KR20160119614A - Encapsulant for orgarnic light emitting display and preparation method using the same - Google Patents
Encapsulant for orgarnic light emitting display and preparation method using the same Download PDFInfo
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- KR20160119614A KR20160119614A KR1020150048539A KR20150048539A KR20160119614A KR 20160119614 A KR20160119614 A KR 20160119614A KR 1020150048539 A KR1020150048539 A KR 1020150048539A KR 20150048539 A KR20150048539 A KR 20150048539A KR 20160119614 A KR20160119614 A KR 20160119614A
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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Abstract
Description
The present invention relates to an encapsulant for an organic light emitting display and a method of manufacturing an organic light emitting display using the encapsulant.
2. Description of the Related Art [0002] Flat panel display devices that are lightweight and thin and easy to realize high image quality have been rapidly commercialized and spread in accordance with the development of semiconductor manufacturing technology and image processing technology. Such flat panel display devices include a liquid crystal display (LCD) Display (PDP), or organic light emitting diode display (OLED).
OLED display devices are devices that emit light from outside by applying an electric field from outside to self-emit light. They are known to have excellent brightness, color contrast, viewing angle, response speed, and environmental resistance. They are used for low-voltage direct drive, (Anode electrode) and a cathode electrode (cathode electrode), electrons and holes are injected from the outside, and light emitted by the recombination energy is applied to the panel electrode And an arbitrary image is implemented.
Such organic materials used in the OLED display devices are inevitably vulnerable to oxygen or air. When the organic material comes into contact with oxygen or air, a spontaneous oxidation reaction occurs, and as a result, the lifetime of the OLED display device is significantly reduced. As a method for preventing oxidation of organic materials applied to the OLED display device and ensuring a device lifetime characteristic of a commercially available level, there has been studied a technique of encapsulating oxygen and moisture from the outside.
Conventionally, as a sealing technique in an OLED display device, a method of sealing a organic device by applying a glass cap to an organic light emitting diode has been used. This has a problem in that the sealing ability against moisture permeation is excellent but the thickness of the device is increased, the process is complicated, the manufacturing cost is high, the product is vulnerable to external impact, and as a result, it is difficult to apply to a large area OLED display device.
An object of the present invention is to provide an encapsulant for an organic light emitting display device excellent in oxygen and moisture barrier properties.
In addition, the present invention relates to an organic light emitting display device including the encapsulation material.
It is another object of the present invention to provide a method of manufacturing an organic light emitting diode display having improved defect rate and luminous efficiency in an organic light emitting diode display.
1. An encapsulant for an organic light emitting display device comprising a first coating layer formed of silane sol and a second coating layer comprising graphene alternately laminated.
2. The encapsulating material for an organic light emitting display device according to 1 above, wherein the silane sol is formed from a composition for forming a first coating layer comprising an alkoxysilane compound, an acid catalyst, an alcohol solvent and water.
3. The encapsulating material for an organic light emitting display device according to 2 above, wherein the alkoxysilane compound is contained in an amount of 20 to 60% by weight based on the total weight of the composition for forming the first coating layer.
4. The encapsulant according to item 1 above, wherein the graphene has a thickness of 0.3 to 5 nm.
5. The encapsulant for an organic light emitting display according to any one of the above 1 to 4, wherein the sealing material has a WVTR of 10 -6 to 10 -4 g / m 2 / day.
6. forming an organic light emitting device on top of a substrate; And
Laminating an encapsulant for an organic light emitting display device in which a first coating layer formed of a silane sol and a second coating layer containing graphene are alternately stacked on the organic light emitting device,
Wherein the graphene is produced by hydrothermal expansion of expandable graphite.
7. The method of claim 6, wherein the graphene is at least one stripper selected from the group consisting of cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium dodecylbenzenesulfonate (SDBS) Mixing expandable graphite and water;
Heating the mixed liquid containing the expandable graphite to 400 to 500 ° C to obtain hydrothermal expanded graphite; And
Applying a shear force to the hydrothermally expanded graphite mixed solution obtained by mixing the dispersion medium and the dispersant in the hydrothermally expanded graphite.
8. The method of claim 6, wherein the step of laminating the encapsulant on the organic light emitting device comprises: forming a first coating layer with a composition for forming a first coating layer containing an alkoxysilane compound; And forming a second coating layer with a composition for forming a second coating layer including graphene, wherein the second coating layer is formed on the organic light emitting device.
9. The method of claim 8, wherein a first coating layer or a second coating layer is applied to the upper surface of the organic light emitting device.
10. The method of claim 6, wherein the step of laminating the sealing material on the organic light emitting device comprises the steps of: forming a first coating layer on a base film with a composition for forming a first coating layer containing an alkoxysilane compound; Wherein the step of forming the second coating layer with the composition for forming the second coating layer is repeated at least once or more to form an encapsulation material and bonding the encapsulation material to the organic light emitting display device .
11. The method of manufacturing an organic light emitting display device of claim 10, wherein a first coating layer or a second coating layer is applied to the upper surface of the base film.
12. The method of manufacturing an organic light emitting display according to the above 10, wherein the sealing material and the organic light emitting element are bonded together with an adhesive.
13. The method of manufacturing an organic light emitting display according to claim 6, wherein the silane sol is formed of a composition for forming a first coating layer comprising an alkoxysilane compound, an acid catalyst, an alcohol solvent and water.
14. The method of manufacturing an organic light emitting display according to 13 above, wherein the alkoxysilane compound is contained in an amount of 20 to 60% by weight based on the total weight of the composition for forming the first coating layer.
15. The method of manufacturing an organic light emitting display according to 6 above, wherein said graphene has a thickness of 0.3 to 5 nm.
16. The method of claim 6, wherein the organic light emitting device comprises a cathode electrode, an organic light emitting layer, and an anode electrode.
17. An organic light emitting display device comprising an encapsulant according to item 5 above.
The sealing material according to the present invention can effectively protect the organic light emitting display device from the external environment by significantly reducing the moisture permeability of oxygen or moisture by sequentially laminating the coating layers each including graphene and silane sol.
Since the encapsulant according to the present invention includes a thin film of graphene, the uniformity can be ensured when forming the coating layer, and the effect of decreasing the moisture permeability can be ensured uniformly.
INDUSTRIAL APPLICABILITY The method of manufacturing an organic light emitting diode display according to the present invention can effectively prevent the inflow of oxygen or moisture and can manufacture an organic light emitting display device having a significantly low defect rate.
[0001] The present invention relates to an encapsulant for an organic light emitting display and a method of manufacturing an organic light emitting display using the encapsulant. More particularly, the present invention relates to a sealing material for an organic light emitting diode By effectively blocking oxygen or moisture, the organic light emitting display device can be manufactured in a process of manufacturing an organic light emitting display device and an organic light emitting display device capable of minimizing the influence of the external environment at the time of using the product, And an encapsulating material for a device.
Hereinafter, the present invention will be described in more detail.
≪ Encapsulant >
An organic light emitting display device is an apparatus which applies an electric field to a fluorescent compound to emit light without a separate light source. When oxygen or moisture enters from the outside, deterioration of the fluorescent compound occurs, There was an easy problem. Accordingly, the present invention has the above-described problems, which are obtained by sequentially laminating coating layers each containing graphene and a silane sol, by significantly reducing the moisture permeability of oxygen or moisture.
The sealing material according to the present invention has a structure in which a first coating layer formed of a silane sol and a second coating layer containing graphene are alternately laminated.
The first coating layer
The first coating layer formed of a silane sol is bonded to a second coating layer containing graphening described later to serve as a binder. The silane sol has an appropriate adhesive force to prevent graphene from being desorbed in the coating layer.
The silane sol may be formed of a composition for forming a first coating layer containing an alkoxysilane compound, an acid catalyst, an alcohol-based solvent, and water.
The alkoxysilane compound according to the present invention is a binder resin, and its kind is not particularly limited, and examples thereof include tetraalkoxysilane compounds such as tetraethoxysilane, tetramethoxysilane and tetra-n-propoxysilane; Methyltrimethoxysilane, methyltriethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, ethyltrimethoxysilane, methyltripropoxysilane, methyltributoxysilane, propyltrimethoxysilane, propyltriethoxysilane, isobutyltri Alkylalkoxysilane of a substituted or unsubstituted straight-chain or branched alkyl group such as methoxymethylsilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, diethoxysilane, Phenyltrimethoxysilane, phenyltriethoxysilane, phenyltripropoxysilane, phenyltributoxysilane; Aminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 2-aminoethyl-3-aminopropyltrimethoxysilane, N -? - (aminoethyl) N- (n-butyl) -3-aminopropyltrimethoxysilane, 3-aminopropylmethyldiethoxysilane; Dimethyldimethoxysilane, diethyldiethoxysilane,? -Glycidyloxypropyltrimethoxysilane,? -Glycidyloxypropyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 3- Capped propyl trimethoxysilane; Tridecafluoro-1,1,2,2-tetrahydrooctylpryethoxysilane, trifluoropropyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, heptadecafluorodecyltriisopropoxysilane, etc. Fluoroalkylsilane, and the like. These may be used alone or in combination of two or more.
Among them, an alkylalkoxysilane compound having an alkyl group of 1 to 20 carbon atoms is most preferable, and a tetraethoxysilane compound is more preferable.
The content of the alkoxysilane compound according to the present invention is not particularly limited, but may be 20 to 60 wt%, preferably 30 to 50 wt%, based on the total weight of the silane sol. When included in the above content range, a sol-gel reaction occurs well, the obtained silane sol has good physical properties and is excellent in adhesion and is easy to form a coating layer.
The acid catalyst according to the present invention promotes the hydrolysis of water and alkoxysilane and imparts a proper degree of crosslinking. The type is not particularly limited, and examples thereof include hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, acetic acid, diluted fluorine And hydrofluoric acid. These may be used alone or in combination of two or more. The acid catalyst used may be included in the form of an aqueous solution upon mixing.
The content of the acid catalyst according to the present invention is not particularly limited, but may be 0.01 to 10% by weight, preferably 0.05 to 5% by weight based on the total weight of the silane sol. When it is included in the above content range, a coating layer can be formed with a proper degree of crosslinking.
The kind of the alcohol-based solvent according to the present invention is not particularly limited, but a hydrophilic alcohol-based solvent is preferably used. Examples of the solvent include methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, amyl alcohol, tert-amyl alcohol, 1-ethyl-1-propanol, 2-methyl-1-butanol, n-hexanol or cyclohexanol, etc., These may be used alone or in combination of two or more. Of these, ethanol, n-butanol, n-propanol, n-pentanol and the like are preferable, and n-propanol is more preferable from the viewpoint of improvement of stability with the carbon nanotube dispersion.
The content of the alcoholic solvent according to the present invention is not particularly limited, but may be 10 to 70% by weight, preferably 20 to 50% by weight, based on the total weight of the silane sol. When included in the above content range, the reactivity of the sol-gel reaction can be further improved.
The water according to the present invention is a component which undergoes a hydrolysis reaction with alkoxysilane and the content thereof is not particularly limited and may be 5 to 60% by weight, preferably 8 to 35% by weight, . When it is included in the above content range, sufficient hydrolysis can be carried out and excellent adhesion to the substrate can be obtained.
The silane sol according to the present invention can be prepared by reacting the above-described components under predetermined conditions. The reaction conditions are not particularly limited. For example, the silane sol may include heating and stirring at 30 to 90 占 폚, The time is not particularly limited, and can be, for example, 4 to 30 hours. Also, the reactor may include a reflux condenser, and may include a step of concentrating the product by rotary evaporation after the reaction, and then diluting the product with a specific solvent.
The second coating layer
Graphene is a layered compound in which carbons are arranged like a honeycomb hexagonal net. The second coating layer containing graphene acts as a filter to prevent penetration of oxygen or moisture due to the structural characteristics of graphene. .
The graphene can be produced from graphite in which a plurality of layers are stacked. When each layer is exfoliated, it is possible to obtain a graphene sheet in the form of one or more layers.
In order to further improve the effect of reducing the moisture permeability according to the structural characteristics of the graphene described above, it is more preferable to use a thin film of graphene. In this respect, the thickness of the graphene may be 0.3 to 5 nm, May be between 0.5 and 2 nm. In the case of having the thickness in the above-mentioned range, it is judged that it is possible to uniformly disperse in the second coating layer in addition to the effect described above, thereby realizing the effect of lowering the moisture permeability uniformly.
And the second coating layer may be formed of a composition for forming a second coating layer comprising graphene and a dispersion medium.
The kind of the dispersion medium is not particularly limited, and examples thereof include water and an alcohol-based solvent, and water can be preferably used.
The composition for forming the second coating layer may further contain additives such as a dispersant and a surfactant, if necessary.
The encapsulant according to the present invention may be a structure in which a plurality of first coating layers and a plurality of second coating layers are repeatedly laminated as long as the first coating layer and the second coating layer are alternately laminated.
The encapsulant according to the present invention may have a remarkably low moisture permeability by being formed with the above-described structure and may be, for example, a water vapor transmission ratio (WVTR) of 10 -6 to 10 -4 g / m 2 / day , And has a moisture permeability within the above range, it is suitable for use in an OLED.
≪ Method of manufacturing organic light emitting display device >
The present invention relates to an organic light emitting diode (OLED) display, and by using an encapsulation material having the above-described structure, it is possible to minimize the inflow of oxygen or moisture, improve the luminous efficiency of the organic light emitting layer, .
Hereinafter, embodiments of the present invention will be described in detail.
First, an organic light emitting device is formed on a substrate (S1).
The substrate and the organic light emitting element can be used without any particular limitation as commonly used in the art.
The substrate can be appropriately selected depending on the requirements of the product to be applied. For example, a glass substrate can be used.
The organic light emitting device may include a cathode electrode, an organic light emitting layer, and an anode electrode. In addition, configurations applicable in the art may be used without any particular limitation.
Next, a step of laminating an encapsulating material on the organic light emitting device is performed (S2).
An encapsulant for an organic light emitting display device in which a first coating layer formed of a silane sol and a second coating layer containing graphene are alternately stacked is laminated on the organic light emitting device.
Here, the graphene used in the second coating layer is prepared by hydrothermal expansion of expandable graphite. In this case, it is possible to form graphene as a thin film, thereby reducing the moisture permeability according to the structural characteristics of graphene The effect can be further improved and at the same time the graphene can be uniformly dispersed in the second coating layer, thereby realizing a uniform effect in the coating layer.
Examples of the method for producing the graphene include at least one stripper selected from the group consisting of cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium dodecylbenzene sulfonate (SDBS), swellable Mixing expandable graphite and water; Heating the mixed liquid containing the expandable graphite to 400 to 500 ° C to obtain hydrothermal expanded graphite; And applying a shear force to the hydrothermally expanded graphite mixed solution obtained by mixing the hydrothermally expanded graphite with a dispersion medium and a dispersant.
More specifically, at least one exfoliating agent selected from the group consisting of expandable graphite, cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium dodecylbenzene sulfonate (SDBS) And water.
Water is a component for effectively expanding the expandable graphite. It dissolves the releasing agents CTAB, TBAOH, and SDBS to help them intercalate between the layers of the expandable graphite, and hydrothermal expansion at a suitable temperature range described later Thereby expanding the respective layers of the expandable graphite and stabilizing the expanded structure.
The content of water is not particularly limited, but may be, for example, 2000 to 6500 parts by weight, preferably 3200 to 5000 parts by weight, based on 100 parts by weight of expandable graphite. When it is included in the above range, it is judged that hydrothermal swellability is further improved within the temperature range described later.
Cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH), and sodium dodecylbenzene sulfonate (SDBS), when the expandable graphite of layered structure is hydrothermally expanded, the intercalation effect of each expanded layer continues So that the hydrothermally expanded graphite having remarkably improved expansion ratio can be produced.
The content of the releasing agent is not particularly limited, and may be, for example, 50 to 120 parts by weight, preferably 80 to 100 parts by weight, based on 100 parts by weight of the expandable graphite. When it is included in the above range, the intercalation phenomenon can be effectively caused, the expansion ratio can be remarkably improved, and the stability of the expanded structure can be improved.
Next, hydrothermally expanded graphite is obtained through hydrothermal expansion by heating the mixed liquid containing the expandable graphite to 400 to 500 ° C.
Hydrothermal expansion is a reaction for synthesizing or altering minerals in the presence of hot water. In the present invention, when heating a solution containing expandable graphite and the above-mentioned releasing agent in the above-mentioned temperature range, The solution containing the release agent penetrates and is gasified, expanding between the layer and the layer to produce hydrothermal expanded graphite.
When the heating temperature is lower than 400 ° C, the expansion ratio of each layer is not easily peeled in the step of applying a shearing force described later, so that it is difficult to produce the graphene of the thin film. When the heating temperature exceeds 500 ° C, And the process proceeds to an excessively high temperature process, which is costly and the process efficiency is lowered
The thermal expansion for obtaining the hydrothermally expanded graphite may be performed by rapidly heating the mixed liquid containing the expandable graphite to 400 to 500 ° C or by heating to 400 to 500 ° C at a proper rate, Various methods can be applied without any particular limitations as long as they are within the allowable range.
For example, the mixed liquid containing the expandable graphite may be heated at a rate of 5 to 20 ° C / min to 400 to 500 ° C, preferably 10 to 15 ° C / min. When heated in the temperature raising rate range, the exfoliating agent and water effectively penetrate into each layer, and the expansion ratio can be further improved.
After the temperature is reached at 400 to 500 ° C., the heating time is not particularly limited, but can be, for example, 30 to 90 minutes, preferably 50 to 70 minutes. It is judged that the expansion rate is remarkably increased within the temperature and time range.
The properties of hydrothermally expanded graphite produced through the heating step are not particularly limited, but may have an apparent density of 0.01 to 0.1 g / mm 3 , and preferably 0.02 to 0.05 g / mm 3 . When the above-mentioned range is satisfied, it is judged that each layer can be effectively peeled off in a step of applying a shearing force described later, whereby a thin film of graphene can be produced.
Finally, the graphene of the thin film is prepared by applying a shear force to the hydrothermally expanded graphite mixed with hydrothermal expanded graphite, dispersion medium and dispersant.
The hydrothermally expanded graphite produced is in a state in which each layer is in an expanded state and the interlayer coupling force is weakened. Therefore, when a physical shearing force is applied, each layer is peeled off due to a slip phenomenon between the respective layers to produce graphene.
The step of applying the shearing force may be performed without any particular limitations as long as it is a commonly used method in the art, and may be performed, for example, by dispersing with a high pressure disperser or a bead mill. In this case, the shearing force can be effectively applied to the hydrothermally expanded graphite by the dispersion.
In order to improve the peeling efficiency in the step of applying the shearing force, a dispersant and a dispersant are included, and further used dispersing agent includes cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium At least one compound selected from the group consisting of dodecylbenzene sulfonate (SDBS) can be used.
The kind of the dispersion medium is not particularly limited, but at least one compound selected from the group consisting of water, an alcohol solvent, dimethylsulfoxide (DMSO) and dimethylformamide (DMF) may be used.
In the step of applying the shear force to the hydrothermally expanded graphite mixture liquid, when the high pressure disperser is used, the pressure is not particularly limited, but may be, for example, 700 to 2000 bar, preferably 1000 to 1500 bar, The shearing force is sufficient, so that it is possible to effectively peel off the interlayer.
When the high-pressure disperser is used, the size of the nozzle is not particularly limited. For example, the size of the nozzle may be 50 to 300 μm, preferably 100 to 200 μm. . ≪ / RTI >
In the step of applying the shear force to the hydrothermally expanded graphite mixed solution, when the bead mill is dispersed, the size of the beads used in the above step is not particularly limited, but may be, for example, 0.05 to 0.3 mm , In which case it is judged to be more effective for the production of the thin film graphene.
When the bead mill is used, the dispersion speed is not particularly limited, but may be, for example, 1800 to 2800 rpm, preferably 2200 to 2500 rpm. When the bead mill is rotated in the above range, The frictional force is effectively applied to the expanded graphite, so that each layer can be effectively separated.
The components for the laminating step of the encapsulant according to the present invention are not limited to the graphene produced by the above method, but the composition for forming the first coating layer and the composition for forming the second coating layer, which are used for the first coating layer and the second coating layer, Lt; / RTI >
As an example of the step (S2) of laminating the sealing material according to the present invention, a first coating layer is formed with a composition for forming a first coating layer containing an alkylsilane compound; And forming a second coating layer using a composition for forming a second coating layer including graphene, which are repeated at least once, and then stacked on the organic light emitting device.
Here, the first coating layer or the second coating layer may be applied to the upper surface of the organic light emitting device, that is, the order of stacking is not particularly limited as long as they are intersected.
Even in this case, the components used may be the same as those used in the above-described components.
Another example of the step (S2) of laminating the sealing material according to the present invention is a method for manufacturing a sealing material comprising the steps of forming a first coating layer with a composition for forming a first coating layer containing an alkylsilane compound on a base film, The step of forming the second coating layer with the composition for forming the second coating layer may be repeated at least once or more to form the sealing material and bonding the sealing material to the organic light emitting element.
Here, the first coating layer or the second coating layer may be applied to the upper surface of the base film, that is, the order of lamination is not particularly limited as long as they are intersected.
A method of bonding the encapsulant to the organic light emitting device is not particularly limited, but may be, for example, an adhesive bonding.
Also in this case, the components used may be the same as those used in the above-described components.
<Organic light-emitting display device>
The present invention relates to an organic light emitting diode (OLED) display device having the above-described encapsulation material. The OLED display device according to the present invention can be manufactured according to the method of the present invention, and effectively prevents the inflow of oxygen and moisture. Is significantly lower.
The organic light emitting diode display according to the present invention may further include a configuration used in the art within the scope of the present invention.
Claims (17)
Laminating an encapsulant for an organic light emitting display device in which a first coating layer formed of a silane sol and a second coating layer containing graphene are alternately stacked on the organic light emitting device,
Wherein the graphene is produced by hydrothermal expansion of expandable graphite.
Heating the mixed liquid containing the expandable graphite to 400 to 500 ° C to obtain hydrothermal expanded graphite; And
Applying a shear force to the hydrothermally expanded graphite mixed solution obtained by mixing the dispersion medium and the dispersant in the hydrothermally expanded graphite.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060113884A (en) | 2003-08-05 | 2006-11-03 | 테크니체 우니베르시테트 브라운츠바이그 차롤오-빌헬미나 | Use of a layer consisting of hydrophobic, linear or two-dimensional polycyclic aromatics as a barrier layer or an encapsulation and electric components constructed with a layer of this type and comprising organic polymers |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060113884A (en) | 2003-08-05 | 2006-11-03 | 테크니체 우니베르시테트 브라운츠바이그 차롤오-빌헬미나 | Use of a layer consisting of hydrophobic, linear or two-dimensional polycyclic aromatics as a barrier layer or an encapsulation and electric components constructed with a layer of this type and comprising organic polymers |
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