WO2011052503A1 - 有機el素子の製造方法 - Google Patents
有機el素子の製造方法 Download PDFInfo
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- WO2011052503A1 WO2011052503A1 PCT/JP2010/068700 JP2010068700W WO2011052503A1 WO 2011052503 A1 WO2011052503 A1 WO 2011052503A1 JP 2010068700 W JP2010068700 W JP 2010068700W WO 2011052503 A1 WO2011052503 A1 WO 2011052503A1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
Definitions
- the present invention relates to a method for manufacturing an organic EL element, an illumination device, and a planar light source.
- the organic EL element is a kind of light-emitting element, and includes a pair of electrodes and one or more organic layers disposed between the electrodes. As the one or more organic layers, one or more light emitting layers that emit light are provided. “EL” is an abbreviation for “Electro Luminescence”.
- An organic EL element is formed by laminating layers such as electrodes and organic layers in a predetermined order.
- a method for forming the organic layer use of a coating method with a simple process has been studied.
- a coating liquid containing a material that becomes an organic layer is applied and formed on a surface on which the organic layer is to be formed, and the coating liquid is solidified. Thereby, an organic layer is formed.
- a coating liquid can be performed using, for example, a nozzle having a slit-like discharge port for discharging the coating liquid.
- a belt-shaped coating film can be formed by scanning the nozzle or the object to be coated while the coating liquid discharged from the nozzle is in contact with the surface to be formed.
- a strip-like coating film is formed on the surface to be formed.
- a plurality of strip-shaped coating films can also be formed.
- a plurality of strip-shaped coating films are formed by using a nozzle in which one or more partitions are provided in one slit-shaped discharge port.
- each organic EL element is formed at a predetermined interval not only in the longitudinal direction of the slit-like discharge port but also in its short direction (application direction).
- the coating liquid is applied to unnecessary portions between organic EL elements adjacent in the coating direction, so the coating film applied to unnecessary portions is removed. Therefore, there is a problem that the number of steps increases.
- an object of the present invention is to provide a method for producing an organic EL element, which is capable of producing an organic EL element by a simple process by applying a coating liquid having an intended width to form an organic layer.
- the present invention has a pair of electrodes and one or more organic layers disposed between the electrodes, and the organic EL element manufacturing method is provided with one or more light emitting layers as the one or more organic layers. It is.
- This manufacturing method includes a step of forming one electrode of the pair of electrodes, a step of forming one or a plurality of organic layers, and a step of forming the other electrode of the pair of electrodes.
- a coating liquid that includes a material to be an organic layer, in which an object to be an organic EL element is disposed with a surface on which the organic layer is formed facing downward.
- a nozzle having a plurality of slit-like discharge ports for discharging the nozzle upward and a notch portion recessed downwardly formed at each end portion of the slit-like discharge port is disposed below the substrate. Then, while maintaining the state in which the coating liquid discharged from the nozzle is in contact with the body to be coated, a coating process for relatively moving the nozzle and the body to be coated in a predetermined coating direction; The coating liquid is applied to the surface to be formed by alternately repeating a non-coating step in which the nozzle and the body to be coated are relatively moved in the coating direction while maintaining a state where the liquid is separated from the body to be coated.
- the organic layer is formed by forming a film and solidifying the applied coating solution.
- the nozzle has a pair of nozzle main bodies disposed opposite to each other with a width in the short direction of the slit-shaped discharge port, and a thickness of the width in the short direction of the slit-shaped discharge port.
- a shim that is sandwiched between the nozzle bodies and is provided in an area excluding the slit-like discharge ports, and that defines a width in the longitudinal direction of the slit-like discharge ports, and an outer edge of the pair of nozzle bodies at the notch You may make it arrange
- the notch may be formed to be inclined from the upper end to the lower end so as to be separated from the slit-like discharge port.
- the present invention also relates to a lighting device including the organic electroluminescence element manufactured by the manufacturing method.
- the present invention also relates to a planar light source including an organic electroluminescence element manufactured by the manufacturing method.
- an organic EL element can be produced by a simple process by applying a pattern with an intended width of a coating solution to be an organic layer.
- FIG. 4 is a side view of the nozzle 13.
- FIG. 4 is a top view of the nozzle 13.
- FIG. 4 is a cross-sectional view taken along a section line IV-IV in FIG. 2.
- FIG. 5 is a cross-sectional view taken along the section line VV in FIG. 2.
- 3 is a side view of a shim 21.
- FIG. It is a top view of the to-be-coated body used as an organic EL element. It is a figure which shows the condition of the board
- the method for producing an organic EL element of the present invention is a method for producing an organic EL element having a pair of electrodes and one or more organic layers disposed between the electrodes.
- the organic EL element is provided with one or more light emitting layers as the one or more organic layers.
- the organic EL device manufacturing method of the present invention includes a step of forming one electrode of a pair of electrodes, a step of forming one or a plurality of organic layers, and the other electrode of the pair of electrodes. Process.
- the organic EL element is usually formed on a support substrate 1 made of glass or resin, and is formed by laminating electrodes and organic layers constituting the organic EL element on the support substrate 1 in a predetermined order.
- a plurality of organic EL elements are formed in a matrix on the support substrate 1 (see FIG. 7). That is, a plurality of organic EL elements are formed on the support substrate 1 with a predetermined interval in the arrangement direction Y and with a predetermined interval in the coating direction X perpendicular to the arrangement direction Y.
- An organic EL element in which a cathode corresponding to the other of the electrodes is stacked in this order from the support substrate 1 side will be described.
- a plurality of anodes are formed in a matrix on the support substrate 1 by a predetermined method described later. That is, on the support substrate 1, a plurality of anodes are formed at a predetermined interval in the arrangement direction Y and at a predetermined interval in the coating direction X.
- Each anode has a flat plate shape, and is formed in, for example, a substantially rectangular shape in plan view.
- a hole injection layer is formed on each anode.
- the hole injection layer is formed, for example, so that its outer edge substantially coincides with the outer edge of each anode in plan view.
- the hole injection layer may be patterned only on the anode by a method using a predetermined nozzle, as in the method of forming the light emitting layer described later. preferable.
- a light emitting layer provided as one of one or more organic layers is formed on the hole injection layer.
- the step of forming the light emitting layer corresponds to the step of forming one or a plurality of organic layers. Therefore, the step of forming one or a plurality of organic layers will be described through the description of the step of forming the light emitting layer.
- the substrate on which the anode and the hole injection layer are formed on the support substrate 1 corresponds to a coated body to be an organic EL element, and the surface of the hole injection layer is formed on the organic layer. This corresponds to surface 2 (the hatched region in FIG. 7).
- the light emitting layer is formed by the step of forming one or a plurality of organic layers.
- the pattern may be formed by a coating method using a predetermined nozzle, and all the organic layers of the plurality of organic layers are formed in the same manner as the method of forming the light emitting layer described later. More preferably, the pattern is formed by a coating method using a predetermined nozzle.
- an object to be coated which becomes an organic EL element, is arranged with the surface on which the organic layer is formed facing downward, and a coating liquid containing a material that becomes the organic layer is discharged upward.
- a nozzle having a plurality of slit-like discharge ports and a notch that is recessed downwardly formed at both ends of the slit-like discharge port is disposed below the object to be coated.
- the coating liquid is applied to the surface to be formed by alternately repeating a non-coating step in which the nozzle and the body to be coated are relatively moved in the coating direction while maintaining a state where the liquid is separated from the body to be coated.
- the organic layer is formed by forming a film and solidifying the applied coating solution.
- the state in which the coating liquid is in contact with the object to be coated means a state in which the coating liquid is attached to the body to be coated.
- a method of discharging the coating liquid upward from the nozzle there are a method using capillary force and / or static pressure, a method using pump power, and the like.
- a cap coat method in which a coating solution is applied by discharging the coating solution upward using capillary force and static pressure will be described.
- FIG. 1 is a diagram schematically showing a cap coater system 11 used for forming a light emitting layer.
- “upper” means “upward in the vertical direction”
- “lower” means “lower in the vertical direction”.
- the configuration and the structure of the nozzle 13 and the like will be described on the premise of the arrangement when applying the coating liquid.
- the cap coater system 11 mainly includes a surface plate 12, a nozzle 13, and a tank 14.
- the coated body 19 is held on the lower surface of the surface plate 12.
- the coated body 19 is held on the surface plate 12 with the surface to be formed (the surface of the hole injection layer in the present embodiment) on which the organic layer (the light emitting layer in the present embodiment) is formed facing downward.
- the surface plate 12 holds the object 19 by vacuum suction, for example.
- the surface plate 12 reciprocates in the horizontal direction by displacement driving means such as an electric motor and a hydraulic machine (not shown).
- the moving direction of the surface plate 12 corresponds to the application direction X, and the direction perpendicular to the vertical direction Z and the application direction X corresponds to the arrangement direction Y.
- the nozzle 13 includes a plurality of slit-like discharge ports for discharging a coating liquid containing a material that becomes an organic layer upward, and notched portions 25 that are recessed downwardly formed at both ends of the slit-like discharge port. It is arranged below the application body 19.
- four slit-shaped ejection openings are arranged at predetermined intervals in the arrangement direction Y. 2 is a side view of the nozzle 13
- FIG. 3 is a top view of the nozzle 13
- FIG. 4 is a cross-sectional view taken along the section line IV-IV in FIG. 2
- FIG. 5 is a sectional view taken along line VV.
- FIG. 6 is a side view of the shim 21.
- the nozzle 13 preferably includes a pair of nozzle bodies 22 and a shim 21 sandwiched between the nozzle bodies 22 as shown in FIGS.
- the pair of nozzle bodies 22 are disposed to face each other with a width in the short direction of the slit-like discharge port 23.
- the shim 21 has a width in the short direction of the slit-like discharge port 23, is provided in an area excluding the slit-like discharge port sandwiched by the nozzle body, and has a longitudinal width of the slit-like discharge port. Stipulate.
- the distance between the pair of nozzle bodies 22 is defined by the thickness of the shim 21 to be sandwiched. That is, the shim 21 functions as a spacer. Since the width in the short direction (corresponding to the coating direction X in the present embodiment) of the slit-like discharge port 23 is defined by the distance between the pair of nozzle bodies 22, the distance between the pair of nozzle bodies 22 is defined. The thickness of the shim 21 is defined. The width in the short direction of the slit-like discharge port 23 is appropriately set according to the properties of the coating liquid and the thickness of the coating film, and can be adjusted by changing the thickness of the shim 21.
- the width of the slit-like discharge port 23 in the short direction is usually about 0.01 mm to 1 mm, preferably 50 ⁇ m to 500 ⁇ m, and more preferably 50 ⁇ m to 200 ⁇ m.
- the pair of nozzle main bodies 22 are respectively formed with columnar cavities extending in the arrangement direction Y and having a semicircular bottom surface. When the two are bonded together, a cylindrical cavity extending in the arrangement direction Y is formed. Has been. When the pair of nozzle main bodies 22 are bonded together with the shim 21 interposed therebetween, the semi-cylindrical cavities formed in the nozzle main bodies 22 function as the manifold 24.
- the plurality of slit-like discharge ports 23 have their longitudinal directions aligned with the arrangement direction Y (direction perpendicular to the coating direction X and the vertical direction Z), and each of the slit-like discharge ports 23 is arranged in the arrangement direction Y. Arranged at predetermined intervals.
- Each slit-like discharge port 23 is formed in the vertical direction Z from the upper end of the nozzle 13 to the manifold 24 and communicates with the manifold 24. Since the manifold 24 is filled with the coating solution, the coating solution is supplied from the manifold 24 to the slit-like discharge ports 23 by capillary force.
- the width in the longitudinal direction (arrangement direction Y) of the slit-like discharge ports 23 is set to the width in the arrangement direction Y of the coating film, and is, for example, 10 mm to 300 mm.
- the width in the short direction of the slit-like discharge port 23 is defined by the thickness of the shim 21, but in this embodiment, not only the width in the short direction (the application direction X) of the slit-like discharge port 23,
- the width in the longitudinal direction (array direction Y) is also defined by the shim 21.
- the shim 21 of the present embodiment is provided in a region excluding the slit-like discharge ports, and the plate body 21a extending in the arrangement direction Y and the width of the slit-like discharge port 23 in the arrangement direction Y are opened to each other to form a plate body And a plurality of plate-like non-liquid passage portions 21b extending upward from 21a (see FIG. 6).
- the plate body 21a is disposed below the manifold 24 so as to extend in the arrangement direction Y, and the non-liquid passage portion 21b is provided in an area excluding an area where the slit-like discharge port 23 is provided (liquid passage area).
- the plate body 21a and the non-liquid passage portion 21b are integrally formed.
- the “region where the slit-like discharge port 23 is provided” may be referred to as a liquid passing region. In the region where the non-liquid passage portion 21b is provided, the upward movement of the coating liquid from the manifold 24 is hindered by the non-liquid passage portion 21b, so that the coating liquid is not discharged.
- a space (slit-like discharge port 23) communicating with the manifold 24 is formed in a region (liquid passage region) sandwiched between the plurality of non-liquid passage portions 21b, so that the coating liquid filled in the manifold 24 is filled with the coating liquid.
- the ink is discharged upward through the slit-like discharge port 23.
- the coating liquid is selectively discharged from the respective slit-like discharge ports 23 provided at predetermined intervals in the arrangement direction Y.
- the shim 21 having the non-liquid-permeable portion 21b By using the shim 21 having the non-liquid-permeable portion 21b, the shim 21 that is normally used to define the width in the short direction of the slit-like discharge port 23 is changed to the width in the longitudinal direction of the slit-like discharge port 23. Since it can also be used as a defining member, there is no need to separately provide a member for defining the width in the longitudinal direction of the slit-like discharge port 23, and the apparatus configuration is simplified. In order to define the width in the longitudinal direction of the slit-shaped discharge port 23, a predetermined member may be disposed so that the coating liquid is not discharged from other than the slit-shaped discharge port 23. As another embodiment, You may use things other than a shim for a simple member.
- the width in the short direction of the slit-like discharge port 23 can be easily adjusted by replacing the shim 21, it is preferable to configure the nozzle 13 using the shim 21, but the shim 21 is not used.
- a nozzle in which a non-liquid-permeable portion is integrally formed may be used.
- the nozzle 13 has a notch 25 that is recessed downward and formed at both ends of the slit-like discharge port 23.
- the partition is formed flush with the tip of the slit-like discharge port.
- the coating liquid discharged from the slit-shaped discharge port and in contact with the surface to be formed spreads in the longitudinal direction of the slit-shaped discharge port through the tip end surface of the partition
- the width of the coating film tends to be wider than the width in the longitudinal direction of the slit-like discharge port.
- the coating liquid discharged from the slit-like discharge port and in contact with the surface to be formed may not spread in the direction in which the notch is recessed.
- the outer edge of the pair of nozzle bodies and the outer edge of the shim are substantially flush with each other in the notch. That is, it is preferable that the outer edge of the shim is formed along the outer edges of the pair of nozzle bodies in the notch.
- the outer edge of the shim that inclines downward from both ends of the slit-like discharge port and the outer edges of the pair of nozzle bodies overlap each other in the notch portion when viewed from one side in the application direction X.
- the nozzle is configured.
- the width of the coating film may be wider than the intended width, but the outer edges of the pair of nozzle bodies and the outer edge of the shim as shown in FIG.
- the notch is formed so as to be inclined from the slit-shaped discharge port from the upper end to the lower end.
- the nozzle 13 is supported so as to be displaceable in the vertical direction Z, and is driven to be displaced in the vertical direction Z by displacement driving means such as an electric motor and a hydraulic machine.
- the coating liquid 17 applied to the coated body 19 is stored in the tank 14.
- the coating liquid 17 is a liquid containing an organic material that becomes a light emitting layer.
- the coating liquid 17 is a solution in which a light emitting material described later is dissolved in a solvent.
- the manifold 24 of the nozzle 13 and the tank 14 communicate with each other via a coating liquid supply pipe 16.
- the coating liquid 17 accommodated in the tank 14 is supplied to the manifold 24 through the coating liquid supply pipe 16 and is further applied to the coated body 19 through the slit-like discharge port 23.
- the tank 14 is supported so as to be displaceable in the vertical direction Z, and is driven to be displaced in the vertical direction Z by displacement driving means such as an electric motor and a hydraulic machine.
- the tank 14 further includes a liquid level sensor 18 that detects the liquid level of the coating liquid 17.
- the position of the coating liquid 17 is detected by a liquid level sensor 18.
- the liquid level sensor 18 is realized by an optical sensor or an ultrasonic vibration sensor, for
- the coating liquid 17 supplied from the tank 14 to the slit-like discharge port 23 via the coating liquid supply pipe 16 is a pressure (static pressure) generated according to the height of the liquid level in the tank 14 and the slit-like discharge port 23. Is extruded from the slit-like discharge port 23 in accordance with the force generated by the capillary action.
- the discharge amount of the coating liquid 17 extruded from the slit-like discharge port 23 is the vertical position of the tank 14 in order to control the relative difference between the liquid level position in the tank 14 and the liquid level position in the nozzle 13. It can adjust by controlling. Since the manifold 24 communicates with all the slit-like discharge ports 23, the liquid level of the coating liquid at all the slit-like discharge ports 23 can be controlled simultaneously by controlling the liquid level in the tank 14.
- the cap coater system 11 further includes a control unit realized by a microcomputer or the like.
- This control unit controls the displacement driving means described above.
- the control unit controls the displacement driving means the position of the nozzle 13 and the tank 14 in the vertical direction Z and the displacement of the surface plate 12 in the application direction X are controlled.
- the control unit controls the displacement driving means based on the detection result of the liquid level sensor 18. Then, by adjusting the position of the tank 14 in the vertical direction Z, the height of the coating liquid 17 extruded from the slit-like discharge port 23 can be controlled.
- the coating liquid is applied in a pattern to a rectangular region arranged in a matrix (5 rows ⁇ 4 columns) as shown in FIG. can do.
- the cap coater system 11 applies the coating liquid in a pattern by repeating the following coating process and non-coating process.
- the nozzle 13 and the coated body 19 are relatively moved in a predetermined coating direction while maintaining the state in which the coating liquid discharged from the nozzle 13 is in contact with the coated body 19.
- the tank 14 is raised so that the liquid level of the coating liquid in the tank 14 is higher than the upper end of the nozzle 13, so that the coating liquid is discharged from the slit-shaped discharge port 23 and discharged from the slit-shaped discharge port 23.
- the nozzle 13 is raised so that the coating liquid comes into contact with the substrate 19.
- the distance between the coated body 19 and the nozzle 13 is appropriately set according to the properties of the coating liquid and the thickness of the coating film.
- the distance between the coated body 19 and the nozzle 13 is set to, for example, about 0.05 mm to 0.3 mm, and preferably about 0.2 mm to 0.3 mm.
- the substrate 19 is moved to one side in the coating direction X (right side in FIG. 1).
- the movement of the object 19 is stopped.
- four strip-shaped coating films are formed.
- a coating film having a coating film thickness of about 5 ⁇ m to 500 ⁇ m can be formed.
- the coated body 19 is moved when the coating liquid is applied, but the nozzle 13 may be moved to the other side of the coating direction X (leftward in FIG. 1). Both of the bodies 19 may be moved.
- Non-coating process In the non-application process, the nozzle and the object to be applied are relatively moved in the application direction while maintaining the state where the application liquid is separated from the object to be applied.
- both the nozzle 13 and the tank 14 are lowered so that the coating liquid is separated from the coated body.
- the coating liquid was discharged from the slit-like discharge port 23.
- the coating liquid in the tank 14 was discharged.
- the coated body 19 is moved by a predetermined distance in one of the coating directions X (rightward in FIG. 1). At this time, since the coating liquid is separated from the body 19 to be coated, the coating liquid is not applied to the body 19 to be coated.
- the coating liquid can be applied to both the coating direction X and the arrangement direction Y.
- the two-dimensional pattern application of the coating liquid is performed. It can be performed.
- the coating liquid can be applied with an intended coating width.
- the coating solution contains a material to be a layer to be formed (an organic material to be a light emitting layer in this embodiment) and a solvent.
- a solvent for the coating solution a solvent having a predetermined boiling point may be used alone, or a plurality of types of solvents may be used in combination.
- a material that dissolves a material to be a layer to be formed is preferable, and examples of the solvent include the following.
- Chloroform (boiling point 61 ° C.), methylene chloride (boiling point 40 ° C.), 1,1-dichloroethane (boiling point 57 ° C.), 1,2-dichloroethane (boiling point 83 ° C.), 1,1,1-trichloroethane (boiling point 74 ° C.), Aliphatic chlorinated solvents such as 1,1,2-trichloroethane (boiling point 113 ° C), chlorobenzene (boiling point 132 ° C), o-dichlorobenzene (boiling point 180 ° C), m-dichlorobenzene (boiling point 173 ° C), p-di Aromatic chlorine solvents such as chlorobenzene (boiling point 174 ° C), aliphatic ether solvents such as tetrahydrofuran (boiling point 66 ° C),
- Aromatic hydrocarbon solvents cyclohexane (boiling point 81 ° C), methylcyclohexane (boiling point 101 ° C), n-pentane (boiling point 36 ° C), n-hexane (boiling point 69 ° C), n-heptane (boiling point 98 ° C) N-octane (boiling point 126 ° C.), n-nonane (boiling point 151 ° C.), n-decane (boiling point 174 ), Decalin (cis body has a boiling point of 196 ° C., trans body has a boiling point of 187 ° C.), aliphatic hydrocarbon solvents such as bicyclohexyl (boiling point of 217 to 233 ° C.), acetone (boiling point of 56 ° C.), methyl ethyl ketone (bo
- the coating liquid preferably contains a solvent having a boiling point of less than 170 ° C. in an amount of 50% by weight or more based on the coating liquid.
- the concentration of the material to be a layer to be formed is appropriately set depending on the viscosity and solubility of the coating solution, and is usually 10% by weight or less, preferably 0.001% by weight to 5% by weight or less. More preferably, the content is 0.01% by weight to 2% by weight or less.
- the light emitting layer can be patterned by solidifying the coating film formed by coating as described above.
- the coating film can be solidified by removing the solvent.
- the solvent can be removed by heat drying or vacuum drying.
- the coating film may be solidified by applying light or heat after the coating film is formed. it can.
- an organic EL element can be formed by forming a cathode on the light emitting layer.
- the organic EL element having a configuration in which the anode, the hole injection layer, the light emitting layer, and the cathode are stacked in this order from the support substrate 1 side has been described above, but the organic EL element is not limited to this configuration.
- the layer structure of an organic EL element, the structure of each layer, and an example of the formation method of each layer are demonstrated.
- the organic EL element includes a pair of electrodes (anode and cathode) and one or more organic layers disposed between the electrodes, and one or more light-emitting layers are provided as the one or more organic layers. Provided. Between the anode and the cathode, not only the light emitting layer but also an organic layer different from the light emitting layer may be provided, and further an inorganic layer may be provided. Hereinafter, a layer provided between the anode and the cathode will be described. Of these, a layer containing an organic substance corresponds to an organic layer.
- the organic layer that can be formed using a coating method among a plurality of types of organic layers is preferably formed by patterning by the coating method using the predetermined nozzle described above as a method for forming the light emitting layer.
- the organic substance constituting the organic layer may be a low molecular compound or a high molecular compound, or a mixture of a low molecular compound and a high molecular compound, but the high molecular compound is generally more soluble in a solvent.
- a polymer compound is preferable because it is good, and a polymer compound having a polystyrene-equivalent number average molecular weight of 10 3 to 10 8 is preferable.
- Examples of the layer provided between the cathode and the light emitting layer include an electron injection layer, an electron transport layer, and a hole blocking layer.
- the layer close to the cathode is called an electron injection layer
- the layer close to the light emitting layer is called an electron transport layer.
- Examples of the layer provided between the anode and the light emitting layer include a hole injection layer, a hole transport layer, and an electron block layer.
- a layer close to the anode is referred to as a hole injection layer
- a layer close to the light emitting layer is referred to as a hole transport layer.
- anode / light emitting layer / cathode b) anode / hole injection layer / light emitting layer / cathode c) anode / hole injection layer / light emitting layer / electron injection layer / cathode d) anode / hole injection layer / light emitting layer / Electron transport layer / cathode e) anode / hole injection layer / light emitting layer / electron transport layer / electron injection layer / cathode f) anode / hole transport layer / light emitting layer / cathode g) anode / hole transport layer / light emitting layer / Electron injection layer / cathode h) anode / hole transport layer / light emitting layer / electron transport layer / cathode i) anode / hole transport layer / light emitting layer / electron transport layer / electron injection layer / electron injection layer
- the organic EL element may be further covered with a sealing member such as a sealing film or a sealing plate for sealing.
- a sealing member such as a sealing film or a sealing plate for sealing.
- an insulating layer having a thickness of 2 nm or less may be provided adjacent to the electrode in order to further improve the adhesion with the electrode or improve the charge injection property from the electrode.
- a thin buffer layer may be inserted between each of the aforementioned layers in order to improve adhesion at the interface or prevent mixing.
- the order of the layers to be laminated, the number of layers, and the thickness of each layer can be appropriately set in consideration of light emission efficiency and element lifetime.
- a glass, plastic, and silicon substrate, and a laminate of these are used.
- a substrate on which an electric circuit is formed in advance may be used as a substrate for forming the organic EL element thereon.
- a transparent or translucent electrode is used for the anode.
- the transparent electrode or translucent electrode thin films of metal oxides, metal sulfides, metals, and the like having high electrical conductivity can be used, and those having high light transmittance are preferably used.
- a thin film made of indium oxide, zinc oxide, tin oxide, ITO, indium zinc oxide (Indium Zinc Oxide: abbreviation IZO), gold, platinum, silver, copper, or the like is used.
- ITO, IZO Alternatively, a thin film made of tin oxide is preferably used.
- Examples of a method for producing the anode include a vacuum deposition method, a sputtering method, an ion plating method, and a plating method. Further, an organic transparent conductive film such as polyaniline or a derivative thereof, polythiophene or a derivative thereof may be used as the anode.
- a material that reflects light may be used for the anode, and the material is preferably a metal, metal oxide, or metal sulfide having a work function of 3.0 eV or more.
- the film thickness of the anode can be appropriately selected in consideration of light transmittance and electric conductivity, and is, for example, 10 nm to 10 ⁇ m, preferably 20 nm to 1 ⁇ m, and more preferably 50 nm to 500 nm. .
- ⁇ Hole injection layer As the hole injection material constituting the hole injection layer, oxides such as vanadium oxide, molybdenum oxide, ruthenium oxide, and aluminum oxide, phenylamine type, starburst type amine type, phthalocyanine type, amorphous carbon, polyaniline, And polythiophene derivatives.
- oxides such as vanadium oxide, molybdenum oxide, ruthenium oxide, and aluminum oxide, phenylamine type, starburst type amine type, phthalocyanine type, amorphous carbon, polyaniline, And polythiophene derivatives.
- Examples of the method for forming the hole injection layer include film formation from a solution containing a hole injection material.
- the solvent used for film formation from a solution is not particularly limited as long as it can dissolve the hole injection material.
- the solvent exemplified when forming the light emitting layer, water, or the like is used. Can do.
- a film forming method from a solution As a film forming method from a solution, a spin coating method, a casting method, a micro gravure coating method, a gravure coating method, a bar coating method, a roll coating method, a wire bar coating method, a dip coating method, a spray coating method, a screen printing method
- the coating method include a flexographic printing method, an offset printing method, and an ink jet printing method
- the hole injection layer is preferably formed by a coating method using the predetermined nozzle described above as a method for forming a light emitting layer.
- the thickness of the hole injection layer is appropriately set in consideration of the electrical characteristics and the ease of film formation, and is, for example, 1 nm to 1 ⁇ m, preferably 2 nm to 500 nm, more preferably 5 nm to 200 nm. is there.
- ⁇ Hole transport layer> As the hole transport material constituting the hole transport layer, polyvinylcarbazole or a derivative thereof, polysilane or a derivative thereof, a polysiloxane derivative having an aromatic amine in a side chain or a main chain, a pyrazoline derivative, an arylamine derivative, a stilbene derivative, Triphenyldiamine derivative, polyaniline or derivative thereof, polythiophene or derivative thereof, polyarylamine or derivative thereof, polypyrrole or derivative thereof, poly (p-phenylene vinylene) or derivative thereof, or poly (2,5-thienylene vinylene) or Examples thereof include derivatives thereof.
- hole transport materials include polyvinyl carbazole or derivatives thereof, polysilane or derivatives thereof, polysiloxane derivatives having aromatic amine compound groups in the side chain or main chain, polyaniline or derivatives thereof, polythiophene or derivatives thereof, poly Preferred is a polymeric hole transport material such as arylamine or a derivative thereof, poly (p-phenylene vinylene) or a derivative thereof, or poly (2,5-thienylene vinylene) or a derivative thereof, more preferably polyvinyl carbazole or a derivative thereof. , Polysilane or a derivative thereof, and a polysiloxane derivative having an aromatic amine in the side chain or main chain. In the case of a low-molecular hole transport material, it is preferably used by being dispersed in a polymer binder.
- the method for forming the hole transport layer is not particularly limited, but in the case of a low molecular hole transport material, film formation from a mixed solution containing a polymer binder and a hole transport material can be exemplified.
- molecular hole transport materials include film formation from a solution containing a hole transport material.
- the solvent used for film formation from a solution is not particularly limited as long as it can dissolve a hole transport material.
- those exemplified as the solvent used in forming a light emitting layer can be used.
- the same coating method as the above-described film formation method of the injection layer in the hole can be mentioned, and the hole transport layer has the predetermined nozzle described above as a method of forming the light emitting layer. It is preferable to form by the coating method used.
- polystyrene examples include vinyl chloride and polysiloxane.
- the film thickness of the hole transport layer is appropriately set in consideration of the electrical characteristics and the ease of film formation, and is, for example, 1 nm to 1 ⁇ m, preferably 2 nm to 500 nm, more preferably 5 nm to 200 nm. It is.
- the light emitting layer is usually formed of an organic substance that mainly emits fluorescence and / or phosphorescence, or this organic substance and a dopant that assists the organic substance.
- the dopant is added, for example, in order to improve the luminous efficiency and change the emission wavelength.
- the organic substance may be a low molecular compound or a high molecular compound, and the light emitting layer preferably contains a high molecular compound having a polystyrene-equivalent number average molecular weight of 10 3 to 10 8 .
- Examples of the light emitting material constituting the light emitting layer include the following dye materials, metal complex materials, polymer materials, and dopant materials.
- dye-based materials include cyclopentamine derivatives, tetraphenylbutadiene derivative compounds, triphenylamine derivatives, oxadiazole derivatives, pyrazoloquinoline derivatives, distyrylbenzene derivatives, distyrylarylene derivatives, pyrrole derivatives, thiophene ring compounds. Pyridine ring compounds, perinone derivatives, perylene derivatives, oligothiophene derivatives, oxadiazole dimers, pyrazoline dimers, quinacridone derivatives, coumarin derivatives, and the like.
- Metal complex materials examples include rare earth metals such as Tb, Eu, and Dy, or Al, Zn, Be, Ir, Pt, etc. as a central metal, and oxadiazole, thiadiazole, phenylpyridine, phenylbenzimidazole, quinoline.
- Examples include metal complexes having a structure as a ligand, for example, iridium complexes, platinum complexes and other metal complexes having light emission from a triplet excited state, aluminum quinolinol complexes, benzoquinolinol beryllium complexes, benzoxazolyl zinc A complex, a benzothiazole zinc complex, an azomethylzinc complex, a porphyrin zinc complex, a phenanthroline europium complex, and the like can be given.
- metal complexes having a structure as a ligand for example, iridium complexes, platinum complexes and other metal complexes having light emission from a triplet excited state, aluminum quinolinol complexes, benzoquinolinol beryllium complexes, benzoxazolyl zinc A complex, a benzothiazole zinc complex, an azomethylzinc complex, a porphyrin zinc complex, a phenanthroline europium complex, and the
- Polymer material As polymer materials, polyparaphenylene vinylene derivatives, polythiophene derivatives, polyparaphenylene derivatives, polysilane derivatives, polyacetylene derivatives, polyfluorene derivatives, polyvinylcarbazole derivatives, the above dye materials and metal complex light emitting materials are polymerized. The thing etc. can be mentioned.
- materials that emit blue light include distyrylarylene derivatives, oxadiazole derivatives, and polymers thereof, polyvinylcarbazole derivatives, polyparaphenylene derivatives, polyfluorene derivatives, and the like.
- polymer materials such as polyvinyl carbazole derivatives, polyparaphenylene derivatives, and polyfluorene derivatives are preferred.
- examples of materials that emit green light include quinacridone derivatives, coumarin derivatives, and polymers thereof, polyparaphenylene vinylene derivatives, polyfluorene derivatives, and the like. Of these, polymer materials such as polyparaphenylene vinylene derivatives and polyfluorene derivatives are preferred.
- examples of materials that emit red light include coumarin derivatives, thiophene ring compounds, and polymers thereof, polyparaphenylene vinylene derivatives, polythiophene derivatives, and polyfluorene derivatives.
- polymer materials such as polyparaphenylene vinylene derivatives, polythiophene derivatives, and polyfluorene derivatives are preferable.
- Dopant material examples include perylene derivatives, coumarin derivatives, rubrene derivatives, quinacridone derivatives, squalium derivatives, porphyrin derivatives, styryl dyes, tetracene derivatives, pyrazolone derivatives, decacyclene, phenoxazone, and the like. Note that the thickness of such a light emitting layer is usually about 2 nm to 200 nm.
- a predetermined coating method in addition to the method described above, a vacuum deposition method, a transfer method, or the like can be used.
- the above-described application method using a predetermined nozzle is preferable, but as other methods, spin coating method, casting method, micro gravure coating method, gravure coating method, bar coating method , Roll coating method, wire bar coating method, dip coating method, slit coating method, spray coating method and nozzle coating method, and gravure printing method, screen printing method, flexographic printing method, offset printing method, reverse printing method And an application method such as an inkjet printing method.
- Electrode transport material constituting the electron transport layer
- known materials can be used, such as oxadiazole derivatives, anthraquinodimethane or derivatives thereof, benzoquinone or derivatives thereof, naphthoquinone or derivatives thereof, anthraquinones or derivatives thereof, tetracyanoanthra Quinodimethane or derivatives thereof, fluorenone derivatives, diphenyldicyanoethylene or derivatives thereof, diphenoquinone derivatives, or metal complexes of 8-hydroxyquinoline or derivatives thereof, polyquinoline or derivatives thereof, polyquinoxaline or derivatives thereof, polyfluorene or derivatives thereof, etc. Can be mentioned.
- electron transport materials include oxadiazole derivatives, benzoquinone or derivatives thereof, anthraquinones or derivatives thereof, metal complexes of 8-hydroxyquinoline or derivatives thereof, polyquinoline or derivatives thereof, polyquinoxaline or derivatives thereof, polyfluorenes Or a derivative thereof, preferably 2- (4-biphenylyl) -5- (4-tert-butylphenyl) -1,3,4-oxadiazole, benzoquinone, anthraquinone, tris (8-quinolinol) aluminum, and polyquinoline. preferable.
- the method for forming the electron transport layer there are no particular restrictions on the method for forming the electron transport layer, but for low molecular weight electron transport materials, vacuum deposition from powder or film formation from a solution or a molten state can be exemplified.
- the material include film formation from a solution or a molten state.
- a polymer binder may be used in combination.
- the film formation method from a solution include the same application method as the film formation method of the hole injection layer described above, and the electron transport layer uses the predetermined nozzle described above as a method of forming a light emitting layer. It is preferable to form by a conventional coating method.
- the film thickness of the electron transport layer is appropriately set in consideration of the electrical characteristics and the ease of film formation, and is, for example, 1 nm to 1 ⁇ m, preferably 2 nm to 500 nm, and more preferably 5 nm to 200 nm. .
- an optimal material is appropriately selected according to the type of the light emitting layer, and an alloy containing at least one of alkali metal, alkaline earth metal, alkali metal and alkaline earth metal, alkali A metal or alkaline earth metal oxide, halide, carbonate, or a mixture of these substances can be given.
- alkali metals, alkali metal oxides, halides, and carbonates include lithium, sodium, potassium, rubidium, cesium, lithium oxide, lithium fluoride, sodium oxide, sodium fluoride, potassium oxide, potassium fluoride , Rubidium oxide, rubidium fluoride, cesium oxide, cesium fluoride, lithium carbonate, and the like.
- alkaline earth metals, alkaline earth metal oxides, halides and carbonates include magnesium, calcium, barium, strontium, magnesium oxide, magnesium fluoride, calcium oxide, calcium fluoride, barium oxide, Examples thereof include barium fluoride, strontium oxide, strontium fluoride, and magnesium carbonate.
- the electron injection layer may be composed of a laminate in which two or more layers are laminated, and examples thereof include LiF / Ca.
- the electron injection layer is formed by vapor deposition, sputtering, printing, or the like.
- the thickness of the electron injection layer is preferably about 1 nm to 1 ⁇ m.
- a material for the cathode As a material for the cathode, a material having a small work function, easy electron injection into the light emitting layer, and high electrical conductivity is preferable. Moreover, in the organic EL element which takes out light from the anode side, since the light from the light emitting layer is reflected to the anode side by the cathode, a material having a high visible light reflectance is preferable as the cathode material.
- an alkali metal, an alkaline earth metal, a transition metal, a group 13 metal of the periodic table, or the like can be used.
- cathode material examples include lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, aluminum, scandium, vanadium, zinc, yttrium, indium, cerium, samarium, europium, terbium, ytterbium, and the like.
- An alloy, graphite, or a graphite intercalation compound is used.
- alloys include magnesium-silver alloys, magnesium-indium alloys, magnesium-aluminum alloys, indium-silver alloys, lithium-aluminum alloys, lithium-magnesium alloys, lithium-indium alloys, calcium-aluminum alloys, and the like.
- a transparent conductive electrode made of a conductive metal oxide, a conductive organic material, or the like can be used.
- the conductive metal oxide include indium oxide, zinc oxide, tin oxide, ITO, and IZO
- examples of the conductive organic substance include polyaniline or a derivative thereof, polythiophene or a derivative thereof, and the like.
- the cathode may be composed of a laminate in which two or more layers are laminated. In some cases, the electron injection layer is used as a cathode.
- the film thickness of the cathode is appropriately set in consideration of electric conductivity and durability, and is, for example, 10 nm to 10 ⁇ m, preferably 20 nm to 1 ⁇ m, and more preferably 50 nm to 500 nm.
- Examples of the method for producing the cathode include a vacuum deposition method, a sputtering method, and a laminating method in which a metal thin film is thermocompression bonded.
- Examples of the material for the insulating layer include metal fluorides, metal oxides, and organic insulating materials.
- an organic EL element provided with an insulating layer having a thickness of 2 nm or less an organic EL element having an insulating layer having a thickness of 2 nm or less adjacent to the cathode and an insulating layer having a thickness of 2 nm or less adjacent to the anode are provided. Can be mentioned.
- the application method using capillary force and static pressure using a predetermined nozzle has been described above through the explanation of the cap coater system 11.
- the present invention is not limited to this, and the method using capillary force, static
- the present invention can also be applied to a method using pressure and a method using a pump.
- the width in the short direction of the slit-like discharge port may be increased.
- the discharge amount of the coating liquid can be controlled by using the power of the pump.
- the coating liquid is separated from the object to be coated by lowering the nozzle, but the pump power or the tank is lowered without lowering the nozzle.
- the coating liquid can be retracted into the slit-like discharge port, and the coating liquid can be separated from the coated body.
- the nozzle and the object to be coated may be relatively moved in the coating direction while maintaining the state where the coating liquid is separated from the object to be coated. Even in this case, since the coating liquid is separated from the coated body, the coating liquid is not applied to the coated body.
- the organic EL element described above can be suitably used for a curved or planar illumination device, or a planar light source used as a light source for a scanner or a backlight for a display device.
- cleaned glass was prepared as a substrate.
- the coating solution was applied onto the substrate using a capillary coating system (trade name “CAP Coater III” manufactured by Hirano Techseed Co., Ltd.) as a coating apparatus.
- a capillary coating system (trade name “CAP Coater III” manufactured by Hirano Techseed Co., Ltd.)
- a solvent for the coating solution a mixed solution of anisole and cyclohexylbenzene (weight ratio 1: 1) was used.
- the polymer light emitting material was dissolved in this mixed solvent so that the concentration became 1% by weight, and a coating solution was prepared.
- a nozzle provided with two slit discharge ports in the arrangement direction Y for discharging the coating solution upward was used. Notches that are recessed downward are formed at both ends of each slit-like discharge port.
- the shim is arranged so as to be integrated with the non-fluid portion other than the area where the slit-like discharge port and the manifold communicate with each other, and the outer edge of the nozzle body and the outer edge of the shim at the notch are arranged so as to be substantially flush with each other. .
- the width in the application direction X (short direction) of each slit-like discharge port is 300 ⁇ m, and the width in the arrangement direction Y (longitudinal direction) of the slit-like discharge ports is 70 mm.
- the two slit discharge ports are provided with an interval of 20 mm in the arrangement direction Y.
- the coating process was applied twice by repeating the coating process and the non-coating process.
- the coating speed was 0.5 m / min
- the coating liquid was applied with a distance of 250 ⁇ m between the upper end of the nozzle and the substrate.
- Example 2 A coating solution was applied in a pattern in the same manner as in Example except that only the nozzle used for coating was changed.
- a nozzle in which notches were not formed at both ends of each slit-like discharge port was used. That is, the upper end of the slit-like discharge port is flush with both ends of the slit-like discharge port.
- FIG. 8 is a diagram showing the state of the substrate coated with the coating liquid in the example
- FIG. 9 is a diagram showing the state of the substrate coated with the coating liquid in the comparative example.
- the portion where the coating solution is applied is hatched.
- a broken line parallel to a portion where the coating liquid is applied and a portion intended to be coated is hatched, and further a portion where the coating liquid is coated and is not intended to be coated. Has been given.
- a coating film having a width corresponding to the width (70 mm) in the arrangement direction Y of the slit-like discharge ports could be formed on the substrate on which the coating liquid was applied with the nozzle in which the notch was formed.
- the coating liquid when the coating liquid is applied with a nozzle having no notch and the width of the slit-shaped ejection openings in the arrangement direction Y defined only by the shim, the coating liquid spreads in the arrangement direction Y (the nozzle longitudinal direction) The coating solution was thinly applied even to the portion that was used as the liquid passing portion, and the target pattern could not be obtained.
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Abstract
Description
塗布工程では、ノズル13から吐出される塗布液が前記被塗布体19に接液した状態を維持したまま、前記ノズル13と前記被塗布体19とを所定の塗布方向に相対移動する。
非塗布工程では、塗布液を前記被塗布体から離液させた状態を維持したまま、前記ノズルと被塗布体とを前記塗布方向に相対移動する。
a)陽極/発光層/陰極
b)陽極/正孔注入層/発光層/陰極
c)陽極/正孔注入層/発光層/電子注入層/陰極
d)陽極/正孔注入層/発光層/電子輸送層/陰極
e)陽極/正孔注入層/発光層/電子輸送層/電子注入層/陰極
f)陽極/正孔輸送層/発光層/陰極
g)陽極/正孔輸送層/発光層/電子注入層/陰極
h)陽極/正孔輸送層/発光層/電子輸送層/陰極
i)陽極/正孔輸送層/発光層/電子輸送層/電子注入層/陰極
j)陽極/正孔注入層/正孔輸送層/発光層/陰極
k)陽極/正孔注入層/正孔輸送層/発光層/電子注入層/陰極
l)陽極/正孔注入層/正孔輸送層/発光層/電子輸送層/陰極
m)陽極/正孔注入層/正孔輸送層/発光層/電子輸送層/電子注入層/陰極
n)陽極/発光層/電子注入層/陰極
o)陽極/発光層/電子輸送層/陰極
p)陽極/発光層/電子輸送層/電子注入層/陰極
さらに有機EL素子は、2層以上の発光層を有していてもよく、また2層以上の発光層を有し、電荷を発生する電荷発生層を発光層間に介在させたいわゆるマルチフォトン型の素子を構成してもよい。
基板には例えばガラス、プラスチック、およびシリコン基板、並びにこれらを積層したものなどが用いられる。また有機EL素子をその上に形成するための基板として、予め電気回路が形成されたものを用いてもよい。
陽極を通して発光層からの光を取出す構成の有機EL素子の場合、この陽極には透明又は半透明の電極が用いられる。透明電極または半透明電極としては、電気伝導度の高い金属酸化物、金属硫化物および金属などの薄膜を用いることができ、光透過率の高いものが好適に用いられる。具体的には酸化インジウム、酸化亜鉛、酸化スズ、ITO、インジウム亜鉛酸化物(IndiumZinc Oxide:略称IZO)、金、白金、銀、および銅などから成る薄膜が用いられ、これらの中でもITO、IZO、または酸化スズから成る薄膜が好適に用いられる。陽極の作製方法としては、真空蒸着法、スパッタリング法、イオンプレーティング法、メッキ法などを挙げることができる。また、該陽極として、ポリアニリンもしくはその誘導体、ポリチオフェンもしくはその誘導体などの有機の透明導電膜を用いてもよい。
正孔注入層を構成する正孔注入材料としては、酸化バナジウム、酸化モリブデン、酸化ルテニウム、および酸化アルミニウムなどの酸化物や、フェニルアミン系、スターバースト型アミン系、フタロシアニン系、アモルファスカーボン、ポリアニリン、およびポリチオフェン誘導体などを挙げることができる。
正孔輸送層を構成する正孔輸送材料としては、ポリビニルカルバゾール若しくはその誘導体、ポリシラン若しくはその誘導体、側鎖若しくは主鎖に芳香族アミンを有するポリシロキサン誘導体、ピラゾリン誘導体、アリールアミン誘導体、スチルベン誘導体、トリフェニルジアミン誘導体、ポリアニリン若しくはその誘導体、ポリチオフェン若しくはその誘導体、ポリアリールアミン若しくはその誘導体、ポリピロール若しくはその誘導体、ポリ(p-フェニレンビニレン)若しくはその誘導体、又はポリ(2,5-チエニレンビニレン)若しくはその誘導体などを挙げることができる。
発光層は通常、主として蛍光及び/又はりん光を発光する有機物、またはこの有機物とこれを補助するドーパントとから形成される。ドーパントは、例えば発光効率の向上や、発光波長を変化させるために加えられる。なお有機物は、低分子化合物でも高分子化合物でもよく、発光層は、ポリスチレン換算の数平均分子量が、103~108である高分子化合物を含むことが好ましい。発光層を構成する発光材料としては、例えば以下の色素系材料、金属錯体系材料、高分子系材料、ドーパント材料を挙げることができる。
色素系材料としては、例えば、シクロペンダミン誘導体、テトラフェニルブタジエン誘導体化合物、トリフェニルアミン誘導体、オキサジアゾール誘導体、ピラゾロキノリン誘導体、ジスチリルベンゼン誘導体、ジスチリルアリーレン誘導体、ピロール誘導体、チオフェン環化合物、ピリジン環化合物、ペリノン誘導体、ペリレン誘導体、オリゴチオフェン誘導体、オキサジアゾールダイマー、ピラゾリンダイマー、キナクリドン誘導体、クマリン誘導体などを挙げることができる。
金属錯体系材料としては、例えばTb、Eu、Dyなどの希土類金属、またはAl、Zn、Be、Ir、Ptなどを中心金属に有し、オキサジアゾール、チアジアゾール、フェニルピリジン、フェニルベンゾイミダゾール、キノリン構造などを配位子に有する金属錯体を挙げることができ、例えばイリジウム錯体、白金錯体などの三重項励起状態からの発光を有する金属錯体、アルミニウムキノリノール錯体、ベンゾキノリノールベリリウム錯体、ベンゾオキサゾリル亜鉛錯体、ベンゾチアゾール亜鉛錯体、アゾメチル亜鉛錯体、ポルフィリン亜鉛錯体、フェナントロリンユーロピウム錯体などを挙げることができる。
高分子系材料としては、ポリパラフェニレンビニレン誘導体、ポリチオフェン誘導体、ポリパラフェニレン誘導体、ポリシラン誘導体、ポリアセチレン誘導体、ポリフルオレン誘導体、ポリビニルカルバゾール誘導体、上記色素系材料や金属錯体系発光材料を高分子化したものなどを挙げることができる。
ドーパント材料としては、例えばペリレン誘導体、クマリン誘導体、ルブレン誘導体、キナクリドン誘導体、スクアリウム誘導体、ポルフィリン誘導体、スチリル系色素、テトラセン誘導体、ピラゾロン誘導体、デカシクレン、フェノキサゾンなどを挙げることができる。なお、このような発光層の厚さは、通常約2nm~200nmである。
電子輸送層を構成する電子輸送材料としては、公知のものを使用でき、オキサジアゾール誘導体、アントラキノジメタン若しくはその誘導体、ベンゾキノン若しくはその誘導体、ナフトキノン若しくはその誘導体、アントラキノン若しくはその誘導体、テトラシアノアンスラキノジメタン若しくはその誘導体、フルオレノン誘導体、ジフェニルジシアノエチレン若しくはその誘導体、ジフェノキノン誘導体、又は8-ヒドロキシキノリン若しくはその誘導体の金属錯体、ポリキノリン若しくはその誘導体、ポリキノキサリン若しくはその誘導体、ポリフルオレン若しくはその誘導体などを挙げることができる。
電子注入層を構成する材料としては、発光層の種類に応じて最適な材料が適宜選択され、アルカリ金属、アルカリ土類金属、アルカリ金属およびアルカリ土類金属のうちの1種類以上含む合金、アルカリ金属若しくはアルカリ土類金属の酸化物、ハロゲン化物、炭酸塩、またはこれらの物質の混合物などを挙げることができる。アルカリ金属、アルカリ金属の酸化物、ハロゲン化物、および炭酸塩の例としては、リチウム、ナトリウム、カリウム、ルビジウム、セシウム、酸化リチウム、フッ化リチウム、酸化ナトリウム、フッ化ナトリウム、酸化カリウム、フッ化カリウム、酸化ルビジウム、フッ化ルビジウム、酸化セシウム、フッ化セシウム、炭酸リチウムなどを挙げることができる。また、アルカリ土類金属、アルカリ土類金属の酸化物、ハロゲン化物、炭酸塩の例としては、マグネシウム、カルシウム、バリウム、ストロンチウム、酸化マグネシウム、フッ化マグネシウム、酸化カルシウム、フッ化カルシウム、酸化バリウム、フッ化バリウム、酸化ストロンチウム、フッ化ストロンチウム、炭酸マグネシウムなどを挙げることができる。電子注入層は、2層以上を積層した積層体で構成されてもよく、例えばLiF/Caなどを挙げることができる。電子注入層は、蒸着法、スパッタリング法、印刷法などにより形成される。電子注入層の膜厚としては、1nm~1μm程度が好ましい。
陰極の材料としては、仕事関数の小さく、発光層への電子注入が容易で、電気伝導度の高い材料が好ましい。また陽極側から光を取出す有機EL素子では、発光層からの光を陰極で陽極側に反射するために、陰極の材料としては可視光反射率の高い材料が好ましい。陰極には、例えばアルカリ金属、アルカリ土類金属、遷移金属および周期表13族金属などを用いることができる。陰極の材料としては、例えばリチウム、ナトリウム、カリウム、ルビジウム、セシウム、ベリリウム、マグネシウム、カルシウム、ストロンチウム、バリウム、アルミニウム、スカンジウム、バナジウム、亜鉛、イットリウム、インジウム、セリウム、サマリウム、ユーロピウム、テルビウム、イッテルビウムなどの金属、前記金属のうちの2種以上の合金、前記金属のうちの1種以上と、金、銀、白金、銅、マンガン、チタン、コバルト、ニッケル、タングステン、錫のうちの1種以上との合金、またはグラファイト若しくはグラファイト層間化合物などが用いられる。合金の例としては、マグネシウム-銀合金、マグネシウム-インジウム合金、マグネシウム-アルミニウム合金、インジウム-銀合金、リチウム-アルミニウム合金、リチウム-マグネシウム合金、リチウム-インジウム合金、カルシウム-アルミニウム合金などを挙げることができる。また、陰極としては導電性金属酸化物および導電性有機物などから成る透明導電性電極を用いることができる。具体的には、導電性金属酸化物として酸化インジウム、酸化亜鉛、酸化スズ、ITO、およびIZOを挙げることができ、導電性有機物としてポリアニリンもしくはその誘導体、ポリチオフェンもしくはその誘導体などを挙げることができる。なお、陰極は、2層以上を積層した積層体で構成されていてもよい。なお、電子注入層が陰極として用いられる場合もある。
絶縁層の材料としては、金属フッ化物、金属酸化物、有機絶縁材料などを挙げることができる。膜厚2nm以下の絶縁層を設けた有機EL素子としては、陰極に隣接して膜厚2nm以下の絶縁層を設けたもの、陽極に隣接して膜厚2nm以下の絶縁層を設けたものを挙げることができる。
塗工に用いるノズルのみを代えて実施例と同様に塗布液をパターン塗布した。比較例では、各スリット状吐出口の両端に切り欠きが形成されていないノズルを用いた。すなわちスリット状吐出口の両端には、スリット状吐出口の上端と面一の面が形成されている。
2 有機層の形成される被形成面
11 キャップコーターシステム
12 定盤
13 ノズル
14 タンク
16 塗布液供給管
17 塗布液
18 液面センサー
19 被塗布体
21 シム
21a 板体
21b 非通液部
22 ノズル本体
23 スリット状吐出口
24 マニホールド
25 切り欠き部
X 塗布方向
Y 配列方向
Z 鉛直方向
Claims (5)
- 一対の電極と、該電極間に配置される1層以上の有機層とを有し、前記1層以上の有機層として1層以上の発光層が設けられる有機EL素子の製造方法であって、
一対の電極のうちの一方の電極を形成する工程と、1または複数の有機層を形成する工程と、一対の電極のうちの他方の電極を形成する工程とを有し、
前記1または複数の有機層を形成する工程では、
有機EL素子となる被塗布体を、前記有機層の形成される被形成面を下方に向けて配置し、
有機層となる材料を含む塗布液を上方に吐出する複数のスリット状吐出口と、このスリット状吐出口の各両端部に形成される下方に凹む切り欠き部とを有するノズルを、前記被塗布体の下方に配置し、
前記ノズルから吐出される塗布液が前記被塗布体に接液した状態を維持したまま、前記ノズルと前記被塗布体とを所定の塗布方向に相対移動する塗布工程と、前記塗布液を前記被塗布体から離液させた状態を維持したまま、前記ノズルと被塗布体とを前記塗布方向に相対移動する非塗布工程とを交互に繰り返すことにより、前記被形成面に塗布液を塗布成膜し、当該塗布成膜した塗布液を固化することによって前記有機層を形成する、有機EL素子の製造方法。 - 前記ノズルは、
前記スリット状吐出口の短手方向の幅を開けて相対して配置される一対のノズル本体と、
前記スリット状吐出口の短手方向の幅の厚みを有し、前記ノズル本体に挟持されてスリット状吐出口を除く領域に設けられ、スリット状吐出口の長手方向の幅を規定するシムと、を備え、
前記切り欠き部において前記一対のノズル本体の外縁と前記シムの外縁とは、略面一に配置されている、請求項1記載の有機EL素子の製造方法。 - 前記切り欠き部は、上端から下端に向けて前記スリット状吐出口から離間するように傾斜して形成されている、請求項1または2記載の有機EL素子の製造方法。
- 請求項3記載の製造方法によって製造された有機エレクトロルミネッセンス素子を備える照明装置。
- 請求項3記載の製造方法によって製造された有機エレクトロルミネッセンス素子を備える面状光源。
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US13/504,169 US9118013B2 (en) | 2009-10-28 | 2010-10-22 | Method for producing organic EL element |
CN201080048864.0A CN102598862B (zh) | 2009-10-28 | 2010-10-22 | 有机el元件的制造方法 |
EP10826635.4A EP2496054B1 (en) | 2009-10-28 | 2010-10-22 | Method for producing organic el element |
KR20127013013A KR20120085822A (ko) | 2009-10-28 | 2010-10-22 | 유기 el 소자의 제조 방법 |
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JP2010070599A (ja) * | 2008-09-17 | 2010-04-02 | Dow Corning Toray Co Ltd | 液状ダイボンディング剤 |
KR20130081528A (ko) * | 2012-01-09 | 2013-07-17 | 삼성디스플레이 주식회사 | 증착 마스크 및 이를 이용한 증착 설비 |
CN107961932A (zh) * | 2016-10-19 | 2018-04-27 | 鲍德温·伊梅克股份公司 | 喷雾喷嘴装置 |
EP3528963B1 (en) | 2016-10-19 | 2022-09-14 | Baldwin Jimek AB | Arrangement at spray nozzle chamber |
SE543963C2 (en) | 2020-02-28 | 2021-10-12 | Baldwin Jimek Ab | Spray applicator and spray unit comprising two groups of spray nozzles |
KR20230072591A (ko) * | 2021-11-18 | 2023-05-25 | 주식회사 엘지에너지솔루션 | 다이 코팅용 착탈식 심, 다이 코팅용 착탈식 심의 제작 방법, 및 다이 코팅용 착탈식 심이 구비된 다이 코터 |
KR20230094865A (ko) * | 2021-12-21 | 2023-06-28 | 주식회사 엘지에너지솔루션 | 슬롯 다이 코터 및 이를 포함하는 다레인 이중 코팅 장치 |
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US9118013B2 (en) | 2015-08-25 |
JP2011096435A (ja) | 2011-05-12 |
EP2496054B1 (en) | 2019-01-02 |
US20120268006A1 (en) | 2012-10-25 |
CN102598862B (zh) | 2014-12-24 |
EP2496054A4 (en) | 2013-12-18 |
JP4983890B2 (ja) | 2012-07-25 |
TW201125181A (en) | 2011-07-16 |
CN102598862A (zh) | 2012-07-18 |
KR20120085822A (ko) | 2012-08-01 |
EP2496054A1 (en) | 2012-09-05 |
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