CN104425754A - Organic light-emitting device and preparation method for same - Google Patents

Organic light-emitting device and preparation method for same Download PDF

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Publication number
CN104425754A
CN104425754A CN201310386249.6A CN201310386249A CN104425754A CN 104425754 A CN104425754 A CN 104425754A CN 201310386249 A CN201310386249 A CN 201310386249A CN 104425754 A CN104425754 A CN 104425754A
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layer
nitride
silicon oxynitride
inorganic barrier
barrier layer
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周明杰
钟铁涛
王平
陈吉星
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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 CN201310386249.6A priority Critical patent/CN104425754A/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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/84—Passivation; Containers; Encapsulations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/84—Passivation; Containers; Encapsulations
    • H10K50/844—Encapsulations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass

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  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

The invention discloses an organic light-emitting device. The organic light-emitting device comprises an anode, a luminous layer, a cathode and a packaging cover, which are sequentially laminated, wherein the luminous layer and the cathode are packaged on the anode by virtue of the packaging cover; the packaging cover comprises a first silicon oxynitride layer formed on the surface of the cathode, a first inorganic barrier layer formed on the surface of the first silicon oxynitride layer, a second silicon oxynitride layer formed on the surface of the first inorganic barrier layer and a second inorganic barrier layer formed on the surface of the second silicon oxynitride layer; a material for the first inorganic barrier layer comprises telluride, nitride and metal; a material for the second inorganic barrier layer comprises metal oxide, nitride and metal; the telluride is at least one of antimony tritelluride, bismuth telluride, cadmium telluride, diindium tritelluride, tin telluride and lead telluride; the nitride is at least one of trisilicon tetranitride, aluminum nitride, boron nitride, hafnium nitride, tantalum nitride and titanium nitride. The organic light-emitting device is longer in service life. The invention also provides a preparation method for the organic light-emitting 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
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is that the luminous organic material preparing one deck tens nanometer thickness on ito glass makes luminescent layer, has the metal electrode of one deck low work function above luminescent layer.When electrode being added with voltage, luminescent layer just produces light radiation.
After organic electroluminescence device is subject to moisture and moisture erosion, the material of organic electroluminescence device inner member can be caused to occur aging and then lost efficacy, thus the life-span of described organic electroluminescence device is shorter.
Summary of the invention
Based on this, be necessary organic electroluminescence device providing a kind of life-span longer and preparation method thereof.
A kind of organic electroluminescence device, comprise the anode, luminescent layer and the negative electrode that stack gradually, it is characterized in that: described organic electroluminescence device also comprises cap, described luminescent layer and negative electrode are packaged on described anode by described cap, and described cap comprises the first silicon oxynitride layer being formed at described cathode surface, the first inorganic barrier layer being formed at described first silicon oxynitride layer surface, is formed at second silicon oxynitride layer on described first inorganic barrier layer surface and is formed at second inorganic barrier layer on described second silicon oxynitride layer surface; The material of described first inorganic barrier layer comprise tellurides, nitride and metal, the material of described second inorganic layer comprises metal oxide, nitride and metal; Described tellurides is selected from least one in three antimony tellurides, bismuth telluride, cadmium telluride, three telluride two indiums, telluride tin and lead telluride, described nitride is selected from least one in silicon nitride, aluminium nitride, boron nitride, hafnium nitride, tantalum nitride and titanium nitride, described metal is selected from least one in silver, aluminium, nickel, gold, copper and platinum, and described metal oxide is selected from least one in meta-aluminic acid magnesium, bismuth titanates, chromic acid nickel, cobalt-chromate, lutetium acid iron and yttrium aluminate.
Wherein in an embodiment, the thickness of described first silicon oxynitride layer is 150nm ~ 200nm; The thickness of described first inorganic barrier layer is 100nm ~ 200nm; The thickness of described second silicon oxynitride layer is 150nm ~ 200nm; The thickness of described second inorganic barrier layer is 100nm ~ 200nm.
Wherein in an embodiment, described in described first inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described tellurides.
Wherein in an embodiment, described in described second inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described metal oxide.
Wherein in an embodiment, described cap coordinates with described anode and is formed with host cavity, and described luminescent layer and negative electrode are all contained in described host cavity.
A preparation method for organic electroluminescence device, comprises the following steps:
Luminescent layer is prepared at anode surface;
Negative electrode is prepared on described luminescent layer surface; And
Prepare cap at described cathode surface, described luminescent layer and negative electrode are packaged on described anode by described cap, and described cap comprises the first silicon oxynitride layer being formed at described cathode surface, be formed at first inorganic barrier layer on described first silicon oxynitride layer surface, be formed at second silicon oxynitride layer on described first inorganic barrier layer surface and be formed at second inorganic barrier layer on described second silicon oxynitride layer surface, the material of described first inorganic barrier layer comprise tellurides, nitride and metal, the material of described second inorganic layer comprises metal oxide, nitride and metal, described tellurides is selected from three antimony tellurides, bismuth telluride, cadmium telluride, three telluride two indiums, at least one in telluride tin and lead telluride, described nitride is selected from silicon nitride, aluminium nitride, boron nitride, hafnium nitride, at least one in tantalum nitride and titanium nitride, described metal is selected from silver, aluminium, nickel, gold, at least one in copper and platinum, described metal oxide is selected from meta-aluminic acid magnesium, bismuth titanates, chromic acid nickel, cobalt-chromate, lutetium acid iron and yttrium aluminate at least one.
Wherein in an embodiment, the thickness of described first silicon oxynitride layer is 150nm ~ 200nm; The thickness of described first inorganic barrier layer is 100nm ~ 200nm; The thickness of described second silicon oxynitride layer is 150nm ~ 200nm; The thickness of described second inorganic barrier layer is 100nm ~ 200nm.
Wherein in an embodiment, described in described first inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described tellurides.
Wherein in an embodiment, described in described second inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described metal oxide.
Wherein in an embodiment, described first silicon oxynitride layer and the equal using plasma of described second silicon oxynitride layer strengthen chemical vapour deposition technique preparation, unstrpped gas is hmds, ammonia and oxygen, carrier gas is argon gas, the flow-rate ratio of wherein said hmds, ammonia and oxygen is (6 ~ 14): (2 ~ 18): (2 ~ 18), temperature is 40 ~ 60 DEG C, and air pressure is 30 ~ 60Pa, and power is 0.1 ~ 0.5W/cm 2.
Above-mentioned organic electroluminescence device and preparation method thereof, cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer, the second inorganic barrier layer that stack gradually, four layers of cooperation can the effectively luminescent layer of material to organic electroluminescence device and the corrosion of negative electrode such as block water oxygen, improve water oxygen resistant ability, thus the life-span of organic electroluminescence device is longer.
Accompanying drawing explanation
Fig. 1 is the structural representation of the organic electroluminescence device of an embodiment;
Fig. 2 is the flow chart of the preparation method of the organic electroluminescent of an embodiment.
Embodiment
Below in conjunction with the drawings and specific embodiments, organic electroluminescence device and preparation method thereof is illustrated further.
Refer to Fig. 1, the organic electroluminescence device 100 of an execution mode comprises the anode 10 with anode pattern, functional layer 20, negative electrode 30 and the cap 40 that stack gradually.
Anode 10 is electro-conductive glass or organic PETG (PET) film substrate that conducts electricity.Anode 10 has the ITO layer that preparation has anode pattern.In present embodiment, the thickness of ITO layer is 100nm.The thickness of certain ITO layer is not limited to 100nm, also can select other thickness as required.
Functional layer 20 is formed at anode 10 surface.Functional layer 20 comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer that stack gradually.Be appreciated that hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, now functional layer 20 only comprises luminescent layer.
In present embodiment, the material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3).CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.The thickness of hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adjust as required.
Negative electrode 30 is formed at functional layer 20 surface.The thickness of negative electrode is 100nm.The material of negative electrode 30 is aluminium (Al).
Cap 40 is formed at the surface of negative electrode 30.In present embodiment, cap 40 covers at functional layer 20 and negative electrode 30, and the edge of cap 40 and anode 10 affixed, thus functional layer 20 and negative electrode 30 to be encapsulated on anode 10.Cap 40 is formed with host cavity.Host cavity is the groove of the surface indentation from cap 40.Functional layer 20 and negative electrode 30 are contained in host cavity by cap 40.
Cap 40 comprises the first silicon oxynitride layer 41, first inorganic barrier layer 42, second silicon oxynitride layer 43 and the second inorganic barrier layer 44 stacked gradually.
First silicon oxynitride layer 41 is formed at the surface of negative electrode 30, and the part surface of the end face of covered cathode 30 and functional layer 20 and anode 10, thus functional layer 20 and negative electrode 30 are encapsulated on anode 10.The material of the first silicon oxynitride layer 41 is SiO xn y, the effect intercepting water oxygen can be played.The thickness of the first silicon oxynitride layer 41 is 150nm ~ 200nm.
First inorganic barrier layer 42 is formed at the surface of the first silicon oxynitride layer 41.The material of the first inorganic barrier layer 42 comprises tellurides, nitride and metal.Tellurides is selected from three antimony telluride (Sb 2te 3), bismuth telluride (Bi 2te), cadmium telluride (CdTe), three telluride two indium (In 2te 3), at least one in telluride tin (SnTe) and lead telluride (PbTe).Nitride is selected from silicon nitride (Si 3n 4), at least one in aluminium nitride (AlN), boron nitride (BN), hafnium nitride (HfN), tantalum nitride (TaN) and titanium nitride (TiN).Metal is selected from least one in silver (Ag), aluminium (Al), nickel (Ni), gold (Au), copper (Cu) and platinum (Pt).The thickness of the first inorganic barrier layer 42 is 100nm ~ 200nm.
Further, in the first inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of metal is 10% ~ 30%, and all the other are tellurides.
Second silicon oxynitride layer 43 is formed at the surface of the first inorganic barrier layer 42.The material of the second silicon oxynitride layer 43 is SiO xn y, the effect intercepting water oxygen can be played.The thickness of the second silicon oxynitride layer 43 is 150nm ~ 200nm.
Second inorganic barrier layer 44 is formed at the surface of the second silicon oxynitride layer 43.The material of the second inorganic barrier layer 44 comprises metal oxide, nitride and metal.Metal oxide is selected from meta-aluminic acid magnesium (MgAl 2o 4), bismuth titanates (Bi 2ti 4o 11), chromic acid nickel (CrNiO 4), cobalt-chromate (CoCr 2o 4), lutetium acid iron (Fe 2luO 4) and yttrium aluminate (Y 3al 5o 12) at least one.Nitride is selected from silicon nitride (Si 3n 4), at least one in aluminium nitride (AlN), boron nitride (BN), hafnium nitride (HfN), tantalum nitride (TaN) and titanium nitride (TiN).Metal is selected from least one in silver (Ag), aluminium (Al), nickel (Ni), gold (Au), copper (Cu) and platinum (Pt).The thickness of the second inorganic barrier layer 44 is 100nm ~ 200nm.
Further, in the second inorganic barrier layer 44, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of metal is 10% ~ 30%, and all the other are metal oxide.
In above-mentioned organic electroluminescence device 100, cap 40 comprises the first silicon oxynitride layer 41, first inorganic barrier layer 42, second silicon oxynitride layer 43 and the second inorganic barrier layer 44 stacked gradually, four layers of cooperation can the corrosion of effective block water oxygen, cap 40 is encapsulated in functional layer 20 and negative electrode 30 on anode 10, effectively can improve water oxygen resistant ability, thus the life-span of organic electroluminescence device 100 is longer.
Be appreciated that the host cavity of cap 40 can omit, now direct host cavity be set on anode 10.
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, on anode 10, form functional layer 20.
Functional layer 20 comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, the electron injecting layer that stack gradually.
Anode 10 can be electro-conductive glass substrate or organic PETG (PET) film substrate that conducts electricity.Anode 10 has the ITO layer that preparation has anode pattern.In present embodiment, the thickness of ITO layer is 100nm.The thickness of certain ITO layer is not limited to 100nm, also can select other thickness as required.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
In present embodiment, the material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
It should be noted that, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer also can adopt other materials as required.Hole injection layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, and now functional layer 20 only comprises luminescent layer.
Step S120, functional layer 20 surface formed negative electrode 30.
The material of negative electrode 30 is aluminium (Al).The thickness of negative electrode 30 is 100nm.Negative electrode 30 is formed by vacuum evaporation, and vacuum degree is 5 × 10 -5pa, evaporation rate is
Step S130, prepare cap 40 on negative electrode 30 surface.
Cap 40 is formed at the surface of negative electrode 30.In present embodiment, cap 40 covers at functional layer 20 and negative electrode 30, and the edge of cap 40 and anode 10 affixed, thus functional layer 20 and negative electrode 30 to be encapsulated on anode 10.Cap 40 is formed with host cavity.Host cavity is the groove of the surface indentation from cap 40.Functional layer 20 and negative electrode 30 are contained in host cavity by cap 40.
Cap 40 comprises the first silicon oxynitride layer 41, first inorganic barrier layer 42, second silicon oxynitride layer 43 and the second inorganic barrier layer 44 stacked gradually.
First silicon oxynitride layer 41 is formed at the surface of negative electrode 30, and the part surface of the end face of covered cathode 30 and functional layer 20 and anode 10, thus functional layer 20 and negative electrode 30 are encapsulated on anode 10.
The material of the first silicon oxynitride layer 41 is SiO xn y, the effect intercepting water oxygen can be played.The thickness of the first silicon oxynitride layer 41 is 150nm ~ 200nm.
In present embodiment, the first silicon oxynitride layer 41 using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).The flow-rate ratio of hmds, ammonia and oxygen is (6 ~ 14): (2 ~ 18): (2 ~ 18).The flow-rate ratio of hmds and carrier gas is (6 ~ 14): (70 ~ 80).Temperature is 40 ~ 60 DEG C, and air pressure is 30 ~ 60Pa, and power is 0.1 ~ 0.5W/cm 2.Specifically in the present embodiment, the flow of HMDS is the flow 70 ~ 80sccm of 6 ~ 14sccm, Ar, NH 3flow 2 ~ 18sccm, O 2flow 2 ~ 18sccm.
The structural formula of HMDS is:
First inorganic barrier layer 42 is formed at the surface of the first silicon oxynitride layer 41.The material of the first inorganic barrier layer 42 comprises tellurides, nitride and metal.Tellurides is selected from three antimony telluride (Sb 2te 3), bismuth telluride (Bi 2te), cadmium telluride (CdTe), three telluride two indium (In 2te 3), at least one in telluride tin (SnTe) and lead telluride (PbTe).Nitride is selected from silicon nitride (Si 3n 4), at least one in aluminium nitride (AlN), boron nitride (BN), hafnium nitride (HfN), tantalum nitride (TaN) and titanium nitride (TiN).Metal is selected from least one in silver (Ag), aluminium (Al), nickel (Ni), gold (Au), copper (Cu) and platinum (Pt).The thickness of the first inorganic barrier layer 42 is 100nm ~ 200nm.
Further, in the first inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of metal is 10% ~ 30%, and all the other are tellurides.
First inorganic barrier layer 42 is prepared by magnetron sputtering, and background vacuum is 1 × 10 -5pa ~ 1 × 10 -3pa.
Second silicon oxynitride layer 43 is formed at the surface of the first inorganic barrier layer 42.The material of the second silicon oxynitride layer 43 second silicon oxynitride layer 43 is SiO xn y, the effect intercepting water oxygen can be played.The thickness of the second silicon oxynitride layer 43 is 150nm ~ 200nm.
In present embodiment, the second silicon oxynitride layer 43 using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).The flow-rate ratio of hmds, ammonia and oxygen is (6 ~ 14): (2 ~ 18): (2 ~ 18).The flow-rate ratio of hmds and carrier gas is (6 ~ 14): (70 ~ 80).Temperature is 40 ~ 60 DEG C, and air pressure is 30 ~ 60Pa, and power is 0.1 ~ 0.5W/cm 2.Specifically in the present embodiment, the flow of HMDS is the flow 70 ~ 80sccm of 6 ~ 14sccm, Ar, NH 3flow 2 ~ 18sccm, O 2flow 2 ~ 18sccm.
The structural formula of HMDS is:
Second inorganic barrier layer 44 is formed at the surface of the second silicon oxynitride layer 43.The material of the second inorganic barrier layer 44 comprises metal oxide, nitride and metal.Metal oxide is selected from meta-aluminic acid magnesium (MgAl 2o 4), bismuth titanates (Bi 2ti 4o 11), chromic acid nickel (CrNiO 4), cobalt-chromate (CoCr 2o 4), lutetium acid iron (Fe 2luO 4) and yttrium aluminate (Y 3al 5o 12) at least one.Nitride is selected from silicon nitride (Si 3n 4), at least one in aluminium nitride (AlN), boron nitride (BN), hafnium nitride (HfN), tantalum nitride (TaN) and titanium nitride (TiN).Metal is selected from least one in silver (Ag), aluminium (Al), nickel (Ni), gold (Au), copper (Cu) and platinum (Pt).The thickness of the second inorganic barrier layer 44 is 100nm ~ 200nm.
Second inorganic barrier layer 44 is prepared by magnetron sputtering, and background vacuum is 1 × 10 -5pa ~ 1 × 10 -3pa.
Further, in the second inorganic barrier layer 44, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of metal is 10% ~ 30%, and all the other are metal oxide.
Be appreciated that the host cavity of cap 40 can omit, now direct host cavity be set on anode 10.
The preparation method of above-mentioned organic electroluminescence device, preparation technology is simple, easily preparation in enormous quantities.
Below in conjunction with specific embodiment, organic electroluminescence device preparation method provided by the invention is described in detail.
Embodiment 1
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap; Wherein, brace "/" represents layer structure, and colon ": " represents doping, lower same.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 100nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 10sccm, Ar flow 75sccm, NH 3flow 10sccm, O 2flow 10sccm, temperature 60 C, air pressure 50Pa, power 0.2W/cm 2.The thickness 200nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material comprises Sb 2te 3, Si 3n 4and Ag, Si 3n 4mass percentage be the mass percentage of 40%, Ag be 20%, all the other are Sb 2te 3, background vacuum 1 × 10 -5pa, thickness 200nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 10sccm, Ar flow 75sccm, NH 3flow 10sccm, O 2flow 10sccm, temperature 60 C, air pressure 50Pa, power 0.2W/cm 2.The thickness 200nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material comprises MgAl 2o 4, Si 3n 4and Ag, Si 3n 4mass percentage be the mass percentage of 40%, Ag be 20%, all the other are MgAl 2o 4, background vacuum 1 × 10 -5pa, thickness 200nm;
The structure of cap is SiO xn y/ Sb 2te 3: Si 3n 4: Ag/SiO xn y/ MgAl 2o 4: Si 3n 4: Ag, wherein, "/" represents separation between layers, and colon ": " represents at least bi-material doping or mixing, lower same.
Embodiment 2
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 100nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 12sccm, Ar flow 77sccm, NH 3flow 15sccm, O 2flow 10sccm, temperature 50 C, air pressure 50Pa, power 0.2W/cm 2.The thickness 180nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material comprises Bi 2te, AlN and Al, the mass percentage of AlN is the mass percentage of 10%, Al is 15%, and all the other are Bi 2te, background vacuum 1 × 10 -5pa, thickness 100nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 12sccm, Ar flow 77sccm, NH 3flow 15sccm, O 2flow 10sccm, temperature 50 C, air pressure 50Pa, power 0.2W/cm 2.The thickness 180nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material comprises Bi 2ti 4o 11, AlN and Al, AlN mass percentage be the mass percentage of 10%, Al be 15%, all the other are Bi 2ti 4o 11, background vacuum 1 × 10 -5pa, thickness 100nm;
The structure of cap is SiO xn y/ Bi 2te:AlN:Al/SiO xn y/ Bi 2ti 4o 11: AlN:Al
Embodiment 3
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 100nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 8sccm, Ar flow 75sccm, NH 3flow 5sccm, O 2flow 8sccm, temperature 50 C, air pressure 60Pa, power 0.5W/cm 2.The thickness 170nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material comprises CdTe, BN and Ni, and the mass percentage of BN is the mass percentage of 30%, Ni is 15%, and all the other are CdTe, background vacuum 1 × 10 -5pa, thickness 150nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 8sccm, Ar flow 75sccm, NH 3flow 5sccm, O 2flow 8sccm, temperature 50 C, air pressure 60Pa, power 0.5W/cm 2.The thickness 170nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material comprises CrNiO 4, BN and Ni, BN mass percentage be the mass percentage of 30%, Ni be 15%, all the other are CrNiO 4, background vacuum 1 × 10 -5pa, thickness 150nm;
The structure of cap is SiO xn y/ CdTe:BN:Ni/SiO xn y/ CrNiO 4: BN:Ni
Embodiment 4
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 150nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 14sccm, Ar flow 70sccm, NH 3flow 18sccm, O 2flow 18sccm, temperature 40 DEG C, air pressure 30Pa, power 0.1W/cm 2.The thickness 160nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material comprises In 2te 3, HfN and Au, HfN mass percentage be the mass percentage of 20%, Au be 20%, all the other are In 2te 3, background vacuum 5 × 10 -5pa, thickness 150nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 14sccm, Ar flow 70sccm, NH 3flow 18sccm, O 2flow 18sccm, temperature 40 DEG C, air pressure 30Pa, power 0.1W/cm 2.The thickness 160nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material comprises CoCr 2o 4, HfN and Au, HfN mass percentage be the mass percentage of 20%, Au be 20%, all the other are CoCr 2o 4, background vacuum 5 × 10 -5pa, thickness 150nm;
The structure of cap is SiO xn y/ In 2te 3: HfN:Au/SiO xn y/ CoCr 2o 4: HfN:Au
Embodiment 5
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 120nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 6sccm, Ar flow 80sccm, NH 3flow 2sccm, O 2flow 2sccm, temperature 45 C, air pressure 40Pa, power 0.3W/cm 2.The thickness 150nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material comprises SnTe, TaN and Cu, and the mass percentage of TaN is the mass percentage of 25%, Cu is 10%, and all the other are SnTe, background vacuum 5 × 10 -5pa, thickness 120nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 6sccm, Ar flow 80sccm, NH 3flow 2sccm, O 2flow 2sccm, temperature 45 C, air pressure 40Pa, power 0.3W/cm 2.The thickness 150nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material comprises Fe 2luO 4, TaN and Cu, TaN mass percentage be the mass percentage of 25%, Cu be 10%, all the other are Fe 2luO 4, background vacuum 5 × 10 -5pa, thickness 120nm;
The structure of cap is SiO xn y/ SnTe:TaN:Cu/SiO xn y/ Fe 2luO 4: TaN:Cu
Embodiment 6
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 100nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 6sccm, Ar flow 75sccm, NH 3flow 15sccm, O 2flow 5sccm, temperature 45 C, air pressure 40Pa, power 0.3W/cm 2.The thickness 160nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material comprises PbTe, TiN and Pt, and the mass percentage of TiN is the mass percentage of 20%, Pt is 30%, and all the other are PbTe, background vacuum 1 × 10 -3pa, thickness 110nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 6sccm, Ar flow 75sccm, NH 3flow 15sccm, O 2flow 5sccm, temperature 45 C, air pressure 40Pa, power 0.3W/cm 2.The thickness 160nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material comprises Y 3al 5o 12, TiN and Pt, TiN mass percentage be the mass percentage of 20%, Pt be 30%, all the other are Y 3al 5o 12, background vacuum 1 × 10 -3pa, thickness 110nm;
The structure of cap is SiO xn y/ PbTe:TiN:Pt/SiO xn y/ Y 3al 5o 12: TiN:Pt
Comparative example
The present embodiment prepares structure: ITO/NPB:MoO 3/ TCTA/TPBI:Ir (ppy) 3/ Bphen/Bphen:CsN 3the organic electroluminescence device of/Al/ cap.
The preparation method of above-mentioned organic electroluminescence device, comprises the following steps:
1, on anode, functional layer is formed.
Anode 10 is electro-conductive glass.Anode 10 has the ITO layer that preparation has anode pattern.The thickness of ITO layer is 100nm.
Anode 10 surface formation functional layer 20 before first carry out preliminary treatment to remove the pollutant on substrate 10 surface, and carry out surface active increase anode 10 surface oxygen content to improve the work function on anode 10 surface.Be specially, adopted successively by anode 10 and remove each Ultrasonic Cleaning 5min of acetone, ethanol, ionized water and ethanol, dry up afterwards with nitrogen, baking box is dried.
The material of hole injection layer comprises N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamines (NPB) and the molybdenum oxide (MoO be entrained in NPB 3).MoO 3mass percentage be 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of hole transmission layer is 4,4 ', 4 "-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer is 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of luminescent layer comprises material of main part and is entrained in the guest materials in material of main part.Material of main part is 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and guest materials is that three (2-phenylpyridines) close iridium (Ir (ppy) 3).The mass percentage of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer is 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
The material of electron injecting layer comprises Bphen and is entrained in the nitrine caesium (CsN in Bphen 3), CsN 3mass percentage be 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation, and vacuum degree is 3 × 10 -5pa, evaporation rate is
2, negative electrode is formed on functional layer surface.
The material of negative electrode is aluminium.The thickness of negative electrode is 100nm.Negative electrode is formed by vacuum evaporation, and vacuum degree is 5 × 10 -5pa, evaporation rate is
3, cap is prepared at cathode surface.
Cap is formed at the surface of negative electrode, and the end face of covered cathode and functional layer and the part surface of anode, thus functional layer and negative electrode are encapsulated on anode.
Cap comprises the first silicon oxynitride layer, the first inorganic barrier layer, the second silicon oxynitride layer and the second inorganic barrier layer that stack gradually.
First silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 6sccm, Ar flow 75sccm, NH 3flow 15sccm, O 2flow 5sccm, temperature 45 C, air pressure 40Pa, power 0.3W/cm 2.The thickness 160nm of the first silicon oxynitride layer;
First inorganic barrier layer is prepared by magnetron sputtering, and material is PbTe, background vacuum 1 × 10 -3pa, thickness 110nm;
Second silicon oxynitride layer using plasma strengthens chemical vapour deposition technique (PECVD) preparation.Unstrpped gas is hmds (HMDS), ammonia (NH 3) and oxygen, carrier gas is argon gas (Ar).HMDS flow 6sccm, Ar flow 75sccm, NH 3flow 15sccm, O 2flow 5sccm, temperature 45 C, air pressure 40Pa, power 0.3W/cm 2.The thickness 160nm of the second silicon oxynitride layer;
Second inorganic barrier layer is prepared by magnetron sputtering, and material is Y 3al 5o 12, background vacuum 1 × 10 -3pa, thickness 110nm.
The structure of cap is SiO xn y/ PbTe/SiO xn y/ Y 3al 5o 12
The embodiment of the present invention and the preparation used by comparative example and tester are: high vacuum coating equipment (scientific instrument development center, Shenyang Co., Ltd, pressure <1 × 10-3Pa), magnetron sputtering apparatus (scientific instrument development center, Shenyang Co., Ltd), current-voltage tester (Keithly company of the U.S., 2400), color luminance meter (Konica Minolta, model: CS-100A) model:.
Refer to table 1, table 1 is depicted as the test result of the aqueous vapor penetrance (Water Vapor Transmission Rate) of organic electroluminescence device prepared by embodiment 1 ~ embodiment 6 and comparative example.The aqueous vapor penetrance of the organic electroluminescence device of embodiment 1 ~ embodiment 6 preparation is all less than 10 as can be seen from Table 1 - 6g/m 2/ day, much smaller than the aqueous vapor penetrance (10 of organic electroluminescence device prepared by comparative example -4g/m 2/ day) waterproof effect is better, and effectively can reduce the erosion of outside aqueous vapor to organic electroluminescence device, thus improve the life-span of organic electroluminescence device.
Table 1
WVTR(g/m 2/day)
Embodiment 1 4.4×10 -6
Embodiment 2 4.8×10 -6
Embodiment 3 5.2×10 -6
Embodiment 4 5.7×10 -6
Embodiment 5 5.9×10 -6
Embodiment 6 6.1×10 -6
Comparative example 4.1×10 -4
Refer to table 2, it is 1000cd/m at original intensity that table 2 is depicted as organic electroluminescence device prepared by embodiment 1 ~ embodiment 6 and comparative example 2condition under life-span (brightness is reduced to original intensity 70% time used).
Table 2
As can be seen from Table 2, the starting brightness of the organic electroluminescence device of embodiment 1 ~ embodiment 6 preparation is 1000cd/m 2time, the life-span reaches more than 23070 hours, and the life-span is longer.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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, comprise the anode, luminescent layer and the negative electrode that stack gradually, it is characterized in that: described organic electroluminescence device also comprises cap, described luminescent layer and negative electrode are packaged on described anode by described cap, and described cap comprises the first silicon oxynitride layer being formed at described cathode surface, the first inorganic barrier layer being formed at described first silicon oxynitride layer surface, is formed at second silicon oxynitride layer on described first inorganic barrier layer surface and is formed at second inorganic barrier layer on described second silicon oxynitride layer surface; The material of described first inorganic barrier layer comprise tellurides, nitride and metal, the material of described second inorganic layer comprises metal oxide, nitride and metal; Described tellurides is selected from least one in three antimony tellurides, bismuth telluride, cadmium telluride, three telluride two indiums, telluride tin and lead telluride, described nitride is selected from least one in silicon nitride, aluminium nitride, boron nitride, hafnium nitride, tantalum nitride and titanium nitride, described metal is selected from least one in silver, aluminium, nickel, gold, copper and platinum, and described metal oxide is selected from least one in meta-aluminic acid magnesium, bismuth titanates, chromic acid nickel, cobalt-chromate, lutetium acid iron and yttrium aluminate.
2. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described first silicon oxynitride layer is 150nm ~ 200nm; The thickness of described first inorganic barrier layer is 100nm ~ 200nm; The thickness of described second silicon oxynitride layer is 150nm ~ 200nm; The thickness of described second inorganic barrier layer is 100nm ~ 200nm.
3. organic electroluminescence device according to claim 1, is characterized in that, described in described first inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described tellurides.
4. organic electroluminescence device according to claim 1, is characterized in that, described in described second inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described metal oxide.
5. organic electroluminescence device according to claim 1, is characterized in that, described cap coordinates with described anode and is formed with host cavity, and described luminescent layer and negative electrode are all contained in described host cavity.
6. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
Luminescent layer is prepared at anode surface;
Negative electrode is prepared on described luminescent layer surface; And
Prepare cap at described cathode surface, described luminescent layer and negative electrode are packaged on described anode by described cap, and described cap comprises the first silicon oxynitride layer being formed at described cathode surface, be formed at first inorganic barrier layer on described first silicon oxynitride layer surface, be formed at second silicon oxynitride layer on described first inorganic barrier layer surface and be formed at second inorganic barrier layer on described second silicon oxynitride layer surface, the material of described first inorganic barrier layer comprise tellurides, nitride and metal, the material of described second inorganic layer comprises metal oxide, nitride and metal, described tellurides is selected from three antimony tellurides, bismuth telluride, cadmium telluride, three telluride two indiums, at least one in telluride tin and lead telluride, described nitride is selected from silicon nitride, aluminium nitride, boron nitride, hafnium nitride, at least one in tantalum nitride and titanium nitride, described metal is selected from silver, aluminium, nickel, gold, at least one in copper and platinum, described metal oxide is selected from meta-aluminic acid magnesium, bismuth titanates, chromic acid nickel, cobalt-chromate, lutetium acid iron and yttrium aluminate at least one.
7. the preparation method of organic electroluminescence device according to claim 6, is characterized in that, the thickness of described first silicon oxynitride layer is 150nm ~ 200nm; The thickness of described first inorganic barrier layer is 100nm ~ 200nm; The thickness of described second silicon oxynitride layer is 150nm ~ 200nm; The thickness of described second inorganic barrier layer is 100nm ~ 200nm.
8. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that, described in described first inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, and the mass percentage of described metal is 10% ~ 30%, and all the other are described tellurides.
9. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: described in described second inorganic barrier layer, the mass percentage of nitride is 10% ~ 40%, the mass percentage of described metal is 10% ~ 30%, and all the other are described metal oxide.
10. the preparation method of organic electroluminescence device according to claim 6, it is characterized in that: described first silicon oxynitride layer and the equal using plasma of described second silicon oxynitride layer strengthen chemical vapour deposition technique preparation, unstrpped gas is hmds, ammonia and oxygen, carrier gas is argon gas, the flow-rate ratio of wherein said hmds, ammonia and oxygen is (6 ~ 14): (2 ~ 18): (2 ~ 18), temperature is 40 ~ 60 DEG C, air pressure is 30 ~ 60Pa, and power is 0.1 ~ 0.5W/cm 2.
CN201310386249.6A 2013-08-29 2013-08-29 Organic light-emitting device and preparation method for same Pending CN104425754A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104377317A (en) * 2013-08-16 2015-02-25 三星显示有限公司 Thin film encapsulation layer manufacturing apparatus and method of manufacturing display apparatus using the same
WO2020199496A1 (en) * 2019-04-01 2020-10-08 深圳市华星光电半导体显示技术有限公司 Display panel and packaging method for display panel

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104377317A (en) * 2013-08-16 2015-02-25 三星显示有限公司 Thin film encapsulation layer manufacturing apparatus and method of manufacturing display apparatus using the same
CN104377317B (en) * 2013-08-16 2019-04-30 三星显示有限公司 Thin-film encapsulation layer manufacturing equipment and the method for showing equipment using its manufacture
WO2020199496A1 (en) * 2019-04-01 2020-10-08 深圳市华星光电半导体显示技术有限公司 Display panel and packaging method for display panel

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Application publication date: 20150318