WO2006100889A1 - Procede pour former une couche el organique - Google Patents

Procede pour former une couche el organique Download PDF

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Publication number
WO2006100889A1
WO2006100889A1 PCT/JP2006/304063 JP2006304063W WO2006100889A1 WO 2006100889 A1 WO2006100889 A1 WO 2006100889A1 JP 2006304063 W JP2006304063 W JP 2006304063W WO 2006100889 A1 WO2006100889 A1 WO 2006100889A1
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WO
WIPO (PCT)
Prior art keywords
layer
organic
coating
forming
unit
Prior art date
Application number
PCT/JP2006/304063
Other languages
English (en)
Japanese (ja)
Inventor
Nobuhiko Takashima
Yousuke Takashima
Masaaki Murayama
Seiichi Tobisawa
Original Assignee
Konica Minolta Holdings, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Konica Minolta Holdings, Inc. filed Critical Konica Minolta Holdings, Inc.
Priority to JP2007509175A priority Critical patent/JP5125503B2/ja
Publication of WO2006100889A1 publication Critical patent/WO2006100889A1/fr

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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
    • H10K71/50—Forming devices by joining two substrates together, e.g. lamination techniques
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
    • H10K2102/301—Details of OLEDs
    • H10K2102/311—Flexible OLED
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/805—Electrodes
    • H10K59/8051—Anodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/87—Passivation; Containers; Encapsulations
    • H10K59/873—Encapsulations
    • 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
    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour

Definitions

  • the present invention relates to a method for forming an organic EL layer of an organic EL (electral luminance) element used as a surface light source, a display panel, or the like.
  • the organic EL element includes a first electrode (anode or cathode) formed on a substrate, an organic EL layer having an organic compound layer including a light emitting layer stacked thereon, and a layer stacked on the light emitting layer. It is a thin film type element having a second electrode (cathode or anode).
  • a voltage is applied to such an organic EL element, electrons are injected from the cathode into the organic EL layer and holes are injected from the cathode. It is known that light is obtained by releasing energy as light when the electrons and holes recombine in the light emitting layer and the energy level returns from the conduction band to the valence band.
  • the organic EL element is a thin film type element
  • a surface light source such as a backlight.
  • a display device is configured by using an organic EL panel in which a predetermined number of organic EL elements as pixels are formed on a substrate as a display panel, it is highly visible and has no viewing angle dependency. There are advantages that cannot be obtained with the device.
  • JP-A-9-102393 and JP-A-2002-170676 when forming an organic EL layer of an organic EL element, as described in JP-A-9-102393 and JP-A-2002-170676, vapor deposition, sputtering, CVD, Various methods such as PVD and solvent coating can be used. Among these methods, the manufacturing process is simplified, the manufacturing cost is reduced, the workability is improved, and the backlight and illumination light source are flexible. It is known that a wet film forming method such as a coating method is advantageous from the viewpoint of application to a large area device.
  • JP 2002-170676 discloses a single wafer glass substrate. A method for forming an organic compound layer on a plate by spin coating is described. Japanese Patent Application Laid-Open No.
  • 2003-142260 describes a method of sequentially forming an organic compound layer on a single wafer substrate by an ink jet method.
  • Each of these methods uses a single-wafer substrate as a substrate, so there is a limit to increasing production efficiency. From these situations, use a roll-shaped substrate that is highly likely to increase production efficiency, and then form various layers that make up the organic EL element on the substrate. Manufacturing methods (roll-to-roll method) are being studied.
  • a method is known in which a roll-like long film is supplied and a light-emitting layer is formed on the film while being conveyed by a wet coating method, and then wound into a rolled core.
  • Patent Document 1 As a method of manufacturing an organic EL display using a plastic film as a light-transmitting substrate, a cathode, one or a plurality of light-emitting layers made of an organic material, and an anode layer on the plastic film, an organic material is used.
  • a method of producing a pattern of one or a plurality of light-emitting layers and patterning a cathode by a vacuum and a single roll method by vapor deposition under vacuum see, for example, Patent Document 2.
  • Patent Document 1 JP-A-10-77467
  • Patent Document 2 Pamphlet of International Publication No. 01/5194
  • the present invention has been made in view of the above situation, and an object thereof is to provide a method of forming an organic EL layer for a high-quality organic EL element with high productivity.
  • An organic EL element having an anode layer including at least a first electrode, an organic EL layer including an organic compound layer including a light emitting layer, and a cathode layer including a second electrode in this order on a strip-shaped flexible support.
  • the organic EL layer is formed using a manufacturing apparatus having a supply unit, a pattern coating and drying unit for forming the light emitting layer on the anode layer, and a recovery unit.
  • the supply section is supplied with a strip-shaped flexible support A on which an anode layer including at least a first electrode is formed in a roll state, and includes a first accumulator section before the pattern coating and drying section, and a second accumulator section later.
  • the accumulator section, and the pattern coating / drying section includes a pattern coating section for forming a coating film for forming a light emitting layer under atmospheric pressure conditions using a wet pattern forming coating apparatus with a coating liquid for forming an organic EL layer.
  • Solvent in the organic EL layer under atmospheric pressure conditions 1 unit of the organic EL layer drying unit for forming the organic EL layer, and the pattern coating / drying unit has at least one unit of the pattern coating / drying unit, and the pattern coating / drying unit Then, the organic EL layer is formed on the anode layer to form a strip-like flexible support B, and the recovery unit forms a winding roll on the winding core.
  • the wet pattern formation coating apparatus operates in response to the intermittent conveyance of the strip-shaped flexible support A, operates when the strip-shaped flexible support A is stopped, and performs pattern formation coating.
  • the method for forming an organic EL layer according to any one of claims 1 to 3, wherein:
  • the said pattern application part has the holding means of a strip
  • the wet coating / drying unit applies a coating solution for forming an organic compound layer by a wet coating apparatus to form an organic compound layer under atmospheric pressure conditions and a solvent in the organic compound layer by applying the organic compound layer under atmospheric pressure conditions.
  • a coating solution for forming an organic compound layer by a wet coating apparatus to form an organic compound layer under atmospheric pressure conditions and a solvent in the organic compound layer by applying the organic compound layer under atmospheric pressure conditions.
  • the organic EL layer and the organic compound layer have a dew point temperature of 20 ° C. or less and conformity with JISB 9920, and the measured cleanliness is class 5 or less, and the organic EL layer drying unit, the organic compound layer drying unit, The method for forming an organic EL layer according to any one of claims 1 to 12, wherein the organic EL layer is formed in an atmospheric pressure of 10 to 45 ° C except for a heat treatment portion.
  • a method of forming an organic EL layer for a high-quality organic EL element with high productivity can be provided, and a stable organic EL element can be produced.
  • FIG. 1 is a schematic cross-sectional view showing an example of a layer structure of an organic EL element.
  • FIG. 2 is a schematic view of a manufacturing apparatus having a pattern application / drying unit for forming layers up to an organic EL layer.
  • FIG. 3 is an enlarged schematic view of a portion indicated by P in FIG.
  • FIG. 4 is a schematic view of a manufacturing apparatus having a wet coating 'drying unit and a pattern coating' drying unit that form up to an organic EL layer.
  • FIG. 5 is a schematic diagram of a manufacturing apparatus having a wet coating / drying section before and after a pattern coating / drying section for forming an organic EL layer.
  • FIG. 6 is an enlarged schematic plan view of a portion indicated by Q in FIG. Explanation of symbols
  • Electron injection layer (electron transport layer)
  • Embodiments according to the present invention will be described with reference to FIGS. 1 to 6, but the present invention is not limited thereto.
  • FIG. 1 is a schematic cross-sectional view showing an example of the layer structure of an organic EL element.
  • FIG. 1 (a) is a schematic cross-sectional view showing the constituent layers of an organic EL element on which a sealing film is formed.
  • FIG. 1 (b) is a schematic cross-sectional view showing the constituent layers of an organic EL element formed by adhering a sealing film via an adhesive.
  • the layer structure of the organic EL element shown in Fig. 1 (a) will be described.
  • la indicates the organic EL element.
  • the organic EL element la includes a first electrode (anode) 102, a hole transport layer 103, a light emitting layer 104, an electron injection layer 105, a second electrode (cathode) 106, and a sealing material on a substrate 101. It has a stop layer 107 in this order.
  • lb represents an organic EL device.
  • the organic EL element lb is formed on a substrate 101 with a first electrode (anode) 102, a hole transport layer (hole injection layer) 103, a light emitting layer 104, an electron injection layer 105, and a second electrode (cathode). ) 106, an adhesive layer 108, and a sealing film 109 are provided in this order.
  • a hole injection layer (not shown) may be provided between the first electrode (anode) 102 and the light emitting layer 104 or the hole transport layer 103.
  • an electron transport layer may be provided between the second electrode (cathode) 106 and the light emitting layer 104 or the electron injection layer 105.
  • a gas barrier film (not shown) between the anode (first electrode) 102 and the substrate 101.
  • the present invention relates to a method for forming the light emitting layer 104 shown in the figure.
  • the layer structure of the organic EL element shown in this figure is an example, but other typical organic EL elements Examples of the layer structure include the following structures.
  • the organic EL layer means a layer structure sandwiched between an anode and a cathode in the layer structure shown in FIG. Each layer constituting the organic EL element will be described later.
  • FIG. 2 is a schematic diagram of a manufacturing apparatus having a pattern coating / drying unit for forming layers up to the organic EL layer.
  • the following is a method for forming an organic EL layer having a hole transport layer, a light-emitting layer, and an electron transport layer on a strip-shaped flexible support having a first electrode that is patterned and formed as an example. This will be described with reference to the drawings.
  • reference numeral 2 denotes a manufacturing apparatus for forming up to the organic EL layer, which is one of the constituent layers of the organic EL element, under atmospheric pressure conditions.
  • the manufacturing apparatus 2 includes a supply unit 201, a cleaning surface modification processing unit 202 for a strip-shaped flexible support, a first charge removal processing unit 203, a first accumulator unit 204, a pattern coating / drying unit 205, The heat treatment unit 206, the second static elimination processing unit 207, the second accumulator 208, and the recovery unit B209 are provided.
  • the strip-shaped flexible support A201a in which the gas barrier film and the anode layer including the first electrode are already formed in this order is wound around the winding core and supplied in a roll state. It has become.
  • 201b shows a strip-like flexible support A201a in a roll state.
  • the first electrode (see FIGS. 1 and 6) is formed by patterning (see FIG. 6).
  • the cleaning surface modification processing unit 202 includes an anode layer (not shown) including the first electrode of the strip-shaped flexible support A201a sent from the supply unit 201 before being applied by the pattern application / drying unit 205. ) It has cleaning surface modification processing means 202a for cleaning and modifying the surface.
  • the cleaning surface modification means 202a include a low-pressure mercury lamp, an excimer lamp, a plasma cleaning apparatus, and the like.
  • the conditions for cleaning surface modification with a low-pressure mercury lamp include, for example, wavelength 184.
  • the condition for performing the cleaning surface modification treatment by irradiating a 2 nm low-pressure mercury lamp with an irradiation intensity of 5 to 20 mW / cm 2 and a distance of 5 to 15 mm is mentioned.
  • atmospheric pressure plasma is preferably used as a condition for the cleaning surface modification treatment by the plasma cleaning apparatus.
  • cleaning conditions argon gas containing 1 to 5% by volume of oxygen is used, and cleaning surface modification treatment is performed at a frequency of 100 KHz to 150 MHz, a voltage of 10 V to 10 KV, and an irradiation distance of 5 to 20 mm.
  • Examples of the charge removal processing means used in the first charge removal processing unit 203 include a light irradiation method, a corona discharge method, and the like, and these can be appropriately selected and used as necessary.
  • Light irradiation type generates weak ions
  • corona discharge type generates air ions by corona discharge. The air ions are attracted to the charged object to compensate for the opposite polarity charge and neutralize the static electricity.
  • a static eliminator using corona discharge and a static eliminator using soft X-rays can be used. Since the first charge removal processing section removes the charge of the base material, the adhesion of the dust and the dielectric breakdown are prevented, thereby improving the yield of the element.
  • the first accumulator unit 204 moves the roll 204a in the vertical direction (in the direction of the arrow in the figure), and the conveyance speed and pattern application of the belt-like flexible support A201a conveyed from the supply unit 201. It is arranged to adjust the difference from the pattern application speed of the drying unit 205, and has a function of accumulating a belt-like flexible support A201a of a certain length, before and after the first accumulator unit 204. It has become possible to change the operation of the strip-shaped flexible support A201a.
  • the roll length 204a can be adjusted according to the speed difference.
  • the roll 204a is preferably a non-contact roll capable of transporting the layer forming surface in a non-contact manner.
  • the pattern coating / drying unit 205 shown in the figure includes a pattern coating unit that forms a light emitting layer under an atmospheric pressure condition by using a wet pattern formation coating apparatus with an organic EL layer forming coating solution, and an atmospheric pressure condition.
  • the organic EL layer drying section that removes the solvent in the organic EL layer and forms the organic EL layer is provided as one unit.
  • This figure shows the case of having 3 units (first pattern application / drying unit 205a, second pattern application 'drying unit 205b, and third pattern application' drying unit 205c). All have the same configuration.
  • the coating liquid for forming an organic EL layer refers to a coating liquid for forming a hole transport layer, a coating liquid for forming a light emitting layer, and a coating liquid for forming an electron transport layer.
  • the first pattern application 'drying unit 205a is a first pattern coating unit 205al that forms a hole transport layer under atmospheric pressure conditions by a wet pattern formation coating apparatus using a hole transport layer forming coating solution 205a, and under atmospheric pressure conditions.
  • the second pattern coating / drying unit 205b includes a second pattern coating unit 205bl that forms a coating film for forming a light emitting layer under atmospheric pressure conditions by using a wet pattern forming coating apparatus with a coating solution for forming a light emitting layer. And a light emitting layer drying section 205b 2 for removing the solvent in the light emitting layer and forming the light emitting layer.
  • the third pattern coating / drying unit 205b includes a second pattern coating unit 205bl that forms an electron transport layer under an atmospheric pressure condition by a wet pattern formation coating apparatus using an electron transport layer forming coating solution, and an electron under an atmospheric pressure condition. It has an electron transport layer drying section 205c2 that removes the solvent in the transport layer and forms an electron transport layer.
  • the first pattern application unit 205al includes a wet pattern formation application device 205al l and a holding table 205al 2 which is a means for holding the belt-like flexible support A.
  • the second pattern coating unit 205 bl is a holding means for holding a belt-like flexible support formed with a wet pattern formation coating device 205 bl l and a hole transport layer sent from the first pattern coating and drying unit 205 a. It has 20 5bl 2 pedestals.
  • the third pattern applicator 205cl is a wet pattern forming applicator 205cl and a second pattern applicator, a holder 205cl that is a means for holding the belt-like flexible support on which the light emitting layer sent from the dryer 205b is formed. And 2.
  • the heat treatment unit 206 includes a heat treatment unit 206a provided on the rear side of the hole transport layer drying unit 205a2, a heat treatment unit 206b provided on the rear side of the light emitting layer drying unit 205b2, and a hole transport layer drying unit.
  • a heat treatment unit 206c provided on the rear side of the unit 205c2.
  • the belt-like flexible support is kept flat.
  • a suction table may be used as long as it can be fixed.
  • the suction table include a mechanism having a suction hole on the table, a mechanism having a porous surface on which the table is placed, and a table that electrostatically attracts, and can be appropriately selected and used.
  • a table having a mechanism in which the mounting surface is porous is used.
  • the first pattern application / drying unit 205a fixes the band-shaped flexible support A201a conveyed from the supply unit 201 on the holding base 205al 2 and uses the wet pattern formation coating apparatus 205al 1 to
  • the hole transport layer forming coating solution is applied to the region excluding the end of the first electrode formed on the flexible support A201a, and the solvent in the hole transport layer is removed from the hole transport layer drying unit 20
  • the hole transport layer 201c is formed by removing with 5a2.
  • the formed hole transport layer 201c is subjected to heat treatment by the heat treatment unit 206a.
  • the first pattern coating is provided on the belt-like flexible support A on which the first electrode conveyed from the previous step is formed.
  • Alignment mark 4 (see FIG. 6) is detected by the detector of the alignment detection means arranged in the first pattern application unit 205al, and the belt-like flexible support A is adsorbed and fixed on the holding table.
  • the wet pattern formation coating device 205al l is aligned according to the alignment mark, and the hole layer formation coating is applied to the region of the first electrode except a part of the end portion of the patterned first electrode. The liquid is applied on the electrode.
  • the second pattern coating / drying unit 205b fixes the belt-like flexible support on which the hole transport layer 201c conveyed from the first pattern coating / drying unit 205a is formed on the holding table 205bl2. Then, using a wet pattern formation coating apparatus 205bl l, the coating solution for forming the light emitting layer is applied to the pattern of the first electrode, applied onto the formed hole transport layer 201c, and the solvent in the light emitting layer is removed from the light emitting layer drying unit 205b2 To remove the light emitting layer 201d. The formed light emitting layer is subjected to heat treatment by the heat treatment unit 206b.
  • the third pattern coating / drying unit 205c fixes the belt-like flexible support on which the light emitting layer 201d conveyed from the second pattern coating / drying unit 205b is formed on the holding table 205cl2, and performs wet processing.
  • the electron transport layer 201d is applied onto the light emitting layer 201d on which the electron transport layer forming coating solution has been formed by using a pattern forming coating device 205cl1, and the solvent in the electron transport layer is removed by the electron transport layer drying unit 205c2 to remove the electron transport layer 201e.
  • the formed electron transport layer is subjected to a calorie heat treatment in the heat treatment unit 206c.
  • the previous process force is provided on the belt-like flexible support A on which the light emitting layer is formed.
  • Alignment mark 4 (see Fig. 6) is detected by the detector of the alignment detection means arranged in the third pattern application section 205cl, and the strip-shaped flexible support A with the light emitting layer formed on the holding table
  • the wet pattern formation coating apparatus 205cll is aligned according to the alignment mark, and the electron transport layer forming coating solution is applied onto the light emitting layer.
  • the first pattern coating / drying unit 205a to the third pattern coating 'drying unit 205c have the hole transport layer 201c, the light emitting layer 201d, and the electron transport layer 201e except for the end of the first electrode.
  • a belt-like flexible support B on which an organic EL layer is formed is completed.
  • the first pattern application unit 205al to the third pattern application unit 205cl are all applied while being adsorbed and fixed to the holding base, so that the hole transport layer is formed from the first pattern application / drying unit 205a.
  • the moving from the drying unit 205 to the collecting unit 209 is performed after the application of each layer is formed in each unit, and thus is intermittent.
  • Examples of wet coaters that can be used in the wet pattern forming and coating apparatus 205al l include an inkjet method, a flexographic printing method, an offset printing method, a gravure printing method, a screen printing method, and a mask.
  • the use of these wet pattern forming coating machines is the light emitting layer type It is possible to select appropriately according to the material of the composition coating liquid. This figure shows the ink jet method.
  • the second static elimination processing unit 207 performs static elimination on the belt-like flexible support having the electron transport layer 201e formed by the third pattern coating / drying unit 205c, and prevents failure due to static electricity in the next process. It has a function to stop and can be arranged as necessary.
  • the second static elimination processing unit 207 preferably uses the same static elimination processing means as that used for the first static elimination processing unit 203.
  • the second accumulator unit 208 moves the roll 208a in the vertical direction (the direction of the arrow in the figure). It is arranged to adjust the difference in transport speed between the pattern coating / drying unit 205 and the wet coating / drying unit (not shown), and the roll 208a can be added according to the speed difference.
  • the second accumulator unit 208 is intermittently conveyed in a state where the belt-like flexible support is stopped in the pattern application / drying unit 205, so that a certain amount is accumulated in the second accumulator unit 208 and collected in the recovery unit 209. It is also possible to use it in a method of scraping off the amount continuously.
  • the second accumulator unit 208 preferably has the same function as the first accumulator unit 204 and has the same configuration.
  • a strip-shaped flexible support B201f processed by the second static elimination processing unit 207 and having an organic EL layer formed thereon is wound around a winding core as a strip-shaped flexible support B201g in a roll state. It is collected and stored until it is sent to the next process for forming the electron injection layer, the second electrode, the sealing layer and the like.
  • FIG. 3 is an enlarged schematic view of a portion indicated by P in FIG.
  • the strip-shaped flexible support B on which the organic EL layer is formed is cooled to room temperature with a cooling device (not shown) and then scraped off.
  • the light-emitting layer drying unit 205b2 includes a drying air supply header 205b23 having a discharge port 205b21 for discharging a drying air, a drying air supply port 205b22, a non-air opening 205b24, and a transport ronole 205b25. And then sing.
  • the heat treatment unit 206b includes a heat treatment apparatus main body 206bl and a back surface of a belt-like flexible support having a light emitting layer 201d formed on the hole transport layer 201d in accordance with the pattern of the first electrode.
  • the heat treatment unit 206b has a function of further stabilizing the hole transport layer by heat treatment.
  • the hole transport layer drying unit 205a2 and the heat treatment unit 206a and the electron transport layer drying unit 205c2 and the heat treatment unit 206c shown in FIG. 2 have the same structure as the light emitting layer drying unit 205b2 and the heat treatment unit 206b shown in FIG. Have the same function.
  • FIG. 4 is a schematic view of a manufacturing apparatus having a wet coating / drying unit and a pattern coating / drying unit for forming layers up to the organic EL layer.
  • the following is a method for forming an organic EL layer having a hole transport layer, a light-emitting layer, and an electron transport layer on a strip-like flexible support having a first electrode that is patterned and formed as an example. I will explain it.
  • reference numeral 3 denotes a manufacturing apparatus for forming up to the organic EL layer, which is one of the constituent layers of the organic EL element, under atmospheric pressure conditions.
  • the production apparatus 3 includes a supply unit 301, a cleaning surface modification processing unit 302 for the strip-shaped flexible support, a static elimination processing unit A303, a wet coating / drying unit 304, a static elimination processing unit B3 05, and a first accumulator.
  • the strip-shaped flexible support A301a in which the gas barrier film and the anode layer including the first electrode are already formed in this order is wound around the winding core and supplied in a roll state. It has become.
  • 301b shows the roll-shaped flexible support A301a in a roll state.
  • the first electrode (see FIGS. 1 and 6) is formed by patterning (see FIGS. 1 and 6).
  • the cleaning surface modification processing unit 302 is an anode layer (not shown) including the first electrode of the strip-shaped flexible support A301a that has been fed by the supply unit 301 before being applied by the wet application / drying unit 304. And cleaning surface modification processing means 302a for cleaning and modifying the surface.
  • the cleaning surface modification processing means 302a is the same as the cleaning surface modification processing means 202a shown in FIG. 2, has the same function, and can perform the cleaning surface modification processing under the same conditions.
  • the static elimination processing unit A303 has a function of removing static electricity from the belt-like flexible support A301a processed by the cleaning surface modification processing unit 302, and preventing a failure due to static electricity in the next process, It can be installed as needed.
  • the static elimination processing unit A303 has the same static elimination processing means as the first static elimination processing unit 203 shown in FIG. 2, and has the same function.
  • the wet coating / drying unit 304 has a backup roll 304a for holding the strip-shaped flexible support A301a and a belt on the strip-shaped flexible support A301a held by the backup roll 304a. Formed on the first electrode on the strip-shaped flexible support A301a and the wet coating machine 304b that applies the coating solution for forming the hole transport layer to the first electrode formed by turning under atmospheric pressure conditions And a hole transport layer drying section 304c for removing the solvent in the hole transport layer 301c under atmospheric pressure.
  • Examples of the wet coater that can be used for the wet coater 304b include a die coating method, a screen printing method, a flexographic printing method, a Mayer bar method, a cap coating method, a spray coating method, a casting method, a roll coating method, It is possible to use a coating machine such as bar coating or gravure coating.
  • the use of these wet coaters can be appropriately selected according to the material of the organic compound layer forming coating liquid organic compound layer.
  • the heat treatment unit 308 includes a heat treatment unit 308a disposed after the hole transport layer drying unit 304c, a heat treatment unit 308b disposed after the light emitting layer drying unit 307a2, and an electron transport layer drying unit.
  • the heat treatment unit 308c is disposed after the drying unit 307b2, and all have the same structure.
  • the heat treatment unit 308a heat-treats from the back surface side of the belt-shaped flexible support having the hole transport layer 301d formed by the hole transport layer drying unit 304c by the back surface heat transfer method, and further stabilizes it. It is preferable to dispose as necessary.
  • the heat treatment unit 308b heat-treats from the back side of the belt-like flexible support having the light emitting layer 201e formed by the light emitting layer drying unit 307al by the back surface heat transfer method, and further stabilizes the light emitting layer 20 le. It is preferable to dispose as necessary.
  • the heat treatment unit 308c is heat-treated by the back surface heat transfer method from the back side of the belt-like flexible support having the electron transport layer 201f formed by the electron transport layer drying unit 307bl, and is further stabilized by the electron transport layer. It has a function of 20 mm and is preferably disposed as necessary.
  • the first accumulator unit 306 adjusts the difference in the conveyance speed between the wet coating 'drying unit 304 and the pattern coating' drying unit 307 by moving the roll 306a in the vertical direction (the arrow direction in the figure).
  • the roll 306a can be added according to the speed difference.
  • the roll 306a is preferably a non-contact roll capable of transporting the hole transport layer surface in a non-contact manner.
  • the pattern coating / drying unit 307 includes a pattern coating unit that forms a light emitting layer under a atmospheric pressure condition by using a wet pattern forming coating apparatus with a coating solution for forming a light emitting layer.
  • the first pattern coating / drying unit 307a with the drying unit for removing the solvent as one unit, and the pattern coating unit for forming the electron transport layer under the atmospheric pressure condition by the wet pattern formation coating device using the coating liquid for forming the electron transport layer And an electron transport layer drying section that removes the solvent in the electron transport layer under atmospheric pressure conditions, and a second pattern application / drying section 307b.
  • the first pattern application 'drying unit 307a and the second pattern application' drying unit 307b have the same configuration.
  • the first pattern coating / drying unit 307a is a first pattern coating unit 307al that forms a light emitting layer under an atmospheric pressure condition by using a wet pattern forming coating apparatus with a light emitting layer forming coating solution. And a light emitting layer drying section 307a2 for removing the solvent.
  • the second pattern coating / drying unit 307b includes a first pattern coating unit 307bl that forms an electron transport layer under an atmospheric pressure condition by a wet pattern formation coating apparatus using an electron transport layer forming coating solution, and an atmospheric pressure condition. And an electron transport layer drying section 307b2 for removing the solvent in the electron transport layer.
  • the static elimination processing section B has a function of performing static elimination on the band-shaped flexible support having the hole transport layer 301d formed by the wet coating / drying section 304 and preventing a failure due to static electricity in the next process. And can be arranged as necessary.
  • the first pattern application unit 307al has a wet pattern formation application device 307al and a holding table 307al 2 which is a holding means for the strip-shaped flexible support A on which the hole transport layer is formed.
  • the second pattern coating unit 307bl includes a wet pattern formation coating device 307bl and a holding base that is a holding means for the belt-like flexible support A on which the light emitting layer sent from the first pattern coating and drying unit 307a is formed. 307bl 2.
  • the first pattern application unit 307al and the second pattern application unit 307bl include alignment detection means (see Fig. 6) and application position correction control means (Fig. 6).
  • the holding table 307al 2 (307bl 2) is the same as the holding table shown in FIG.
  • the first pattern coating / drying unit 307a fixes the belt-shaped flexible support A on which the hole transport layer transported from the wet coating / drying unit 304 is formed on the holding table 307al 2, and performs wet processing.
  • a coating solution for forming a light emitting layer is applied onto the sending layer, and the solvent in the light emitting layer is removed by the light emitting layer drying unit 307a2 to form the light emitting layer 301e.
  • the formed light emitting layer 301e is subjected to heat treatment in the heat treatment unit 308b.
  • the wet pattern forming coating device 3 07 When coating is performed by the wet pattern forming coating device 3 07all in the first pattern coating 'drying unit 307a, it is provided on the belt-like flexible support A on which the hole transport layer to be transported is formed.
  • the alignment mark 4 (see Fig. 6) is detected by the detector of the alignment detection means arranged in the first pattern application section 307al, and the belt-like flexible support A is adsorbed and fixed on the holding table.
  • the wet pattern forming and coating device 307al l is aligned according to the alignment mark, and light emission is performed in accordance with the pattern of the first electrode except for a part of the end portion of the first electrode formed by patterning.
  • a layer-forming coating solution is applied onto the electrode.
  • the second pattern coating / drying unit 307b fixes the belt-shaped flexible support on which the light emitting layer 301e conveyed from the first pattern coating / drying unit 307a is formed on the holding table 307bl 2, and is wet.
  • the pattern forming coating apparatus 307bl l applies the electron transport layer forming coating solution onto the light emitting layer 201d, and the solvent in the electron transport layer is removed by the electron transport layer drying unit 307b2 to remove the electron transport layer 301f. Form.
  • the formed electron transport layer is subjected to heat treatment in the heat treatment unit 308c.
  • the wet pattern forming coating device 3 07bl l in the second pattern coating / drying unit 307b When coating is performed by the wet pattern forming coating device 3 07bl l in the second pattern coating / drying unit 307b, it is provided on the belt-like flexible support A on which the light emitting layer conveyed from the previous step is formed.
  • Alignment mark 4 (see Fig. 6) is detected by the detector of the alignment detection means arranged in the third pattern application section 307bl, and the strip-shaped flexible support A on which the light emitting layer is formed is placed on the holding table.
  • the wet pattern formation coating device 307bl is aligned according to the alignment mark, and the electron transport layer forming coating solution is applied on the light emitting layer.
  • a belt-like flexible support B having a layer formed thereon is completed.
  • the wet pattern formation coating apparatus 307al l (307b 11) is the same as the wet pattern formation coating apparatus shown in FIG. This figure shows the case where an ink jet coating device is used.
  • the static elimination processing unit C309 performs static elimination on the belt-like flexible support having the electron transport layer 30 If formed by the second pattern coating / drying unit 307b, and prevents a failure due to static electricity in the next process. It has a function and can be arranged as required. In addition, it is preferable to use the same static elimination processing means as the static elimination processing means used for the static elimination processing section A as the static elimination processing means used for the static elimination processing section B305 and the static elimination processing section C309.
  • the second accumulator unit 309 is configured such that when a wet application / drying unit (not shown) is disposed after the second accumulator unit 308, the roll 208a moves in the vertical direction (the direction of the arrow in the figure). , Arranged to adjust the difference in transport speed between the pattern coating / drying unit 307 and the wet coating / drying unit (not shown), and the roll 31 la can be added according to the speed difference. .
  • the second accumulator unit 311 is intermittently transported while the belt-like flexible support is stopped in the pattern application / drying unit 207, so that a certain amount is accumulated in the second accumulator unit 311 and collected in the collection unit 312. It is also possible to use it in a method of scraping off the amount continuously.
  • the second accumulator unit 311 preferably has the same function as the first accumulator unit 306 and has the same configuration.
  • the strip-shaped flexible support B301g which is processed by the static elimination processing unit C and formed with the organic EL layer, is wound around the winding core and collected as a rolled strip-shaped flexible support B301h. It is stored until it is sent to the next process for forming the electron injection layer, the second electrode, the sealing layer and the like.
  • the belt-shaped flexible support B on which the organic EL layer is formed is cooled to room temperature with a cooling device (not shown) and then wound up.
  • FIG. 5 is a schematic diagram of a manufacturing apparatus having a wet coating / drying unit before and after a pattern coating / drying unit for forming up to an organic EL layer.
  • the following is a method for forming an organic EL layer having a hole transport layer, a light-emitting layer, and an electron transport layer on a strip-shaped flexible support having a first electrode that is patterned and formed as an example. I will explain it.
  • the manufacturing apparatus 4 indicates the shape up to the organic EL layer, which is one of the constituent layers of the organic EL element, under atmospheric pressure conditions.
  • the manufacturing apparatus to be formed is shown.
  • the manufacturing apparatus 4 includes a supply unit 401, a belt-like flexible substrate cleaning surface modification processing unit 402, a static elimination processing unit a403, a first wet coating / drying unit 404, a heat processing unit 405, and a static elimination treatment.
  • a processing unit d414 and a recovery unit 415 are provided.
  • the manufacturing apparatus 4 shown in the figure includes a first wet application / drying unit 404 and a heat treatment unit 406 before the first accumulator unit 407, and a second wet application / drying unit 412 after the second accumulator unit 411. And a heat treatment unit 413 are provided.
  • the strip-shaped flexible support A401a in which the gas barrier film and the anode layer including the first electrode are already formed in this order is wound around the winding core and supplied in a roll state. It has become.
  • 401b shows the roll-shaped flexible support A401a in a roll state.
  • the first electrode (see FIGS. 1 and 6) is formed by patterning (see FIGS. 1 and 6).
  • the cleaning surface modification processing unit 402 has an anode layer (including a first electrode of the strip-shaped flexible support A401a sent from the supply unit 401 before being applied by the first wet coating / drying unit 404. (Not shown) cleaning surface modification processing means 402a for cleaning and modifying the surface.
  • the neutralization processing unit a403 has a function of performing static neutralization of the belt-like flexible support A 401a processed by the cleaning surface modification processing unit 402, and preventing a failure due to static electricity in the next process. It can be arranged as necessary.
  • the charge removal processing unit a403 has the same charge removal processing means as the first charge removal processing unit 203 shown in FIG. 2, and has the same function.
  • the first wet coating / drying unit 404 is formed with a hole transport layer on the back-up opening 404a holding the strip-shaped flexible support A401a and the strip-shaped flexible support A401a held by the backup roll 404a.
  • a transport layer drying section 405c For removing the solvent of the hole transport layer formed on the first electrode on the wet flexible coater 404b and the strip-shaped flexible support A401a under atmospheric pressure conditions.
  • the wet coater 404b is the same as the wet coater 304b shown in FIG.
  • the heat treatment unit 405 heat-treats from the back side of the belt-shaped flexible support A having the hole transport layer 401c formed by the hole transport layer drying unit 405c by the back surface heat transfer method, and further stabilizes the holes. It has a function of forming the transport layer 401 d and is preferably disposed as necessary.
  • the static elimination processing unit b406 performs static elimination on the belt-shaped flexible support A on which the hole transport layer 40 Id formed in the first wet coating / drying unit is formed, and a failure caused by static electricity in the next process. It has a function to prevent this, and can be installed as necessary.
  • the static elimination processing unit b406 preferably uses the same static elimination processing unit as that used in the first static elimination processing unit 203 shown in FIG.
  • the first accumulator unit 407 adjusts the difference in transport speed between the wet coating / drying unit 404 and the pattern coating / drying unit 408 by moving the roll 407a in the vertical direction (the arrow direction in the figure).
  • the roll 407a can be added according to the speed difference.
  • the roll 406a is preferably a non-contact roll that can transport the hole transport layer surface in a non-contact manner.
  • the first pattern application / drying unit 408 includes a pattern application unit 408a and a light emitting layer drying unit 408b.
  • the pattern coating part 408a is a belt-shaped flexible support holding base 408a2 in which the hole transport layer 40 Id is formed, and a large amount of coating solution for forming the light emitting layer is formed on the hole transport layer 401d in accordance with the pattern of the first electrode.
  • the light emitting layer drying unit 408b has a function of removing the solvent in the light emitting layer under atmospheric pressure conditions, and has the same configuration as the light emitting layer drying unit 205b2 shown in FIG.
  • the holding table 408a2 is not particularly limited as long as the belt-like flexible support can be fixed while maintaining flatness, and it is preferable to use a holding table having the same structure as the holding table shown in FIG.
  • the pattern is provided on the belt-like flexible support A on which the hole transport layer to be transported is formed.
  • Alignment mark 4 (see Fig. 6) is detected by the detector of the alignment detection means arranged in the pattern application unit 408a, and the belt-like flexible support A on which the hole transport layer is formed is held on the holding base.
  • Wet-fixed on top and forms wet pattern according to alignment mark.Applicator 408al is aligned and aligned with the pattern of the first electrode except for a part of the end of the first electrode formed by patterning. Then, the light emitting layer forming coating solution is applied onto the electrode.
  • the heat treatment unit 409 heat-treats from the back side of the belt-like flexible support having the light-emitting layer 401e formed by the light-emitting layer drying unit 408b by a back-surface heat transfer method, thereby obtaining a more stable light-emitting layer. It has a function, and it is preferable to arrange as needed.
  • the heat treatment unit 409 is shown in FIG. It has the same configuration as the heat treatment part 206b.
  • the charge removal processing unit c410 has a function of removing charges from the belt-like flexible support on which the light emitting layer is formed, and preventing a failure caused by static electricity in the next step, and is disposed as necessary. Is becoming possible.
  • the static elimination processing unit c410 preferably uses the same static elimination processing unit as the static elimination processing unit used in the first static elimination processing unit 203 shown in FIG.
  • the second accumulator unit 411 adjusts the difference in conveyance speed between the pattern coating 'drying unit 408 and the wet coating' drying unit 412 by moving the roll 411a in the vertical direction (the arrow direction in the figure).
  • the roll 411a can be added according to the speed difference.
  • the second accumulator unit 411 has the same configuration as the first accumulator unit 407.
  • the second wet coating / drying unit 412 is formed with a backup roll 412a holding the belt-like flexible support on which the light emitting layer 401e is formed, and a light emitting layer 40le held on the backup roll 412a.
  • Wet coater 412b that coats the belt-shaped flexible support with a coating solution for forming an electron transport layer under atmospheric pressure, and an electron transport layer drying unit that removes the solvent of the formed electron transport layer under atmospheric pressure. 412c.
  • the electron transport layer drying section 412c has the same configuration as the light emitting layer drying section 205b2 shown in FIG.
  • the wet coater 412b is the same as the wet coater 304b shown in FIG.
  • the heat treatment unit 413 heat-treats from the back side of the belt-like flexible support having the electron transport layer 401f formed by the electron transport layer drying unit 412c by the back surface heat transfer method, and further stabilizes the electron transport layer 40 If It is preferable to dispose as necessary.
  • the heat treatment unit 413 has the same configuration as the heat treatment unit 206b shown in FIG.
  • the static elimination processing unit d414 performs static elimination on the band-shaped flexible support having the electron transport layer 401f formed by the second wet coating / drying unit 412 and prevents a failure due to static electricity in the next process. And can be arranged as required.
  • the static elimination processing unit d414 preferably uses the same static elimination processing means as that used in the first static elimination processing unit 203 shown in FIG.
  • a strip-shaped flexible support B401g which is processed by the static elimination processing unit d414, and on which the organic EL layer is formed, is wound around the winding core as a rolled strip-shaped flexible support B401h. It is collected and stored until it is sent to the next process for forming the electron injection layer, the second electrode, the sealing layer and the like.
  • the strip-shaped flexible support B on which the organic EL layer is formed is cooled to room temperature with a cooling device (not shown) and then wound up.
  • the coating apparatus 4 shown in this figure is performed in a state where the coating of the light emitting layer forming coating solution in the pattern coating / drying unit 408 is stopped, and when the light emitting layer is completely coated, the next light emitting layer Intermittent conveyance is performed to apply the forming coating solution.
  • the first wet application 'drying unit 404 the hole transport layer is continuously applied, and the first wet adjustment' drying unit 404 and the pattern application 'drying unit 408 adjust the speed difference.
  • the accumulator section 407 is adjusted so that the required length can be stored.
  • the second wet coating / drying unit 412 is continuously coated with an electron transport layer, and the second difference is that the speed difference between the pattern coating / drying unit 408 and the second wet coating / drying unit 412 is adjusted.
  • the accumulator unit 411 is adjusted so that the required length can be stored.
  • FIG. 6 is an enlarged schematic plan view of a portion indicated by Q in FIG.
  • FIG. 6 (a) is an enlarged schematic plan view of the pattern application part indicated by Q in FIG.
  • FIG. 6 (b) is an enlarged schematic plan view of the band-shaped flexible support in a state in which a hole transport layer is formed on the first electrode conveyed from the wet coating / drying unit.
  • A shows a wet pattern forming coating apparatus for pattern coating of the blue light emitting layer forming coating liquid
  • B shows a wet pattern forming coating apparatus for pattern coating of the green light emitting layer forming coating liquid
  • C Shows a wet pattern forming coating apparatus for pattern coating the red light emitting layer forming coating liquid.
  • a wet pattern forming coating apparatus 205bl is configured.
  • Each of the wet pattern forming and coating apparatuses A to C shown in the figure shows a case where an ink jet head is used, and is hereinafter also simply referred to as a head.
  • Reference numeral 205bl 3 denotes a stage to which the head 205bl 1 is attached, and the head 205bl ll is disposed on the stage 205bl3 so as to be movable in the width direction (arrow direction in the figure).
  • 205 bl4 is a state in which the hole transport layer 201 c is formed on the first electrode 102 in the stage 205 bl 3.
  • the stage to be mounted so as to be movable in the transport direction (arrow direction in the figure) of the belt-like flexible support is shown.
  • the first electrode 102 is patterned on the strip-shaped flexible support 201m, and is provided in the longitudinal direction of the strip-shaped flexible support 201m continuously at regular intervals.
  • each wet pattern forming coating apparatus A to C may be disposed independently, or each wet pattern forming coating apparatus A to C may be combined. It is preferable to select appropriately according to need.
  • This figure shows a case where wet pattern forming and coating apparatuses A to C are arranged together.
  • Alignment mark 4 is at least two places on the lower right end and upper left end (or upper right end and lower left end) of first electrode 102 with respect to the conveyance direction of strip-shaped flexible support A (the direction of the arrow in the figure). It is preferable from the relation of determining the position of the head 205bl. Of course, the alignment mark 4 may be provided on the lower right end, upper right end, left lower end, and left upper end of the first electrode 102.
  • the hole transport layer 201c is formed by applying and drying the entire surface in the first pattern application / drying unit 205b (see FIG. 2), leaving the end 102a of the first electrode 102.
  • An example of the detection device 3 is a CCD camera.
  • the belt-like flexible support having the hole transport layer 201c, the stage 205bl3, the stage 205bl4, and the head 205bl1 are driven according to the detection information of the alignment mark 4 by the detection device 3 according to the detection information of the coating position correction (non- It can be controlled by (shown).
  • FIG. 5 shows a process of applying a light emitting layer forming coating solution on the first electrode 102 arranged in a pattern according to the pattern of the first electrode 102 in the pattern application unit shown in FIG. Shown below when the manufacturing equipment is used.
  • the alignment mark 4 provided on the first electrode 102 is detected by the detection device provided in the pattern coating / drying unit 408, whereby the belt-like flexible film having the hole transport layer 401d formed thereon is detected.
  • the support is sucked and fixed onto the holding table 408a2.
  • the stage 205bl 3 moves based on the information that the belt-like flexible support is sucked and fixed onto the holding table 408a2, and the position of the head is determined.
  • the coating solution for forming the blue light emitting layer is applied from head A (see FIG. 6), and the coating solution for forming the green light emitting layer is applied from head B (see FIG. 6). Then, a red light emitting layer forming coating solution is applied onto the first electrode 102 from the head C (see FIG. 6). As the stage 205 bl3 moves in the width direction, each of the first electrodes 102 in which the blue light emitting layer forming coating liquid, the green light emitting layer forming coating liquid, and the red light emitting layer forming coating liquid are patterned is used. Applied to.
  • the stage 205bl4 moves in the transport direction by the pitch of the first electrode 102, and is used for forming a blue light emitting layer in the same manner as S4.
  • a coating solution, a green light emitting layer forming coating solution, and a red light emitting layer forming coating solution are applied to each of the patterned first electrodes 102.
  • S4 and S5 are repeated until all of the patterned first electrodes 102 are coated with the blue light emitting layer forming coating solution, the green light emitting layer forming coating solution, and the red light emitting layer forming coating solution.
  • the conveyance of the belt-like flexible support is stopped at the pattern application unit 408a, while the wet coating and drying unit 404 and the heat treatment unit 406 are continuously transporting the holes.
  • the first accumulator unit 407 operates to adjust the speed difference between the pattern coating unit 408a, the wet coating / drying unit 404, and the heat treatment unit 405.
  • the formed belt-like flexible support is stored.
  • each drying section shown in FIGS. 2 to 6 are determined in consideration of drying unevenness of each formed coating film, rough coating of the coating surface, and the like. .:! ⁇ Airflow drying of 5m / s, width direction wind velocity 0.1 ⁇ : 10%.
  • the heating conditions in the heat treatment section shown in Figs. 2 to 6 are those that consider the improvement in smoothness of the hole transport layer, light emitting layer, electron transport layer, etc., removal of residual solvent, curing, etc. Decomposes organic compounds that constitute the hole transport layer, light-emitting layer, electron transport layer, etc. at a temperature of -30 to + 30 ° C with respect to the glass transition temperature of the transport layer, light-emitting layer, electron transport layer, etc. It is preferable to perform heat treatment of the back surface heat transfer system at a temperature that does not exceed the temperature.
  • the coating liquid for forming the hole transport layer and the coating liquid for forming the electron transport layer are applied by the wet coater shown in FIGS.
  • it is preferably 0.2 to 10% with respect to the average conveyance speed.
  • the formation of the hole transport layer, the light emitting layer, the electron transport layer, etc. maintains the performance of the hole transport layer, the light emitting layer, the electron transport layer, etc.
  • the dew point temperature is -20 ° C or less
  • the measured cleanliness is class 5 or less, excluding the drying section and heat treatment section.
  • the strip-shaped flexible support B on which an organic EL layer (a hole transport layer, a light emitting layer, an electron transport layer, etc.) is formed is wound around a winding core and recovered as a roll, and the organic EL maintain performance of the layers, taking into account the non-light emission failure or the like, it is good preferable to store under a reduced pressure of 10- 5 10 Pa.
  • the storage period is preferably 1 hour to 200 hours in consideration of the removal of oxygen and trace moisture due to the deterioration of the organic EL layer. In some cases, it may be stored in a heated environment.
  • a strip-shaped flexible support A having an anode layer including a first electrode is used, and an organic EL layer (hole transport layer) is formed on the first electrode.
  • an organic EL layer hole transport layer
  • Light emitting layer, electron transport layer to form a strip-shaped flexible support B, and then the organic compound to form the strip-shaped flexible support B on a winding core in the form of a strip-shaped flexible support B
  • Pattern application ⁇ By placing the accumulator part before and after the drying part, when applying the coating solution for forming the light emitting layer, it is possible to stop and apply the light, so that accurate and stable light emission is possible. Formation of the layer became possible. [0122] 2) Furthermore, the application position correction control means makes it possible to place the wet pattern forming application device at an accurate position according to the alignment mark, eliminating the misalignment of the light emitting layer, and making it accurate and stable. A light emitting layer can be formed.
  • Pattern application ⁇ The accumulator section is placed before and after the drying section, so that wet coating equipment and pattern coating equipment with different coating speeds can be used in combination, enabling continuous production and improving productivity. It became.
  • the hole transport layer according to the present invention is made of a hole transport material having a function of transporting holes, and in a broad sense, a hole injection layer and an electron blocking layer are also included in the hole transport layer.
  • the hole transport layer can be provided as a single layer or multiple layers. When a plurality of hole transport layers are provided, it is necessary to increase the wet coating / drying section in accordance with the number of layers, and it is preferable to increase the heat treatment section at the same time.
  • each light emitting layer (blue light emitting layer, green light emitting layer, red light emitting layer) is preferably selected in the range of 2 to lOOnm, and more preferably in the range of 2 to 20nm. . There are no particular restrictions on the thickness of the blue, green, and red light emitting layers, but the blue light emitting layer is preferably the thickest among the three color light layers.
  • the light-emitting layer according to the present invention is a blue light-emitting layer having a maximum emission wavelength of 430 to 480 nm, a green light-emitting layer having a wavelength of 10 to 550 nm, and a red light-emitting layer having a range of 600 to 640 nm.
  • a blue light-emitting layer having a maximum emission wavelength of 430 to 480 nm
  • a green light-emitting layer having a wavelength of 10 to 550 nm
  • a red light-emitting layer having a range of 600 to 640 nm.
  • it includes at least three layers with different emission spectra in the range of these emission maximum wavelengths. If it is 3 layers or more, there is no restriction in particular. When there are more than four layers, there may be a plurality of layers having the same emission spectrum.
  • a plurality of light emitting compounds may be mixed in each light emitting layer within the range where the maximum wavelength is maintained.
  • the blue light emitting layer may be used by mixing a blue light emitting compound having a maximum wavelength of 430 to 480 nm and a green light emitting compound having the same wavelength of 510 to 550 nm.
  • the material used for the light emitting layer is not particularly limited. For example, Toray Research Center, Inc. The latest trends in flat panel displays The current state of EL displays and the latest technological trends Various materials such as those described on pages 228-332 can be mentioned.
  • the light emitting layer formed by applying the coating solution for forming the light emitting layer with a wet pattern forming coating machine and drying it is an electron or hole injected from the electrode, the electron injection layer, or the hole transport layer. Is a layer that emits light by recombination, and the light emitting portion may be in the layer of the light emitting layer or at the interface between the light emitting layer and the adjacent layer.
  • Examples of the strip-shaped flexible support used for the strip-shaped flexible support A on which the anode layer including the first electrode according to the present invention has already been formed include a transparent resin film.
  • the resin film include polyesters such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), polyethylene, polypropylene, cellophane, cellulose diacetate, cenorelose triacetate, cenorelose acetate butyrate, cenorelose Cellulose esters such as cetate propionate (CAP), cellulose acetate phthalate (TAC), cellulose nitrate or their derivatives, polyvinylidene chloride, polyvinylenoleoleconole, polyethylene butyl alcohol, syndiotactic polystyrene, polycarbonate, Norbornene resin, polymethylpentene, polyetherketone, polyimide, polyethersulfone (PES), polyphenylene sulfide, polysulf
  • an electrode material made of a metal, an alloy, an electrically conductive compound, or a mixture thereof having a high work function (4 eV or more) is preferably used.
  • electrode materials include conductive transparent materials such as metals such as Au, Cul, indium tinoxide (ITO), SnO and ZnO. It is also possible to use an amorphous material such as IDIX ⁇ (InO ⁇ ⁇ ) that can produce a transparent conductive film.
  • these electrode materials may be formed into a thin film by a method such as vapor deposition or sputtering, and a pattern having a desired shape may be formed by a single photolithography method.
  • the electrode material It is also possible to form a pattern through a mask of the desired shape when depositing or sputtering the electrode material. Or when using the substance which can be apply
  • the sheet resistance is preferably several hundred ⁇ / mouth or less.
  • the film thickness is a force depending on the material, and is usually selected in the range of 10 to 1000 nm, preferably 10 to 200 nm.
  • a hole injection layer may exist between the anode and the light emitting layer or the hole transport layer.
  • the injection layer is a layer that is provided between the electrode and the organic layer in order to lower the drive voltage and increase the luminance of the light emission.
  • anode buffer layer (hole injection layer) The details of the anode buffer layer (hole injection layer) are described in JP-A-9-45479, JP-A-9-260062, JP-A-8-288069 and the like.
  • One layer of phthalocyanine buffer typified by copper phthalocyanine
  • one layer of oxide buffer typified by vanadium oxide
  • one layer of amorphous carbon buffer typified by vanadium oxide
  • polymer buffer using a conductive polymer such as polyaniline (emeraldine) or polythiophene, etc.
  • the thickness of the anode buffer layer (hole injection layer) is preferably in the range of 0.1 ⁇ to 5 ⁇ ⁇ ⁇ , although it depends on the material desired to be a very thin film.
  • a gas barrier film may be formed on the surface of the resin film used as the belt-like flexible support, if necessary.
  • the gas barrier film include an inorganic film, an organic film, or a hybrid film of both.
  • the water vapor permeability is preferably 0.01 g / m 2 'day' atm or less.
  • the oxygen permeability 10- 3 g / m 2 / day or less is preferably a high barrier film follows the water vapor transmission rate 10- 5 g / m 2 / day .
  • any material may be used as long as it has a function of suppressing intrusion of elements such as moisture and oxygen that cause deterioration of the element.
  • silicon oxide, silicon dioxide, silicon nitride, or the like is used. I can do it.
  • the order of lamination of the inorganic layer and the organic layer is not particularly limited, but it is preferable to laminate the layers alternately several times.
  • the method of forming the nano film for example, vacuum deposition, sputtering, reactive sputtering, molecular beam epitaxy, cluster-one ion beam, ion plating, plasma polymerization, atmospheric pressure Plasma polymerization method, plasma CV Forces capable of using D method, laser CVD method, thermal CVD method, coating method, etc. Specially, those by atmospheric pressure plasma polymerization method as described in 2004-68143 are particularly preferable.
  • the hole transporting material has any of hole injection or transport and electron barrier properties, and may be either organic or inorganic.
  • triazole derivatives oxadiazole derivatives, imidazole derivatives, polyarylalkane derivatives, pyrazoline derivatives and pyrazolone derivatives, vinylene diamine derivatives, arylamine derivatives, amino-substituted chalcone derivatives, oxazole derivatives, styrylanthracene derivatives, fluorenone Derivatives, hydrazone derivatives, stilbene derivatives, silazane derivatives, aniline copolymers, conductive polymer oligomers, particularly thiophene oligomers, and the like.
  • a borfilin compound an aromatic tertiary amine compound and a styrylamine compound, particularly an aromatic tertiary amine compound.
  • aromatic tertiary amine compounds and styrylamine compounds include N, N, N ′, N ′ —tetraphenyl-1,4′—diaminophenyl; N, N′—diphenyl-1, N, N ′ —bis.
  • a polymer material in which these materials are introduced into a polymer chain or these materials are used as a polymer main chain can also be used.
  • Inorganic compounds such as P-type-Si and p-type-SiC can also be used as hole injection materials and hole transport materials.
  • the thickness of the hole transport layer is not particularly limited, but is usually about 5 nm to 5 zm, preferably 5 to 200 nm.
  • the hole transport layer may have a single layer structure composed of one or more of the above materials. It is also possible to use a hole transport layer having a high p property doped with impurities. Examples thereof include those described in JP-A-41-297076, JP-A-2000-196140, JP-A-2001-102175, J. Appl. Phys., 95, 5773 (2004), etc. It is done. It is preferable to use such a high p property hole transport layer because an organic EL device with lower power consumption can be produced.
  • Examples of the layer provided adjacent to the light emitting layer include a blocking layer.
  • Examples of the blocking layer include a hole blocking layer and an electron blocking layer.
  • the blocking layer is provided as necessary in addition to the basic constituent layer of the organic compound thin film.
  • the hole blocking layer has a function of an electron transport layer in a broad sense, and is made of a hole blocking material that has a function of transporting electrons but has a very small ability to transport holes.
  • the structure of the electron transport layer described later can be used as a hole blocking layer according to the present invention, if necessary, and the hole blocking layer is preferably provided adjacent to the light emitting layer.
  • the light emitting layer has a plurality of light emitting layers having different emission colors
  • the light emitting layer whose emission maximum wavelength is the shortest is preferably closest to the anode among all the light emitting layers, In such a case, it is preferable to provide an additional hole blocking layer between the shortest wave layer and the light emitting layer next to the anode next to the anode.
  • 50% by mass or more of the compound contained in the hole blocking layer provided at the position has an ionization potential of 0.3 eV or more larger than the host compound of the shortest wave emitting layer.
  • the ionization potential is defined by the energy required to emit electrons at the H ⁇ M ⁇ (highest occupied molecular orbital) level of a compound to the vacuum level.
  • the ionization potential can be obtained by the method shown below. I can do it.
  • the ionization potential can be obtained by rounding off the second decimal place of the value (eV unit conversion value) calculated by optimizing the structure using B3LYP / 6_31G *.
  • the reason why this calculated value is effective is that there is a high correlation between the calculated value obtained by this method and the experimental value.
  • the ionization potential can also be obtained by a direct measurement method using photoelectron spectroscopy.
  • a direct measurement method using photoelectron spectroscopy For example, a low-energy electron spectrometer “Model AC-lj” manufactured by Riken Keiki Co., Ltd. or a method known as ultraviolet photoelectron spectroscopy can be preferably used.
  • the electron blocking layer has a function of a hole transport layer in a broad sense, and is made of a material having a function of transporting holes and a very small ability to transport electrons, and transports holes.
  • the probability of recombination of electrons and holes can be improved.
  • the structure of the positive hole transport layer mentioned later can be used as an electron blocking layer as needed.
  • the film thickness of the hole blocking layer and the electron transporting layer according to the present invention is preferably 3 nm to:! OOnm, and more preferably 5 nm to 30 nm.
  • a known host compound and a known phosphorescent compound are used in order to increase the light emission efficiency of the light emitting layer.
  • the host compound is a compound contained in the light-emitting layer, the mass ratio of which is 20% or more, and the amount of phosphorescent phosphorescence at room temperature (25 ° C).
  • a child yield is defined as a compound of less than 0.1.
  • the phosphorescence quantum yield is less than 0.01.
  • a plurality of host compounds may be used in combination. By using multiple types of host compounds, it is possible to adjust the charge transfer, and the organic EL layer can be made highly efficient.
  • these host compounds compounds having a hole transporting ability and an electron transporting ability, preventing the emission of longer wavelengths, and having a high Tg (glass transition temperature) are preferable.
  • the following materials are disclosed in Japanese Laid-Open Patent Publication Nos. 2001-257076, 2002-308855, 2001-313179, 2002-319491, 2001. — No. 357977, No. 2002-334786, No. 2002-8860, No. 2002-334787, No. 2002-15871, No. 2002-334788, No. 2002-43056, No.
  • the light-emitting layer has a plurality of light-emitting layers, it is easy to obtain uniform film properties over the entire light-emitting layer that 50% by mass or more of the host compound in each layer is the same compound. Furthermore, it is more preferable that the phosphorescence energy of the host compound is 2.9 eV or more because it is advantageous for efficiently suppressing energy transfer from the dopant and obtaining high luminance. preferable.
  • Phosphorescence emission energy refers to the peak energy of the 0-0 band of phosphorescence emission measured by measuring the photoluminescence of the deposited film of lOOnm on the substrate with the host compound.
  • the host compound is an organic EL element using the organic EL layer of the present invention
  • the organic EL element Considering the deterioration of the child over time (decrease in brightness, deterioration of film properties), market needs as a light source, etc.
  • the phosphorescence energy is 2.9 eV or more and Tg is 90 ° C or more.
  • the phosphorescent energy is 2.9 eV or more and Tg is 90 ° C or more.
  • Tg is more preferably 100 ° C or higher.
  • a phosphorescent compound is a compound in which light emission from an excited triplet is observed, and is a compound that emits phosphorescence at room temperature (25 ° C). A compound having a rate of 0.01 or more at 25 ° C. When used in combination with the host compound described above, an organic EL device with higher luminous efficiency can be obtained.
  • the phosphorescent compound according to the present invention preferably has a phosphorescence quantum yield of 0.1 or more.
  • the above phosphorescence quantum yield can be measured by the method described on page 398 (1992 edition, Maruzen) of Spectroscopic II, 4th edition, Experimental Chemistry Course 7.
  • the phosphorescence quantum yield in a solution can be measured using various solvents, but the phosphorescent compound used in the present invention can be obtained if the phosphorescence quantum yield is achieved in any solvent. ,.
  • the light emission of a phosphorescent compound can be described in two types in principle.
  • One is the recombination of the carriers on the host compound to which carriers are transported, resulting in the generation of an excited state of the host compound. When this energy is transferred to the phosphorescent compound, light is emitted from the phosphorescent compound.
  • the other is the energy transfer type, and the other is that the phosphorescent compound becomes a carrier trap, which is on the phosphorescent compound.
  • the carrier trap type in which carrier recombination occurs and light emission from the phosphorescent compound is obtained, but in either case, the excited state energy of the phosphorescent compound is the excitation of the phosphine H compound. The condition is that it is lower than the energy of the state.
  • the phosphorescent compound can be appropriately selected from known compounds used for the light emitting layer of the organic EL layer.
  • the phosphorescent compound is preferably a complex compound containing a group 8-10 metal in the periodic table of elements, more preferably an iridium compound, an osmium compound, or a platinum compound (platinum complex compound). Of these, rare earth complexes, and most preferred are iridium compounds.
  • the phosphorescent maximum wavelength of the phosphorescent compound is not particularly limited, and in principle, a central metal, a ligand, a substituent of the ligand, and the like are selected. so The emission wavelength obtained can be changed.
  • the external extraction efficiency at room temperature of light emission of the organic EL element using the organic EL layer according to the present invention is 1. It is preferable that the ratio is 0 or more, more preferably 5% or more.
  • the external extraction quantum efficiency (%) the number of photons emitted outside the organic EL element / the number of electrons sent to the organic EL element XI 00.
  • a hue improvement filter such as a color filter may be used in combination, or a color conversion filter that converts the emission color from the organic EL element into multiple colors using a phosphor may be used in combination.
  • a color conversion filter When a color conversion filter is used, the maximum light emission of the organic EL element is preferably 480 nm or less.
  • an electron transport material also serving as a hole blocking material
  • any material that has a function of transmitting electrons injected from the cathode to the light emitting layer is acceptable. It is possible to select and use any of the known compounds of the known compounds, such as nitro-substituted fluorene derivatives, diphenylquinone derivatives, thiopyran dioxide derivatives, carbodiimides, fluorenylidenemethane derivatives, anthraquinodis. Examples include methane and anthrone derivatives, oxadiazole derivatives, and the like.
  • a thiadiazole derivative in which an oxygen atom of the oxaziazole ring is substituted with a sulfur atom, and a quinoxaline derivative having a quinoxaline ring known as an electron withdrawing group can also be used as an electron transport material.
  • a polymer material in which these materials are introduced into a polymer chain or these materials are used as a polymer main chain can also be used.
  • Metal complexes of 8_quinolinol derivatives such as tris (8-quinolinol) aluminum (Alq), tris (5,7-dichloro-1-8-quinolinol) aluminum, tris (5,7-jib mouthpiece) _8_quinolinol) aluminum, tris (2-methyl _8_quinolinol) aluminum, tris (5-methyl_8_quinolinol) aluminum, bis (8-quinolinol) zinc (Znq) etc., and the central metal of these metal complexes Placed on In, Mg, Cu, Ca, Sn, Ga or Pb
  • Alternative metal complexes can also be used as electron transport materials.
  • metal-free or metal phthalocyanine or those having an end substituted with an alkyl group or a sulfonic acid group can be preferably used as the electron transport material.
  • Distyrylpyrazine derivatives can also be used as electron transport materials, and n-type-Si, n-type-SiC and other inorganic semiconductors should be used as electron-transport materials as well as hole injection layers and hole-transport layers. Force S is possible.
  • limiting in particular about the film thickness of an electron carrying layer Usually, about 5 nm-5 zm, Preferably it is 5-200 nm.
  • the electron transport layer may have a single layer structure composed of one or more of the above materials.
  • an electron transport layer having a high n property doped with impurities can be used.
  • examples thereof include Japanese Patent Application Laid-Open No. 4-297076, Japanese Patent Application Laid-Open No. 10-270172, Japanese Patent Application Laid-Open No. 2000-196140, Japanese Patent Application Laid-Open No. 2001-102175, J. Appl. Phys., 95, 5773 (2004). ) Etc. are mentioned. It is preferable to use such an n-type electron transport layer because a device with lower power consumption can be manufactured.
  • a transparent gas barrier layer with a thickness of about 90 nm was formed by atmospheric pressure plasma discharge treatment.
  • the water vapor transmission rate by a method based on JlSk-7129B it was 10 ⁇ 3 g / m 2 / day or less.
  • the oxygen transmission rate by a method based on JlSk-7126B it was 10 ⁇ 3 g / m 2 / day or less.
  • first electrode layer On the formed barrier layer, a 120 nm thick ITO (indium tin oxide) was formed using a plasma ion plating apparatus. Thereafter, a pattern having a width of 110 / im and a spacing of 34 ⁇ m was formed through a photolithography process.
  • ITO indium tin oxide
  • the host material polyvinyl carbazole (PVK) was prepared by dissolving 5% by mass of the dopant material Ir (ppy) 3 in 1,2-dichloroethane to form a 1% solution as a coating solution for forming an organic compound layer.
  • Alq was dissolved in 1,2-dichloroethane to prepare a 0.5% by mass solution as a coating solution for forming an electron transport layer.
  • Holes are formed on the first electrode layer of the belt-like flexible support having the gas barrier layer and the first electrode layer in this order on the prepared winding core using the manufacturing apparatus shown in FIG. Change the environmental conditions (dew point temperature, cleanliness) until the transport layer, light-emitting layer, and electron transport layer are formed as shown in Table 1 to form an organic EL layer, heat treatment, charge removal, and room temperature After cooling to the same temperature as in Example 1, sample rolls Nos. 101 to 107 were formed as a wound roll shape on the core. The cleanliness is the value measured according to JISB 9920, and the cleanliness was changed by changing the filter.
  • the hole transport layer was formed by applying and drying the following hole transport layer forming coating solution by a wet coating method using an etatrusion coating machine, followed by heat treatment.
  • the light-emitting layer is aligned with the wet pattern coating device according to the alignment mark, and is used for forming the light-emitting layer according to the pattern of the first electrode formed as shown in Fig. 6 while being held by the holding means.
  • the coating liquid was formed with a wet pattern coating apparatus.
  • the following electron transport layer forming coating solution was applied and dried by a wet coating method using an etatrusion coater, followed by heat treatment.
  • the cleaning surface modification treatment of the belt-shaped flexible support was performed using a low-pressure mercury lamp with a wavelength of 184.9 nm and an irradiation intensity of 15 mW / cm 2 The distance was 10 mm.
  • the charge removal treatment was performed using a static eliminator with weak X-rays.
  • the coating solution for forming the hole transport layer was applied so that the thickness after drying was 50 nm.
  • the coating solution for forming the light emitting layer was applied so that the thickness after drying was lOOnm.
  • the coating solution for forming the electron transport layer was coated so that the thickness after drying was 30 nm.
  • the transport speed was 2m / min.
  • the coating temperature of the coating solution for forming the hole transport layer, the coating solution for forming the light emitting layer, and the coating solution for forming the electron transport layer is 25 ° C, and the other ambient temperature is 25 ° C except for the drying device and heat treatment device. Performed under atmospheric pressure conditions.
  • the light emitting layer drying section and the heat treatment section shown in Fig. 3 are used.
  • the height from the slit nozzle type discharge port to the film forming surface is 100 m. m
  • a heat treatment was subsequently performed at a temperature of 220 ° C. in the heat treatment section to form a light emitting layer.
  • the drying unit and the heat treatment apparatus having the same structure as the light emitting layer drying unit and the heat treatment unit shown in Fig. 3 are used.
  • an electron transport layer was formed by subsequently performing a heat treatment at a temperature of 200 ° C. in the heat treatment section.
  • the discharge wind speed was measured with a hot air anemometer model 6113 manufactured by Kanomax Co., Ltd., and the wind speed distribution in the width direction was calculated by the following formula.
  • Wind speed distribution (maximum wind speed-minimum wind speed) / average wind speed X I 00
  • a LiF layer (electron injection layer) with a thickness of 0.5 nm is vapor-deposited under a vacuum of 5 X 10 _4 Pa so that it is perpendicular to the first electrode through the mask.
  • a sealing layer is subsequently formed by vapor deposition, cooled to room temperature, A winding roll was formed on the winding core.
  • Table 1 shows the results of visually confirming the non-light-emitting failure on sample Nos. 101 to 107 manufactured in this state and evaluating according to the following evaluation rank.
  • the prepared sample was stored at a constant temperature of 80 ° C for 1 week, and when it was driven at a constant current of 2.5 mA / cm 2 , it was visually checked for the presence of no light emission. Evaluation rank of non-luminous failure ⁇ : Non-luminous failure is not confirmed,
  • sample No. 101 it is presumed that a non-luminous failure has occurred due to the amount of moisture contained in the sample, and in the case of sample No. 104, due to adhering foreign matter. The effectiveness of the present invention was confirmed.
  • Samples Nos. 201 to 206 were used under the same conditions except that the conditions under which sample No. 104 produced in Example 1 was stored were changed as shown in Table 2 and processed. The storage period was 5 days.
  • the lifetime of the light emitting layer attached to the fabricated sample Nos. 201 to 206 is the time required for the luminance to be half of the initial luminance when driven at a constant current of 2.5 mA / cm 2 (half time)
  • Table 2 shows the results of the evaluation using as a life index. Incidentally, the lifetime (relative value) indicates a relative value when storage conditions was 100 life time of 1 X 10- 5 Pa.

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Abstract

La présente invention concerne un procédé pour former une couche EL organique pour former un élément EL organique de qualité élevée avec une productivité élevée sans augmenter le coût. Le procédé pour former la couche EL organique d’un élément EL organique en utilisant un système de fabrication comportant une partie d’alimentation, une partie de revêtement de motif/séchage et une partie de récupération, est caractérisé en ce que la partie d’alimentation est alimentée avec un support A souple de bande enroulée sur lequel une couche d’anode comprenant une première électrode est formée, une première partie d’accumulateur et une seconde partie d’accumulateur sont formées respectivement à l’avant et à l’arrière de la partie de revêtement de motif/séchage qui présente au moins une unité consistant en une partie de revêtement de motif et une partie de séchage de la couche EL organique, une couche EL organique est formée sur la couche d’anode sous forme d’un support B souple de bande au niveau de la partie de revêtement de motif/séchage puis enroulée au niveau de la partie de récupération.
PCT/JP2006/304063 2005-03-23 2006-03-03 Procede pour former une couche el organique WO2006100889A1 (fr)

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