CN104638120A - Transparent organic light-emitting device and method for manufacturing same - Google Patents
Transparent organic light-emitting device and method for manufacturing same Download PDFInfo
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- CN104638120A CN104638120A CN201310561368.0A CN201310561368A CN104638120A CN 104638120 A CN104638120 A CN 104638120A CN 201310561368 A CN201310561368 A CN 201310561368A CN 104638120 A CN104638120 A CN 104638120A
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Abstract
The invention discloses a transparent organic light-emitting device which comprises a packaging layer. The packaging layer comprises a mixed barrier layer, a first silicon oxynitride film layer, an inorganic barrier layer and a second silicon oxynitride film layer; the mixed barrier layer is made of organic compounds, first metal fluorides and second metal fluorides; the organic compounds include at least one type of TAPC, NPB, Alq<3>, m-MTDATA, BCP and TPBi; the first metal fluorides include at least one type of magnesium fluorides, aluminum fluorides and sodium aluminum fluorides; the second metal fluorides include at least one type of lanthanum fluorides, neodymium fluorides and gadolinium fluorides; the first silicon oxynitride film layer and the second silicon oxynitride film layer are made of silicon oxynitride; the inorganic barrier layer is made of at least one type of nitrogen-doped titanium oxides, nitrogen-doped magnesium oxides, nitrogen-doped silicon oxides, nitrogen-doped zirconium oxides, nitrogen-doped zinc oxides and nitrogen-doped aluminum oxides.
Description
Technical field
The present invention relates to organic electroluminescence device technical field, particularly relate to a kind of transparent organic electroluminescent device and preparation method thereof.
Background technology
For existing organic electroluminescence device (OLED), according to the difference of the surface of emission of light, can be divided three classes: bottom-emission organic electroluminescence device (BOLED), top light emitting organic electroluminescence device (TEOLED) and transparent organic electroluminescent device (TOLED).Transparent organic electroluminescent device (TOLED) is with the difference of top light emitting organic electroluminescence device (TEOLED) and bottom organic electroluminescence device (BOLED): negative electrode and anode all adopt transparent material, thus the light produced in photophore is penetrated from negative electrode and anode two sides simultaneously.Its two sides all can utilizing emitted light when powering up for transparent organic electroluminescent device (TOLED), and becomes the characteristic of transparence when not powering up, and opens a special applications direction in display field.
At present, also there is life-span shorter problem in transparent organic electroluminescent device (TOLED), and this is mainly because the oxygen that invades and steam cause.On the one hand, oxygen is quencher, and luminous quantum efficiency can be made significantly to decline, meanwhile, oxygen can with luminescent layer generation oxidation, the carbonyls of generation is also effective quencher; On the other hand, the impact of steam is more apparent, and its main failure mode is the organic compound generation hydrolysis made in transparent devices, also can react with negative electrode simultaneously, its stability is declined greatly, thus causes transparent devices to lose efficacy, reduce useful life.Therefore; in order to effectively suppress the degeneration of transparent organic electroluminescent device (TOLED) in long-term work process and inefficacy; with the life-span making steady operation reach enough, the encapsulation technology playing seal protection effect has just become a break-through point of solution transparent organic electroluminescent device (TOLED) life problems.
Conventional transparent organic electroluminescent device (TOLED) encapsulation technology is in substrate, adopt cover plate to encapsulate.Cover plate encapsulation need seal cover plate and substrate with fluid sealant, and the porousness of fluid sealant makes oxygen and steam be easy to infiltrate transparent devices inside, therefore adopts during this packaged type and generally also needs to add drier in device.Along with the drier in transparent devices adsorbs a large amount of oxygen and steam, drier is made to lose absorbability at short notice, cause in transparent devices, building up oxygen and steam, thus the life-span of transparent devices is significantly declined, the encapsulation requirement of long-life transparent organic electroluminescent device can not be reached.The glass cover-plate of usual employing or the light transmittance of metal cover board lower, the light extraction efficiency of transparent devices can be reduced, affect transparent devices visual effect in actual applications.Meanwhile, the glass cover-plate usually adopted or metal cover board are fragility material, easily crack, and after encapsulation, transparent devices can seem very thick and heavy, is not suitable for flexible and transparent device.Therefore; how to reduce oxygen and steam to the infiltration of transparent devices; improve the life-span of transparent devices; the light extraction efficiency of transparent devices can't be reduced simultaneously; and want to be applicable to flexible and transparent device; effective protection is formed to flexible and transparent device, become current technical staff the problem that will solve in a hurry, this proposes high requirement to package material.
Summary of the invention
For solving the problem, first aspect present invention provides a kind of transparent organic electroluminescent device, namely arranges encapsulated layer on the surface at transparent cathode; First, encapsulated layer provided by the invention has very high compactness, and effectively reduce outside oxygen, steam isoreactivity material to the erosion of the organic compound in transparent organic electroluminescent device and electrode, water resistance (WVTR) reaches as high as 2.11 × 10
-6g/m
2day, thus effective protection is defined to transparent devices, make the life-span of device reach more than 20300 hours (T70@1000cd/m
2); Secondly, encapsulated layer provided by the invention has good light transmission, therefore can not reduce the light extraction efficiency of transparent devices, affects transparent devices visual effect in actual applications; Finally, encapsulated layer provided by the invention also goes for flexible and transparent organic electroluminescence device, forms effective protection to flexible and transparent device.Second aspect present invention additionally provides a kind of preparation method of transparent organic electroluminescent device, and the package material that this method for packing adopts is cheap, and preparation technology is simple, easy large area preparation.
First aspect, the invention provides a kind of transparent organic electroluminescent device, the organic luminescence function layer, transparent cathode and the encapsulated layer that comprise transparent anode conductive substrates and be cascading on the surface in described transparent anode conductive substrates; Described encapsulated layer comprises the mixing barrier layer be cascading on described transparent cathode surface, the first silicon oxynitride film, inorganic barrier layer and the second silicon oxynitride film;
The material on described mixing barrier layer includes organic compounds and the first metal fluoride be entrained in described organic compound and the second metal fluoride; Described organic compound is 1,1-bis-((4-N, N '-two (p-methylphenyl) amine) phenyl) cyclohexane (TAPC), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq
3), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl amino) triphenylamine (m-MTDATA), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP) and 1, at least one in 3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi); Described first metal fluoride is magnesium fluoride (MgF
2), aluminum fluoride (AlF
3) and aluminium sodium fluoride (Na
3alF
6) at least one; Described second metal fluoride is lanthanum fluoride (LaF
3), neodymium fluoride (NdF
3) and gadolinium fluoride (GdF) at least one;
The material of described first silicon oxynitride film and described second silicon oxynitride film is all silicon oxynitride compound (SiO
xn
y, wherein 0.01 < x≤1.5,0.01 < y≤1.3,0.5 < x+y < 2);
The material of described inorganic barrier layer comprises the titanium oxide (TiO of N doping
2: N), the magnesium oxide (MgO:N) of N doping, the silica (SiO of N doping
2: N), the zirconia (ZrO of N doping
2: N), the zinc oxide (ZnO:N) of N doping and the aluminium oxide (Al of N doping
2o
3: N) at least one.
The obstruct water oxygen performance of the metal fluoride in mixing barrier layer is good, organic compound has good pliability, therefore, material includes organic compounds and is entrained in the mixing barrier layer structure densification of the metal fluoride in organic compound, effectively blocking oxygen and water vapor permeable can enter device inside, also can alleviate the stress between rete simultaneously; Adulterate in the material of inorganic barrier layer nitrogen, can improve compactness and the corrosion resistance of inorganic barrier layer, and therefore, inorganic barrier layer also has good oxygen and water vapor rejection ability; The molecular structure of the silicon oxynitride in silicon oxynitride film has inorganic and organic functional group simultaneously, silicon oxynitride compound is made to have the high barrier of inorganic matter and organic adhesive and pliability, oxygen and water vapor permeable path can be extended further, while improving rete barrier property, also can improve the adhesiveness of inorganic barrier layer, and effectively can reduce the stress between rete.Encapsulated layer is the dense composite film that mixing barrier layer, the first silicon oxynitride film, inorganic barrier layer and the multiple rete of the second silicon oxynitride film are laminated; overcome deficiency and defect that monofilm layer brings; extend oxygen and water vapor permeable path; effectively reduce outside oxygen, steam isoreactivity material to the erosion of the organic compound in transparent organic electroluminescent device and electrode, thus defines effective protection to transparent devices.
Preferably, the mass fraction described in the material on described mixing barrier layer shared by the first metal fluoride is 10% ~ 20%, and the mass fraction shared by described second metal fluoride is 10% ~ 20%.
Preferably, the thickness on described mixing barrier layer is 100nm ~ 200nm; The thickness of described first silicon oxynitride film is 150nm ~ 200nm; The thickness of described inorganic barrier layer is 50nm ~ 100nm; The thickness of described second silicon oxynitride film is 150nm ~ 200nm.
Preferably, described transparent anode conductive substrates is transparent conducting glass substrate or electrically conducting transparent plastic-substrates.
More preferably, the material of described transparent conducting glass substrate comprises indium tin oxide (ITO), aluminium zinc oxide (AZO) or indium-zinc oxide (IZO);
The material of described electrically conducting transparent plastic-substrates comprises PETG (PET), polysulfones ether (PES), polyethylene naphthalate (PEN) or polyimides (PI).
Encapsulated layer can to rigid transparent substrates (clear glass substrate) and flexible and transparent substrate (transparent plastic substrate); especially flexible and transparent substrate is encapsulated; this is because the pliability on silicon oxynitride film in thin layer and mixing barrier layer can realize flexible and transparent device can tortuosity, thus effective protection can be formed to flexible and transparent device.
Preferably, described organic luminescence function layer comprises luminescent layer, and comprises at least one in hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer;
Hole injection layer adopts common used material in industry, be preferably N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB) and be entrained in N, N'-diphenyl-N, molybdenum trioxide (MoO in N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB)
3);
Hole transmission layer adopts common used material in industry, is preferably 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA);
Luminescent layer adopts common used material in industry, and preferably, 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];
Electron transfer layer adopts common used material in industry, is preferably 4,7-diphenyl-1,10-phenanthroline (Bphen);
Electron injecting layer adopts common used material in industry, the cesium azide (CsN being preferably 4,7-diphenyl-1,10-phenanthroline (Bphen) and being entrained in 4,7-diphenyl-1,10-phenanthroline (Bphen)
3);
Negative electrode is transparent cathode (dielectric layer/metal level/dielectric layer structure etc. that dielectric layer tramp metal layer is formed), and material is preferably the sandwich that zinc sulphide (ZnS)/silver (Ag)/zinc sulphide (ZnS) is formed.
Second aspect, present invention also offers a kind of preparation method of transparent organic electroluminescent device, comprises the steps:
First electrically conducting transparent substrate surface forms transparent anode conductive substrates, then adopt the method for vacuum evaporation to stack gradually on the surface in described transparent anode conductive substrates and prepare organic luminescence function layer and transparent cathode;
Prepare encapsulated layer on the surface at described transparent cathode, described encapsulated layer comprises the mixing barrier layer be cascading on described transparent cathode surface, the first silicon oxynitride film, inorganic barrier layer and the second silicon oxynitride film;
Adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at described transparent cathode, the material on described mixing barrier layer includes organic compounds and the first metal fluoride be entrained in described organic compound and the second metal fluoride; Described organic compound is 1,1-bis-((4-N, N '-two (p-methylphenyl) amine) phenyl) cyclohexane (TAPC), N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB), oxine aluminium (Alq
3), 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl amino) triphenylamine (m-MTDATA), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP) and 1, at least one in 3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi); Described first metal fluoride is magnesium fluoride (MgF
2), aluminum fluoride (AlF
3) and aluminium sodium fluoride (Na
3alF
6) at least one; Described second metal fluoride is lanthanum fluoride (LaF
3), neodymium fluoride (NdF
3) and gadolinium fluoride (GdF) at least one;
Using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on described mixing barrier layer surface, and the material of described first silicon oxynitride film is silicon oxynitride compound (SiO
xn
y, wherein 0.01 < x≤1.5,0.01 < y≤1.3,0.5 < x+y < 2);
Adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in described first silicon oxynitride film, the material of described inorganic barrier layer comprises the titanium oxide (TiO of N doping
2: N), the magnesium oxide (MgO:N) of N doping, the silica (SiO of N doping
2: N), the zirconia (ZrO of N doping
2: N), the zinc oxide (ZnO:N) of N doping and the aluminium oxide (Al of N doping
2o
3: N) at least one;
Using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and the material of described second silicon oxynitride film is silicon oxynitride compound (SiO
xn
y, wherein 0.01 < x≤1.5,0.01 < y≤1.3,0.5 < x+y < 2).
The depositing temperature of plasma enhanced chemical vapor deposition technology is low, to the structure of device and impact on physical properties little, the thickness of the film made, compactness and uniformity are good, strong adhesion.
Preferably, the process conditions preparing the vacuum evaporation that described mixing barrier layer adopts are: vacuum degree is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
Preferably, the process conditions of described plasma enhanced chemical vapor deposition method are: operating pressure is 10Pa ~ 50Pa, and depositing temperature is 40 DEG C ~ 60 DEG C, and radio-frequency power is 0.1W/cm
2~ 1W/cm
2; The source of the gas adopted in the process of described deposition first silicon oxynitride film and the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of described hmds (HMDS) is 6sccm ~ 14sccm, described ammonia (NH
3) flow be 2sccm ~ 18sccm, described oxygen (O
2) flow be 2sccm ~ 18sccm, the flow of described argon gas (Ar) is 70sccm ~ 80sccm; The structural formula of described hmds (HMDS) is as shown in P:
Preferably, the process conditions of described magnetron sputtering method are: vacuum degree is 1 × 10
-5pa ~ 1 × 10
-3pa, accelerating voltage is 300V ~ 800V, and magnetic field is 50G ~ 200G, and target-substrate distance is 50mm ~ 80mm, and power density is 1W/cm
2~ 40W/cm
2; The target adopted in the process of described Slag coating inorganic barrier layer is titanium oxide (TiO
2), magnesium oxide (MgO), silica (SiO
2), zirconia (ZrO
2), zinc oxide (ZnO) and aluminium oxide (Al
2o
3) at least one, working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of described argon gas (Ar) is 5sccm ~ 10sccm, described ammonia (NH
3) flow be 10sccm ~ 20sccm.
Preferably, the mass fraction described in the material on described mixing barrier layer shared by the first metal fluoride is 10% ~ 20%, and the mass fraction shared by described second metal fluoride is 10% ~ 20%.
Preferably, the thickness on described mixing barrier layer is 100nm ~ 200nm; The thickness of described first silicon oxynitride film is 150nm ~ 200nm; The thickness of described inorganic barrier layer is 50nm ~ 100nm; The thickness of described second silicon oxynitride film is 150nm ~ 200nm.
Preferably, described transparent anode conductive substrates is transparent conducting glass substrate or electrically conducting transparent plastic-substrates.
More preferably, the material of described transparent conducting glass substrate comprises indium tin oxide (ITO), aluminium zinc oxide (AZO) or indium-zinc oxide (IZO);
The material of described electrically conducting transparent plastic-substrates comprises PETG (PET), polysulfones ether (PES), polyethylene naphthalate (PEN) or polyimides (PI).
Preferably, described organic luminescence function layer comprises luminescent layer, and comprises at least one in hole injection layer, hole transmission layer, electron transfer layer and electron injecting layer;
Hole injection layer adopts common used material in industry, be preferably N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB) and be entrained in N, N'-diphenyl-N, molybdenum trioxide (MoO in N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB)
3);
Hole transmission layer adopts common used material in industry, is preferably 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA);
Luminescent layer adopts common used material in industry, and preferably, 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];
Electron transfer layer adopts common used material in industry, is preferably 4,7-diphenyl-1,10-phenanthroline (Bphen);
Electron injecting layer adopts common used material in industry, the cesium azide (CsN being preferably 4,7-diphenyl-1,10-phenanthroline (Bphen) and being entrained in 4,7-diphenyl-1,10-phenanthroline (Bphen)
3);
Negative electrode is transparent cathode (dielectric layer/metal level/dielectric layer structure etc. that dielectric layer tramp metal layer is formed), and material is preferably the sandwich that zinc sulphide (ZnS)/silver (Ag)/zinc sulphide (ZnS) is formed.
Obtain described transparent organic electroluminescent device by above-mentioned steps, comprise the transparent anode conductive substrates, light emitting functional layer, transparent cathode and the encapsulated layer that are cascading.
Compared with prior art, the present invention has following beneficial effect:
1, the encapsulating structure of transparent organic electroluminescent device provided by the invention refer to transparent cathode arrange on the surface comprise mixing barrier layer, encapsulated layer that the first silicon oxynitride film, inorganic barrier layer and the multiple rete of described second silicon oxynitride film are laminated, encapsulation layer structure is fine and close, overcome deficiency and defect that monofilm layer brings, there is very high barrier property, effectively reduce outside oxygen, steam isoreactivity material to the erosion of the organic compound in transparent organic electroluminescent device and electrode, water resistance (WVTR) reaches as high as 2.11 × 10
-6g/m
2day, defines effective protection to transparent devices, makes the life-span of device reach more than 20300 hours (T70@1000cd/m
2);
2, the encapsulated layer of transparent organic electroluminescent device provided by the invention has good light transmission, therefore can not reduce the light extraction efficiency of transparent devices, affects transparent devices visual effect in actual applications;
3, the encapsulated layer of transparent organic electroluminescent device provided by the invention can to rigid transparent substrates (clear glass substrate) and flexible and transparent substrate (transparent plastic substrate), especially flexible and transparent substrate is encapsulated, this is because the pliability on silicon oxynitride film in thin layer and mixing barrier layer can realize flexible and transparent device can tortuosity, thus effective protection can be formed to flexible and transparent device, for flexible display technologies brings breakthrough progress;
4, the package material of the method for packing employing of transparent organic electroluminescent device provided by the invention is cheap, and preparation technology is simple, easy large area preparation.
Accompanying drawing explanation
Fig. 1 is the structural representation of the transparent organic electroluminescent device in embodiment 1;
Fig. 2 is the encapsulation layer structure schematic diagram of the transparent organic electroluminescent device in Fig. 1.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with accompanying drawing and preferred embodiment, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not used in restriction the present invention.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1:
Fig. 1 is the structural representation of the transparent organic electroluminescent device in embodiment 1; As shown in Figure 1, the transparent organic electroluminescent device in embodiment 1 comprise be cascading from the bottom to top ito glass substrate (10), organic luminescence function layer (20), transparent cathode (30) and encapsulated layer (40); Wherein organic electroluminescent functional layer (20) comprises the hole injection layer (21), hole transmission layer (22), luminescent layer (23), electron transfer layer (24) and the electron injecting layer (25) that are cascading from the bottom to top.Fig. 2 is the structural representation of the encapsulated layer of transparent organic electroluminescent device in Fig. 1; As shown in Figure 2, encapsulated layer (40) is included in mixing barrier layer (41) that transparent cathode (30) is cascading on the surface, the first silicon oxynitride film (42), inorganic barrier layer (43) and the second silicon oxynitride film (44).
A preparation method for transparent organic electroluminescent device, comprises the steps:
(1) pre-treatment of ito glass substrate (10): first by ito glass successively with acetone cleaning, ethanol purge, washed with de-ionized water and ethanol purge, all clean with supersonic wave cleaning machine, individual event washing cleaning 5 minutes, dry up with nitrogen, stove-drying is stand-by; Then surface activation process is carried out to the ito glass after cleaning, to increase the oxygen content of conductive surface layer, improve the work function of conductive layer surface; The thickness of ito glass substrate is 100nm;
(2) preparation of organic luminescence function layer (20): adopt on the method for vacuum evaporation ito glass substrate surface after treatment and prepare organic luminescence function layer, organic luminescence function layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that are cascading;
Hole injection layer (21), material comprises N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB) and be entrained in N, N'-diphenyl-N, molybdenum trioxide (MoO in N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB)
3), molybdenum trioxide (MoO
3) shared by mass fraction be 30%, thickness is 10nm, and the vacuum degree of the vacuum evaporation of employing is 1 × 10
-5pa, evaporation rate is
Hole transmission layer (22), material comprises 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA), and thickness is 30nm, and the vacuum degree of the vacuum evaporation of employing is 1 × 10
-5pa, evaporation rate is
Luminescent layer (23), main material comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBI), and object material comprises three (2-phenylpyridines) and closes iridium [Ir (ppy)
3], the mass fraction shared by object material is 5%, and thickness is 20nm, and the vacuum degree of the vacuum evaporation of employing is 1 × 10
-5pa, evaporation rate is
Electron transfer layer (24), material comprises 4,7-diphenyl-1,10-phenanthroline (Bphen), and thickness is 10nm, and the vacuum degree of the vacuum evaporation of employing is 1 × 10
-5pa, evaporation rate is
Electron injecting layer (25), the cesium azide (CsN that material comprises 4,7-diphenyl-1,10-phenanthroline (Bphen) and is entrained in 4,7-diphenyl-1,10-phenanthroline (Bphen)
3), cesium azide (CsN
3) shared by mass fraction be 30%, thickness is 20nm, and the vacuum degree of the vacuum evaporation of employing is 1 × 10
-5pa, evaporation rate is
(3) preparation of transparent cathode (30): adopt the method for vacuum evaporation to prepare negative electrode on the surface at organic luminescence function layer, material comprises the sandwich that zinc sulphide (ZnS)/silver (Ag)/zinc sulphide (ZnS) is formed, the thickness of zinc sulphide (ZnS) is 30nm, the thickness of silver (Ag) is 10nm, and the vacuum degree of the vacuum evaporation of employing is 1 × 10
-5pa, evaporation rate is
(4) preparation of encapsulated layer (40):
A) preparation on barrier layer (41) is mixed: adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at transparent cathode, vacuum degree is 1 × 10
-5pa, evaporation rate is
aluminium sodium fluoride (the Na that the material mixing barrier layer comprises 1,1-bis-((4-N, N '-two (p-methylphenyl) amine) phenyl) cyclohexane (TAPC) and is entrained in 1,1-bis-((4-N, N '-two (p-methylphenyl) amine) phenyl) cyclohexane (TAPC)
3alF
6) and lanthanum fluoride (LaF
3); Aluminium sodium fluoride (Na
3alF
6) shared by mass fraction be 15%, lanthanum fluoride (LaF
3) shared by mass fraction be 15%; The thickness on mixing barrier layer is 200nm;
B) preparation of the first silicon oxynitride film (42): using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on mixing barrier layer surface, and operating pressure is 40Pa, and depositing temperature is 50 DEG C, and radio-frequency power is 0.5W/cm
2; Depositing the source of the gas adopted in the process of the first silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 10sccm, ammonia (NH
3) and oxygen (O
2) flow be 10sccm, the flow of argon gas (Ar) is 75sccm; The thickness of the first silicon oxynitride film is 200nm;
C) preparation of inorganic barrier layer (43): adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in the first silicon oxynitride film, vacuum degree is 1 × 10
-5pa, accelerating voltage is 500V, and magnetic field is 150G, and target-substrate distance is 60mm, and power density is 20W/cm
2; The material of inorganic barrier layer comprises the aluminium oxide (Al of N doping
2o
3: N); The target adopted in the process of Slag coating inorganic barrier layer is aluminium oxide (Al
2o
3), working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of argon gas (Ar) is 8sccm, ammonia (NH
3) flow be 20sccm; The thickness of inorganic barrier layer is 80nm;
D) preparation of the second silicon oxynitride film (44): using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and operating pressure is 40Pa, and depositing temperature is 50 DEG C, and radio-frequency power is 0.5W/cm
2; Depositing the source of the gas adopted in the process of the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 10sccm, ammonia (NH
3) and oxygen (O
2) flow be 10sccm, the flow of argon gas (Ar) is 75sccm; The thickness of the second silicon oxynitride film is 200nm;
The water resistance (WVTR) of the transparent organic electroluminescent device that the present embodiment obtains is 2.02 × 10
-6g/m
2day, the life-span is 20422 hours.
Ca film electrical testing method is adopted to test the vapor permeability of the present embodiment organic electroluminescence device, concrete grammar is: deposit calcium film on the glass substrate, then on calcium film, prepare the encapsulated layer of the present embodiment, by glass substrate and encapsulated layer, calcium film is sealed, then vapor permeability (WVTR is calculated by the electrical parameter of test Ca film, g/m2day), formula is:
Embodiment 2:
A preparation method for transparent organic electroluminescent device, comprises the steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
A) preparation on barrier layer is mixed: adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at transparent cathode, vacuum degree is 1 × 10
-5pa, evaporation rate is
the material on mixing barrier layer comprises N, N'-diphenyl-N, N'-bis-(1-naphthyls)-1,1'-biphenyl-4,4'-diamines (NPB) and be entrained in N, N'-diphenyl-N, aluminum fluoride (AlF in N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines (NPB)
3) and neodymium fluoride (NdF
3); Aluminum fluoride (AlF
3) shared by mass fraction be 20%, neodymium fluoride (NdF
3) shared by mass fraction be 10%; The thickness on mixing barrier layer is 200nm;
B) preparation of the first silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on mixing barrier layer surface, and operating pressure is 10Pa, and depositing temperature is 40 DEG C, and radio-frequency power is 0.1W/cm
2; Depositing the source of the gas adopted in the process of the first silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 12sccm, ammonia (NH
3) flow be 15sccm, oxygen (O
2) flow be 10sccm, the flow of argon gas (Ar) is 77sccm; The thickness of the first silicon oxynitride film is 180nm;
C) preparation of inorganic barrier layer: adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in the first silicon oxynitride film, vacuum degree is 1 × 10
-5pa, accelerating voltage is 300V, and magnetic field is 50G, and target-substrate distance is 50mm, and power density is 1W/cm
2; The material of inorganic barrier layer comprises the zinc oxide (ZnO:N) of N doping; The target adopted in the process of Slag coating inorganic barrier layer is zinc oxide (ZnO), and working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of argon gas (Ar) is 10sccm, ammonia (NH
3) flow be 10sccm; The thickness of inorganic barrier layer is 100nm;
D) preparation of the second silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and operating pressure is 10Pa, and depositing temperature is 40 DEG C, and radio-frequency power is 0.1W/cm
2; Depositing the source of the gas adopted in the process of the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 12sccm, ammonia (NH
3) flow be 15sccm, oxygen (O
2) flow be 10sccm, the flow of argon gas (Ar) is 77sccm; The thickness of the second silicon oxynitride film is 180nm;
The water resistance (WVTR) of the transparent organic electroluminescent device that the present embodiment obtains is 2.05 × 10
-6g/m
2day, the life-span is 20382 hours.
Embodiment 3:
A preparation method for transparent organic electroluminescent device, comprises the steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
A) preparation on barrier layer is mixed: adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at transparent cathode, vacuum degree is 1 × 10
-5pa, evaporation rate is
the material on mixing barrier layer comprises oxine aluminium (Alq
3) and be entrained in oxine aluminium (Alq
3) in magnesium fluoride (MgF
2) and gadolinium fluoride (GdF); Magnesium fluoride (MgF
2) shared by mass fraction be 10%, the mass fraction shared by gadolinium fluoride (GdF) is 20%; The thickness on mixing barrier layer is 100nm;
B) preparation of the first silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on mixing barrier layer surface, and operating pressure is 50Pa, and depositing temperature is 60 DEG C, and radio-frequency power is 1W/cm
2; Depositing the source of the gas adopted in the process of the first silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 8sccm, ammonia (NH
3) flow be 5sccm, oxygen (O
2) flow be 8sccm, the flow of argon gas (Ar) is 75sccm; The thickness of the first silicon oxynitride film is 170nm;
C) preparation of inorganic barrier layer: adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in the first silicon oxynitride film, vacuum degree is 1 × 10
-5pa, accelerating voltage is 800V, and magnetic field is 200G, and target-substrate distance is 80mm, and power density is 1W/cm
2; The material of inorganic barrier layer comprises the zirconia (ZrO of N doping
2: N); The target adopted in the process of Slag coating inorganic barrier layer is zirconia (ZrO
2), working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of argon gas (Ar) is 5sccm, ammonia (NH
3) flow be 15sccm; The thickness of inorganic barrier layer is 50nm;
D) preparation of the second silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and operating pressure is 50Pa, and depositing temperature is 60 DEG C, and radio-frequency power is 40W/cm
2; Depositing the source of the gas adopted in the process of the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 8sccm, ammonia (NH
3) flow be 5sccm, oxygen (O
2) flow be 8sccm, the flow of argon gas (Ar) is 75sccm; The thickness of the second silicon oxynitride film is 170nm;
The water resistance (WVTR) of the transparent organic electroluminescent device that the present embodiment obtains is 2.06 × 10
-6g/m
2day, the life-span is 20340 hours.
Embodiment 4:
A preparation method for transparent organic electroluminescent device, comprises the steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
A) preparation on barrier layer is mixed: adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at transparent cathode, vacuum degree is 5 × 10
-5pa, evaporation rate is
the material on mixing barrier layer comprises 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine (m-MTDATA) and be entrained in 4,4', the aluminium sodium fluoride (Na in 4''-tri-(N-3-methylphenyl-N-phenyl amino) triphenylamine (m-MTDATA)
3alF
6) and lanthanum fluoride (LaF
3); Aluminium sodium fluoride (Na
3alF
6) shared by mass fraction be 16%, lanthanum fluoride (LaF
3) shared by mass fraction be 13%; The thickness on mixing barrier layer is 130nm;
B) preparation of the first silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on mixing barrier layer surface, and operating pressure is 30Pa, and depositing temperature is 50 DEG C, and radio-frequency power is 0.8W/cm
2; Depositing the source of the gas adopted in the process of the first silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 14sccm, ammonia (NH
3) and oxygen (O
2) flow be 18sccm, the flow of argon gas (Ar) is 70sccm; The thickness of the first silicon oxynitride film is 160nm;
C) preparation of inorganic barrier layer: adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in the first silicon oxynitride film, vacuum degree is 5 × 10
-5pa, accelerating voltage is 400V, and magnetic field is 100G, and target-substrate distance is 60mm, and power density is 20W/cm
2; The material of inorganic barrier layer comprises the silica (SiO of N doping
2: N); The target adopted in the process of Slag coating inorganic barrier layer is silica (SiO
2), working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of argon gas (Ar) is 9sccm, ammonia (NH
3) flow be 17sccm; The thickness of inorganic barrier layer is 70nm;
D) preparation of the second silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and operating pressure is 30Pa, and depositing temperature is 50 DEG C, and radio-frequency power is 0.5W/cm
2; Depositing the source of the gas adopted in the process of the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 14sccm, ammonia (NH
3) and oxygen (O
2) flow be 18sccm, the flow of argon gas (Ar) is 70sccm; The thickness of the second silicon oxynitride film is 160nm;
The water resistance (WVTR) of the transparent organic electroluminescent device that the present embodiment obtains is 2.07 × 10
-6g/m
2day, the life-span is 20326 hours.
Embodiment 5:
A preparation method for transparent organic electroluminescent device, comprises the steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
A) preparation on barrier layer is mixed: adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at transparent cathode, vacuum degree is 5 × 10
-5pa, evaporation rate is
aluminum fluoride (the AlF that the material mixing barrier layer comprises 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP) and is entrained in 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP)
3) and neodymium fluoride (NdF
3); Aluminum fluoride (AlF
3) shared by mass fraction be 16%, neodymium fluoride (NdF
3) shared by mass fraction be 11%; The thickness on mixing barrier layer is 140nm;
B) preparation of the first silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on mixing barrier layer surface, and operating pressure is 45Pa, and depositing temperature is 55 DEG C, and radio-frequency power is 0.9W/cm
2; Depositing the source of the gas adopted in the process of the first silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 6sccm, ammonia (NH
3) flow be 2sccm, oxygen (O
2) flow be 2sccm, the flow of argon gas (Ar) is 80sccm; The thickness of the first silicon oxynitride film is 150nm;
C) preparation of inorganic barrier layer: adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in the first silicon oxynitride film, vacuum degree is 5 × 10
-5pa, accelerating voltage is 500V, and magnetic field is 150G, and target-substrate distance is 70mm, and power density is 30W/cm
2; The material of inorganic barrier layer comprises the magnesium oxide (MgO:N) of N doping; The target adopted in the process of Slag coating inorganic barrier layer is magnesium oxide (MgO), and working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of argon gas (Ar) is 7sccm, ammonia (NH
3) flow be 12sccm; The thickness of inorganic barrier layer is 60nm;
D) preparation of the second silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and operating pressure is 50Pa, and depositing temperature is 50 DEG C, and radio-frequency power is 30W/cm
2; Depositing the source of the gas adopted in the process of the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 6sccm, ammonia (NH
3) flow be 2sccm, oxygen (O
2) flow be 2sccm, the flow of argon gas (Ar) is 80sccm; The thickness of the second silicon oxynitride film is 150nm;
The water resistance (WVTR) of the transparent organic electroluminescent device that the present embodiment obtains is 2.08 × 10
-6g/m
2day, the life-span is 20314 hours.
Embodiment 6:
A preparation method for transparent organic electroluminescent device, comprises the steps:
(1), (2), (3) are with embodiment 1;
(4) preparation of encapsulated layer:
A) preparation on barrier layer is mixed: adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at transparent cathode, vacuum degree is 1 × 10
-3pa, evaporation rate is
magnesium fluoride (the MgF that the material mixing barrier layer comprises 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi) and is entrained in 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi)
2) and gadolinium fluoride (GdF); Magnesium fluoride (MgF
2) shared by mass fraction be 12%, the mass fraction shared by gadolinium fluoride (GdF) is 12%; The thickness on mixing barrier layer is 120nm;
B) preparation of the first silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on mixing barrier layer surface, and operating pressure is 35Pa, and depositing temperature is 45 DEG C, and radio-frequency power is 15W/cm
2; Depositing the source of the gas adopted in the process of the first silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 6sccm, ammonia (NH
3) flow be 15sccm, oxygen (O
2) flow be 5sccm, the flow of argon gas (Ar) is 75sccm; The thickness of the first silicon oxynitride film is 160nm;
C) preparation of inorganic barrier layer: adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in the first silicon oxynitride film, vacuum degree is 1 × 10
-3pa, accelerating voltage is 550V, and magnetic field is 160G, and target-substrate distance is 70mm, and power density is 40W/cm
2; The material of inorganic barrier layer comprises the titanium oxide (TiO of N doping
2: N); The target adopted in the process of Slag coating inorganic barrier layer is titanium oxide (TiO
2), working gas is argon gas (Ar), and reacting gas is ammonia (NH
3); The flow of argon gas (Ar) is 8sccm, ammonia (NH
3) flow be 15sccm; The thickness of inorganic barrier layer is 70nm;
D) preparation of the second silicon oxynitride film: using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and operating pressure is 40Pa, and depositing temperature is 55 DEG C, and radio-frequency power is 0.8W/cm
2; Depositing the source of the gas adopted in the process of the second silicon oxynitride film is hmds (HMDS), ammonia (NH
3) and oxygen (O
2), loading gas is argon gas (Ar); The flow of hmds (HMDS) is 6sccm, ammonia (NH
3) flow be 15sccm, oxygen (O
2) flow be 5sccm, the flow of argon gas (Ar) is 75sccm; The thickness of the second silicon oxynitride film is 160nm;
The water resistance (WVTR) of the transparent organic electroluminescent device that the present embodiment obtains is 2.11 × 10
-6g/m
2day, the life-span is 20300 hours.
Effect example
For the beneficial effect of valid certificates transparent organic electroluminescence device provided by the invention, provide relevant experimental data as follows.
The water resistance of table 1. transparent organic electroluminescent device, useful life and encapsulating face light transmittance information slip
Table 1 is the water resistance of transparent organic electroluminescent device in embodiment 1 ~ 6, useful life and encapsulating face light transmittance information slip.As can be seen from Table 1, the water resistance (WVTR) of organic electroluminescence device provided by the invention reaches as high as 2.11 × 10
-6g/m
2day, the life-span all reaches more than 20300 hours (T70@1000cd/m
2: namely starting brightness is 1000cd/m
2brightness decay is to 70% time used), and the light transmittance of encapsulating face reaches 36% ~ 43%, illustrate that encapsulated layer provided by the invention has very high compactness, effectively reduce outside oxygen, steam isoreactivity material to the erosion of the organic compound in transparent organic electroluminescent device and electrode, thus effective protection is defined to transparent devices, extend the useful life of transparent devices; And encapsulated layer provided by the invention has good light transmission, therefore can not reduce the light extraction efficiency of transparent devices, affect transparent devices visual effect in actual applications.
Encapsulation rete compactness and light transmittance most important for transparent organic electroluminescent device, suitable process conditions can be selected according to device detection result.Certainly, the above is only individual example of the present invention, all according to the structure described in the present patent application the scope of the claims, principle and similar change, all should be contained in the scope of the present patent application patent.
Claims (10)
1. a transparent organic electroluminescent device, the organic luminescence function layer, transparent cathode and the encapsulated layer that comprise transparent anode conductive substrates and be cascading on the surface in described transparent anode conductive substrates, it is characterized in that, described encapsulated layer comprises the mixing barrier layer be cascading on described transparent cathode surface, the first silicon oxynitride film, inorganic barrier layer and the second silicon oxynitride film;
The material on described mixing barrier layer includes organic compounds and the first metal fluoride be entrained in described organic compound and the second metal fluoride; Described organic compound is 1,1-bis-((4-N, N '-two (p-methylphenyl) amine) phenyl) cyclohexane, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine, 2,9-dimethyl-4,7-diphenyl-1, at least one in 10-phenanthroline and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene; Described first metal fluoride is at least one in magnesium fluoride, aluminum fluoride and aluminium sodium fluoride; Described second metal fluoride is at least one in lanthanum fluoride, neodymium fluoride and gadolinium fluoride;
The material of described first silicon oxynitride film and described second silicon oxynitride film is all silicon oxynitride compound;
The material of described inorganic barrier layer comprises at least one in the aluminium oxide of the titanium oxide of N doping, the magnesium oxide of N doping, the silica of N doping, the zirconia of N doping, the zinc oxide of N doping and N doping.
2. transparent organic electroluminescent device according to claim 1, it is characterized in that, mass fraction described in the material on described mixing barrier layer shared by the first metal fluoride is 10% ~ 20%, and the mass fraction shared by described second metal fluoride is 10% ~ 20%.
3. transparent organic electroluminescent device according to claim 1, is characterized in that, the thickness on described mixing barrier layer is 100nm ~ 200nm; The thickness of described first silicon oxynitride film is 150nm ~ 200nm; The thickness of described inorganic barrier layer is 50nm ~ 100nm; The thickness of described second silicon oxynitride film is 150nm ~ 200nm.
4. transparent organic electroluminescent device according to claim 1, is characterized in that, described transparent anode conductive substrates is transparent conducting glass substrate or electrically conducting transparent plastic-substrates.
5. a preparation method for transparent organic electroluminescent device, is characterized in that, comprises the steps:
First prepared by electrically conducting transparent substrate surface anode pattern and form transparent anode conductive substrates, then adopt the method for vacuum evaporation to stack gradually on the surface in described transparent anode conductive substrates and prepare organic luminescence function layer and transparent cathode;
Prepare encapsulated layer on the surface at described transparent cathode, described encapsulated layer comprises the mixing barrier layer be cascading on described transparent cathode surface, the first silicon oxynitride film, inorganic barrier layer and the second silicon oxynitride film;
Adopt vacuum vapour deposition to prepare mixing barrier layer on the surface at described transparent cathode, the material on described mixing barrier layer includes organic compounds and the first metal fluoride be entrained in described organic compound and the second metal fluoride; Described organic compound is 1,1-bis-((4-N, N '-two (p-methylphenyl) amine) phenyl) cyclohexane, N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-methylphenyl-N-phenyl is amino) triphenylamine, 2,9-dimethyl-4,7-diphenyl-1, at least one in 10-phenanthroline and 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene; Described first metal fluoride is at least one in magnesium fluoride, aluminum fluoride and aluminium sodium fluoride; Described second metal fluoride is at least one in lanthanum fluoride, neodymium fluoride and gadolinium fluoride;
Using plasma strengthens chemical vapour deposition technique and prepare the first silicon oxynitride film on described mixing barrier layer surface, and the material of described first silicon oxynitride film is silicon oxynitride compound;
Adopt magnetron sputtering method to prepare inorganic barrier layer on the surface in described first silicon oxynitride film, the material of described inorganic barrier layer comprises at least one in the aluminium oxide of the titanium oxide of N doping, the magnesium oxide of N doping, the silica of N doping, the zirconia of N doping, the zinc oxide of N doping and N doping;
Using plasma strengthens chemical vapour deposition technique and prepares the second silicon oxynitride film on the surface at described inorganic barrier layer, and the material of described second silicon oxynitride film is silicon oxynitride compound.
6. the preparation method of transparent organic electroluminescent device according to claim 5, is characterized in that, the process conditions preparing the vacuum evaporation that described mixing barrier layer adopts are: vacuum degree is 1 × 10
-5pa ~ 1 × 10
-3pa, evaporation rate is
7. the preparation method of transparent organic electroluminescent device according to claim 5, it is characterized in that, the process conditions of described plasma enhanced chemical vapor deposition method are: operating pressure is 10Pa ~ 50Pa, and depositing temperature is 40 DEG C ~ 60 DEG C, and radio-frequency power is 0.1W/cm
2~ 1W/cm
2; The source of the gas adopted in the process of described deposition first silicon oxynitride film and the second silicon oxynitride film is hmds, ammonia and oxygen, and loading gas is argon gas; The flow of described hmds is 6sccm ~ 14sccm, and the flow of described ammonia is 2sccm ~ 18sccm, and the flow of described oxygen is 2sccm ~ 18sccm, and the flow of described argon gas is 70sccm ~ 80sccm.
8. the preparation method of transparent organic electroluminescent device according to claim 5, is characterized in that, the process conditions of described magnetron sputtering method are: vacuum degree is 1 × 10
-5pa ~ 1 × 10
-3pa, accelerating voltage is 300V ~ 800V, and magnetic field is 50G ~ 200G, and target-substrate distance is 50mm ~ 80mm, and power density is 1W/cm
2~ 40W/cm
2; The target adopted in the process of described Slag coating inorganic barrier layer is at least one in titanium oxide, magnesium oxide, silica, zirconia, zinc oxide and aluminium oxide, and working gas is argon gas, and reacting gas is ammonia; The flow of described argon gas is 5sccm ~ 10sccm, and the flow of described ammonia is 10sccm ~ 20sccm.
9. the preparation method of transparent organic electroluminescent device according to claim 5, it is characterized in that, mass fraction described in the material on described mixing barrier layer shared by the first metal fluoride is 10% ~ 20%, and the mass fraction shared by described second metal fluoride is 10% ~ 20%.
10. the preparation method of transparent organic electroluminescent device according to claim 5, is characterized in that, the thickness on described mixing barrier layer is 100nm ~ 200nm; The thickness of described first silicon oxynitride film is 150nm ~ 200nm; The thickness of described inorganic barrier layer is 50nm ~ 100nm; The thickness of described second silicon oxynitride film is 150nm ~ 200nm.
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