CN104064675A - Organic electroluminescent device and preparation method thereof - Google Patents

Organic electroluminescent device and preparation method thereof Download PDF

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CN104064675A
CN104064675A CN201310092194.8A CN201310092194A CN104064675A CN 104064675 A CN104064675 A CN 104064675A CN 201310092194 A CN201310092194 A CN 201310092194A CN 104064675 A CN104064675 A CN 104064675A
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layer
ion barrier
barrier layer
electron transfer
organic electroluminescence
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周明杰
冯小明
张振华
王平
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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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    • 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]
    • H10K50/18—Carrier blocking layers
    • 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]
    • H10K50/14—Carrier transporting layers
    • H10K50/16—Electron transporting layers
    • H10K50/165—Electron transporting layers comprising dopants
    • 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
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass

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  • Engineering & Computer Science (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
  • Manufacturing & Machinery (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

Disclosed is an organic electroluminescent device. The organic electroluminescent device comprises a substrate, an anode, a cavity transmission layer, a luminescent layer, a cavity barrier layer, an ion barrier layer, an electron transmission layer, a cathode and a packaging cover which are successively stacked. The materials of the ion barrier layer are selected from at least one from titanium oxides, zinc oxides, zirconium oxides and tin oxides. The materials of the electron transmission layer comprise an electron transmission material and a doping material doped in the electron transmission material. The doping material is lithium, sodium, potassium, rubidium or caesium. The electron transmission material is 2-(4-biphenylyl)-5-(4-tert-butyl)phenyl-1,3,4-oxadiazol, (8-hydroxyquinoline)aluminum, 4,7-diphenyl-phenanthroline, 1,3,5-(1-pheyl-1H-benzimidazole-2-ly)benzene, 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, or a 1,2,4-triazole derivative. The life of the organic electroluminescent device is quite long. The invention also provides a preparation method of an organic electroluminescent device.

Description

Organic electroluminescence device and preparation method thereof
Technical field
The present invention relates to a kind of organic electroluminescence device and preparation method thereof.
Background technology
The principle of luminosity of organic electroluminescence device (OLED) is based under the effect of extra electric field, and electronics is injected into organic lowest unocccupied molecular orbital (LUMO) from negative electrode, and hole is injected into organic highest occupied molecular orbital (HOMO) from anode.Electronics and hole meet at luminescent layer, compound, form exciton, exciton moves under electric field action, and energy is passed to luminescent material, and excitation electron is from ground state transition to excitation state, excited energy, by Radiation-induced deactivation, produces photon, discharges luminous energy.
In existing OLED, in electron transfer layer, conventionally use alkali-metal compound to adulterate, but in alkali-metal compound, alkali metal ion volume is little, diffusivity is strong, and in the organic layer in OLED, diffusion length is long, makes the life-span of organic electroluminescence device shorter.
Summary of the invention
Based on this, be necessary to provide organic electroluminescence device that a kind of life-span grows and preparation method thereof.
A kind of organic electroluminescence device, comprise the substrate stacking gradually, anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode, the material of described ion barrier layer is selected from titanyl compound, the oxide of zinc, at least one in the oxide of zirconium and the oxide of tin, the material of described electron transfer layer comprises electron transport material and is entrained in the dopant material in described electron transport material, described dopant material is lithium, sodium, potassium, rubidium or caesium, described electron transport material is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1, 3, 4-oxadiazole, (oxine)-aluminium, 4, 7-diphenyl-o-phenanthroline, 1, 3, 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthrolene or 1, 2, 4-triazole derivative,
Described organic electroluminescence device also comprises cap, and described cap is packaged in described anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in described substrate.
Therein in an embodiment,, the thickness of described ion barrier layer is 2nm～7nm, the thickness of described electron transfer layer is 50nm～200nm.
In an embodiment, the mass ratio of dopant material and described electron transport material described in described electron transfer layer is 10:100～50:100 therein.
In an embodiment, described ion barrier layer is total two-layer therein, and two-layer ion barrier layer stacks gradually.
Therein in an embodiment, the material of described luminescent layer is mixture or the fluorescent material that material of main part and guest materials doping form, described material of main part is selected from 4, 4'-bis-(9-carbazole) biphenyl, oxine aluminium, 1, 3, 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, at least one in 4'-diamines, described guest materials is selected from 4-(dintrile methyl)-2-butyl-6-(1, 1, 7, 7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans, two (4, 6-difluorophenyl pyridine-N, C2) pyridine formyl closes iridium, two (4, 6-difluorophenyl pyridine)-tetra-(1-pyrazolyl) boric acid closes iridium, two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanedione) close iridium, three (1-phenyl-isoquinolin) close iridium and three (2-phenylpyridine) and close at least one in iridium, described fluorescent material is selected from 4, 4'-bis-(2, 2-diphenylethyllene)-1, 1'-biphenyl, oxine aluminium, 4, two [4-(di-p-tolyl amino) styryl] biphenyl and 5 of 4'-, 6, 11, at least one in 12-tetraphenyl naphthonaphthalene, the mass ratio of described guest materials and described material of main part is 1:100～10:100.
A preparation method for organic electroluminescence device, comprises the following steps:
The anode, hole transmission layer, luminescent layer and the hole blocking layer that stack gradually are prepared in surface at substrate;
Prepare ion barrier layer at the surface sputtering of described hole blocking layer, the material of described ion barrier layer is selected from least one in oxide, the oxide of zirconium and the oxide of tin of titanyl compound, zinc;
Surface at described ion barrier layer adopts thermal resistance evaporation technology, electron transport material and alkali-metal compound are carried out to Evaporation preparation electron transfer layer simultaneously, alkali metal in described alkali-metal compound is lithium, sodium, potassium, rubidium or caesium, described electron transport material is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1, 3, 4-oxadiazole, (oxine)-aluminium, 4, 7-diphenyl-o-phenanthroline, 1, 3, 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthrolene or 1, 2, 4-triazole derivative,
Negative electrode is prepared on surface at described electron transfer layer; And
Use cap that described anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode are packaged in described substrate.
In an embodiment, the thickness of described ion barrier layer is 2nm～7nm therein, and the thickness of described electron transfer layer is 50nm～200nm.
In an embodiment, described alkali-metal compound is alkali-metal fluoride, alkali-metal carbonate compound, alkali-metal triazo-compound, alkali-metal nitride or alkali-metal hydroboron therein.
In an embodiment, described cap is formed with host cavity therein, and described anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode are contained in described host cavity.
In an embodiment, described ion barrier layer is total two-layer therein, and two-layer ion barrier layer stacks gradually.
Above-mentioned organic electroluminescence device and preparation method thereof, the dopant material in electron transfer layer is lithium, sodium, potassium, rubidium or caesium, adopts the electron transfer layer of doped structure, has reduced the drive current of organic electroluminescence device; The ion barrier layer that inorganic material forms is set between electron transfer layer and luminescent layer, ion barrier layer is comparatively form compact and stable, ion barrier layer has good diffusion-restricted effect to alkali metal, can stop that alkali metal spreads to luminescent layer, avoid causing exciton cancellation, make the life-span of organic electroluminescence device longer.
Brief description of the drawings
Fig. 1 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 2 is the preparation method's of the organic electroluminescence device of an execution mode flow chart.
Embodiment
Below in conjunction with the drawings and specific embodiments, organic electroluminescence device and preparation method thereof is further illustrated.
Refer to Fig. 1, the organic electroluminescence device 100 of an execution mode comprises the substrate 10, anode 20, hole transmission layer 30, luminescent layer 40, hole blocking layer 50, ion barrier layer 60, electron transfer layer 70, negative electrode 80 and the cap 90 that stack gradually.
The material of substrate 10 is glass.
Anode 20 is formed at the surface of substrate 10.The material of anode 20 is transparent conductive oxide.Concrete, the material of anode 20 is selected from least one in indium tin oxide (ITO), indium-zinc oxide (IZO), aluminium zinc oxide (AZO) and gallium zinc oxide (GZO), is preferably ITO.The thickness of anode 20 is 70nm～200nm.
Hole transmission layer 30 is formed at the surface of anode 20.The material of hole transmission layer 30 is mixture or the hole mobile material that hole mobile material and dopant form.Hole mobile material is selected from N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, 4'-diamines (NPB), 4, 4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine (m-MTDATA), N, N'-diphenyl-N, N'-bis-(3-aminomethyl phenyl)-1, 1'-biphenyl-4, 4'-diamines (TPD), N, N, N', N '-tetramethoxy phenyl)-benzidine (MeO-TPD), 2, two (the N of 7-, N-bis-(4-methoxyphenyl) amino)-9, 9-spiral shell two fluorenes (MeO-Sprio-TPD), 4, 4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) and 1, 1-bis-(4-(N, N '-bis-(p-tolyl) amino) phenyl) at least one in cyclohexane (TAPC).Dopant is selected from 2,3, and 5,6-tetrafluoro-7,7 ', 8,8 '-tetra-cyanogen quinone-bismethanes (F4-TCNQ), 1,3,4,5,7,8-hexafluoro-tetra-cyanogen-diformazan is to naphthoquinones (F6-TNAP) and 2,2'-(2,5-dicyano-3,6-difluoro cyclohexane-2,5-diene-Isosorbide-5-Nitrae-bis-subunit) at least one in two malononitrile (F2-HCNQ).In mixture, the mass ratio of dopant and hole mobile material is 2:100～30:100.The thickness of hole transmission layer 30 is 20nm～60nm.
Luminescent layer 40 is formed at the surface of hole transmission layer 30.The material of luminescent layer 40 is mixture or the fluorescent material that material of main part and guest materials doping form.Material of main part is selected from 4,4'-bis-(9-carbazole) biphenyl (CBP), oxine aluminium (Alq 3), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi) and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, at least one in 4'-diamines (NPB).Guest materials is selected from 4-(dintrile methyl)-2-butyl-6-(1, 1, 7, 7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), two (4, 6-difluorophenyl pyridine-N, C2) pyridine formyl closes iridium (FIrpic), two (4, 6-difluorophenyl pyridine)-tetra-(1-pyrazolyl) boric acid closes iridium (FIr6), two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanedione) close iridium (Ir (MDQ) 2 (acac)), three (1-phenyl-isoquinolin) close iridium (Ir (piq) 3) and three (2-phenylpyridines) close at least one in iridium (Ir (ppy) 3).The mass ratio of guest materials and material of main part is 1:100～10:100.Fluorescent material is selected from 4,4'-bis-(2,2-diphenylethyllene)-1,1'-biphenyl (DPVBi), oxine aluminium (Alq 3), 4, at least one in two [4-(di-p-tolyl amino) styryl] biphenyl (DPAVBi) of 4'-and 5,6,11,12-tetraphenyl naphthonaphthalene (Rubrene).The material of luminescent layer 40 is preferably oxine aluminium (Alq 3).The thickness of luminescent layer 40 is 5nm～20nm, is preferably 15nm.
Hole blocking layer 50 is formed at the surface of luminescent layer 40.The material of hole blocking layer 50 is selected from two (2-methyl-oxine-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium (BAlq), oxine gallium (Gaq 3), oxine indium (Inq 3), oxine zinc (Znq 2), oxine beryllium (Beq 2) and three (5-methylol-oxine) aluminium (AlOq) at least one.The thickness of hole blocking layer 50 is 5nm～10nm.
The material of hole blocking layer 50 is organometallic complex, has better film forming stability and compactness, and its thermal stability is good, can play a very good protection to luminescent layer 40; Meanwhile, hole blocking layer 50 blocking holes transmit to electron transfer layer 70 from luminescent layer 40, control the recombination region of exciton at luminescent layer 40.
Ion barrier layer 60 is formed at the surface of hole blocking layer 50.The material of ion barrier layer 60 is selected from least one in oxide, the oxide of zirconium and the oxide of tin of titanyl compound, zinc.Titanyl compound is titanium monoxide (TiO) or titanium dioxide (TiO 2).The oxide of zinc is zinc oxide (ZnO).The oxide of zirconium is zirconium dioxide (ZrO 2).The oxide of tin is tin monoxide (SnO) or tin ash (SnO 2).The material of ion barrier layer 60 is preferably TiO 2, ZnO, ZrO 2or SnO 2.The thickness of ion barrier layer 60 is 2nm～7nm.
Further, ion barrier layer 60 is total two-layer, and two-layer ion barrier layer 60 stacks gradually.
Electron transfer layer 70 is formed at the surface of ion barrier layer 60.The material of electron transfer layer 70 comprises electron transport material and is entrained in the dopant material in electron transport material.Dopant material is lithium (Li), sodium (Na), potassium (K), rubidium (Rb) or caesium (Cs).Electron transport material is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1,3,4-oxadiazole (PBD), (oxine)-aluminium (Alq3), 4,7-diphenyl-o-phenanthroline (Bphen), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi), 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene (BCP) or 1,2,4-triazole derivative (TAZ).In electron transfer layer 70, the mass ratio of dopant material and electron transport material is 10:100～50:100.The thickness of electron transfer layer 70 is 50nm～200nm.
Negative electrode 80 is formed at the surface of electron transfer layer 70.The material of negative electrode 80 is silver (Ag), aluminium (Al), samarium (Sm), ytterbium (Yb), magnesium silver alloy (Mg-Ag) or magnadure (Mg-Al), is preferably silver.The thickness of negative electrode is 70nm～200nm, is preferably 100nm.
Cap 90 is covered on negative electrode 80.Cap 90 is formed with host cavity 92.Host cavity 92 is the groove from the surface of cap 90 depression.Cap 90 is covered on negative electrode 80 surfaces and anode 20, hole transmission layer 30, luminescent layer 40, hole blocking layer 50, ion barrier layer 60, electron transfer layer 70 and negative electrode 80 is contained in to host cavity 92.The edge of cap 90 is tightly connected by packaging plastic (not shown) and substrate 10, thereby cap 90 is encapsulated in anode 20, hole transmission layer 30, luminescent layer 40, hole blocking layer 50, ion barrier layer 60, electron transfer layer 70 and negative electrode 80 in substrate 10.In present embodiment, the material of cap 90 is glass.
Above-mentioned organic electroluminescence device 100, the dopant material in electron transfer layer 70 is lithium, sodium, potassium, rubidium or caesium, adopts the electron transfer layer 70 of doped structure, has reduced the drive current of organic electroluminescence device; The ion barrier layer 60 that inorganic material forms is set between electron transfer layer 70 and luminescent layer 40, ion barrier layer 60 is comparatively form compact and stable, 60 pairs of alkali metal of ion barrier layer have good diffusion-restricted effect, can stop that alkali metal spreads to luminescent layer 40, avoid causing exciton cancellation, make the life-span of organic electroluminescence device 100 longer; The material of hole blocking layer 50 is organometallic complex, has better film forming stability and compactness, and its thermal stability is good, can play a very good protection to luminescent layer 40; Meanwhile, hole blocking layer 50 blocking holes transmit to electron transfer layer 70 from luminescent layer 40, control the recombination region of exciton at luminescent layer 40.
Be appreciated that other functional layers also can be set in this organic electroluminescence device 100 as required.
Please refer to Fig. 2, the preparation method of the organic electroluminescence device 100 of an execution mode, it comprises the following steps:
Step S110, prepare on the surface of substrate 10 anode 20, hole transmission layer 30, luminescent layer 40 and the hole blocking layer 50 that stack gradually.
The material of substrate 10 is glass.
In present embodiment, before forming anode 20, substrate 10 surfaces first substrate 10 is carried out to pre-treatment, pre-treatment comprises: substrate 10 is placed on and in the deionized water that contains washing agent, carries out ultrasonic cleaning, after cleaning up, use successively isopropyl alcohol, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
Anode 20 is formed at the surface of substrate 10.The material of anode 20 is transparent conductive oxide.Concrete, the material of anode 20 is selected from least one in indium tin oxide (ITO), indium-zinc oxide (IZO), aluminium zinc oxide (AZO) and gallium zinc oxide (GZO), is preferably ITO.The thickness of anode 20 is 70nm～200nm.Anode 20, in vacuum coating system, is prepared by magnetron sputtering, and vacuum degree is 1 × 10 -5pa～1 × 10 -3pa.
Hole transmission layer 30 is formed at the surface of anode 20.The material of hole transmission layer 30 is mixture or the hole mobile material that hole mobile material and dopant form.Hole mobile material is selected from N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, 4'-diamines (NPB), 4, 4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine (m-MTDATA), N, N'-diphenyl-N, N'-bis-(3-aminomethyl phenyl)-1, 1'-biphenyl-4, 4'-diamines (TPD), N, N, N', N '-tetramethoxy phenyl)-benzidine (MeO-TPD), 2, two (the N of 7-, N-bis-(4-methoxyphenyl) amino)-9, 9-spiral shell two fluorenes (MeO-Sprio-TPD), 4, 4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) and 1, 1-bis-(4-(N, N '-bis-(p-tolyl) amino) phenyl) at least one in cyclohexane (TAPC).Dopant is selected from 2,3, and 5,6-tetrafluoro-7,7 ', 8,8 '-tetra-cyanogen quinone-bismethanes (F4-TCNQ), 1,3,4,5,7,8-hexafluoro-tetra-cyanogen-diformazan is to naphthoquinones (F6-TNAP) and 2,2'-(2,5-dicyano-3,6-difluoro cyclohexane-2,5-diene-Isosorbide-5-Nitrae-bis-subunit) at least one in two malononitrile (F2-HCNQ).In mixture, the mass ratio of dopant and hole mobile material is 2:100～30:100.The thickness of hole transmission layer 30 is 20nm～60nm.In present embodiment, hole transmission layer 30 is prepared by evaporation, and evaporation is 1 × 10 at vacuum pressure -5pa～1 × 10 -3under Pa, carry out, the evaporation speed of hole mobile material is 0.02nm/s～1nm/s.
Luminescent layer 40 is formed at the surface of hole transmission layer 30.The material of luminescent layer 40 is mixture or the fluorescent material that material of main part and guest materials doping form.Material of main part is selected from 4,4'-bis-(9-carbazole) biphenyl (CBP), oxine aluminium (Alq 3), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi) and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, at least one in 4'-diamines (NPB).Guest materials is selected from 4-(dintrile methyl)-2-butyl-6-(1, 1, 7, 7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), two (4, 6-difluorophenyl pyridine-N, C2) pyridine formyl closes iridium (FIrpic), two (4, 6-difluorophenyl pyridine)-tetra-(1-pyrazolyl) boric acid closes iridium (FIr6), two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanedione) close iridium (Ir (MDQ) 2 (acac)), three (1-phenyl-isoquinolin) close iridium (Ir (piq) 3) and three (2-phenylpyridines) close at least one in iridium (Ir (ppy) 3).The mass ratio of guest materials and material of main part is 1:100～10:100.Fluorescent material is selected from 4,4'-bis-(2,2-diphenylethyllene)-1,1'-biphenyl (DPVBi), oxine aluminium (Alq 3), 4, at least one in two [4-(di-p-tolyl amino) styryl] biphenyl (DPAVBi) of 4'-and 5,6,11,12-tetraphenyl naphthonaphthalene (Rubrene).The material of luminescent layer 40 is preferably oxine aluminium (Alq 3).The thickness of luminescent layer 40 is 5nm～20nm, is preferably 15nm.In present embodiment, luminescent layer 40 is prepared by evaporation, and evaporation is 1 × 10 at vacuum pressure -5pa～1 × 10 -3under Pa, carry out, the evaporation speed of luminescent layer is 0.1nm/s～1nm/s.
Hole blocking layer 50 is formed at the surface of luminescent layer 40.The material of hole blocking layer 50 is selected from two (2-methyl-oxine-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium (BAlq), oxine gallium (Gaq 3), oxine indium (Inq 3), oxine zinc (Znq 2), oxine beryllium (Beq 2) and three (5-methylol-oxine) aluminium (AlOq) at least one.The thickness of hole blocking layer 50 is 5nm～10nm.In present embodiment, hole blocking layer 50 is prepared by evaporation, and evaporation is 1 × 10 at vacuum pressure -5pa～1 × 10 -3under Pa, carry out, evaporation speed is 0.1nm/s～1nm/s.
The material of hole blocking layer 50 is organometallic complex, has better film forming stability and compactness, and its thermal stability is good, can play a very good protection to luminescent layer 40; Meanwhile, hole blocking layer 50 blocking holes transmit to electron transfer layer 70 from luminescent layer 40, control the recombination region of exciton at luminescent layer 40.Hole blocking layer 50 can play a protective role to luminescent layer 40, while avoiding preparing ion barrier layer 60, luminescent layer 40 is caused damage.
Step S120, prepare ion barrier layer 60 at the surface sputtering of hole blocking layer 50.
Ion barrier layer 60 is formed at the surface of hole blocking layer 50.The material of ion barrier layer 60 is selected from least one in oxide, the oxide of zirconium and the oxide of tin of titanyl compound, zinc.Titanyl compound is titanium monoxide (TiO) or titanium dioxide (TiO 2).The oxide of zinc is zinc oxide (ZnO).The oxide of zirconium is zirconium dioxide (ZrO 2).The oxide of tin is tin monoxide (SnO) or tin ash (SnO 2).The material of ion barrier layer 60 is preferably TiO 2, ZnO, ZrO 2or SnO 2.The thickness of ion barrier layer 60 is 2nm～7nm.Ion barrier layer 60, in vacuum coating system, is prepared by magnetron sputtering, and vacuum degree is 1 × 10 -5pa～1 × 10 -3pa, sputter rate is 0.2nm/s～2nm/s.
Further, ion barrier layer 60 is total two-layer, and two-layer ion barrier layer 60 stacks gradually.
The surface of step S130, ion barrier layer 60 adopts thermal resistance evaporation technology, and electron transport material and alkali-metal compound are carried out to Evaporation preparation electron transfer layer 70 simultaneously.
Alkali metal is compound, rubidium or the caesium of lithium, sodium, potassium.Alkali-metal compound is alkali-metal fluoride, alkali-metal carbonate compound, alkali-metal triazo-compound, alkali-metal nitride or alkali-metal hydroboron, as lithium carbonate (Li 2cO 3), Lithium Azide (LiN 3), lithium fluoride (LiF), cesium azide (CsN 3), cesium carbonate (Cs 2cO 3), cesium fluoride (CsF), potassium borohydride (KBH 4), rubidium carbonate (Rb 2cO 3), lithium nitride (Li 3n), sodium fluoride (NaF).
Electron transport material is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1,3,4-oxadiazole (PBD), (oxine)-aluminium (Alq3), 4,7-diphenyl-o-phenanthroline (Bphen), 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBi), 2,9-dimethyl-4,7-biphenyl-1,10-phenanthrolene (BCP) or 1,2,4-triazole derivative (TAZ).
In this step, in evaporate process, alkali-metal compound, through adding thermal decomposition, forms alkali-metal-doped in electron transport material.
In electron transfer layer 70, the mass ratio of alkali metal and electron transport material is 10:100～50:100.The thickness of electron transfer layer 70 is 50nm～200nm.
In present embodiment, evaporation is 1 × 10 at vacuum pressure -5pa～1 × 10 -3under Pa, carry out, the evaporation speed of electron transport material is 0.2nm/s～1nm/s.The evaporation speed of alkali-metal compound is 0.1nm/s～0.5nm/s.
Step S140, prepare negative electrode 80 on the surface of electron transfer layer 70.
Negative electrode 80 is formed at the surface of electron transfer layer 70.The material of negative electrode 80 is silver (Ag), aluminium (Al), samarium (Sm), ytterbium (Yb), magnesium silver alloy (Mg-Ag) or magnadure (Mg-Al), is preferably silver.The thickness of negative electrode is 70nm～200nm, is preferably 100nm.
In present embodiment, evaporation is 1 × 10 at vacuum pressure -5pa～1 × 10 -3under Pa, carry out, evaporation speed is 0.2m/s～2nm/s.
Step S150, use cap 90 just anode 20, hole transmission layer 30, luminescent layer 40, hole blocking layer 50, ion barrier layer 60, electron transfer layer 70 and negative electrode 80 are packaged in substrate 10.
Cap 90 is formed with host cavity 92.Host cavity 92 is the groove from the surface of cap 90 depression.Cap 90 is covered on negative electrode 80 surfaces and anode 20, hole transmission layer 30, luminescent layer 40, hole blocking layer 50, ion barrier layer 60, electron transfer layer 70 and negative electrode 80 is contained in to host cavity 92.
The edge of cap 90 supports substrate 10, at the edge-coating packaging plastic of cap 90, cap 90 and substrate 10 are tightly connected, thereby cap 90 is encapsulated in anode 20, hole transmission layer 30, luminescent layer 40, hole blocking layer 50, ion barrier layer 60, electron transfer layer 70 and negative electrode 80 in substrate 10.
Above-mentioned organic electroluminescence device preparation method, technique is simple.
Below in conjunction with specific embodiment, the preparation method of organic electroluminescence device provided by the invention is elaborated.
The preparation used of the embodiment of the present invention and comparative example and tester are: test is high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd) with Preparation equipment, the USB4000 fiber spectrometer testing electroluminescent spectrum of U.S. marine optics Ocean Optics, the Keithley2400 test electric property of Keithley company of the U.S., CS-100A colorimeter test brightness and the colourity of Japanese Konica Minolta company.
Embodiment 1
The manufacture method of the Organnic electroluminescent device of the present embodiment, comprises following step:
Step 1, provide substrate, substrate is placed in the deionized water that contains washing agent and carries out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
Step 2, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, at substrate surface sputter preparation sun, material is that ITO thickness is 100nm, and sputter rate is 0.5nm/s;
Step 3, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, pass through vacuum thermal evaporation technology on the surface of anode, prepare hole transmission layer, luminescent layer and hole blocking layer.The material of hole transmission layer comprises MeO-TPD and is entrained in the F6-TNAP in MeO-TPD, and the mass ratio of F6-TNAP and MeO-TPD is 5:100, and thickness is 60nm, and the evaporation speed of MeO-TPD is 1nm/s, and the evaporation speed of F6-TNAP is 0.05nm/s; The material of luminescent layer is Alq 3, thickness is 15nm, evaporation speed is 0.5nm/s; The material of hole blocking layer is BAlq, and thickness is 10nm, and evaporation speed is 1nm/s.
Step 4, be 1 × 10 in vacuum degree -4in the magnetron sputtering coating system of Pa, adopt low frequency sputtering technology, prepare ion barrier layer, material is TiO 2, sputtering rate is 0.02nm/s, thickness is 2nm.
Step 5, be 1 × 10 in vacuum degree -4in the vacuum thermal evaporation film system of Pa, evaporation is prepared electron transfer layer, at evaporating Al q 3time, evaporate Li simultaneously 2cO 3, Alq 3evaporation rate remain 1nm/s, Li 2cO 3evaporation rate be 0.1nm/s, thickness is 50nm, wherein Li and Alq 3mass ratio be 10:100.
Step 6, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, prepare negative electrode at the surperficial evaporation of electron transfer layer, material is Ag, and thickness is 100nm, and evaporation speed is 0.2nm/s.
Step 7, use glass packaging lid are encapsulated in anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in substrate.
Embodiment 2
The manufacture method of the Organnic electroluminescent device of the present embodiment, comprises following step:
Step 1, provide substrate, substrate is placed in the deionized water that contains washing agent and carries out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
Step 2, be 1 × 10 in vacuum degree -5in the vacuum coating system of Pa, at substrate surface sputter preparation sun, material is that GZO thickness is 70nm, and sputter rate is 0.1nm/s;
Step 3, be 1 × 10 in vacuum degree -5in the vacuum coating system of Pa, pass through vacuum thermal evaporation technology on the surface of anode, prepare hole transmission layer, luminescent layer and hole blocking layer.The material of hole transmission layer comprises NPB and is entrained in the F4-TCNQ in NPB, and the mass ratio of F4-TCNQ and NPB is 10:100, and thickness is 40nm, and the evaporation speed of NPB is 1nm/s, and the evaporation speed of F4-TCNQ is 0.1nm/s; The material of luminescent layer is DPAVBi, and thickness is 10nm, and evaporation speed is 0.2nm/s; The material of hole blocking layer is Gaq 3, thickness is 10nm, evaporation speed is 0.5nm/s.
Step 4, be 1 × 10 in vacuum degree -5in the magnetron sputtering coating system of Pa, adopt low frequency sputtering technology, prepare ion barrier layer, material is ZrO 2, sputtering rate is 0.05nm/s, thickness is 7nm.
Step 5, be 1 × 10 in vacuum degree -54in the vacuum thermal evaporation film system of Pa, evaporation is prepared electron transfer layer, in evaporation Bphen, evaporates Cs simultaneously 2cO 3, the evaporation rate of Bphen remains 0.2nm/s, Cs 2cO 3evaporation rate be 0.1nm/s, thickness is 200nm, wherein the mass ratio of Cs and Bphen is 50:100.
Step 6, be 1 × 10 in vacuum degree -5in the vacuum coating system of Pa, prepare negative electrode at the surperficial evaporation of electron transfer layer, material is Ag, and thickness is 200nm, and evaporation speed is 2nm/s.
Step 7, use glass packaging lid are encapsulated in anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in substrate.
Embodiment 3
The manufacture method of the Organnic electroluminescent device of the present embodiment, comprises following step:
Step 1, provide substrate, substrate is placed in the deionized water that contains washing agent and carries out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
Step 2, be 1 × 10 in vacuum degree -3in the vacuum coating system of Pa, prepare negative electrode in substrate surface sputter, material is that AZO thickness is 200nm, and sputter rate is 2nm/s;
Step 3, be 1 × 10 in vacuum degree -3in the vacuum coating system of Pa, pass through vacuum thermal evaporation technology on the surface of anode, prepare hole transmission layer, luminescent layer and hole blocking layer.The material of hole transmission layer comprises TPD and is entrained in the F2-HCNQ in TPD, and the mass ratio of F2-HCNQ and TPD is 30:100, and thickness is 20nm, and the evaporation speed of TPD is 0.9nm/s, and the evaporation speed of F2-HCNQ is 0.3nm/s; The material of luminescent layer is Alq 3, thickness is 15nm, evaporation speed is 1nm/s; The material of hole blocking layer is Inq 3, thickness is 7nm, evaporation speed is 0.1nm/s.
Step 4, be 1 × 10 in vacuum degree -3in the magnetron sputtering coating system of Pa, adopt low frequency sputtering technology, prepare ion barrier layer, material is SnO 2, sputtering rate is 0.1nm/s, thickness is 5nm.
Step 5, be 1 × 10 in vacuum degree -3in the vacuum thermal evaporation film system of Pa, evaporation is prepared electron transfer layer, in evaporation TAZ, evaporates Rb simultaneously 2cO 3, the evaporation rate of TAZ remains 0.5nm/s, Rb 2cO 3evaporation rate be 0.1nm/s, thickness is 80nm, wherein the mass ratio of Rb and TAZ is 20:100.
Step 6, be 1 × 10 in vacuum degree -3in the vacuum coating system of Pa, prepare negative electrode at the surperficial evaporation of electron transfer layer, material is Al, and thickness is 100nm, and evaporation speed is 0.5nm/s.
Step 7, use glass packaging lid are encapsulated in anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in substrate.
Embodiment 4
The manufacture method of the Organnic electroluminescent device of the present embodiment, comprises following step:
Step 1, provide substrate, substrate is placed in the deionized water that contains washing agent and carries out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
Step 2, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, prepare negative electrode in substrate surface sputter, material is that ITO thickness is 100nm, and sputter rate is 0.5nm/s;
Step 3, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, pass through vacuum thermal evaporation technology on the surface of anode, prepare hole transmission layer, luminescent layer and hole blocking layer.The material of hole transmission layer comprises m-MTDATA and is entrained in the F4-TCNQ in m-MTDATA, and the mass ratio of F4-TCNQ and m-MTDATA is 2:100, and thickness is 40nm, and the evaporation speed of m-MTDATA is 1nm/s, and the evaporation speed of F4-TCNQ is 0.02nm/s; The material of luminescent layer is DPVBi, and thickness is 5nm, and evaporation speed is 0.1nm/s; The material of hole blocking layer is Znq 2, thickness is 5nm, evaporation speed is 0.1nm/s.
Step 4, be 1 × 10 in vacuum degree -4in the magnetron sputtering coating system of Pa, adopt low frequency sputtering technology, prepare ion barrier layer, material is ZnO, and sputtering rate is 0.1nm/s, and thickness is 5nm.
Step 5, be 1 × 10 in vacuum degree -4in the vacuum thermal evaporation film system of Pa, evaporation is prepared electron transfer layer, in evaporation TPBi, evaporates KBH simultaneously 4, the evaporation rate of TPBi remains 1nm/s, KBH 4evaporation rate be 0.2nm/s, thickness is 100nm, wherein the mass ratio of K and TPBi is 20:100.
Step 6, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, prepare negative electrode at the surperficial evaporation of electron transfer layer, material is Ag, and thickness is 100nm, and evaporation speed is 0.5nm/s.
Step 7, use glass packaging lid are encapsulated in anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in substrate.
Comparative example
The manufacture method of the Organnic electroluminescent device of the present embodiment, comprises following step:
Step 1, provide substrate, substrate is placed in the deionized water that contains washing agent and carries out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
Step 2, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, prepare negative electrode in substrate surface sputter, material is that ITO thickness is 100nm, and sputter rate is 0.5nm/s;
Step 3, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, pass through vacuum thermal evaporation technology on the surface of anode, prepare hole transmission layer, luminescent layer and hole blocking layer.The material of hole transmission layer comprises MeO-TPD and is entrained in the F6-TNAP in MeO-TPD, and the mass ratio of F6-TNAP and MeO-TPD is 5:100, and thickness is 60nm, and the evaporation speed of MeO-TPD is 1nm/s, and the evaporation speed of F6-TNAP is 0.05nm/s; The material of luminescent layer is Alq 3, thickness is 15nm, evaporation speed is 0.5nm/s; The material of hole blocking layer is BAlq, and thickness is 10nm, and evaporation speed is 0.5nm/s.
Step 4, be 1 × 10 in vacuum degree -4in the vacuum thermal evaporation film system of Pa, evaporation is prepared electron transfer layer, at evaporating Al q 3time, evaporate Li simultaneously 2cO 3, Alq 3evaporation rate remain 1nm/s, Li 2cO 3evaporation rate be 0.1nm/s, thickness is 50nm, wherein the mass ratio of Cs and Bphen is 10:100.
Step 5, be 1 × 10 in vacuum degree -4in the vacuum coating system of Pa, prepare negative electrode at the surperficial evaporation of electron transfer layer, material is Ag, and thickness is 100nm, and evaporation speed is 0.2nm/s.
Step 6, use glass packaging lid are encapsulated in anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in substrate.
Table 1
Refer to table 1, table 1 is the luminescent properties data of the device of embodiment 1～4 and comparative example making, and the data of surveying are to be 1000cd/m in initial brightness 2under, service time when initial brightness 70% is arrived in brightness decay.As can be seen from Table 1, the life-span of the organic electroluminescence device of embodiment 1～4 preparation is longer, and with respect to comparative example, the life-span of the organic electroluminescence device of embodiment 1～4 preparation has improved respectively 54%, 62%, 73%, 50%.Thereby can find out Organnic electroluminescent device provided by the invention, can improve the life-span of organic electroluminescence device by ion barrier layer is set.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.

Claims (10)

1. an organic electroluminescence device, it is characterized in that, comprise the substrate stacking gradually, anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode, the material of described ion barrier layer is selected from titanyl compound, the oxide of zinc, at least one in the oxide of zirconium and the oxide of tin, the material of described electron transfer layer comprises electron transport material and is entrained in the dopant material in described electron transport material, described dopant material is lithium, sodium, potassium, rubidium or caesium, described electron transport material is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1, 3, 4-oxadiazole, (oxine)-aluminium, 4, 7-diphenyl-o-phenanthroline, 1, 3, 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthrolene or 1, 2, 4-triazole derivative,
Described organic electroluminescence device also comprises cap, and described cap is packaged in described anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode in described substrate.
2. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described ion barrier layer is 2nm～7nm, and the thickness of described electron transfer layer is 50nm～200nm.
3. organic electroluminescence device according to claim 1, is characterized in that, the mass ratio of dopant material and described electron transport material described in described electron transfer layer is 10:100～50:100.
4. organic electroluminescence device according to claim 1, is characterized in that, described ion barrier layer is total two-layer, and two-layer ion barrier layer stacks gradually.
5. organic electroluminescence device according to claim 1, it is characterized in that, the material of described luminescent layer is mixture or the fluorescent material that material of main part and guest materials doping form, described material of main part is selected from 4, 4'-bis-(9-carbazole) biphenyl, oxine aluminium, 1, 3, 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene and N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1, 1'-biphenyl-4, at least one in 4'-diamines, described guest materials is selected from 4-(dintrile methyl)-2-butyl-6-(1, 1, 7, 7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans, two (4, 6-difluorophenyl pyridine-N, C2) pyridine formyl closes iridium, two (4, 6-difluorophenyl pyridine)-tetra-(1-pyrazolyl) boric acid closes iridium, two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanedione) close iridium, three (1-phenyl-isoquinolin) close iridium and three (2-phenylpyridine) and close at least one in iridium, described fluorescent material is selected from 4, 4'-bis-(2, 2-diphenylethyllene)-1, 1'-biphenyl, oxine aluminium, 4, two [4-(di-p-tolyl amino) styryl] biphenyl and 5 of 4'-, 6, 11, at least one in 12-tetraphenyl naphthonaphthalene, the mass ratio of described guest materials and described material of main part is 1:100～10:100.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
The anode, hole transmission layer, luminescent layer and the hole blocking layer that stack gradually are prepared in surface at substrate;
Prepare ion barrier layer at the surface sputtering of described hole blocking layer, the material of described ion barrier layer is selected from least one in oxide, the oxide of zirconium and the oxide of tin of titanyl compound, zinc;
Surface at described ion barrier layer adopts thermal resistance evaporation technology, electron transport material and alkali-metal compound are carried out to Evaporation preparation electron transfer layer simultaneously, alkali metal in described alkali-metal compound is lithium, sodium, potassium, rubidium or caesium, described electron transport material is 2-(4-xenyl)-5-(4-the tert-butyl group) phenyl-1, 3, 4-oxadiazole, (oxine)-aluminium, 4, 7-diphenyl-o-phenanthroline, 1, 3, 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthrolene or 1, 2, 4-triazole derivative,
Negative electrode is prepared on surface at described electron transfer layer; And
Use cap that described anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode are packaged in described substrate.
7. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: the thickness of described ion barrier layer is 2nm～7nm, and the thickness of described electron transfer layer is 50nm～200nm.
8. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: described alkali-metal compound is alkali-metal fluoride, alkali-metal carbonate compound, alkali-metal triazo-compound, alkali-metal nitride or alkali-metal hydroboron.
9. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: described cap is formed with host cavity, described anode, hole transmission layer, luminescent layer, hole blocking layer, ion barrier layer, electron transfer layer and negative electrode are contained in described host cavity.
10. the preparation method of organic electroluminescence device according to claim 6, is characterized in that: described ion barrier layer is total two-layer, and two-layer ion barrier layer stacks gradually.
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Application publication date: 20140924