind of.More preferably, the material of the second electron injecting layer is LiF.
Preferably, the thickness of electron injecting layer is 0.5～10nm.More preferably, the thickness of electron injecting layer is 1nm.
Negative electrode is arranged on electron injecting layer.
The material of negative electrode is zinc compound, work function for the metal of-4.0eV～-5.5eV and silicon compound are according to mass ratio 1:(0.5～2): the composite material that (1～5) is mixed to form.
Preferably, the material of negative electrode is zinc compound, work function for the metal of-4.0eV～-5.5eV and silicon compound are according to mass ratio 1:(1～2): the composite material that (3～5) are mixed to form.
Particularly, zinc compound is zinc oxide (ZnO), zinc sulphide (ZnS), zinc selenide (ZnSe) and zinc chloride (ZnCl
2) in a kind of, the metal that work function is-4.0eV～-5.5eV is a kind of in aluminium (Al), silver (Ag), platinum (Pt) and golden (Au), silicon compound is silicon monoxide (SiO), silicon dioxide (SiO
2) and sodium metasilicate (Na
2siO
3) in a kind of.
Preferably, the thickness of negative electrode is 80～300nm.
Negative electrode prepared by the present invention is comprised of zinc compound, silicon compound and metal, zinc compound refractive index is larger, be greater than the refractive index of organic layer, therefore, light is not launched total reflection can be occurred from luminescent layer, avoided the loss of total reflection, meanwhile, the transparency range of zinc compound is wider, has reached micron order, can make most of visible ray see through, improve the transmitance of device; Silicon compound particle is larger, is microspheroidal, makes the adding of silicon compound inner formation of rete arrange orderly micro-sphere structure, thus light encounter micro-spherical particle and can form in the middle of scattering makes to get back to device to the light scattering of both sides transmitting, improve light extraction efficiency; Metal improves the concentration of electronics, thereby is conducive to improve the exciton recombination probability of device, and the reflection that simultaneously improves negative electrode, meanwhile, also can improve the stability of device.
Second aspect, the invention provides a kind of preparation method of organic electroluminescence device, comprises the following steps:
Clean conductive anode substrate of glass is provided;
In described conductive anode substrate of glass, thermal resistance evaporation is prepared hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively, and the condition of described thermal resistance evaporation is pressure 5 * 10
-5～2 * 10
-3pa, the evaporation speed of described hole injection layer and electron injecting layer is 1～10nm/s, the evaporation speed of described hole transmission layer, luminescent layer and electron transfer layer is 0.1～1nm/s;
On described electron injecting layer, prepare negative electrode, described negative electrode is prepared by electron beam evaporation plating, concrete operations are for be-4.0eV～-5.5eV by zinc compound, work function metal and silicon compound is according to mass ratio 1:(0.5～2): (1～5) is mixed to get composite material, wherein, described zinc compound is a kind of in zinc oxide, zinc sulphide, zinc selenide and zinc chloride, the metal that described work function is-4.0eV～-5.5eV is a kind of in aluminium, silver, platinum and gold, and described silicon compound is a kind of in silicon monoxide, silicon dioxide and sodium metasilicate; By described composite material by electron beam evaporation plating on described electron injecting layer, condition is energy density 10～100W/cm
2, obtain described negative electrode;
After above step completes, obtain described organic electroluminescence device.
Preferably, conductive anode substrate of glass is a kind of in indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) and indium-zinc oxide glass (IZO).More preferably, conductive anode substrate of glass is ITO.
Preferably, conductive anode substrate of glass is carried out to photoetching treatment, be then cut into needed size.
By the cleaning to conductive anode substrate of glass, remove surperficial organic pollution.
Particularly, the clean operation of conductive anode substrate of glass is: conductive anode substrate of glass is used to liquid detergent, each ultrasonic cleaning of deionized water 15min successively, remove surperficial organic pollution, obtain clean conductive anode substrate of glass.
By the method for thermal resistance evaporation, in clean conductive anode substrate of glass, evaporation arranges hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively.Wherein, the condition of thermal resistance evaporation is pressure 5 * 10
-5～2 * 10
-3pa, the evaporation speed of hole injection layer and electron injecting layer is 1～10nm/s, the evaporation speed of described hole transmission layer, luminescent layer and electron transfer layer is 0.1～1nm/s.
Preferably, the material of hole injection layer is molybdenum trioxide (MoO
3), tungstic acid (WO
3) and vanadic oxide (V
2o
5) in a kind of.More preferably, the material of hole injection layer is WO
3.
Preferably, the thickness of hole injection layer is 20～80nm.More preferably, the thickness of hole injection layer is 30nm.
Preferably, the material of hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, a kind of in 4'-diamines (NPB).More preferably, the material of hole transmission layer is NPB.
Preferably, the thickness of hole transmission layer is 20～60nm.More preferably, the thickness of hole transmission layer is 40nm.
Preferably, the material of luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis-(betanaphthyl) anthracene (ADN), 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1,1 '-biphenyl (BCzVBi) and oxine aluminium (Alq
3) in a kind of.More preferably, the material of luminescent layer is Alq
3.
Preferably, the thickness of luminescent layer is 5～40nm.More preferably, the thickness of luminescent layer is 20nm.
The material of electron transfer layer is to have higher electron mobility, effectively the organic molecule material of conduction electron.
Preferably, the material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,2, a kind of in 4-triazole derivative and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi).
More preferably, 1,2,4-triazole derivative is 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ).More preferably, the material of electron transfer layer is Bphen.
Preferably, the thickness of electron transfer layer is 40～200nm.More preferably, the thickness of electron transfer layer is 100nm.
Preferably, the material of electron injecting layer is cesium carbonate (Cs
2cO
3), cesium fluoride (CsF), nitrine caesium (CsN
3) and lithium fluoride (LiF) in a kind of.More preferably, the material of the second electron injecting layer is LiF.
Preferably, the thickness of electron injecting layer is 0.5～10nm.More preferably, the thickness of electron injecting layer is 1nm.
Negative electrode is arranged on electron injecting layer by the method for electron beam evaporation plating.
Electron beam evaporation plating condition is energy density 10～100W/cm
2.
Concrete operations are for be-4.0eV～-5.5eV by zinc compound, work function metal and silicon compound is according to mass ratio 1:(0.5～2): (1～5) is mixed to get composite material, wherein, zinc compound is a kind of in zinc oxide, zinc sulphide, zinc selenide and zinc chloride, the metal that work function is-4.0eV～-5.5eV is a kind of in aluminium, silver, platinum and gold, and silicon compound is a kind of in silicon monoxide, silicon dioxide and sodium metasilicate; By composite material by electron beam evaporation plating on electron injecting layer, obtain negative electrode.
Preferably, the metal that is-4.0eV～-5.5eV by zinc compound, work function and silicon compound are according to mass ratio 1:(1～2): (3～5) are mixed to get composite material.
Preferably, the thickness of negative electrode is 80～300nm.
Negative electrode prepared by the present invention is comprised of zinc compound, silicon compound and metal, zinc compound refractive index is larger, be greater than the refractive index of organic layer, therefore, light is not launched total reflection can be occurred from luminescent layer, avoided the loss of total reflection, meanwhile, the transparency range of zinc compound is wider, has reached micron order, can make most of visible ray see through, improve the transmitance of device; Silicon compound particle is larger, is microspheroidal, makes the adding of silicon compound inner formation of rete arrange orderly micro-sphere structure, thus light encounter micro-spherical particle and can form in the middle of scattering makes to get back to device to the light scattering of both sides transmitting, improve light extraction efficiency; Metal improves the concentration of electronics, thereby is conducive to improve the exciton recombination probability of device, and the reflection that simultaneously improves negative electrode, meanwhile, also can improve the stability of device.
The present invention has following beneficial effect:
(1) cathode material of the organic electroluminescence device that prepared by the present invention is the composite material that zinc compound, silicon compound and metal mixed form, make luminous energy more effectively arrive at conductive anode substrate of glass, thereby improve the luminous efficiency of device, and improved electronic injection ability, the stability of device.
(2) preparation method of the present invention is simple, be easy to control and operation, and raw material easily obtains.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structure chart of the organic electroluminescence device that provides of the embodiment of the present invention 1;
Fig. 2 is the current density of organic electroluminescence device and the graph of a relation of current efficiency that the organic electroluminescence device that provides of the embodiment of the present invention 1 and comparative example provide.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Be below specific embodiment and comparative example part, wherein, "/" represents stacked, and ": " represents the mass ratio of the former with the latter.
Embodiment 1
A preparation method for organic electroluminescence device, comprises the following steps:
(1) by ito glass liquid detergent, each ultrasonic cleaning of deionized water 15min for substrate, obtain clean conductive anode substrate of glass;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 8 * 10
-5under the condition of Pa, thermal resistance evaporation hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively in clean conductive anode substrate of glass;
Particularly, in the present embodiment, the material of hole injection layer is WO
3, thickness is 30nm; The material of hole transmission layer is NPB, and thickness is 40nm; The material of luminescent layer is Alq3, and thickness is 20nm; The material of electron transfer layer is Bphen, and thickness is 100nm; The material of electron injecting layer is LiF, and thickness is 1nm;
Wherein, WO
3with the evaporation speed of LiF be 3nm/s, the evaporation speed of NPB, Alq3 and Bphen is 0.2nm/s;
(3) at pressure, be 8 * 10
-5under the condition of Pa, on electron injecting layer, prepare negative electrode:
Particularly, by ZnSe, SiO
2according to mass ratio 1:1:3, be mixed to get composite material with Ag, by this composite material by electron beam evaporation plating on electron injecting layer, condition is energy density 35W/cm
2, obtaining negative electrode, thickness is 250nm;
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: ITO/WO
3/ NPB/Alq3/Bphen/LiF/ZnSe:SiO
2: Ag (1:1:3).
Fig. 1 is the structural representation of the organic electroluminescence device of the present embodiment.As shown in Figure 1, the structure of this organic electroluminescence device comprises conductive anode substrate of glass 10, hole injection layer 20, hole transmission layer 30, luminescent layer 40, electron transfer layer 50, electron injecting layer 60 and the negative electrode 70 stacking gradually.
Embodiment 2
A preparation method for organic electroluminescence device, comprises the following steps:
(1) by AZO liquid detergent, each ultrasonic cleaning of deionized water 15min for substrate of glass, obtain clean conductive anode substrate of glass;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 2 * 10
-3under the condition of Pa, thermal resistance evaporation hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively in clean conductive anode substrate of glass;
Particularly, in the present embodiment, the material of hole injection layer is MoO
3, thickness is 80nm; The material of hole transmission layer is NPB, and thickness is 60nm; The material of luminescent layer is ADN, and thickness is 5nm; The material of electron transfer layer is TAZ, and thickness is 200nm; The material of electron injecting layer is CsF, and thickness is 10nm;
Wherein, MoO
3with the evaporation speed of CsF be 10nm/s, the evaporation speed of NPB, ADN and TAZ is 0.1nm/s;
(3) at pressure, be 2 * 10
-3under the condition of Pa, on electron injecting layer, prepare negative electrode:
Particularly, ZnO, SiO and Al are mixed to get to composite material according to mass ratio 1:0.5:1, by this composite material by electron beam evaporation plating on electron injecting layer, condition is energy density 100W/cm
2, obtaining negative electrode, thickness is 80nm;
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: AZO/MoO
3/ NPB/ADN/TAZ/CsF/ZnO:SiO:Al (1:1:3).
Embodiment 3
A preparation method for organic electroluminescence device, comprises the following steps:
(1) by IZO liquid detergent, each ultrasonic cleaning of deionized water 15min for substrate of glass, obtain clean conductive anode substrate of glass;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 5 * 10
-5under the condition of Pa, thermal resistance evaporation hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively in clean conductive anode substrate of glass;
Particularly, in the present embodiment, the material of hole injection layer is WO
3, thickness is 20nm; The material of hole transmission layer is TAPC, and thickness is 30nm; The material of luminescent layer is BCzVBi, and thickness is 40nm; The material of electron transfer layer is TPBi, and thickness is 60nm; The material of electron injecting layer is Cs
2cO
3, thickness is 0.5nm;
Wherein, WO
3and Cs
2cO
3evaporation speed be 1nm/s, the evaporation speed of TAPC, BCzVBi and TPBi is 1nm/s;
(3) at pressure, be 5 * 10
-5under the condition of Pa, on electron injecting layer, prepare negative electrode:
Particularly, by ZnS, Na
2siO
3according to mass ratio 1:2:5, be mixed to get composite material with Pt, by this composite material by electron beam evaporation plating on electron injecting layer, condition is energy density 10W/cm
2, obtaining negative electrode, thickness is 300nm;
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: IZO/WO
3/ TAPC/BCzVBi/TPBi/Cs
2cO
3/ ZnS:Na
2siO
3: Pt (1:2:5).
Embodiment 4
A preparation method for organic electroluminescence device, comprises the following steps:
(1) by IZO liquid detergent, each ultrasonic cleaning of deionized water 15min for substrate of glass, obtain clean conductive anode substrate of glass;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 5 * 10
-4under the condition of Pa, thermal resistance evaporation hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively in clean conductive anode substrate of glass;
Particularly, in the present embodiment, the material of hole injection layer is V
2o
5, thickness is 30nm; The material of hole transmission layer is TCTA, and thickness is 20nm; The material of luminescent layer is DCJTB, and thickness is 5nm; The material of electron transfer layer is Bphen, and thickness is 40nm; The material of electron injecting layer is CsN
3, thickness is 1nm;
Wherein, V
2o
5and CsN
3evaporation speed be 5nm/s, the evaporation speed of TCTA, DCJTB and Bphen is 0.2nm/s;
(3) at pressure, be 5 * 10
-4under the condition of Pa, on electron injecting layer, prepare negative electrode:
Particularly, by ZnCl
2, SiO
2according to mass ratio 1:2:3, be mixed to get composite material with Au, by this composite material by electron beam evaporation plating on electron injecting layer, condition is energy density 50W/cm
2, obtaining negative electrode, thickness is 200nm;
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: IZO/V
2o
5/ TCTA/DCJTB/Bphen/CsN
3/ ZnCl
2: SiO
2: Au (1:2:3).
Comparative example
A preparation method for organic electroluminescence device, comprises the following steps:
(1) by ito glass liquid detergent, each ultrasonic cleaning of deionized water 15min for substrate, obtain clean conductive anode substrate of glass;
(2) in high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), pressure is 8 * 10
-5under the condition of Pa, thermal resistance evaporation hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode successively in clean conductive anode substrate of glass;
Particularly, in the present embodiment, the material of hole injection layer is WO
3, thickness is 30nm; The material of hole transmission layer is NPB, and thickness is 40nm; The material of luminescent layer is Alq3, and thickness is 20nm; The material of electron transfer layer is Bphen, and thickness is 100nm; The material of electron injecting layer is LiF, and thickness is 1nm; The material of negative electrode is Ag, and thickness is 150;
Wherein, WO
3, LiF and Ag evaporation speed be 3nm/s, the evaporation speed of NPB, Alq3 and Bphen is 0.2nm/s;
After above step completes, obtain a kind of organic electroluminescence device, structure is specifically expressed as: ITO/WO
3/ NPB/Alq3/Bphen/LiF/Ag.
Utilize the Keithley2400 test electric property of U.S. Keithley company, colorimeter (Japanese Konica Minolta company, model: CS-100A) test brightness and colourity, fiber spectrometer (U.S. marine optics company, model: USB4000) testing electroluminescent spectrum.
Fig. 2 is the organic electroluminescence device of embodiment 1 and the current density of the organic electroluminescence device of comparative example and the graph of a relation of current efficiency.Wherein, curve 1 is the current density of organic electroluminescence device and the graph of a relation of current efficiency of embodiment 1; The current density of organic electroluminescence device and the graph of a relation of current efficiency that curve 2 provides for comparative example.
As can see from Figure 2, under different current densities, the current efficiency of embodiment 1 is large than comparative example all, the maximum current efficiency of embodiment 1 is 13.25cd/A, and that comparative example is only 10.44cd/A, this explanation, in organic electroluminescence device prepared by the present invention, luminous energy more effectively arrives at conductive anode substrate of glass, has higher transmitance and light extraction efficiency.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. an organic electroluminescence device, it is characterized in that, comprise the conductive anode substrate of glass stacking gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode, the material of described negative electrode is zinc compound, the metal that work function is-4.0eV～-5.5eV and silicon compound are according to mass ratio 1:(0.5～2): the composite material that (1～5) is mixed to form, wherein, described zinc compound is zinc oxide, zinc sulphide, a kind of in zinc selenide and zinc chloride, the metal that described work function is-4.0eV～-5.5eV is aluminium, silver, a kind of in platinum and gold, described silicon compound is silicon monoxide, a kind of in silicon dioxide and sodium metasilicate.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, described conductive anode substrate of glass is a kind of in indium tin oxide glass, aluminium zinc oxide glass and indium-zinc oxide glass.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, the material of described hole injection layer is a kind of in molybdenum trioxide, tungstic acid and vanadic oxide; The material of hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4''-tri-(carbazole-9-yl) triphenylamine and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, a kind of in 4'-diamines; The material of luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans, 9,10-bis-(betanaphthyl) anthracene, 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1, a kind of in 1 '-biphenyl and oxine aluminium; The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline, 1,2, a kind of in 4-triazole derivative and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene; The material of electron injecting layer is a kind of in cesium carbonate, cesium fluoride, nitrine caesium and lithium fluoride.
4. organic electroluminescence device as claimed in claim 1, it is characterized in that, the material of described negative electrode is zinc compound, work function for the metal of-4.0eV～-5.5eV and silicon compound are according to mass ratio 1:(1～2): the composite material that (3～5) are mixed to form.
5. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
Clean conductive anode substrate of glass is provided;
In described conductive anode substrate of glass, thermal resistance evaporation is prepared hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer successively, and the condition of described thermal resistance evaporation is pressure 5 * 10
-5～2 * 10
-3pa, the evaporation speed of described hole injection layer and electron injecting layer is 1～10nm/s, the evaporation speed of described hole transmission layer, luminescent layer and electron transfer layer is 0.1～1nm/s;
On described electron injecting layer, prepare negative electrode, described negative electrode is prepared by electron beam evaporation plating, concrete operations are for be-4.0eV～-5.5eV by zinc compound, work function metal and silicon compound is according to mass ratio 1:(0.5～2): (1～5) is mixed to get composite material, wherein, described zinc compound is a kind of in zinc oxide, zinc sulphide, zinc selenide and zinc chloride, the metal that described work function is-4.0eV～-5.5eV is a kind of in aluminium, silver, platinum and gold, and described silicon compound is a kind of in silicon monoxide, silicon dioxide and sodium metasilicate; By described composite material by electron beam evaporation plating on described electron injecting layer, condition is energy density 10～100W/cm
2, obtain described negative electrode;
After above step completes, obtain described organic electroluminescence device.
6. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, described conductive anode substrate of glass is a kind of in indium tin oxide glass, aluminium zinc oxide glass and indium-zinc oxide glass.
7. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the material of described hole injection layer is a kind of in molybdenum trioxide, tungstic acid and vanadic oxide; The material of hole transmission layer is 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane, 4,4', 4''-tri-(carbazole-9-yl) triphenylamine and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, a kind of in 4'-diamines; The material of luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans, 9,10-bis-(betanaphthyl) anthracene, 4,4 '-bis-(9-ethyl-3-carbazole vinyl)-1, a kind of in 1 '-biphenyl and oxine aluminium; The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline, 1,2, a kind of in 4-triazole derivative and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene; The material of electron injecting layer is a kind of in cesium carbonate, cesium fluoride, nitrine caesium and lithium fluoride.
8. the preparation method of organic electroluminescence device as claimed in claim 5, it is characterized in that, the metal that is-4.0eV～-5.5eV by described zinc compound, work function and silicon compound are according to mass ratio 1:(1～2): (3～5) are mixed to get composite material.
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