CN104183717A - Organic light-emitting device and preparation method thereof - Google Patents

Organic light-emitting device and preparation method thereof Download PDF

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Publication number
CN104183717A
CN104183717A CN201310192463.8A CN201310192463A CN104183717A CN 104183717 A CN104183717 A CN 104183717A CN 201310192463 A CN201310192463 A CN 201310192463A CN 104183717 A CN104183717 A CN 104183717A
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luminescent layer
layer
main part
mass ratio
bis
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周明杰
钟铁涛
王平
张娟娟
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Priority to CN201310192463.8A priority Critical patent/CN104183717A/en
Publication of CN104183717A publication Critical patent/CN104183717A/en
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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
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/30—Coordination compounds
    • H10K85/341—Transition metal complexes, e.g. Ru(II)polypyridine complexes
    • H10K85/342—Transition metal complexes, e.g. Ru(II)polypyridine complexes comprising iridium
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/615—Polycyclic condensed aromatic hydrocarbons, e.g. anthracene
    • H10K85/624—Polycyclic condensed aromatic hydrocarbons, e.g. anthracene containing six or more rings
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/631—Amine compounds having at least two aryl rest on at least one amine-nitrogen atom, e.g. triphenylamine

Abstract

The invention discloses an organic light-emitting device which includes a conductive anode substrate, a hole injection layer, a hole transmission layer, a light-emitting layer, an electron transmission layer, an electron injection layer and a cathode layer, which are sequentially laminated. The material of the light-emitting layer is mixture formed through mixing of an object material, a first subject material and a second subject material. In the light-emitting layer of the organic light-emitting device, a mass ratio of the object material and the first subject material is reduced in an echelon manner from a side close to the hole transmission layer to a side far from the hole transmission layer, and the mass ratio of the object material and the second subject material is improved in an echelon manner from the side close to the hole transmission layer to the side far from the hole transmission layer. Through gradual mixing of the subject materials and the object material, the energy conversion efficiency of subjects and an object is improved. The invention also discloses a preparation method for the organic light-emitting device.

Description

Organic electroluminescence device and preparation method thereof
Technical field
The present invention relates to organic electroluminescent field, relate in particular to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) has advantages of that some are unique: (1) OLED belongs to diffused area source, does not need by extra light-conducting system, to obtain large-area white light source as light-emitting diode (LED); (2) due to the diversity of luminous organic material, OLED illumination is the light of design color as required, no matter be little Molecule OLEDs at present, or polymer organic LED (PLED) has all obtained and has comprised white-light spectrum at the light of interior all colours; (3) OLED can make on as glass, pottery, metal, plastic or other material at multiple substrate, freer when this makes to design lighting source; (4) adopt the mode of making OLED demonstration to make OLED illumination panel, can in illumination, show information; (5) OLED also can be used as controlled look in illuminator, allows user to regulate light atmosphere according to individual demand.
The luminous efficiency of organic electroluminescence device is to evaluate the important indicator of organic electroluminescence device performance always.The material of the luminescent layer of traditional organic electroluminescence device normally Uniform Doped the material of main part of guest materials, because the energy conversion efficiency of Subjective and Objective is relatively low, cause the luminous efficiency of traditional organic electroluminescence device poor.
Summary of the invention
Based on this, be necessary to provide organic electroluminescence device that a kind of luminous efficiency is higher and preparation method thereof.
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode layer that stack gradually;
The material of described luminescent layer is the mixture that guest materials, the first material of main part and the second material of main part are mixed to form;
The mass ratio of guest materials described in described luminescent layer and described the first material of main part reduces from the side near described hole transmission layer to the side echelon away from described hole transmission layer;
The mass ratio of guest materials described in described luminescent layer and described the second material of main part improves from the side near described hole transmission layer to the side echelon away from described hole transmission layer;
Described guest materials is that three (2-phenylpyridines) close iridium, acetopyruvic acid two (2-phenylpyridine) iridium or three [2-(p-methylphenyl) pyridine] closes iridium;
Described the first material of main part is 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 9,9 '-(1,3-phenyl) two-9H-carbazole, 4,4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine, 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane or the 3-tert-butyl group-9,10-bis-(2-naphthalene) anthracene;
Described the second material of main part is 2,2 '-(1,3-phenyl) two [5-(4-tert-butyl-phenyl)-1,3,4-oxadiazoles], 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene, 2,8-bis-(diphenyl phosphine oxygen base) dibenzo [b, d] thiophene, 4,7-diphenyl-1,10-phenanthroline or N-aryl benzimidazole;
The mass ratio of guest materials described in described luminescent layer and described the first material of main part is 0.1～10:100;
The mass ratio of guest materials described in described luminescent layer and described the second material of main part is 0.1～10:100.
In one embodiment, described luminescent layer is comprised of the first luminescent layer stacking gradually and thickness is identical, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer, and described the first luminescent layer is laminated on described hole transmission layer;
Described in described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described the 4th luminescent layer and described the 5th luminescent layer, guest materials successively decreases than echelon with the quality of described the first material of main part;
Described in described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described the 4th luminescent layer and described the 5th luminescent layer, guest materials increases progressively than echelon with the quality of described the second material of main part.
In one embodiment, guest materials described in described the first luminescent layer equates with the mass ratio of described the second material of main part with the described guest materials in described the 5th luminescent layer with the mass ratio of described the first material of main part;
Guest materials described in described the 3rd luminescent layer equates with the mass ratio of described the second material of main part with described guest materials with the mass ratio of described the first material of main part;
And the described guest materials in described the second luminescent layer and the mass ratio of described the second material of main part are the twices of the mass ratio of described guest materials in described the first luminescent layer and described the second material of main part.
In one embodiment, the thickness of described luminescent layer is 10nm～30nm.
In one embodiment, the material of described hole injection layer is the hole mobile material doped with metal oxide;
Described metal oxide is MoO 3, WO 3, V 2o 5or ReO 3;
Described hole mobile material is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 4,4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane;
The mass ratio of described metal oxide and described hole mobile material is 25～35:100;
The thickness of described hole injection layer is 10nm～15nm.
In one embodiment, the material of described hole transmission layer is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 4,4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane;
The thickness of described hole transmission layer is 30nm～50nm.
In one embodiment, the material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline, 4,7-diphenyl-1,10-Phen, 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium, oxine aluminium, 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The thickness of described electron transfer layer is 10nm～60nm.
In one embodiment, the material of described electron injecting layer is the electron transport material doped with the first salt and the second salt;
Described the first salt is LiF, LiN 3, Li 3n, CsF, CsN 3or Cs 3n;
Described the second salt is Li 2sO 4, Na 2sO 4, K 2sO 4, Rb 2sO 4or Cs 2sO 4;
Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 4,7-diphenyl-1,10-Phen, 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium, oxine aluminium, 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The mass ratio of described the first salt and described electron transport material is 25～35:100;
The mass ratio of described the second salt and described electron transport material is 6～25:100;
The thickness of described electron injecting layer is 15nm～45nm.
A preparation method for organic electroluminescence device, comprises the steps:
Conductive anode substrate is carried out to surface preparation;
In described conductive anode substrate, evaporation forms hole injection layer and hole transmission layer successively;
On described hole transmission layer, evaporation forms luminescent layer, wherein, the material of described luminescent layer is guest materials, the mixture that the first material of main part and the second material of main part are mixed to form, the mass ratio of guest materials described in described luminescent layer and described the first material of main part reduces from the side near described hole transmission layer to the side echelon away from described hole transmission layer, the mass ratio of guest materials described in described luminescent layer and described the second material of main part improves from the side near described hole transmission layer to the side echelon away from described hole transmission layer, described guest materials is that three (2-phenylpyridines) close iridium, acetopyruvic acid two (2-phenylpyridine) iridium or three [2-(p-methylphenyl) pyridine] closes iridium, described the first material of main part is 4, 4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 9, 9 '-(1, 3-phenyl) two-9H-carbazole, 4, 4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4, 4 '-benzidine, 1, 1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane or the 3-tert-butyl group-9, 10-bis-(2-naphthalene) anthracene, described the second material of main part is 2, 2 '-(1, 3-phenyl) two [5-(4-tert-butyl-phenyl)-1, 3, 4-oxadiazoles], 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthrolene, 2, 8-bis-(diphenyl phosphine oxygen base) dibenzo [b, d] thiophene, 4, 7-diphenyl-1, 10-phenanthroline or N-aryl benzimidazole, the mass ratio of guest materials described in described luminescent layer and described the first material of main part is 0.1～10:100, the mass ratio of guest materials described in described luminescent layer and described the second material of main part is 0.1～10:100, and
On described luminescent layer, evaporation forms electron transfer layer, electron injecting layer and cathode layer successively.
In one embodiment, the described step that evaporation forms luminescent layer on described hole transmission layer is:
On described hole transmission layer, evaporation forms the first identical luminescent layer of thickness successively, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer, described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described the 4th luminescent layer and described the 5th luminescent layer form described luminescent layer, described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described in described the 4th luminescent layer and described the 5th luminescent layer, guest materials successively decreases than echelon with the quality of described the first material of main part, described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described in described the 4th luminescent layer and described the 5th luminescent layer, guest materials increases progressively than echelon with the quality of described the second material of main part.
In the luminescent layer of this organic electroluminescence device, the mass ratio of guest materials and the first material of main part reduces from the side near hole transmission layer to the side echelon away from hole transmission layer, the mass ratio of guest materials and the second material of main part improves from the side near hole transmission layer to the side echelon away from hole transmission layer, by the gradual mixing of material of main part and guest materials, improved the energy conversion efficiency of Subjective and Objective.With respect to traditional organic electroluminescence device, the luminous efficiency of this organic electroluminescence device is higher.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 2 is the structural representation of luminescent layer of an embodiment of organic electroluminescence device as shown in Figure 1;
Fig. 3 is the preparation method's of organic electroluminescence device flow chart as shown in Figure 1.
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.
The organic electroluminescence device of an execution mode as shown in Figure 1, comprises the conductive anode substrate 10, hole injection layer 20, hole transmission layer 30, luminescent layer 40, electron transfer layer 50, electron injecting layer 60 and the cathode layer 70 that stack gradually.
Conductive anode substrate 10 can be indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO).At one, preferably in embodiment, conductive anode substrate 10 is indium tin oxide glass (ITO).
The thickness of the conductive layer of anode conducting substrate 10 can be 80nm～150nm.
The material of hole injection layer 20 can be the hole mobile material doped with metal oxide.
Metal oxide can be MoO 3, WO 3, V 2o 5or ReO 3.
Hole mobile material can be N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines (NPB), 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA), 4,4 '-bis-(9-carbazole) biphenyl (CBP), N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine (TPD) or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC).
The mass ratio of metal oxide and hole mobile material is 25～35:100.
The thickness of hole injection layer 20 can be 10nm～15nm.
The material of hole transmission layer 30 can be N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines (NPB), 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA), 4,4 '-bis-(9-carbazole) biphenyl (CBP), N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine (TPD) or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC).
The thickness of hole transmission layer 30 can be 30nm～50nm.
The mixture that the material of luminescent layer 40 can be mixed to form for guest materials, the first material of main part and the second material of main part.
The mass ratio of guest materials and the first material of main part is 0.1～10:100.
The mass ratio of guest materials and the second material of main part is 0.1～10:100.
The first material of main part is different with the second material of main part.
Guest materials can close iridium (Ir (ppy) for three (2-phenylpyridines) 3), acetopyruvic acid two (2-phenylpyridine) iridium (Ir (ppy) 2(acac)) or three [2-(p-methylphenyl) pyridines] close iridium (Ir (mppy) 3).
The first material of main part can be 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA), 9,9 '-(1,3-phenyl) two-9H-carbazole (mCP), 4,4 '-bis-(9-carbazole) biphenyl (CBP), N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine (TPD), 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC) or the 3-tert-butyl group-9,10-bis-(2-naphthalene) anthracene (MADN).
The second material of main part can be 2,2'-(1,3-phenyl) two [5-(4-tert-butyl-phenyl)-1,3,4-oxadiazoles] (OXD-7), 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene (BCP), 2,8-bis-(diphenyl phosphine oxygen base) dibenzo [b, d] thiophene (PO15), 4,7-diphenyl-1,10-phenanthroline (Bphen) or N-aryl benzimidazole (TPBI).
The thickness of luminescent layer 40 can be 10nm～30nm.
In luminescent layer 40, the mass ratio of guest materials and the first material of main part reduces to the side echelon away from hole transmission layer 30 from the side near hole transmission layer 30, and the mass ratio of guest materials and the second material of main part improves from the side near hole transmission layer 30 to the side echelon away from hole transmission layer 30.
In conjunction with Fig. 2, in a specific embodiment, luminescent layer 40 is comprised of the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49 that stack gradually and thickness is identical, and the first luminescent layer 41 is laminated on hole transmission layer 30.
The material of the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49 is the mixture that guest materials, the first material of main part and the second material of main part are mixed to form, and in above-mentioned each layer, guest materials and the mass ratio of the first material of main part and the mass ratio of guest materials and the second material of main part are single value.
In the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49, guest materials successively decreases than echelon with the quality of the first material of main part, and in the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49, guest materials increases progressively than echelon with the quality of the second material of main part.
In the present embodiment, the first luminescent layer 41 that thickness is identical, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49 altogether five-layer structure form luminescent layer 40.In other embodiments, can also form luminescent layer 40 by two-layer structure, three-decker, four-layer structure, six layers of structure, seven-layer structure etc.
In the present embodiment, in the first luminescent layer 41, guest materials equates with the mass ratio of the second material of main part with the guest materials in the 5th luminescent layer 49 with the mass ratio of the first material of main part, in the 3rd luminescent layer 45, guest materials equates with the mass ratio of the second material of main part with guest materials with the mass ratio of the first material of main part, and the mass ratio of the guest materials in the second luminescent layer 43 and the second material of main part is the twice of the mass ratio of guest materials in the first luminescent layer 41 and the second material of main part.That is to say, in the present embodiment, remember that in the first luminescent layer 41, guest materials equates a with the guest materials in the 5th luminescent layer 49 with the mass ratio of the first material of main part with the mass ratio of the second material of main part, again owing to being echelon doping, in the mass ratio of the guest materials in the second luminescent layer 43 and the second material of main part and the 4th luminescent layer 47, the mass ratio of guest materials and the first material of main part equates to be 2a, guest materials in the 3rd luminescent layer 45 equates to be 3a with the mass ratio of the mass ratio of the first material of main part and guest materials and the second material of main part, guest materials in the 4th luminescent layer 47 equates to be 4a with the mass ratio of guest materials in the mass ratio of the second material of main part and the second luminescent layer 43 and the first material of main part, in the 5th luminescent layer 49, in the mass ratio of guest materials and the second material of main part and the first luminescent layer 41, the mass ratio of guest materials and the first material of main part equates to be 5a.
In other embodiment, guest materials in the first luminescent layer 41 in the mass ratio of guest materials and the first material of main part and the 5th luminescent layer 49 and the mass ratio of the second material of main part also can be unequal, in the 3rd luminescent layer 45, the mass ratio of the mass ratio of guest materials and the first material of main part and guest materials and the second material of main part also can be unequal, and the mass ratio of the guest materials in the second luminescent layer 43 and the second material of main part can not be also the twice of the mass ratio of guest materials in the first luminescent layer 41 and the second material of main part.
The material of electron transfer layer 50 can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 4, and 7-diphenyl-1,10-Phen (BCP), 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium (BAlq), oxine aluminium (Alq 3), 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ) or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI).
Electron transfer layer 50 can thickness be 10nm～60nm.
The material of electron injecting layer 60 can be the electron transport material doped with the first salt and the second salt.
The first salt can be LiF, LiN 3, Li 3n, CsF, CsN 3or Cs 3n.
The second salt can Li 2sO 4, Na 2sO 4, K 2sO 4, Rb 2sO 4or Cs 2sO 4.
Electron transport material can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 4, and 7-diphenyl-1,10-Phen (BCP), 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium (BAlq), oxine aluminium (Alq 3), 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ) or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI).
The mass ratio of the first salt and electron transport material is 25～35:100.
The mass ratio of the second salt and electron transport material is 6～25:100.
The thickness of electron injecting layer 60 can be 15nm～45nm.
The material of cathode layer 70 can be silver (Ag), aluminium (Al) or gold (Au).
The thickness of cathode layer 70 can be 50nm～200nm.
In the luminescent layer 40 of this organic electroluminescence device, the mass ratio of guest materials and the first material of main part reduces from the side near hole transmission layer 30 to the side echelon away from hole transmission layer 30, in luminescent layer 40, the mass ratio of guest materials and the second material of main part improves from the side near hole transmission layer 30 to the side echelon away from hole transmission layer 30, by the gradual mixing of material of main part and guest materials, improved the energy conversion efficiency of Subjective and Objective.With respect to traditional organic electroluminescence device, the luminous efficiency of this organic electroluminescence device is higher.
The preparation method of above-mentioned organic electroluminescence device as shown in Figure 3, comprises the steps:
S10, conductive anode substrate 10 is carried out to surface preparation.
Conductive anode substrate 10 can be indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) or indium-zinc oxide glass (IZO).At one, preferably in embodiment, conductive anode substrate 10 is indium tin oxide glass (ITO).
The thickness of the conductive layer of anode conducting substrate 10 can be 80nm～150nm.
The operation of surface preparation can be: successively conductive anode substrate 10 is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, obtain clean conductive anode substrate 10.Then the conductive layer of clean conductive anode substrate 10 is carried out to surface activation process, increase oxygen content and the work function of the conductive layer of conductive anode substrate 10.
All in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Meanwhile, above-mentioned cleaning all adopts supersonic wave cleaning machine to carry out.
Surface activation process can be for adopting ultraviolet-ozone (UV-ozone) to process 30～50 minutes the anode after cleaning-drying.
S20, in conductive anode substrate 10, evaporation forms hole injection layer 20 and hole transmission layer 30 successively.
Obviously, hole injection layer 20 is formed on the conductive layer of conductive anode substrate 10.
In present embodiment, in vacuum degree, be 1 * 10 -5pa～1 * 10 -3pa, evaporation rate is condition under, on the conductive layer of conductive anode substrate 10, evaporation forms hole injection layer 20.
The material of hole injection layer 20 can be the hole mobile material doped with metal oxide.
Metal oxide can be MoO 3, WO 3, V 2o 5or ReO 3.
Hole mobile material can be N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines (NPB), 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA), 4,4 '-bis-(9-carbazole) biphenyl (CBP), N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine (TPD) or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC).
The mass ratio of metal oxide and hole mobile material is 25～35:100.
The thickness of hole injection layer 20 can be 10nm～15nm.
In present embodiment, in vacuum degree, be 1 * 10 -5pa～1 * 10 -3pa, evaporation rate is condition under, on hole injection layer 20, evaporation forms hole transmission layer 30.
The material of hole transmission layer 30 can be N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines (NPB), 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA), 4,4 '-bis-(9-carbazole) biphenyl (CBP), N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine (TPD) or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC).
The thickness of hole transmission layer 30 can be 30nm～50nm.
S30, on hole transmission layer 30, evaporation forms luminescent layer 40.
In present embodiment, in vacuum degree, be 1 * 10 -5pa～1 * 10 -3pa, evaporation rate is condition under, on hole transmission layer 30, evaporation forms luminescent layer 40.
The mixture that the material of luminescent layer 40 can be mixed to form for guest materials, the first material of main part and the second material of main part.
The mass ratio of guest materials and the first material of main part is 0.1～10:100.
The mass ratio of guest materials and the second material of main part is 0.1～10:100.
The first material of main part is different with the second material of main part.
Guest materials can close iridium (Ir (ppy) for three (2-phenylpyridines) 3), acetopyruvic acid two (2-phenylpyridine) iridium (Ir (ppy) 2(acac)) or three [2-(p-methylphenyl) pyridines] close iridium (Ir (mppy) 3).
The first material of main part can be 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine (TCTA), 9,9 '-(1,3-phenyl) two-9H-carbazole (mCP), 4,4 '-bis-(9-carbazole) biphenyl (CBP), N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine (TPD), 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC) or the 3-tert-butyl group-9,10-bis-(2-naphthalene) anthracene (MADN).
The second material of main part can be 2,2 '-(1,3-phenyl) two [5-(4-tert-butyl-phenyl)-1,3,4-oxadiazoles] (OXD-7), 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene (BCP), 2,8-bis-(diphenyl phosphine oxygen base) dibenzo [b, d] thiophene (PO15), 4,7-diphenyl-1,10-phenanthroline (Bphen) or N-aryl benzimidazole (TPBI).
The thickness of luminescent layer 40 can be 10nm～30nm.
In luminescent layer 40, the mass ratio of guest materials and the first material of main part reduces to the side echelon away from hole transmission layer 30 from the side near hole transmission layer 30, and the mass ratio of guest materials and the second material of main part improves from the side near hole transmission layer 30 to the side echelon away from hole transmission layer 30.
In conjunction with Fig. 2, in a specific embodiment, luminescent layer 40 is comprised of the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49 that stack gradually and thickness is identical, and the first luminescent layer 41 is laminated on hole transmission layer 30.
The material of the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49 is the mixture that guest materials, the first material of main part and the second material of main part are mixed to form, and in above-mentioned each layer, guest materials and the mass ratio of the first material of main part and the mass ratio of guest materials and the second material of main part are single value.
In the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49, guest materials successively decreases than echelon with the quality of the first material of main part, and in the first luminescent layer 41, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49, guest materials increases progressively than echelon with the quality of the second material of main part.
In the present embodiment, the first luminescent layer 41 that thickness is identical, the second luminescent layer 43, the 3rd luminescent layer 45, the 4th luminescent layer 47 and the 5th luminescent layer 49 altogether five-layer structure form luminescent layer 40.In other embodiments, can also form luminescent layer 40 by two-layer structure, three-decker, four-layer structure, six layers of structure, seven-layer structure etc.
In the present embodiment, in the first luminescent layer 41, guest materials equates with the mass ratio of the second material of main part with the guest materials in the 5th luminescent layer 49 with the mass ratio of the first material of main part, in the 3rd luminescent layer 45, guest materials equates with the mass ratio of the second material of main part with guest materials with the mass ratio of the first material of main part, and the mass ratio of the guest materials in the second luminescent layer 43 and the second material of main part is the twice of the mass ratio of guest materials in the first luminescent layer 41 and the second material of main part.That is to say, in the present embodiment, remember that in the first luminescent layer 41, guest materials equates a with the guest materials in the 5th luminescent layer 49 with the mass ratio of the first material of main part with the mass ratio of the second material of main part, again owing to being echelon doping, in the mass ratio of the guest materials in the second luminescent layer 43 and the second material of main part and the 4th luminescent layer 47, the mass ratio of guest materials and the first material of main part equates to be 2a, guest materials in the 3rd luminescent layer 45 equates to be 3a with the mass ratio of the mass ratio of the first material of main part and guest materials and the second material of main part, guest materials in the 4th luminescent layer 47 equates to be 4a with the mass ratio of guest materials in the mass ratio of the second material of main part and the second luminescent layer 43 and the first material of main part, in the 5th luminescent layer 49, in the mass ratio of guest materials and the second material of main part and the first luminescent layer 41, the mass ratio of guest materials and the first material of main part equates to be 5a.
In other embodiment, guest materials in the first luminescent layer 41 in the mass ratio of guest materials and the first material of main part and the 5th luminescent layer 49 and the mass ratio of the second material of main part also can be unequal, in the 3rd luminescent layer 45, the mass ratio of the mass ratio of guest materials and the first material of main part and guest materials and the second material of main part also can be unequal, and the mass ratio of the guest materials in the second luminescent layer 43 and the second material of main part can not be also the twice of the mass ratio of guest materials in the first luminescent layer 41 and the second material of main part.
S40, on luminescent layer 40, evaporation forms electron transfer layer 50, electron injecting layer 60 and cathode layer 70 successively.
In present embodiment, in vacuum degree 1 * 10 -5pa～1 * 10 -3pa, evaporation rate condition under, on luminescent layer 40, evaporation forms electron transfer layer 50.
The material of electron transfer layer 50 can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 4, and 7-diphenyl-1,10-Phen (BCP), 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium (BAlq), oxine aluminium (Alq 3), 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ) or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI).
Electron transfer layer 50 can thickness be 10nm～60nm.
In present embodiment, in vacuum degree 1 * 10 -5pa～1 * 10 -3pa, evaporation rate condition under, on electron transfer layer 50, evaporation forms electron injecting layer 60.
The material of electron injecting layer 60 can be the electron transport material doped with the first salt and the second salt.
The first salt can be LiF, LiN 3, Li 3n, CsF, CsN 3or Cs 3n.
The second salt can Li 2sO 4, Na 2sO 4, K 2sO 4, Rb 2sO 4or Cs 2sO 4.
Electron transport material can be 4,7-diphenyl-1,10-phenanthroline (Bphen), 4, and 7-diphenyl-1,10-Phen (BCP), 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium (BAlq), oxine aluminium (Alq 3), 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole (TAZ) or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI).
The mass ratio of the first salt and electron transport material is 25～35:100.
The mass ratio of the second salt and electron transport material is 6～25:100.
The thickness of electron injecting layer 60 can be 15nm～45nm.
In present embodiment, in vacuum degree 1 * 10 -5pa～1 * 10 -3pa, evaporation rate condition under, on electron injecting layer 60, evaporation forms cathode layer 70.
The material of cathode layer 70 can be silver (Ag), aluminium (Al) or gold (Au).
The thickness of cathode layer 70 can be 50nm～200nm.
In the luminescent layer 40 of the organic electroluminescence device that the preparation method of this organic electroluminescence device prepares, the mass ratio of guest materials and the first material of main part reduces from the side near hole transmission layer 30 to the side echelon away from hole transmission layer 30, in luminescent layer 40, the mass ratio of guest materials and the second material of main part improves from the side near hole transmission layer 30 to the side echelon away from hole transmission layer 30, by the gradual mixing of material of main part and guest materials, improved the energy conversion efficiency of Subjective and Objective.With respect to traditional organic electroluminescence device, the luminous efficiency of this organic electroluminescence device is higher.
Be below specific embodiment and comparative example part, the test and the Preparation equipment that in embodiment, use comprise: high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), the USB4000 fiber spectrometer testing electroluminescent spectrum of U.S. marine optics Ocean Optics, the Keithley2400 test electric property of U.S. Keithley company, CS-100A colorimeter test brightness and the colourity of Japanese Konica Minolta company.
Embodiment 1
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the MoO that adulterated 3nPB, MoO 3with the mass ratio of NPB be 30:100, the thickness of hole injection layer is 12.5nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is NPB, and the thickness of hole transmission layer is 40nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on hole transmission layer, evaporation forms the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer successively.The first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer form luminescent layer.The material of the first luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TCTA and OXD-7, Ir (ppy) 3with the mass ratio of TCTA be 10:100, Ir (ppy) 3with the mass ratio of OXD-7 be 2:100.The material of the second luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TCTA and OXD-7, Ir (ppy) 3with the mass ratio of TCTA be 8:100, Ir (ppy) 3with the mass ratio of OXD-7 be 4:100.The material of the 3rd luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TCTA and OXD-7, Ir (ppy) 3with the mass ratio of TCTA be 6:100, Ir (ppy) 3with the mass ratio of OXD-7 be 6:100.The material of the 4th luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TCTA and OXD-7, Ir (ppy) 3with the mass ratio of TCTA be 4:100, Ir (ppy) 3with the mass ratio of OXD-7 be 8:100.The material of the 5th luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TCTA and OXD-7, Ir (ppy) 3with the mass ratio of TCTA be 2:100, Ir (ppy) 3with the mass ratio of OXD-7 be 10:100.The thickness of the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer is all identical, and the gross thickness of luminescent layer is 30nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on the 5th luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is Bphen, and the thickness of electron transfer layer is 35nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with LiF and Li 2sO 4bphen, the mass ratio of LiF and Bphen is 30:100, Li 2sO 4with the mass ratio of Bphen be 15:100, the thickness of electron injecting layer is 35nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Ag, and the thickness of cathode layer is 125nm.
Embodiment 2
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the WO that adulterated 3tCTA, WO 3with the mass ratio of TCTA be 25:100, the thickness of hole injection layer is 10nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is TCTA, and the thickness of hole transmission layer is 30nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on hole transmission layer, evaporation forms the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer successively.The first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer form luminescent layer.The material of the first luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of mCP and BCP, Ir (ppy) 2(acac) be 8:100 with the mass ratio of mCP, Ir (ppy) 2(acac) be 1.6:100 with the mass ratio of BCP.The material of the second luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of mCP and BCP, Ir (ppy) 2(acac) be 6.4:100 with the mass ratio of mCP, Ir (ppy) 2(acac) be 3.2:100 with the mass ratio of BCP.The material of the 3rd luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of mCP and BCP, Ir (ppy) 2(acac) be 4.8:100 with the mass ratio of mCP, Ir (ppy) 2(acac) be 4.8:100 with the mass ratio of BCP.The material of the 4th luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of mCP and BCP, Ir (ppy) 2(acac) be 3.2:100 with the mass ratio of mCP, Ir (ppy) 2(acac) be 6.4:100 with the mass ratio of BCP.The material of the 5th luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of mCP and BCP, Ir (ppy) 2(acac) be 1.6:100 with the mass ratio of mCP, Ir (ppy) 2(acac) be 8:100 with the mass ratio of BCP.The thickness of the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer is all identical, and the gross thickness of luminescent layer is 27nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the 5th luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is BCP, and the thickness of electron transfer layer is 10nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with LiN 3and Na 2sO 4bCP, LiN 3with the mass ratio of BCP be 25:100, Na 2sO 4with the mass ratio of BCP be 25:100, the thickness of electron injecting layer is 45nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Al, and the thickness of cathode layer is 50nm.
Embodiment 3
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the V that adulterated 2o 5cBP, V 2o 5with the mass ratio of CBP be 35:100, the thickness of hole injection layer is 15nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is CBP, and the thickness of hole transmission layer is 50nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on hole transmission layer, evaporation forms the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer successively.The first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer form luminescent layer.The material of the first luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of CBP and PO15, Ir (mppy) 3with the mass ratio of CBP be 6:100, Ir (mppy) 3with the mass ratio of PO15 be 1.2:100.The material of the second luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of CBP and PO15, Ir (mppy) 3with the mass ratio of CBP be 4.8:100, Ir (mppy) 3with the mass ratio of PO15 be 2.4:100.The material of the 3rd luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of CBP and PO15, Ir (mppy) 3with the mass ratio of CBP be 3.6:100, Ir (mppy) 3with the mass ratio of PO15 be 3.6:100.The material of the 4th luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of CBP and PO15, Ir (mppy) 3with the mass ratio of CBP be 2.4:100, Ir (mppy) 3with the mass ratio of PO15 be 4.8:100.The material of the 5th luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of CBP and PO15, Ir (mppy) 3with the mass ratio of CBP be 1.2:100, Ir (mppy) 3with the mass ratio of PO15 be 6:100.The thickness of the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer is all identical, and the gross thickness of luminescent layer is 24nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the 5th luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is BAlq, and the thickness of electron transfer layer is 60nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with Li 3n and K 2sO 4bAlq, Li 3the mass ratio of N and BAlq is 35:100, K 2sO 4with the mass ratio of BAlq be 6:100, the thickness of electron injecting layer is 15nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Au, and the thickness of cathode layer is 200nm.
Embodiment 4
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the ReO that adulterated 3tPD, ReO 3with the mass ratio of TPD be 30:100, the thickness of hole injection layer is 13nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is TPD, and the thickness of hole transmission layer is 40nm.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on hole transmission layer, evaporation forms the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer successively.The first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer form luminescent layer.The material of the first luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TPD and Bphen, Ir (ppy) 3with the mass ratio of TPD be 4:100, Ir (ppy) 3with the mass ratio of Bphen be 0.8:100.The material of the second luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TPD and Bphen, Ir (ppy) 3with the mass ratio of TPD be 3.2:100, Ir (ppy) 3with the mass ratio of Bphen be 1.6:100.The material of the 3rd luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TPD and Bphen, Ir (ppy) 3with the mass ratio of TPD be 2.4:100, Ir (ppy) 3with the mass ratio of Bphen be 2.4:100.The material of the 4th luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TPD and Bphen, Ir (ppy) 3with the mass ratio of TPD be 1.6:100, Ir (ppy) 3with the mass ratio of Bphen be 3.2:100.The material of the 5th luminescent layer is Ir (ppy) 3, the mixture that is mixed to form of TPD and Bphen, Ir (ppy) 3with the mass ratio of TPD be 0.8:100, Ir (ppy) 3with the mass ratio of Bphen be 4:100.The thickness of the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer is all identical, and the gross thickness of luminescent layer is 24nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the 5th luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is Alq 3, the thickness of electron transfer layer is 30nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with CsF and Rb 2sO 4alq 3, CsF and Alq 3mass ratio be 30:100, Rb 2sO 4and Alq 3mass ratio be 10:100, the thickness of electron injecting layer is 30nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Ag, and the thickness of cathode layer is 100nm.
Embodiment 5
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 1 * 10 -5pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the MoO that adulterated 3tAPC, MoO 3with the mass ratio of TAPC be 25:100, the thickness of hole injection layer is 10nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is TAPC, and the thickness of hole transmission layer is 40nm.
In vacuum degree, be 1 * 10 -4pa, evaporation rate condition under, on hole transmission layer, evaporation forms the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer successively.The first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer form luminescent layer.The material of the first luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of TAPC and TPBI, Ir (ppy) 2(acac) and the mass ratio of TAPC be 2:100, Ir (ppy) 2(acac) and the mass ratio of TPBI be 0.4:100.The material of the second luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of TAPC and TPBI, Ir (ppy) 2(acac) and the mass ratio of TAPC be 1.6:100, Ir (ppy) 2(acac) and the mass ratio of TPBI be 0.8:100.The material of the 3rd luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of TAPC and TPBI, Ir (ppy) 2(acac) and the mass ratio of TAPC be 1.2:100, Ir (ppy) 2(acac) and the mass ratio of TPBI be 1.2:100.The material of the 4th luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of TAPC and TPBI, Ir (ppy) 2(acac) and the mass ratio of TAPC be 0.8:100, Ir (ppy) 2(acac) and the mass ratio of TPBI be 1.6:100.The material of the 5th luminescent layer is Ir (ppy) 2(acac), the mixture that is mixed to form of TAPC and TPBI, Ir (ppy) 2(acac) and the mass ratio of TAPC be 0.4:100, Ir (ppy) 2(acac) and the mass ratio of TPBI be 2:100.The thickness of the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer is all identical, and the gross thickness of luminescent layer is 20nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the 5th luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is TAZ, and the thickness of electron transfer layer is 50nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with CsN 3and Cs 2sO 4tAZ, CsN 3with the mass ratio of TAZ be 30:100, Cs 2sO 4with the mass ratio of TAZ be 10:100, the thickness of electron injecting layer is 30nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Al, and the thickness of cathode layer is 100nm.
Embodiment 6
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 1 * 10 -3pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the WO that adulterated 3nPB, WO 3with the mass ratio of NPB be 30:100, the thickness of hole injection layer is 12nm.
In vacuum degree, be 1 * 10 -3pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is NPB, and the thickness of hole transmission layer is 40nm.
In vacuum degree, be 1 * 10 -3pa, evaporation rate condition under, on hole transmission layer, evaporation forms the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer successively.The first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer form luminescent layer.The material of the first luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of MADN and OXD-7, Ir (mppy) 3with the mass ratio of MADN be 0.5:100, Ir (mppy) 3with the mass ratio of OXD-7 be 0.1:100.The material of the second luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of MADN and OXD-7, Ir (mppy) 3with the mass ratio of MADN be 0.4:100, Ir (mppy) 3with the mass ratio of OXD-7 be 0.2:100.The material of the 3rd luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of MADN and OXD-7, Ir (mppy) 3with the mass ratio of MADN be 0.3:100, Ir (mppy) 3with the mass ratio of OXD-7 be 0.3:100.The material of the 4th luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of MADN and OXD-7, Ir (mppy) 3with the mass ratio of MADN be 0.2:100, Ir (mppy) 3with the mass ratio of OXD-7 be 0.4:100.The material of the 5th luminescent layer is Ir (mppy) 3, the mixture that is mixed to form of MADN and OXD-7, Ir (mppy) 3with the mass ratio of MADN be 0.1:100, Ir (mppy) 3with the mass ratio of OXD-7 be 0.5:100.The thickness of the first luminescent layer, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer is all identical, and the gross thickness of luminescent layer is 10nm.
In vacuum degree, be 1 * 10 -3pa, evaporation rate condition under, on the 5th luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is TPBI, and the thickness of electron transfer layer is 30nm.
In vacuum degree, be 1 * 10 -3pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with Cs 3n and Cs 2sO 4tPBI, Cs 3the mass ratio of N and TPBI is 30:100, Cs 2sO 4with the mass ratio of TPBI be 10:100, the thickness of electron injecting layer is 30nm.
In vacuum degree, be 1 * 10 -3pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Al, and the thickness of cathode layer is 100nm.
Comparative example
An organic electroluminescence device, comprises the conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the negative electrode that stack gradually.Preparation process is:
It is the ito glass of 100nm that conductive layer thickness is provided, and successively ito glass is carried out to liquid detergent cleaning, washed with de-ionized water, acetone cleaning and ethanol and clean, and all in triplicate, each scavenging period is 5min in above-mentioned cleaning, and be 5min interval time.Then the ITO layer of the ito glass cleaning is carried out to surface activation process, increase oxygen content and the work function of ITO layer.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on the ITO of ito glass layer, evaporation forms hole injection layer.The material of hole injection layer is the V that adulterated 2o 5cBP, V 2o 5with the mass ratio of CBP be 30:100, the thickness of hole injection layer is 12nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on hole injection layer, evaporation forms hole transmission layer.The material of hole transmission layer is TCTA, and the thickness of hole transmission layer is 40nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on hole transmission layer, evaporation forms luminescent layer.The material of luminescent layer is the Ir that adulterated (ppy) 3mADN, Ir (ppy) 3with the mass ratio of MADN be 7:100, the thickness of luminescent layer is 20nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on luminescent layer, evaporation forms electron transfer layer.The material of electron transfer layer is Bphen, and the thickness of electron transfer layer is 40nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron transfer layer, evaporation forms electron injecting layer.The material of electron injecting layer is doped with Cs 3the Bphen of N, Cs 3the mass ratio of N and Bphen is 28:100, and the thickness of electron injecting layer is 32.5nm.
In vacuum degree, be 5 * 10 -5pa, evaporation rate condition under, on electron injecting layer, evaporation forms cathode layer.The material of cathode layer is Al, and the thickness of cathode layer is 138nm.
Adopt luminance meter CS-100A and digital sourcemeter Keithley2400 synchro measure, the organic electroluminescence device that embodiment 1～6 and comparative example are made carries out luminous efficiency testing experiment, by programming Control with can be calculated test result as shown in the table:
? Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Comparative example
Efficiency (lm/W) 26.2 25.4 24.7 23.9 23.4 22.5 13.2
The luminous efficiency of the organic electroluminescence device that the luminous efficiency of the organic electroluminescence device that embodiment 1～embodiment 6 prepares as can be seen from the above table prepares apparently higher than comparative example, has approximately improved more than 0.7 times.
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 conductive anode substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the cathode layer that stack gradually;
The material of described luminescent layer is the mixture that guest materials, the first material of main part and the second material of main part are mixed to form;
The mass ratio of guest materials described in described luminescent layer and described the first material of main part reduces from the side near described hole transmission layer to the side echelon away from described hole transmission layer;
The mass ratio of guest materials described in described luminescent layer and described the second material of main part improves from the side near described hole transmission layer to the side echelon away from described hole transmission layer;
Described guest materials is that three (2-phenylpyridines) close iridium, acetopyruvic acid two (2-phenylpyridine) iridium or three [2-(p-methylphenyl) pyridine] closes iridium;
Described the first material of main part is 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 9,9 '-(1,3-phenyl) two-9H-carbazole, 4,4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine, 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane or the 3-tert-butyl group-9,10-bis-(2-naphthalene) anthracene;
Described the second material of main part is 2,2 '-(1,3-phenyl) two [5-(4-tert-butyl-phenyl)-1,3,4-oxadiazoles], 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene, 2,8-bis-(diphenyl phosphine oxygen base) dibenzo [b, d] thiophene, 4,7-diphenyl-1,10-phenanthroline or N-aryl benzimidazole;
The mass ratio of guest materials described in described luminescent layer and described the first material of main part is 0.1～10:100;
The mass ratio of guest materials described in described luminescent layer and described the second material of main part is 0.1～10:100.
2. organic electroluminescence device according to claim 1, it is characterized in that, described luminescent layer is comprised of the first luminescent layer stacking gradually and thickness is identical, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer, and described the first luminescent layer is laminated on described hole transmission layer;
Described in described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described the 4th luminescent layer and described the 5th luminescent layer, guest materials successively decreases than echelon with the quality of described the first material of main part;
Described in described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described the 4th luminescent layer and described the 5th luminescent layer, guest materials increases progressively than echelon with the quality of described the second material of main part.
3. organic electroluminescence device according to claim 1, it is characterized in that, guest materials described in described the first luminescent layer equates with the mass ratio of described the second material of main part with the described guest materials in described the 5th luminescent layer with the mass ratio of described the first material of main part;
Guest materials described in described the 3rd luminescent layer equates with the mass ratio of described the second material of main part with described guest materials with the mass ratio of described the first material of main part;
And the described guest materials in described the second luminescent layer and the mass ratio of described the second material of main part are the twices of the mass ratio of described guest materials in described the first luminescent layer and described the second material of main part.
4. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described luminescent layer is 10nm～30nm.
5. organic electroluminescence device according to claim 1, is characterized in that, the material of described hole injection layer is the hole mobile material doped with metal oxide;
Described metal oxide is MoO 3, WO 3, V 2o 5or ReO 3;
Described hole mobile material is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 4,4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane;
The mass ratio of described metal oxide and described hole mobile material is 25～35:100;
The thickness of described hole injection layer is 10nm～15nm.
6. organic electroluminescence device according to claim 1, is characterized in that, the material of described hole transmission layer is N, N '-diphenyl-N, N '-bis-(1-naphthyl)-1,1 '-biphenyl-4,4 '-diamines, 4,4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 4,4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4,4 '-benzidine or 1,1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane;
The thickness of described hole transmission layer is 30nm～50nm.
7. organic electroluminescence device according to claim 1, it is characterized in that, the material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline, 4,7-diphenyl-1,10-Phen, 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium, oxine aluminium, 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The thickness of described electron transfer layer is 10nm～60nm.
8. organic electroluminescence device according to claim 1, is characterized in that, the material of described electron injecting layer is the electron transport material doped with the first salt and the second salt;
Described the first salt is LiF, LiN 3, Li 3n, CsF, CsN 3or Cs 3n;
Described the second salt is Li 2sO 4, Na 2sO 4, K 2sO 4, Rb 2sO 4or Cs 2sO 4;
Described electron transport material is 4,7-diphenyl-1,10-phenanthroline, 4,7-diphenyl-1,10-Phen, 4-biphenyl phenolic group-bis-(2-methyl-oxine) close aluminium, oxine aluminium, 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1,2,4-triazole or 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene;
The mass ratio of described the first salt and described electron transport material is 25～35:100;
The mass ratio of described the second salt and described electron transport material is 6～25:100;
The thickness of described electron injecting layer is 15nm～45nm.
9. a preparation method for organic electroluminescence device, is characterized in that, comprises the steps:
Conductive anode substrate is carried out to surface preparation;
In described conductive anode substrate, evaporation forms hole injection layer and hole transmission layer successively;
On described hole transmission layer, evaporation forms luminescent layer, wherein, the material of described luminescent layer is guest materials, the mixture that the first material of main part and the second material of main part are mixed to form, the mass ratio of guest materials described in described luminescent layer and described the first material of main part reduces from the side near described hole transmission layer to the side echelon away from described hole transmission layer, the mass ratio of guest materials described in described luminescent layer and described the second material of main part improves from the side near described hole transmission layer to the side echelon away from described hole transmission layer, described guest materials is that three (2-phenylpyridines) close iridium, acetopyruvic acid two (2-phenylpyridine) iridium or three [2-(p-methylphenyl) pyridine] closes iridium, described the first material of main part is 4, 4 ', 4 ' '-tri-(carbazole-9-yl) triphenylamine, 9, 9 '-(1, 3-phenyl) two-9H-carbazole, 4, 4 '-bis-(9-carbazole) biphenyl, N, N '-bis-(3-aminomethyl phenyl)-N, N '-diphenyl-4, 4 '-benzidine, 1, 1-bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane or the 3-tert-butyl group-9, 10-bis-(2-naphthalene) anthracene, described the second material of main part is 2, 2 '-(1, 3-phenyl) two [5-(4-tert-butyl-phenyl)-1, 3, 4-oxadiazoles], 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthrolene, 2, 8-bis-(diphenyl phosphine oxygen base) dibenzo [b, d] thiophene, 4, 7-diphenyl-1, 10-phenanthroline or N-aryl benzimidazole, the mass ratio of guest materials described in described luminescent layer and described the first material of main part is 0.1～10:100, the mass ratio of guest materials described in described luminescent layer and described the second material of main part is 0.1～10:100, and
On described luminescent layer, evaporation forms electron transfer layer, electron injecting layer and cathode layer successively.
10. the preparation method of organic electroluminescence device according to claim 1, is characterized in that, the described step that evaporation forms luminescent layer on described hole transmission layer is:
On described hole transmission layer, evaporation forms the first identical luminescent layer of thickness successively, the second luminescent layer, the 3rd luminescent layer, the 4th luminescent layer and the 5th luminescent layer, described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described the 4th luminescent layer and described the 5th luminescent layer form described luminescent layer, described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described in described the 4th luminescent layer and described the 5th luminescent layer, guest materials successively decreases than echelon with the quality of described the first material of main part, described the first luminescent layer, described the second luminescent layer, described the 3rd luminescent layer, described in described the 4th luminescent layer and described the 5th luminescent layer, guest materials increases progressively than echelon with the quality of described the second material of main part.
CN201310192463.8A 2013-05-22 2013-05-22 Organic light-emitting device and preparation method thereof Pending CN104183717A (en)

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Application publication date: 20141203