CN104078601A - Organic light-emitting diode device and manufacturing method thereof - Google Patents
Organic light-emitting diode device and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to an organic light-emitting diode device and a manufacturing method thereof. The organic light-emitting diode device is of a layer structure, the layer structure is formed by sequentially stacking an anode conductive substrate, a hole injection layer, a hole transmission layer, a light-emitting layer, an electron transmission layer, an electron injection layer and a cathode layer, and the surface of the cathode layer is provided with a mixed barrier layer and an inorganic barrier layer which are alternatively stacked. The organic light-emitting diode device adopts phthalocyanine and fluoride doped organic substance as the mixed barrier layer, enables film layer heat stability to be high and flatness to be good and facilitates film formation of inorganic substance on a film layer, erosion of water, oxygen and other active substrate in the outside to the organic light-emitting diode device can be effectively reduced, accordingly an organic function material and electrodes of the organic light-emitting diode device are effectively protected, the sealing performance requirement of package is met, and the service life of the OLED device can be remarkably prolonged.
Description
Technical field
The present invention relates to field of optoelectronic devices, relate in particular to a kind of organic electroluminescence device.The invention still further relates to the preparation method of this organic electroluminescence device.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.Its typical structure is the luminescent layer of making one deck tens nanometer thickness on ito glass with luminous organic material, and luminescent layer top is provided with the metal electrode of one deck low work function.In the time being added with voltage on electrode, luminescent layer just produces light radiation.
OLED device have active illuminating, luminous efficiency high, low in energy consumption and light, thin, without advantages such as angle limitations, thought to be most likely at by insider the device of new generation that occupies dominance on following illumination and display device market.As a brand-new illumination and Display Technique, the ten years development in the past of OLED technology is swift and violent, has obtained huge achievement.Throw light on because the whole world is increasing and show that producer drops into research and development one after another, having promoted greatly the industrialization process of OLED, making the growth rate of OLED industry surprising, having arrived the eve of scale of mass production at present.
Flexible product is the development trend of organic electroluminescence device, but current short problem of ubiquity life-span, therefore the quality of encapsulation technology directly affects the life-span of device.Main purpose of the present invention is to provide a kind of organic electroluminescence device and preparation method thereof, and this encapsulation technology technique is simple, and waterproof oxygen ability (WVTR) is strong, and the life-span of flexible OLED device is increased significantly.
Summary of the invention
The object of the invention is to solve the problem and shortage that above-mentioned prior art exists, a kind of organic electroluminescence device and preparation method thereof is provided, this organic electroluminescence device adopts the organic substance of doping phthalocyanine thing and fluoride as mixing barrier layer, make rete thermal stability high, evenness is good, be conducive to inorganic matter film forming in the above, can effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device.
The technical scheme that the present invention is directed to above-mentioned technical problem and propose is: a kind of organic electroluminescence devices, this organic electroluminescence device is layer structure, and this layer structure stacks gradually as anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer; Be provided with alternately laminated mixing barrier layer and inorganic barrier layer on described cathode layer surface; Wherein,
The material on described mixing barrier layer is the mixture of phthalein cyanogen thing, organic substance, fluoride and oxide composition; Described phthalein cyanogen thing is the one in CuPc, Phthalocyanine Zinc, FePC, Cobalt Phthalocyanine, manganese phthalocyanine or Nickel Phthalocyanine, described organic substance is N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 4,7-diphenyl-1,10-Phen or 1,3, one in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, described fluoride is LiF, CeF
2, MgF
2, AlF
3, CaF
2or BaF
2in one, described oxide is MoO
3, V
2o
5, WO
3, Cs
2o, Ni
2o or MnO
2in one;
The material of described inorganic barrier layer is TiO
2, MgO, SiO
2, ZrO
2, ZnO or Al
2o
3in one;
Described phthalocyanine thing accounts for the 40～60mol% on described mixing barrier layer, described fluoride accounts for the 10～30mol% on described mixing barrier layer, described oxide accounts for the 10～20mol% on described mixing barrier layer, and the molar percentage that described organic substance accounts for described mixing barrier layer is not more than 40%.
The thickness on described mixing barrier layer is 100nm～200nm.
The thickness of described inorganic barrier layer is 50nm～100nm.
The alternately laminated number of plies of described mixing barrier layer and inorganic barrier layer is 4～6 layers.
The material of described hole injection layer is MoO
3doping content according to 30wt% is doped into N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the doping composite material forming in 4'-diamines;
The material of described hole transmission layer is for adopting 4,4', 4''-tri-(carbazole-9-yl) triphenylamine;
The material of described luminescent layer is the doping composite material that three (2-phenylpyridines) close iridium and be doped to according to the doping content of 5wt% 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) composition;
The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline;
The material of described electron injecting layer is CsN
3mix 4,7-diphenyl-1 according to the doping content of 30wt%, the composite material forming in 10-phenanthroline;
The material of described cathode layer is ZnS, Ag and the ZnS that adopts the method for vacuum evaporation to stack gradually.
The present invention also comprises the preparation method who utilizes above-mentioned organic electroluminescence devices, comprises the steps:
(a), on the anode conductive layer of the anode conducting substrate cleaning up, the method for employing vacuum evaporation stacks gradually prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer;
(b), on described cathode layer, first, adopt the method preparation of vacuum evaporation to mix barrier layer; Then on described mixing barrier layer, adopt the method for magnetron sputtering to prepare inorganic barrier layer; Subsequently, alternately laminated several times preparation mixes barrier layer and inorganic barrier layer successively; Wherein,
The material on described mixing barrier layer is the mixture of phthalein cyanogen thing, organic substance, fluoride and oxide composition; Phthalein cyanogen thing is the one in CuPc, Phthalocyanine Zinc, FePC, Cobalt Phthalocyanine, manganese phthalocyanine or Nickel Phthalocyanine, described organic substance is N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 4,7-diphenyl-1,10-Phen or 1,3, one in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, described fluoride is LiF, CeF
2, MgF
2, AlF
3, CaF
2, BaF
2in one, described oxide is MoO
3, V
2o
5, WO
3, Cs
2o, Ni
2o, MnO
2in one;
The material of described inorganic barrier layer is TiO
2, MgO, SiO
2, ZrO
2, ZnO or Al
2o
3in one;
Described phthalocyanine thing accounts for the 40～60mol% on described mixing barrier layer, described fluoride accounts for the 10～30mol% on described mixing barrier layer, described oxide accounts for the 10～20mol% on described mixing barrier layer, and the molar percentage that described organic substance accounts for described mixing barrier layer is not more than 40%.
The thickness of described inorganic barrier layer is 100nm～200nm; The thickness on described mixing barrier layer is 50nm～100nm.
In described step (a), time prepared by described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer vacuum evaporation, vacuum degree is 1 × 10
-5pa, evaporation rate is
In described step (b), described mixing barrier layer and inorganic barrier layer alternate frequency are 4～6 times.
In described step (a), time prepared by described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer vacuum evaporation, vacuum degree is 1 × 10
-5pa; The evaporation rate of described hole injection layer, hole transmission layer and electron transfer layer is
described luminescent layer and electron injecting layer evaporation rate are
described cathode layer evaporation rate is
Compared with prior art, organic electroluminescence devices of the present invention and preparation method thereof, there is following advantage: organic electroluminescence device of the present invention, adopt the organic substance of doping phthalocyanine thing and fluoride as mixing barrier layer, make rete thermal stability high, evenness is good, be conducive to inorganic matter film forming in the above, can effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, thereby the organic functional material to organic electroluminescence device and electrode have formed effective protection, meet the requirement of the sealing of encapsulation, can improve significantly the life-span of OLED device.
Brief description of the drawings
Fig. 1 is the structural representation of organic electroluminescence device of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.
Organic electroluminescence device of the present invention is layer structure, as shown in Figure 1, this layer structure stacks gradually anode conducting substrate 101, hole injection layer 102, hole transmission layer 103, luminescent layer 104, electron transfer layer 105, electron injecting layer 106, cathode layer 107, mixing barrier layer 108, inorganic barrier layer 109.
In organic electroluminescence device, be provided with alternately laminated mixing barrier layer and the inorganic barrier layer of some layers on above-mentioned cathode layer surface.Mixing barrier layer and the alternately laminated number of plies of inorganic barrier layer is 4～6 layers.
The material of mixing barrier layer is the mixture of phthalein cyanogen thing, organic substance, fluoride and oxide composition; Phthalein cyanogen thing is the one in CuPc, Phthalocyanine Zinc, FePC, Cobalt Phthalocyanine, manganese phthalocyanine or Nickel Phthalocyanine, and organic substance is N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 4,7-diphenyl-1,10-Phen or 1,3, one in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, fluoride is LiF, CeF
2, MgF
2, AlF
3, CaF
2or BaF
2in one, oxide is MoO
3, V
2o
5, WO
3, Cs
2o, Ni
2o or MnO
2in one;
The material of inorganic barrier layer is TiO
2, MgO, SiO
2, ZrO
2, ZnO or Al
2o
3in one;
Phthalocyanine thing accounts for the 40～60mol% that mixes barrier layer, and fluoride accounts for the 10～30mol% that mixes barrier layer, and oxide accounts for the 10～20mol% on described mixing barrier layer, and the molar percentage that organic substance accounts for mixing barrier layer is not more than 40%.
The thickness that mixes barrier layer is 100nm～200nm, and the thickness of inorganic barrier layer is 50nm～100nm.
In organic electroluminescence device, the material of anode conducting substrate 101 comprises anode conductive layer and substrate, its substrate can be glass substrate or organic film substrate, the material of anode conductive layer can be conductive oxide, as, tin indium oxide (ITO), Al-Doped ZnO (AZO), mix indium zinc oxide (IZO) or mix fluorine zinc oxide (FTO), these conductive oxides are prepared on glass substrate, are called for short ito glass, AZO glass, IZO glass, FTO glass.Anode conducting substrate can be made by oneself, also can commercially obtain.In actual applications, can select as required other suitable materials as anode conducting substrate 101.In actual applications, can on anode conducting substrate 101, prepare the anode pattern of required organic electroluminescence device.Anode conducting substrate 101 is prior art, does not repeat them here.
In organic electroluminescence device, material and the thickness of other functional layers are as follows:
The material of hole injection layer is MoO
3doping content according to 30wt% is doped into N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the doping composite material forming in 4'-diamines; Thickness 10nm;
The material of hole transmission layer is for adopting 4,4', 4''-tri-(carbazole-9-yl) triphenylamine; Thickness 30nm
The material of luminescent layer is the doping composite material that three (2-phenylpyridines) close iridium and be doped to according to the doping content of 5wt% 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) composition; Thickness 20nm;
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline; Thickness 10nm;
The material of electron injecting layer is CsN
3mix 4,7-diphenyl-1 according to the doping content of 30wt%, the composite material forming in 10-phenanthroline; Thickness 20nm.
The material of cathode layer adopts ZnS, the Ag and the ZnS that stack gradually, and thickness is 30nm.
To the preparation method of above-mentioned organic electroluminescence device, comprise the steps:
(a), on the anode conductive layer of the anode conducting substrate cleaning up, the method for employing vacuum evaporation stacks gradually prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer;
Time prepared by hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer vacuum evaporation, vacuum degree is 1 × 10
-5pa; The evaporation rate of hole injection layer, hole transmission layer and electron transfer layer is
luminescent layer and electron injecting layer evaporation rate are
cathode layer evaporation rate is
(b), on cathode layer, first, adopt the method preparation of vacuum evaporation to mix barrier layer; Then on mixing barrier layer, adopt the method for magnetron sputtering to prepare inorganic barrier layer; Subsequently, successively prepared by alternately laminated several times mixing barrier layer and inorganic barrier layer; Mixing barrier layer and inorganic barrier layer alternate frequency is 4～6 times.
When vacuum evaporation preparation mixes barrier layer, the vacuum degree of vacuum evaporation is 1 × 10
-5pa～1 × 10
-3pa, the evaporation rate of vacuum evaporation is
when magnetron sputtering is prepared inorganic barrier layer, vacuum degree is 1 × 10
-5pa～1 × 10
-3pa.
Wherein, the material on mixing barrier layer is the mixture of phthalein cyanogen thing, organic substance, fluoride and oxide composition; Phthalein cyanogen thing is the one in CuPc, Phthalocyanine Zinc, FePC, Cobalt Phthalocyanine, manganese phthalocyanine or Nickel Phthalocyanine, and organic substance is N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 4,7-diphenyl-1,10-Phen or 1,3, one in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, fluoride is LiF, CeF
2, MgF
2, AlF
3, CaF
2, BaF
2in one, oxide is MoO
3, V
2o
5, WO
3, Cs
2o, Ni
2o, MnO
2in one;
The material of inorganic barrier layer is TiO
2, MgO, SiO
2, ZrO
2, ZnO or Al
2o
3in one;
Phthalocyanine thing accounts for the 40～60mol% that mixes barrier layer, and fluoride accounts for the 10～30mol% that mixes barrier layer, and oxide accounts for the 10～20mol% that mixes barrier layer, and the molar percentage that organic substance accounts for mixing barrier layer is not more than 40%.
The thickness that mixes barrier layer is 100nm～200nm, and the thickness of inorganic barrier layer is 50nm～100nm.
Be specifically described with 1～6 pair of organic electroluminescence device of the present invention of embodiment and preparation process thereof below:
Embodiment 1
Organic electroluminescence device in the present embodiment is layer structure, and this layer structure is followed successively by:
Anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, cathode layer, mixing barrier layer, inorganic barrier layer.
Specifically be followed successively by the present embodiment: ito glass substrate, MoO
3-NPB layer, TCTA layer, TPBI-Ir (ppy)
3layer, Bphen layer, CsN
3-Bphen layer, ZnS/Ag/ZnS, CuPc-TAPC-LiF-MoO
3layer, TiO
2layer.(brace "/" represents layer structure, and whippletree "-" represents doping mutually.）
Above-mentioned organic electroluminescence device adopts following steps to prepare:
A) pre-treatment of ito glass substrate: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, and described cleaning is all cleaned with supersonic wave cleaning machine, each washing is cleaned 5 minutes, then dries up with nitrogen, then uses stove-drying stand-by; Ito glass after cleaning is also needed to carry out surface activation process, 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;
B) preparation of hole injection layer: by MoO
3be doped in NPB as hole-injecting material, the concentration of doping is 30wt%, and thickness is 10nm, and vacuum degree is 1 × 10
-5pa, evaporation rate is
C) preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
D) luminescent layer: adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) as material of main part, guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
E) preparation of electron transfer layer: evaporation one deck 4 on luminescent layer, 7-diphenyl-1,10-phenanthroline (Bphen) is as electron transfer layer, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
F) preparation of electron injecting layer: with Bphen electron injecting layer material of main part, as by CsN
3mix in Bphen doping content 30wt%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
G) preparation of cathode layer: negative electrode adopts ZnS/Ag/ZnS, and thickness is 100nm, vacuum degree 1 × 10
-5pa, evaporation rate
H) making on mixing barrier layer: adopt the mode of vacuum evaporation to prepare one deck mixing barrier layer on cathode layer, mixing barrier layer is that four kinds of material doping steam work altogether, and one is CuPc(CuPc), another kind is organic substance TAPC, the third is LiF, and the 4th kind is MoO
3, wherein, CuPc proportion is 50mol%, LiF proportion is 30mol%, MoO
3proportion is 16mol%, and organic substance TAPC proportion is 4mol%.Mix the vacuum degree 1 × 10 on barrier layer
-5pa, evaporation rate
thickness 200nm;
I) making of inorganic barrier layer: adopt the method for magnetron sputtering to be made into TiO
2film, the base vacuum degree 1 × 10 of inorganic barrier layer
-5pa, thickness 100nm.When preparation, the flow that passes into Ar is 10sccm, CH
4flow 20sccm;
J) alternately repeat above-mentioned steps h) and i) 6 times.
Embodiment 2
Organic electroluminescence device in the present embodiment is layer structure, and this layer structure is followed successively by:
Anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, cathode layer, mixing barrier layer, inorganic barrier layer.
Specifically be followed successively by the present embodiment: ito glass substrate, MoO
3-NPB layer, TCTA layer, TPBI-Ir (ppy)
3layer, Bphen layer, CsN
3-Bphen layer, ZnS/Ag/ZnS layer, ZnPc-NPB-CeF
2-V
2o
5layer, MgO layer.(brace "/" represents layer structure, and whippletree "-" represents doping mutually.）
Above-mentioned organic electroluminescence device adopts following steps to prepare:
A) pre-treatment of ito glass substrate: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, and described cleaning is all cleaned with supersonic wave cleaning machine, each washing is cleaned 5 minutes, then dries up with nitrogen, then uses stove-drying stand-by; Ito glass after cleaning is also needed to carry out surface activation process, 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;
B) preparation of hole injection layer: by MoO
3be doped in NPB as hole-injecting material, the concentration of doping is 30wt%, and thickness is 10nm, and vacuum degree is 1 × 10
-5pa, evaporation rate is
C) preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
D) luminescent layer: adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) as material of main part, guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
E) preparation of electron transfer layer: evaporation one deck 4 on luminescent layer, 7-diphenyl-1,10-phenanthroline (Bphen) is as electron transfer layer, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
F) preparation of electron injecting layer: with Bphen electron injecting layer material of main part, as by CsN
3mix in Bphen doping content 30wt%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
G) preparation of cathode layer: negative electrode adopts ZnS/Ag/ZnS, and thickness is 100nm, vacuum degree 1 × 10
-5pa, evaporation rate
H) making on mixing barrier layer: adopt the mode of vacuum evaporation to prepare one deck mixing barrier layer on cathode layer, mixing barrier layer is that four kinds of materials doping steam work altogether, and one is ZnPc(Phthalocyanine Zinc), another kind is NPB, the third is CeF
2, the 4th kind is V
2o
5, ZnPc proportion is 40mol%, NPB proportion is 35mol%, CeF
2proportion is 15mol%, V
2o
5proportion is 10mol%, mixes the vacuum degree 5 × 10 on barrier layer
-5pa, evaporation rate
thickness 150nm;
I) making of inorganic barrier layer: adopt the method for magnetron sputtering to be made into MgO film, the base vacuum degree 1 × 10 of inorganic barrier layer
-5pa, thickness 50nm.When preparation, the flow that passes into Ar is 5sccm, CH
4flow 15sccm;
J) alternately repeat above-mentioned steps h) and i) 5 times.
Embodiment 3
Organic electroluminescence device in the present embodiment is layer structure, and this layer structure is followed successively by:
Anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, cathode layer, mixing barrier layer, inorganic barrier layer.
Specifically be followed successively by the present embodiment: ito glass substrate, MoO
3-NPB layer, TCTA layer, TPBI-Ir (ppy)
3layer, Bphen layer, CsN
3-Bphen layer, ZnS/Ag/ZnS, FePc-Alq
3-MgF
2-WO
3layer, SiO
2layer.(brace "/" represents layer structure, and whippletree "-" represents doping mutually.）
Above-mentioned organic electroluminescence device adopts following steps to prepare:
A) pre-treatment of ito glass substrate: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, and described cleaning is all cleaned with supersonic wave cleaning machine, each washing is cleaned 5 minutes, then dries up with nitrogen, then uses stove-drying stand-by; Ito glass after cleaning is also needed to carry out surface activation process, 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;
B) preparation of hole injection layer: by MoO
3be doped in NPB as hole-injecting material, the concentration of doping is 30wt%, and thickness is 10nm, and vacuum degree is 1 × 10
-5pa, evaporation rate is
C) preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
D) luminescent layer: adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) as material of main part, guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
E) preparation of electron transfer layer: evaporation one deck 4 on luminescent layer, 7-diphenyl-1,10-phenanthroline (Bphen) is as electron transfer layer, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
F) preparation of electron injecting layer: with Bphen electron injecting layer material of main part, as by CsN
3mix in Bphen doping content 30wt%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
G) preparation of cathode layer: negative electrode adopts ZnS/Ag/ZnS, and thickness is 100nm, vacuum degree 1 × 10
-5pa, evaporation rate
H) making on mixing barrier layer: adopt the mode of vacuum evaporation to prepare one deck mixing barrier layer on cathode layer, mixing barrier layer is that four kinds of materials doping steam work altogether, and one is FePc(FePC), another kind is Alq
3, the third is MgF
2, the 4th kind is WO
3, FePc proportion is 60mol%, Alq
3proportion is 10mol%MgF
2proportion is 10mol%, WO
3proportion is 20mol%, vacuum degree 1 × 10
-5pa, evaporation rate
thickness 200nm;
I) making of inorganic barrier layer: adopt the method for magnetron sputtering to be made into SiO
2film, the base vacuum degree 1 × 10 of inorganic barrier layer
-5pa, thickness 70nm.When preparation, the flow that passes into Ar is 7sccm, CH
4flow 10sccm;
J) alternately repeat above-mentioned steps h) and i) 6 times.
Embodiment 4
Organic electroluminescence device in the present embodiment is layer structure, and this layer structure is followed successively by:
Anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, cathode layer, mixing barrier layer, inorganic barrier layer.
Specifically be followed successively by the present embodiment: ito glass substrate, MoO
3-NPB layer, TCTA layer, TPBI-Ir (ppy)
3layer, Bphen layer, CsN
3-Bphen layer, ZnS/Ag/ZnS, CoPc-m-MTDATA-AlF
3-Cs
2o layer, ZrO
2layer.(brace "/" represents layer structure, and whippletree "-" represents doping mutually.）
Above-mentioned organic electroluminescence device adopts following steps to prepare:
A) pre-treatment of ito glass substrate: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, and described cleaning is all cleaned with supersonic wave cleaning machine, each washing is cleaned 5 minutes, then dries up with nitrogen, then uses stove-drying stand-by; Ito glass after cleaning is also needed to carry out surface activation process, 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;
B) preparation of hole injection layer: by MoO
3be doped in NPB as hole-injecting material, the concentration of doping is 30wt%, and thickness is 10nm, and vacuum degree is 1 × 10
-5pa, evaporation rate is
C) preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
D) luminescent layer: adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) as material of main part, guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
E) preparation of electron transfer layer: evaporation one deck 4 on luminescent layer, 7-diphenyl-1,10-phenanthroline (Bphen) is as electron transfer layer, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
F) preparation of electron injecting layer: with Bphen electron injecting layer material of main part, as by CsN
3mix in Bphen doping content 30wt%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
G) preparation of cathode layer: negative electrode adopts ZnS/Ag/ZnS, and thickness is 100nm, vacuum degree 1 × 10
-5pa, evaporation rate
H) making on mixing barrier layer: adopt the mode of vacuum evaporation to prepare one deck mixing barrier layer on cathode layer, mixing barrier layer is that four kinds of materials doping steam work altogether, and one is CoPc(Cobalt Phthalocyanine), another kind is m-MTDATA, the third is AlF
3, the 4th kind is Cs
2o, CoPc proportion is 50mol%, m-MTDATA proportion is 15mol%, AlF
3proportion is 20mol%, Cs
2o proportion is 15mol%, mixes the vacuum degree 5 × 10 on barrier layer
-5pa, evaporation rate
thickness 150nm;
I) making of inorganic barrier layer: adopt the method for magnetron sputtering to be made into ZrO
2film, the base vacuum degree 5 × 10 of inorganic barrier layer
-5pa, thickness 100nm, when preparation, passes into Ar flow 10sccm, CH
4flow 20sccm;
J) alternately repeat above-mentioned steps h) and i) 4 times.
Embodiment 5
Organic electroluminescence device in the present embodiment is layer structure, and this layer structure is followed successively by:
Anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, cathode layer, mixing barrier layer, inorganic barrier layer.
Specifically be followed successively by the present embodiment: ito glass substrate, MoO
3-NPB layer, TCTA layer, TPBI-Ir (ppy)
3layer, Bphen layer, CsN
3-Bphen layer, ZnS/Ag/ZnS, MnPc-BCP-CaF
2-Ni
2o layer, ZnO layer.(brace "/" represents layer structure, and whippletree "-" represents doping mutually.）
Above-mentioned organic electroluminescence device adopts following steps to prepare:
A) pre-treatment of ito glass substrate: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, and described cleaning is all cleaned with supersonic wave cleaning machine, each washing is cleaned 5 minutes, then dries up with nitrogen, then uses stove-drying stand-by; Ito glass after cleaning is also needed to carry out surface activation process, 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;
B) preparation of hole injection layer: by MoO
3be doped in NPB as hole-injecting material, the concentration of doping is 30wt%, and thickness is 10nm, and vacuum degree is 1 × 10
-5pa, evaporation rate is
C) preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
D) luminescent layer: adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) as material of main part, guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
E) preparation of electron transfer layer: evaporation one deck 4 on luminescent layer, 7-diphenyl-1,10-phenanthroline (Bphen) is as electron transfer layer, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
F) preparation of electron injecting layer: with Bphen electron injecting layer material of main part, as by CsN
3mix in Bphen doping content 30wt%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
G) preparation of cathode layer: negative electrode adopts ZnS/Ag/ZnS, and thickness is 100nm, vacuum degree 1 × 10
-5pa, evaporation rate
H) making on mixing barrier layer: adopt the mode of vacuum evaporation to prepare one deck mixing barrier layer on cathode layer, mixing barrier layer is that four kinds of materials doping steam work altogether, and one is MnPc(manganese phthalocyanine), another kind is BCP, the third is CaF
2, the 4th kind is Ni
2o, MnPc proportion is 55mol%, BCP proportion is 15mol%CaF
2proportion is 15mol%, Ni
2o proportion is 15mol%, mixes the thickness 150nm on barrier layer, vacuum degree 5 × 10
-5pa, evaporation rate
I) making of inorganic barrier layer: adopt the method for magnetron sputtering to be made into ZnO film, the base vacuum degree 5 × 10 of inorganic barrier layer
-5pa, thickness 80nm.When preparation, the flow that passes into Ar is 5sccm, CH
4flow 20sccm;
J) alternately repeat above-mentioned steps h) and i) 6 times.
Embodiment 6
Organic electroluminescence device in the present embodiment is layer structure, and this layer structure is followed successively by:
Anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer, cathode layer, mixing barrier layer, inorganic barrier layer.
Specifically be followed successively by the present embodiment: ito glass substrate, MoO
3-NPB layer, TCTA layer, TPBI-Ir (ppy)
3layer, Bphen layer, CsN
3-Bphen layer, ZnS/Ag/ZnS, NiPc-TPBi-BaF
2-MnO
2layer, Al
2o
3layer.(brace "/" represents layer structure, and whippletree "-" represents doping mutually.）
Above-mentioned organic electroluminescence device adopts following steps to prepare:
A) pre-treatment of ito glass substrate: acetone cleaning → ethanol cleaning → washed with de-ionized water → ethanol cleans, and described cleaning is all cleaned with supersonic wave cleaning machine, each washing is cleaned 5 minutes, then dries up with nitrogen, then uses stove-drying stand-by; Ito glass after cleaning is also needed to carry out surface activation process, 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;
B) preparation of hole injection layer: by MoO
3be doped in NPB as hole-injecting material, the concentration of doping is 30wt%, and thickness is 10nm, and vacuum degree is 1 × 10
-5pa, evaporation rate is
C) preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) is as hole mobile material, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
D) luminescent layer: adopt 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI) as material of main part, guest materials adopts three (2-phenylpyridines) to close iridium (Ir (ppy)
3), doping content 5%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
E) preparation of electron transfer layer: evaporation one deck 4 on luminescent layer, 7-diphenyl-1,10-phenanthroline (Bphen) is as electron transfer layer, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 10nm;
F) preparation of electron injecting layer: with Bphen electron injecting layer material of main part, as by CsN
3mix in Bphen doping content 30wt%, vacuum degree 1 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
G) preparation of cathode layer: negative electrode adopts ZnS/Ag/ZnS, and thickness is 100nm, vacuum degree 1 × 10
-5pa, evaporation rate
H) making on mixing barrier layer: adopt the mode of vacuum evaporation to prepare one deck mixing barrier layer on cathode layer, mixing barrier layer is that four kinds of materials doping steam work altogether, and one is NiPc(Nickel Phthalocyanine), another kind is TPBi, the third is BaF
2, the 4th kind is MnO
2, NiPc proportion is 60mol%, TPBi proportion is 19mol%, BaF
2proportion is 16mol%, MnO
2proportion is 15mol%, mixes the vacuum degree 1 × 10 on barrier layer
-3pa, evaporation rate
thickness 150nm;
I) making of inorganic barrier layer: adopt the method for magnetron sputtering to be made into Al
2o
3film, the base vacuum degree 1 × 10 of inorganic barrier layer
-3pa, thickness 70nm.When preparation, the flow that passes into Ar is 7sccm, the flow 13sccm of CH4;
J) alternately repeat above-mentioned steps h) and i) 6 times.
Performance test
1～6 pair of organic electroluminescence device of the present invention of above embodiment is carried out to waterproof oxygen ability (WVTR) and transmissivity test, can from following table 1, see, its waterproof oxygen ability reaches 10
-4g/m
2performance more than/day, by the OLED luminescent device of its making, the life-span has also reached average more than 4800 hours.
Table 1
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| WVTR(g/m 2/day) | 6.0E-4 | 6.3E-4 | 6.7E-4 | 7.2E-4 | 7.5E-4 | 8.2E-4 |
| Light transmittance | 63％ | 64％ | 65％ | 67％ | 68％ | 69％ |
| Life-span (hour) | 4945 | 4910 | 4883 | 4845 | 4820 | 4800 |
As can be seen here,, there is following advantage in the preparation method of organic electroluminescence device of the present invention and this organic electroluminescence device:
1. organic electroluminescence device of the present invention; adopt the organic substance of doping phthalocyanine thing and fluoride as mixing barrier layer; make rete thermal stability high; evenness is good; be conducive to inorganic matter film forming in the above, can effectively reduce outside water, the erosion of oxygen isoreactivity material to organic electroluminescence device, thereby the organic functional material to organic electroluminescence device and electrode formed effective protection; meet the requirement of the sealing of encapsulation, the life-span that can improve significantly OLED device.Its waterproof oxygen ability has reached 10
-4g/m
2/ day, by the OLED luminescent device of its making, the life-span has also reached average more than 4800 hours, and encapsulating face light transmittance reaches more than 63%.
2. the preparation method preparation technology of organic electroluminescence device of the present invention is simple, easily prepared by large area, and this technology is specially adapted to the application of flexible OLED device, has solved the encapsulation problem that flexible OLED faces, and has promoted the development of flexible OLED product.
Foregoing; it is only preferred embodiment of the present invention; not for limiting embodiment of the present invention; those of ordinary skill in the art are according to main design of the present invention and spirit; can carry out very easily corresponding flexible or amendment, therefore protection scope of the present invention should be as the criterion with the desired protection range of claims.
Claims (10)
1. an organic electroluminescence device, this organic electroluminescence device is layer structure, this layer structure stacks gradually as anode conducting substrate, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer; It is characterized in that, be provided with alternately laminated mixing barrier layer and inorganic barrier layer on described cathode layer surface; Wherein,
The material on described mixing barrier layer is the mixture of phthalein cyanogen thing, organic substance, fluoride and oxide composition; Described phthalein cyanogen thing is the one in CuPc, Phthalocyanine Zinc, FePC, Cobalt Phthalocyanine, manganese phthalocyanine or Nickel Phthalocyanine, described organic substance is N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 4,7-diphenyl-1,10-Phen or 1,3, one in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, described fluoride is LiF, CeF
2, MgF
2, AlF
3, CaF
2or BaF
2in one, described oxide is MoO
3, V
2o
5, WO
3, Cs
2o, Ni
2o or MnO
2in one;
The material of described inorganic barrier layer is TiO
2, MgO, SiO
2, ZrO
2, ZnO or Al
2o
3in one;
Described phthalocyanine thing accounts for 40～60 mol% on described mixing barrier layer, described fluoride accounts for the 10～30mol% on described mixing barrier layer, described oxide accounts for the 10～20mol% on described mixing barrier layer, and the molar percentage that described organic substance accounts for described mixing barrier layer is not more than 40 %.
2. organic electroluminescence device according to claim 1, is characterized in that, the thickness on described mixing barrier layer is 100nm～200nm.
3. organic electroluminescence device according to claim 1, is characterized in that, the thickness of described inorganic barrier layer is 50nm～100nm.
4. organic electroluminescence device according to claim 1, is characterized in that: the alternately laminated number of plies of described mixing barrier layer and inorganic barrier layer is 4 ~ 6 layers.
5. organic electroluminescence device according to claim 1, is characterized in that:
The material of described hole injection layer is MoO
3doping content according to 30wt% is doped into N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4, the doping composite material forming in 4'-diamines;
The material of described hole transmission layer is for adopting 4,4', 4''-tri-(carbazole-9-yl) triphenylamine;
The material of described luminescent layer is the doping composite material that three (2-phenylpyridines) close iridium and be doped to according to the doping content of 5wt% 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) composition;
The material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline;
The material of described electron injecting layer is CsN
3mix 4,7-diphenyl-1 according to the doping content of 30wt%, the composite material forming in 10-phenanthroline;
The material of described cathode layer is ZnS, Ag and the ZnS that adopts the method for vacuum evaporation to stack gradually.
6. a preparation method for organic electroluminescence device, comprises the steps:
(a), on the anode conductive layer of the anode conducting substrate cleaning up, the method for employing vacuum evaporation stacks gradually prepares hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer;
(b), on described cathode layer, first, adopt the method preparation of vacuum evaporation to mix barrier layer; Then on described mixing barrier layer, adopt the method for magnetron sputtering to prepare inorganic barrier layer; Subsequently, alternately laminated several times mixing barrier layer and inorganic barrier layer successively; Wherein,
The material on described mixing barrier layer is the mixture of phthalein cyanogen thing, organic substance, fluoride and oxide composition; Phthalein cyanogen thing is the one in CuPc, Phthalocyanine Zinc, FePC, Cobalt Phthalocyanine, manganese phthalocyanine or Nickel Phthalocyanine, described organic substance is N, N'-diphenyl-N, N'-bis-(1-naphthyl)-1,1'-biphenyl-4,4'-diamines, oxine aluminium, 4,4', 4''-tri-(N-3-aminomethyl phenyl-N-phenyl amino) triphenylamine, 4,7-diphenyl-1,10-Phen or 1,3, one in 5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene, described fluoride is LiF, CeF
2, MgF
2, AlF
3, CaF
2or BaF
2in one, described oxide is MoO
3, V
2o
5, WO
3, Cs
2o, Ni
2o or MnO
2in one;
The material of described inorganic barrier layer is TiO
2, MgO, SiO
2, ZrO
2, ZnO or Al
2o
3in one;
Described phthalocyanine thing accounts for 40～60 mol% on described mixing barrier layer, described fluoride accounts for the 10～30mol% on described mixing barrier layer, described oxide accounts for the 10～20mol% on described mixing barrier layer, and the molar percentage that described organic substance accounts for described mixing barrier layer is not more than 40 %.
7. preparation method according to claim 6, is characterized in that, the thickness on described mixing barrier layer is 100nm～200nm; The thickness of described inorganic barrier layer is 50nm～100nm.
8. preparation method according to claim 6, it is characterized in that, in described step (a), time prepared by described hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and cathode layer vacuum evaporation, vacuum degree is 1 × 10
-5pa; The evaporation rate of described hole injection layer, hole transmission layer and electron transfer layer is 0.1/s, and described luminescent layer and electron injecting layer evaporation rate are 0.2/s, and described cathode layer evaporation rate is 1/s.
9. preparation method according to claim 6, is characterized in that, in described step (b), described mixing barrier layer and inorganic barrier layer alternate frequency are 4 ~ 6 times.
10. preparation method according to claim 6, is characterized in that, in described step (b), when described vacuum evaporation preparation mixes barrier layer, the vacuum degree of described vacuum evaporation is 1 × 10
-5pa～1 × 10
-3pa, the evaporation rate of described vacuum evaporation is 0.5/s～5/s; When described magnetron sputtering is prepared inorganic barrier layer, vacuum degree is 1 × 10
-5pa～1 × 10
-3pa.
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