CN104518165A - Organic light-emitting device and preparation method thereof - Google Patents
Organic light-emitting device and preparation method thereof Download PDFInfo
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- CN104518165A CN104518165A CN201310456892.1A CN201310456892A CN104518165A CN 104518165 A CN104518165 A CN 104518165A CN 201310456892 A CN201310456892 A CN 201310456892A CN 104518165 A CN104518165 A CN 104518165A
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- H—ELECTRICITY
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- H10K50/844—Encapsulations
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
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Abstract
The invention aims to provide an organic light-emitting device with a packaging layer structure. The packaging layer is composed of silicon oxycarbide barrier layers and inorganic barrier layers which are alternately stacked, wherein the silicon oxycarbide barrier layers are made of silicon oxycarbide, and the inorganic barrier layers are made of B2O3, Al2O3, Ga2O3, In2O3 or Tl2O3. The packaging layer can effectively prevent the erosion of external water, oxygen and other active substances to the organic light-emitting device and prolong the service life of the organic light-emitting device. The invention further provides a preparation method of the organic light-emitting device. The preparation method has the advantages of simple process, cheap raw materials and easy realization of large-area preparation.
Description
Technical field
The present invention relates to field of organic electroluminescence, particularly relate to a kind of organic electroluminescence device and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) is a kind of is luminescent material with organic material, can be the energy conversion device of luminous energy the electric energy conversion applied.It has the outstanding properties such as ultra-thin, self-luminous, response are fast, low-power consumption, has application prospect very widely in fields such as display, illuminations.
Electroluminescent organic material invades responsive especially to oxygen and steam.On the one hand because oxygen is quencher, luminous quantum efficiency can be made significantly to decline, and oxygen also can make its transmittability decline to the oxidation of hole transmission layer; On the other hand, steam can produce hydrolysis to organic compound, its stability is declined greatly, thus causes component failure, shortens the life-span of OLED.Therefore, usually need to carry out packaging protection process to OLED, luminescent device and external environment isolated, divides to prevent water, the intrusion of pernicious gas etc., and then improve stability and the useful life of OLED.
For OLED product, if use traditional OLED encapsulation technology, add encapsulation cover plate in device back, the problems such as weight is large, cost is high, bad mechanical strength can be produced, limit the performance of OLED product.At present, the water oxygen resistant ability of most OLED is not strong, and useful life is shorter, and complicated process of preparation, cost are high.
Summary of the invention
In order to solve the problem; the present invention aims to provide a kind of organic electroluminescence device with encapsulation layer structure; this encapsulated layer can reduce outside water, oxygen isoreactivity material effectively to the erosion of organic electroluminescence device; thus effective protection is formed to device organic functional material and electrode, extend the useful life of organic electroluminescence device.Present invention also offers a kind of preparation method of organic electroluminescence device, this preparation method's technique is simple, cheaper starting materials, is easy to large area preparation.
First aspect, the invention provides a kind of organic electroluminescence device, comprise the anode conducting substrate, light emitting functional layer, negative electrode and the encapsulated layer that stack gradually, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually, and described encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The material on described silicon oxynitride barrier layer is silicon oxynitride;
The material of described inorganic barrier layer is B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3.
Arrange encapsulated layer at cathode outer side, encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer.Preferably, adjacent with negative electrode is silicon oxynitride barrier layer.
Silicon oxynitride barrier layer and inorganic barrier layer obtain better water oxygen barriering effect through repeatedly alternately laminated.Preferably, encapsulated layer is silicon oxynitride barrier layer and the inorganic barrier layer of alternately laminated 3 ~ 5 times.
Preferably, the thickness on silicon oxynitride barrier layer is 150 ~ 200nm.
The material of inorganic barrier layer is B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3.
Preferably, the thickness of inorganic barrier layer is 15 ~ 20nm.
By B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3the rete formed is a kind of ceramic membrane, belongs to dense film, has good water oxygen barrier performance, high temperature high voltage resistant, corrosion-resistant, and hardness is large.Silicon oxynitride has SiO concurrently
2and Si
3n
4feature, there is stable chemical property and higher water preventing ability.Silicon oxynitride provides smooth substrate, and the existence on silicon oxynitride barrier layer can alleviate the stress in thin film of inorganic barrier layer, extends the rete life-span.
Preferably, the material of anode conducting substrate is conducting glass substrate or conduction organic film substrate.More preferably, anode conducting substrate is indium tin oxide (ITO).
Preferably, the thickness of anode conducting substrate is 100nm.
Light emitting functional layer is arranged on anode conducting substrate.
Light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually.
Preferably, the material of hole injection layer is MoO
3the mixture be mixed to form according to mass ratio 1:3 with NPB.
Preferably, the thickness of hole injection layer is 10nm.
Preferably, the material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA).
Preferably, the thickness of hole transmission layer is 40nm.
Preferably, the material of luminescent layer is that three (2-phenylpyridines) close iridium (Ir (ppy)
3) mixture that is mixed to form according to mass ratio 5:95 with 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi).
Preferably, the thickness of luminescent layer is 20nm.
Preferably, the material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen)
Preferably, the thickness of electron transfer layer is 30nm.
Preferably, the material of electron injecting layer is cesium azide (CsN
3) mixture that is mixed to form according to mass ratio 1:3 with Bphen.
Preferably, the thickness of electron injecting layer is 20nm.
Negative electrode is arranged in light emitting functional layer.
Preferably, the material of negative electrode is aluminium (Al).
Preferably, the thickness of negative electrode is 100nm.
Second aspect, the invention provides a kind of preparation method of organic electroluminescence device, comprises the following steps:
S1, provide clean anode conducting substrate, and activation processing is carried out to described anode conducting substrate;
S2, prepare light emitting functional layer and negative electrode in the vacuum evaporation of described anode conducting substrate surface, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually;
S3, strengthen chemical vapour deposition technique at described cathode surface using plasma and prepare silicon oxynitride barrier layer;
S4, atomic layer deposition method is adopted to make inorganic barrier layer at described silicon oxynitride barrier layer surface, the organic electroluminescence device sample on silicon oxynitride barrier layer is had to be placed in the settling chamber of atomic layer deposition system preparation, then in described settling chamber, inject source metal and oxygen source respectively, described source metal is B (CH
3)
3, Al (CH
3)
3, Ga (CH
3)
3, In (CH
3)
3or Tl (CH
3)
3, described oxygen source is steam, obtains described inorganic barrier layer after reaction, and the material of described inorganic barrier layer is B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3;
Repeat step S3 ~ S4 and obtain alternately laminated silicon oxynitride barrier layer and inorganic barrier layer, finally obtain described organic electroluminescence device.
In step S1, by the cleaning of antianode electrically-conductive backing plate, the organic pollution of removing anode conducting substrate surface.
Particularly, the clean operation of anode conducting substrate is: cleaned in supersonic wave cleaning machine with acetone, ethanol, deionized water, ethanol successively by anode conducting substrate, then dry up with nitrogen, stove-drying, obtains the anode conducting substrate cleaned.
Surface activation process is carried out to the anode conducting substrate after cleaning, to increase the oxygen content of conductive surface layer, improves the work function of conductive layer surface.
Preferably, the material of anode conducting substrate is conducting glass substrate or conduction organic film substrate.More preferably, anode conducting substrate is indium tin oxide (ITO).
Preferably, the thickness of anode conducting substrate is 100nm.
In step S2, light emitting functional layer is arranged on anode conducting substrate by vacuum evaporation.
Preferably, during vacuum evaporation light emitting functional layer, condition is vacuum degree 3 × 10
-5pa, evaporation rate
Light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually.
Preferably, the material of hole injection layer is MoO
3the mixture be mixed to form according to mass ratio 1:3 with NPB.
Preferably, the thickness of hole injection layer is 10nm.
Preferably, the material of hole transmission layer is 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA).
Preferably, the thickness of hole transmission layer is 40nm.
Preferably, the material of luminescent layer is that three (2-phenylpyridines) close iridium (Ir (ppy)
3) mixture that is mixed to form according to mass ratio 5:95 with 1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-Ji) benzene (TPBi).
Preferably, the thickness of luminescent layer is 20nm.
Preferably, the material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen)
Preferably, the thickness of electron transfer layer is 30nm.
Preferably, the material of electron injecting layer is cesium azide (CsN
3) mixture that is mixed to form according to mass ratio 1:3 with Bphen.
Preferably, the thickness of electron injecting layer is 20nm.
Negative electrode is arranged in light emitting functional layer by vacuum evaporation.
Preferably, during vacuum evaporation negative electrode, condition is vacuum degree 3 × 10
-5pa, evaporation rate
Preferably, the material of negative electrode is aluminium (Al).
Preferably, the thickness of negative electrode is 100nm.
In step S3, silicon oxynitride barrier layer is arranged on cathode surface by vacuum evaporation.
Using plasma strengthens chemical vapour deposition technique (PECVD) and prepares silicon oxynitride barrier layer, and the stress in thin film of obtained silicon oxynitride is little, has been not easy peeling and has occurred, had good compactness.Preferably, with hmds (HMDS), ammonia, oxygen for source, pass into argon gas, preparation process condition is hmds flow 6 ~ 14sccm, ammonia flow 2 ~ 18sccm, oxygen flow 2 ~ 18sccm, argon flow amount 70 ~ 80sccm.
Preferably, the thickness on silicon oxynitride barrier layer is 150 ~ 200nm.
In step S4, inorganic barrier layer is arranged on silicon oxynitride barrier layer surface by atomic layer deposition method, and by single ald, thin-film material, with stable form close-packed arrays, obtain the film that compactness is good, and smooth surface is smooth.
Particularly, the organic electroluminescence device sample on silicon oxynitride barrier layer is had to be placed in the settling chamber of atomic layer deposition system preparation, then in settling chamber, source metal and oxygen source is injected respectively, alternately be exposed to sample surfaces and react, after multiple ald growth cycle, obtain inorganic barrier layer.
Ald growth cycle is divided into four steps:
The first step: source metal is injected described settling chamber with carrier gas, and be adsorbed on described silicon oxynitride barrier layer, injection length is 10 ~ 20ms, and carrier gas flux is 10 ~ 20sccm;
Second step: inject carrier gas purification settling chamber, remove unnecessary presoma, injection length is 5 ~ 10s, and flow is 10 ~ 20sccm;
3rd step: steam is injected settling chamber with carrier gas, and reacts with described source metal, until the source metal on surface consumes completely, injection length is 10 ~ 20ms, and carrier gas flux is 10 ~ 20sccm;
4th step: inject carrier gas purification settling chamber, avoid the gas-phase reaction of accessory substance, injection length is 5 ~ 10s, and flow is 10 ~ 20sccm.
Preferably, carrier gas is inert gas.
Preferably, the thickness of inorganic barrier layer is 15 ~ 20nm.
After completing steps S3 ~ S4, obtained alternately laminated silicon oxynitride barrier layer and inorganic barrier layer, finally obtain described organic electroluminescence device.
Preferably, step S3 ~ S4 is implemented 3 ~ 5 times, obtains silicon oxynitride barrier layer and the inorganic barrier layer of alternately laminated 3 ~ 5 times.
The present invention has following beneficial effect:
(1) a kind of organic electroluminescence device with encapsulation layer structure provided by the invention, effectively can prevent outside water, oxygen isoreactivity material to the erosion of organic electroluminescence device, have good sealing and longer useful life.
(2) by B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3the rete formed is a kind of ceramic membrane, belong to dense film, have good water oxygen barrier performance, high temperature high voltage resistant, corrosion-resistant, hardness is large.Silicon oxynitride has SiO concurrently
2and Si
3n
4feature, there is stable chemical property and higher water preventing ability.Silicon oxynitride provides smooth substrate, and the existence on silicon oxynitride barrier layer can alleviate the stress in thin film of inorganic barrier layer, extends the rete life-span.
(3) preparation method of a kind of organic electroluminescence device provided by the invention, this preparation method's technique is simple, cheaper starting materials, is easy to large area preparation.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the structure chart of the organic electroluminescence device that the embodiment of the present invention 6 provides.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.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:
A kind of organic electroluminescence device, is obtained by following operating procedure:
(1) clean anode conducting substrate is provided:
Cleaned in supersonic wave cleaning machine with acetone, ethanol, deionized water, ethanol successively by ito glass substrate, individual event washing cleaning 5 minutes, then dry up with nitrogen, stove-drying is stand-by; Surface activation process is carried out to the ito glass after cleaning; ITO thickness is 100nm;
(2) vacuum evaporation light emitting functional layer on ito glass substrate:
Particularly, light emitting functional layer comprises hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
The preparation of hole injection layer: by MoO
3the mixture be mixed to get according to mass ratio 1:3 with NPB as the material of hole injection layer, thickness 10nm, vacuum degree 3 × 10
-5pa, evaporation rate
The preparation of hole transmission layer: adopt 4,4', 4''-tri-(carbazole-9-base) triphenylamine (TCTA) as hole mobile material, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 40nm;
The preparation of luminescent layer: the mixture adopting Ir (ppy) 3 and TPBi to be mixed to form according to mass ratio 5:95 as the material of luminescent layer, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
The preparation of electron transfer layer: evaporation one deck 4,7-diphenyl-1,10-phenanthroline (Bphen) as electron transport material, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 30nm;
The preparation of electron injecting layer: by CsN
3the mixture be mixed to form according to mass ratio 1:3 with Bphen as the material of electron injecting layer, vacuum degree 3 × 10
-5pa, evaporation rate
evaporation thickness 20nm;
(3) negative electrode is prepared on light emitting functional layer surface:
Metallic cathode adopts aluminium (Al), and thickness is 100nm, vacuum degree 3 × 10
-5pa, evaporation rate
(4) encapsulated layer is prepared at cathode outer side:
Encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The making on silicon oxynitride barrier layer: with HMDS, NH
3, O
2for source, pass into argon gas, in PECVD settling chamber, prepare silicon oxynitride film, obtain silicon oxynitride barrier layer, preparation process condition is HMDS flow 10sccm, NH
3flow 10sccm, O
2flow 10sccm, argon flow amount 75sccm, the silicon oxynitride film layer thickness 200nm of generation;
The making of inorganic barrier layer: have the organic electroluminescence device sample on silicon oxynitride barrier layer to be placed in the settling chamber of atomic layer deposition system preparation, then,
A () is by source metal B (CH
3)
3inject settling chamber with nitrogen and deposit on silicon oxynitride barrier layer, injection length is 15ms, and nitrogen flow is 15sccm;
B () nitrogen injection rinses settling chamber, injection length is 7s, and flow is 15sccm;
C then steam is injected settling chamber with nitrogen by (), react with source metal, injection length is 15ms, and nitrogen flow is 15sccm;
D () nitrogen injection rinses settling chamber, injection length is 7s, and flow is 15sccm;
Repetition period (a) ~ (d) step, obtains the inorganic barrier layer that thickness is 20nm, and material is B
2o
3;
Alternately preparation 5 silicon oxynitride barrier layers and inorganic barrier layer, finally obtain organic electroluminescence device.
Embodiment 2:
A kind of organic electroluminescence device, is obtained by following operating procedure:
(1), (2), (3) are with embodiment 1;
(4) encapsulated layer is prepared at cathode outer side:
Encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The making on silicon oxynitride barrier layer: with HMDS, NH
3, O
2for source, pass into argon gas, in PECVD settling chamber, prepare silicon oxynitride film, obtain silicon oxynitride barrier layer, preparation process condition is HMDS flow 14sccm, NH
3flow 18sccm, O
2flow 18sccm, argon flow amount 80sccm, the silicon oxynitride film layer thickness 190nm of generation;
The making of inorganic barrier layer: have the organic electroluminescence device sample on silicon oxynitride barrier layer to be placed in the settling chamber of atomic layer deposition system preparation, then,
A () is by source metal Al (CH
3)
3inject settling chamber with nitrogen and deposit on silicon oxynitride barrier layer, injection length is 20ms, and nitrogen flow is 20sccm;
B () nitrogen injection rinses settling chamber, injection length is 10s, and flow is 20sccm;
C then steam is injected settling chamber with nitrogen by (), react with source metal, injection length is 20ms, and nitrogen flow is 20sccm;
D () nitrogen injection rinses settling chamber, injection length is 10s, and flow is 20sccm; Repetition period (a) ~ (d) step, obtains the inorganic barrier layer that thickness is 19nm, and material is Al
2o
3; Alternately preparation 4 silicon oxynitride barrier layers and inorganic barrier layer, finally obtain organic electroluminescence device.
Embodiment 3:
A kind of organic electroluminescence device, is obtained by following operating procedure:
(1), (2), (3) are with embodiment 1;
(4) encapsulated layer is prepared at cathode outer side:
Encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The making on silicon oxynitride barrier layer: with HMDS, NH
3, O
2for source, pass into argon gas, in PECVD settling chamber, prepare silicon oxynitride film, obtain silicon oxynitride barrier layer, preparation process condition is HMDS flow 12sccm, NH
3flow 15sccm, O
2flow 16sccm, argon flow amount 76sccm, the silicon oxynitride film layer thickness 180nm of generation;
The making of inorganic barrier layer: have the organic electroluminescence device sample on silicon oxynitride barrier layer to be placed in the settling chamber of atomic layer deposition system preparation, then,
A () is by source metal Ga (CH
3)
3inject settling chamber with nitrogen and deposit on silicon oxynitride barrier layer, injection length is 10ms, and nitrogen flow is 10sccm;
B () nitrogen injection rinses settling chamber, injection length is 5s, and flow is 10sccm;
C then steam is injected settling chamber with nitrogen by (), react with source metal, injection length is 10ms, and nitrogen flow is 10sccm;
D () nitrogen injection rinses settling chamber, injection length is 5s, and flow is 10sccm; Repetition period (a) ~ (d) step, obtains the inorganic barrier layer that thickness is 18nm, and material is Ga
2o
3; Alternately preparation 3 silicon oxynitride barrier layers and inorganic barrier layer, finally obtain organic electroluminescence device.
Embodiment 4:
A kind of organic electroluminescence device, is obtained by following operating procedure:
(1), (2), (3) are with embodiment 1;
(4) encapsulated layer is prepared at cathode outer side:
Encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The making on silicon oxynitride barrier layer: with HMDS, NH
3, O
2for source, pass into argon gas, in PECVD settling chamber, prepare silicon oxynitride film, obtain silicon oxynitride barrier layer, preparation process condition is HMDS flow 6sccm, NH
3flow 2sccm, O
2flow 2sccm, argon flow amount 70sccm, the silicon oxynitride film layer thickness 170nm of generation;
The making of inorganic barrier layer: have the organic electroluminescence device sample on silicon oxynitride barrier layer to be placed in the settling chamber of atomic layer deposition system preparation, then,
A () is by source metal In (CH
3)
3inject settling chamber with nitrogen and deposit on silicon oxynitride barrier layer, injection length is 15ms, and nitrogen flow is 17sccm;
B () nitrogen injection rinses settling chamber, injection length is 7s, and flow is 17sccm;
C then steam is injected settling chamber with nitrogen by (), react with source metal, injection length is 15ms, and nitrogen flow is 17sccm;
D () nitrogen injection rinses settling chamber, injection length is 7s, and flow is 17sccm; Repetition period (a) ~ (d) step, obtains the inorganic barrier layer that thickness is 16nm, and material is In
2o
3; Alternately preparation 3 silicon oxynitride barrier layers and inorganic barrier layer, finally obtain organic electroluminescence device.
Embodiment 5:
A kind of organic electroluminescence device, is obtained by following operating procedure:
(1), (2), (3) are with embodiment 1;
(4) encapsulated layer is prepared at cathode outer side:
Encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The making on silicon oxynitride barrier layer: with HMDS, NH
3, O
2for source, pass into argon gas, in PECVD settling chamber, prepare silicon oxynitride film, obtain silicon oxynitride barrier layer, preparation process condition is HMDS flow 8sccm, NH
3flow 5sccm, O
2flow 5sccm, argon flow amount 70sccm, the silicon oxynitride film layer thickness 150nm of generation;
The making of inorganic barrier layer: have the organic electroluminescence device sample on silicon oxynitride barrier layer to be placed in the settling chamber of atomic layer deposition system preparation, then,
A () is by source metal Tl (CH
3)
3inject settling chamber with nitrogen and deposit on silicon oxynitride barrier layer, injection length is 15ms, and nitrogen flow is 11sccm;
B () nitrogen injection rinses settling chamber, injection length is 7s, and flow is 11sccm;
C then steam is injected settling chamber with nitrogen by (), react with source metal, injection length is 15ms, and nitrogen flow is 11sccm;
D () nitrogen injection rinses settling chamber, injection length is 7s, and flow is 11sccm; Repetition period (a) ~ (d) step, obtains the inorganic barrier layer that thickness is 15nm, and material is Tl
2o
3; Alternately preparation 3 silicon oxynitride barrier layers and inorganic barrier layer, finally obtain organic electroluminescence device.
Embodiment 6:
A kind of organic electroluminescence device, is obtained by following operating procedure:
(1), (2), (3) are with embodiment 1;
(4) encapsulated layer is prepared at cathode outer side:
Encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The making on silicon oxynitride barrier layer: with HMDS, NH
3, O
2for source, pass into argon gas, in PECVD settling chamber, prepare silicon oxynitride film, obtain silicon oxynitride barrier layer, preparation process condition is HMDS flow 7sccm, NH
3flow 10sccm, O
2flow 10sccm, argon flow amount 77sccm, the silicon oxynitride film layer thickness 150nm of generation;
The making of inorganic barrier layer: have the organic electroluminescence device sample on silicon oxynitride barrier layer to be placed in the settling chamber of atomic layer deposition system preparation, then,
A () is by source metal B (CH
3)
3inject settling chamber with nitrogen and deposit on silicon oxynitride barrier layer, injection length is 10ms, and nitrogen flow is 15sccm;
B () nitrogen injection rinses settling chamber, injection length is 10s, and flow is 15sccm;
C then steam is injected settling chamber with nitrogen by (), react with source metal, injection length is 10ms, and nitrogen flow is 15sccm;
D () nitrogen injection rinses settling chamber, injection length is 10s, and flow is 15sccm; Repetition period (a) ~ (d) step, obtains the inorganic barrier layer that thickness is 15nm, and material is B
2o
3; Alternately preparation 3 silicon oxynitride barrier layers and inorganic barrier layer, finally obtain organic electroluminescence device.
Fig. 1 is the structural representation of the organic electroluminescence device of the present embodiment.As shown in Figure 1, the structure of this organic electroluminescence device comprises the anode conducting substrate 10, light emitting functional layer 20, negative electrode 30, the encapsulated layer 40(that stack gradually and comprises silicon oxynitride barrier layer 401, inorganic barrier layer 402, silicon oxynitride barrier layer 403, inorganic barrier layer 404, silicon oxynitride barrier layer 405, inorganic barrier layer 406).
Effect example
Life-span (the T70@1000cd/m of test organic electroluminescence device
2), from original intensity 1000cd/m
2decay to the time needed for 70%.The life-span of organic electroluminescence device prepared by the embodiment of the present invention 1 ~ 6 is as shown in table 1.As can be seen from the table, the life time of organic electroluminescence device remains on more than 13000, the longlyest reaches 13495 hours.This illustrates, the organic electroluminescence device of encapsulation layer structure that prepared by the present invention have can prevent outside water, oxygen isoreactivity material to the erosion of organic electroluminescence device effectively, has good sealing and longer useful life.
Table 1
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. an organic electroluminescence device, comprise the anode conducting substrate, light emitting functional layer, negative electrode and the encapsulated layer that stack gradually, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually, it is characterized in that, described encapsulated layer is alternately laminated silicon oxynitride barrier layer and inorganic barrier layer;
The material on described silicon oxynitride barrier layer is silicon oxynitride;
The material of described inorganic barrier layer is B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3.
2. organic electroluminescence device as claimed in claim 1, it is characterized in that, described encapsulated layer is silicon oxynitride barrier layer and the inorganic barrier layer of alternately laminated 3 ~ 5 times.
3. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness on described silicon oxynitride barrier layer is 150 ~ 200nm.
4. organic electroluminescence device as claimed in claim 1, it is characterized in that, the thickness of described inorganic barrier layer is 15 ~ 20nm.
5. a preparation method for organic electroluminescence device, is characterized in that, comprises the following steps:
S1, provide clean anode conducting substrate, and activation processing is carried out to described anode conducting substrate;
S2, prepare light emitting functional layer and negative electrode in the vacuum evaporation of described anode conducting substrate surface, described light emitting functional layer comprises the hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and the electron injecting layer that stack gradually;
S3, strengthen chemical vapour deposition technique at described cathode surface using plasma and prepare silicon oxynitride barrier layer;
S4, atomic layer deposition method is adopted to make inorganic barrier layer at described silicon oxynitride barrier layer surface, the organic electroluminescence device sample on silicon oxynitride barrier layer is had to be placed in the settling chamber of atomic layer deposition system preparation, then in described settling chamber, inject source metal and oxygen source respectively, described source metal is B (CH
3)
3, Al (CH
3)
3, Ga (CH
3)
3, In (CH
3)
3or Tl (CH
3)
3, described oxygen source is steam, obtains described inorganic barrier layer after reaction, and the material of described inorganic barrier layer is B
2o
3, Al
2o
3, Ga
2o
3, In
2o
3or Tl
2o
3;
Repeat step S3 ~ S4 and obtain alternately laminated silicon oxynitride barrier layer and inorganic barrier layer, finally obtain described organic electroluminescence device.
6. the preparation method of organic electroluminescence device as claimed in claim 5, it is characterized in that, plasma enhanced chemical vapor deposition method in step S3 with hmds, ammonia, oxygen for source, pass into argon gas, preparation process condition is hmds flow 6 ~ 14sccm, ammonia flow 2 ~ 18sccm, oxygen flow 2 ~ 18sccm, argon flow amount 70 ~ 80sccm.
7. the preparation method of organic electroluminescence device as claimed in claim 5, it is characterized in that, a manufacturing cycle of the atomic layer deposition method of step S4 is:
A source metal is injected described settling chamber with carrier gas and is deposited on described silicon oxynitride barrier layer by (), injection length is 10 ~ 20ms, and carrier gas flux is 10 ~ 20sccm;
B () is injected carrier gas and is rinsed settling chamber, injection length is 5 ~ 10s, and flow is 10 ~ 20sccm;
C then steam is injected settling chamber with carrier gas by (), react with described source metal, injection length is 10 ~ 20ms, and carrier gas flux is 10 ~ 20sccm;
D () is injected carrier gas and is rinsed settling chamber, injection length is 5 ~ 10s, and flow is 10 ~ 20sccm.
8. the preparation method of organic electroluminescence device as claimed in claim 5, it is characterized in that, described encapsulated layer is silicon oxynitride barrier layer and the inorganic barrier layer of alternately laminated 3 ~ 5 times.
9. the preparation method of organic electroluminescence device as claimed in claim 5, it is characterized in that, the thickness on described silicon oxynitride barrier layer is 150 ~ 200nm.
10. the preparation method of organic electroluminescence device as claimed in claim 5, it is characterized in that, the thickness of described inorganic barrier layer is 15 ~ 20nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109103230A (en) * | 2018-08-27 | 2018-12-28 | 上海天马有机发光显示技术有限公司 | A kind of OLED display panel, the production method of OLED display panel and display device |
| CN109904344A (en) * | 2019-02-28 | 2019-06-18 | 云谷（固安）科技有限公司 | Thin-film packing structure and preparation method thereof |
| WO2020253431A1 (en) * | 2019-06-17 | 2020-12-24 | 南京国兆光电科技有限公司 | Encapsulation structure of organic light-emitting device, and method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109103230A (en) * | 2018-08-27 | 2018-12-28 | 上海天马有机发光显示技术有限公司 | A kind of OLED display panel, the production method of OLED display panel and display device |
| CN109103230B (en) * | 2018-08-27 | 2022-02-08 | 武汉天马微电子有限公司 | OLED display panel, manufacturing method of OLED display panel and display device |
| CN109904344A (en) * | 2019-02-28 | 2019-06-18 | 云谷（固安）科技有限公司 | Thin-film packing structure and preparation method thereof |
| WO2020253431A1 (en) * | 2019-06-17 | 2020-12-24 | 南京国兆光电科技有限公司 | Encapsulation structure of organic light-emitting device, and method |
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