WO2011093120A1 - Élément électroluminescent organique et dispositif d'éclairage - Google Patents

Élément électroluminescent organique et dispositif d'éclairage Download PDF

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Publication number
WO2011093120A1
WO2011093120A1 PCT/JP2011/050251 JP2011050251W WO2011093120A1 WO 2011093120 A1 WO2011093120 A1 WO 2011093120A1 JP 2011050251 W JP2011050251 W JP 2011050251W WO 2011093120 A1 WO2011093120 A1 WO 2011093120A1
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Prior art keywords
layer
light
organic
light emitting
resin
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PCT/JP2011/050251
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English (en)
Japanese (ja)
Inventor
恭雄 當間
邦雅 檜山
健夫 荒井
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コニカミノルタホールディングス株式会社
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Priority to JP2011551788A priority Critical patent/JP5655795B2/ja
Publication of WO2011093120A1 publication Critical patent/WO2011093120A1/fr

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/12—Light sources with substantially two-dimensional radiating surfaces
    • H05B33/22—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of auxiliary dielectric or reflective layers
    • 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
    • H10K59/875—Arrangements for extracting light from the devices
    • H10K59/877—Arrangements for extracting light from the devices comprising scattering means

Definitions

  • the present invention relates to an organic electroluminescence element and a lighting device using the element.
  • ELD electroluminescence display
  • an inorganic electroluminescent element and an organic electroluminescent element are mentioned.
  • Inorganic electroluminescent elements have been used as planar light sources, but an alternating high voltage is required to drive the light emitting elements.
  • the organic electroluminescence device has a configuration in which a light emitting layer containing a compound that emits light (an organic compound thin film containing a fluorescent organic compound) is sandwiched between a cathode and an anode, and injects electrons and holes into the light emitting layer, It is an element that emits light by utilizing light emission (fluorescence / phosphorescence) when excitons (excitons) are generated by recombination and the excitons are deactivated.
  • a transparent conductive layer such as ITO is used for at least one of the electrodes sandwiching the organic compound thin film, and the transparent conductive layer is further supported by a transparent substrate such as glass.
  • Organic EL devices can emit light at a low voltage of several volts to several tens of volts, are self-luminous, have a wide viewing angle, high visibility, and are thin-film, completely solid-state devices that save space. It is attracting attention from the viewpoint of portability.
  • the organic electroluminescence device has a problem that the light extraction efficiency (the ratio of the energy coming out of the substrate to the emitted energy) is low. That is, the light emission of the light emitting layer is not directional and dissipates in all directions, so there is a large loss when guiding light forward from the light emitting layer, and there is a problem that the display screen becomes dark due to insufficient light intensity. .
  • the light emitted from the light emitting layer uses only the light emitted in the forward direction, but the light extraction efficiency (light emission efficiency) in the forward direction derived from multiple reflection based on classical optics is 1 / 2n 2 . It can be approximated, and is almost determined by the refractive index n of the light emitting layer. If the refractive index of the light emitting layer is about 1.7, the light emission efficiency from the organic EL part is simply about 20%. The remaining light propagates in the area direction of the light emitting layer (spray in the lateral direction) or disappears at the metal electrode facing the transparent electrode with the light emitting layer interposed therebetween (absorption in the backward direction).
  • a method of forming a layer containing scattering particles and a low refractive index layer in a matrix having the same refractive index as that of the transparent electrode between the transparent electrode layer and the transparent body, and improving the light extraction efficiency by the light scattering effect For example, see Patent Document 1).
  • This is a method using an inorganic compound such as titania as a high refractive index matrix, and there is no description of a light scattering layer made of a resin containing oxide nanoparticles and a light scattering filler in a resin matrix.
  • a method in which a selective reflection layer is formed on the light emission side and a change in color is suppressed by reflection of light of a specific wavelength (see, for example, Patent Document 3).
  • this method improves the change in color depending on the viewing angle, but the luminance is reduced by the selective reflection layer, and this is used for an organic light emitting layer having different light distribution luminance characteristics depending on the emission wavelength. In such a case, the disadvantage that the brightness at a specific angle is high cannot be improved.
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide an electroluminescent device that greatly improves light extraction efficiency and has small color change and luminance variation depending on an observation angle, and the device. It is in providing the used illuminating device.
  • the inventors of the present invention have an average particle size of 0.1 ⁇ m or more and 0.7 ⁇ m in an organic-inorganic composite material having a refractive index of 1.65 or more and 1.80 or less (hereinafter referred to as composite material).
  • composite material organic-inorganic composite material having a refractive index of 1.65 or more and 1.80 or less.
  • an organic electroluminescence device in which a transparent conductive layer, an organic electroluminescence layer having an electron transport layer, and a counter electrode are sequentially laminated on a transparent substrate, the transparent substrate is an oxide having an average particle diameter of 1 nm to 20 nm on at least one surface.
  • An organic-inorganic composite material composed of nanoparticles and a resin material precursor, and having a refractive index of 1.65 to 1.80 after curing, has an average particle size of 0.1 ⁇ m to 0 ⁇ m.
  • an organic electroluminescence element that is excellent for white illumination, with significantly improved light extraction efficiency compared to the prior art, small changes in color depending on the observation angle, and variations in luminance.
  • Embodiments of an organic electroluminescence element also referred to as an organic EL element
  • a lighting device of the present invention will be described in detail below, but the contents described below are representative examples of the embodiment of the present invention. As long as the gist is not exceeded, it is not limited to these contents.
  • the organic EL device of the present invention is a composite having an oxide nanoparticle having an average particle diameter of 1 nm or more and 20 nm or less and a resin on at least one surface of a transparent substrate, and having a refractive index of 1.65 or more and 1.80 or less.
  • the material has a light scattering layer containing a light scattering filler having an average particle size of 0.1 ⁇ m or more and 0.7 ⁇ m or less, and an electron transport layer having a film thickness of 40 nm or more and 200 nm or less. To do.
  • the transparent substrate is not particularly limited as long as it has high light transmittance.
  • a glass substrate, a resin substrate, a resin film, etc. are preferably mentioned in terms of excellent hardness as a base material and ease of film formation on the surface, but from the viewpoint of lightness and flexibility It is preferable to use a transparent resin film.
  • the transparent resin film that can be preferably used as the transparent substrate in the present invention is not particularly limited, and the material, shape, structure, thickness and the like can be appropriately selected from known ones.
  • polyester resin films such as polyethylene terephthalate (PET), polyethylene naphthalate, modified polyester, polyethylene (PE) resin films, polypropylene (PP) resin films, polystyrene resin films, polyolefin resin films such as cyclic olefin resins, Vinyl resin films such as polyvinyl chloride and polyvinylidene chloride, polyether ether ketone (PEEK) resin film, polysulfone (PSF) resin film, polyether sulfone (PES) resin film, polycarbonate (PC) resin film, polyamide resin Examples include films, polyimide resin films, acrylic resin films, triacetyl cellulose (TAC) resin films, and the like, but wavelengths in the visible range (380 to 78).
  • TAC triacetyl cellulose
  • the resin film transmittance of 80% or more in nm can be preferably applied to a transparent resin film according to the present invention.
  • a transparent resin film according to the present invention is preferably a biaxially stretched polyethylene terephthalate film, a biaxially stretched polyethylene naphthalate film, a polyethersulfone film, or a polycarbonate film, and biaxially stretched. More preferred are polyethylene terephthalate films and biaxially stretched polyethylene naphthalate films.
  • the refractive index of the transparent resin film is preferably 1.50 or more, more preferably 1.60 or more and 1.80 or less.
  • the thickness of the transparent resin film is preferably 50 ⁇ m or more and 250 ⁇ m or less, and more preferably 75 ⁇ m or more and 200 ⁇ m or less.
  • the transparent substrate used in the present invention can be subjected to a surface treatment or an easy adhesion layer in order to ensure the wettability and adhesion of the coating solution.
  • a surface treatment or an easy adhesion layer in order to ensure the wettability and adhesion of the coating solution.
  • a conventionally well-known technique can be used about a surface treatment or an easily bonding layer.
  • the surface treatment includes surface activation treatment such as corona discharge treatment, flame treatment, ultraviolet treatment, high frequency treatment, glow discharge treatment, active plasma treatment, and laser treatment.
  • examples of the easy adhesion layer include polyester, polyamide, polyurethane, vinyl copolymer, butadiene copolymer, acrylic copolymer, vinylidene copolymer, epoxy copolymer and the like.
  • the easy adhesion layer may be a single layer, but may be composed of two or more layers in order to improve adhesion.
  • the light scattering layer preferably has a small difference in refractive index from the transparent substrate, preferably a composite material having a refractive index of 1.65 or more and 1.80 or less, and more preferably a refractive index of 1.65 or more and 1.75. The following is more preferable.
  • the composite material referred to in the present invention refers to a composite of a resin, which is an organic material, and an inorganic material such as oxide nanoparticles.
  • a resin which is an organic material
  • an inorganic material such as oxide nanoparticles.
  • Hybrid materials are preferably used.
  • the resin used for the composite material according to the present invention is not particularly limited, but it is preferable to use a curable resin in view of cost and convenience when forming the layer.
  • the curable resin used in the present invention can be cured by any of ultraviolet and electron beam irradiation or heat treatment, and is mixed with oxide nanoparticles in an uncured state and then cured.
  • it can be used without particular limitation, and examples thereof include silicone resins, epoxy resins, vinyl ester resins, acrylic resins, allyl ester resins, and the like.
  • the curable resin may be an actinic ray curable resin that is cured by being irradiated with ultraviolet rays or electron beams, or may be a thermosetting resin that is cured by heat treatment.
  • Such types of resins can be preferably used, and acrylic resins can be particularly preferably used.
  • ⁇ Acrylic resin examples include monofunctional monomers such as ethyl (meth) acrylate, ethylhexyl (meth) acrylate, styrene, methylstyrene, fluorene acrylate, and N-vinylpyrrolidone.
  • Examples include polyfunctional monomers such as acrylate.
  • the oxide nanoparticles used in the composite material of the present invention are not particularly limited as long as the refractive index of the composite material can be adjusted to a target value, and absorption, emission, fluorescence, etc. occur in the wavelength region to be used. It is preferable to select and use those not present.
  • the composite material formed in the organic EL element has a high light extraction effect due to its high transparency. Therefore, the oxide nanoparticles used in the present invention are 1 nm or more and 20 nm or less. Preferably there is. When the average particle size is less than 1 nm, it is difficult to disperse the particles and the desired performance may not be obtained.
  • the average particle diameter when the average particle diameter exceeds 20 nm, the resulting composite material layer may become turbid depending on the difference in refractive index, resulting in a decrease in transparency, and the oxide nanoparticles acting as an optical scatterer. Therefore, the average particle diameter is preferably 20 nm or less because the contribution to the adjustment of the target refractive index is small.
  • the average particle diameter refers to the volume average value of the diameter (sphere converted particle diameter) when each particle is converted into a sphere having the same volume.
  • the refractive index of the oxide nanoparticles used in the present invention is preferably higher than that of the resin, and the refractive index is preferably 1.6 or more and 2.5 or less.
  • the elements constituting the oxide are Li, Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb. 1 selected from the group consisting of Sr, Y, Nb, Zr, Mo, Ag, Cd, In, Sn, Sb, Cs, Ba, La, Ta, Hf, W, Ir, Tl, Pb, Bi and rare earth metals
  • Metal oxide nanoparticles that are seeds or two or more metals can be used. Specifically, for example, titanium oxide (titania), zinc oxide, aluminum oxide (alumina), zirconium oxide, hafnium oxide, niobium oxide.
  • rare earth oxides can also be used as the metal oxide nanoparticles, specifically, scandium oxide, yttrium oxide, lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, Examples also include terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, and lutetium oxide.
  • titanium oxide and zirconium oxide can be preferably used.
  • oxide nanoparticles As a method for preparing oxide nanoparticles, it is possible to obtain fine particles by spraying and firing the raw material of oxide nanoparticles in a gas phase. Furthermore, a method of preparing particles using plasma, a method of ablating raw material solids with a laser or the like to make fine particles, a method of oxidizing evaporated metal gas to prepare fine particles, and the like can be suitably used. Further, as a method for preparing in the liquid phase, it is possible to prepare a dispersion of oxide nanoparticles dispersed almost as primary particles by using a sol-gel method using an alkoxide or chloride solution as a raw material. Alternatively, it is possible to obtain a dispersion having a uniform particle size by using a reaction crystallization method utilizing a decrease in solubility.
  • the filling rate to resin When filling an oxide nanoparticle of 20 nm or less into resin, when ensuring moldability (fluidity, there is no crack), it is preferable that it is 30 volume% or less. .
  • a certain filling rate is required, so 5 volume% or more, further 10 volume% or more is preferable.
  • the volume fraction of the oxide nanoparticles here is expressed by the formula (x / a) / when the specific gravity of the oxide nanoparticles is a, the content is x grams, and the total volume of the composite material produced is Y milliliters.
  • the content of oxide nanoparticles can be determined by observing a semiconductor crystal image with a transmission electron microscope (TEM) (information on the semiconductor crystal composition can also be obtained by local elemental analysis such as EDX) or given resin composition It can be calculated from the contained mass of a predetermined composition obtained by elemental analysis of ash contained in the product and the specific gravity of crystals of the composition.
  • TEM transmission electron microscope
  • the oxide nanoparticles are preferably subjected to a surface treatment in order to increase the affinity with the resin.
  • a surface treatment for the bonding between the necessary surface treating agent and the particle surface, the following introduction methods are conceivable, but not limited to them.
  • Silane coupling agent A condensation reaction or a hydrogen bond between a silanol group and a hydroxyl group on the particle surface is used.
  • Examples include vinylsilazane, trimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, trimethylalkoxysilane, dimethyldialkoxysilane, methyltrialkoxysilane, hexamethyldisilazane, and the like.
  • Trimethylmethoxysilane, dimethyldimethoxysilane, methyltrimethoxy Silane, hexamethyldisilazane and the like are preferably used.
  • Titanate, aluminate, and zirconate coupling agents are also applicable. Further, zircoaluminate, chromate, borate, stannate, isocyanate and the like can be used. A diketone coupling agent can also be used.
  • Resin-based surface treatment After introducing active species to the particle surface by the methods (1) to (3) above, a method of providing a polymer layer on the surface by graft polymerization, or adsorbing a pre-synthesized polymer dispersant to the particle surface , There is a method of combining. In order to provide a polymer layer more firmly on the particle surface, graft polymerization is preferred, and grafting at a high density is particularly preferred.
  • a resin containing fine particles (a molten state when a thermoplastic resin is used and an uncured state when a curable resin is used) is prepared.
  • a composite material turns into a desired layer by apply
  • a curable resin when used as the resin, it may be prepared by mixing the curable resin dissolved in an organic solvent and the fine particles according to the present invention, or in a monomer solution that is one of the raw materials of the curable resin. It may be prepared by adding and mixing the fine particles according to the present invention and then polymerizing them. Alternatively, it may be prepared by melting an oligomer in which a monomer is partially polymerized or a low molecular weight polymer, and adding and mixing the fine particles according to the present invention thereto.
  • organic solvent used herein examples include lower alcohols having about 1 to 4 carbon atoms, ketones such as acetone, methyl ethyl ketone and methyl isobutyl ketone, esters such as methyl acetate and ethyl acetate, hydrocarbons such as toluene and xylene, and the like. However, it is not particularly limited as long as it has a boiling point lower than that of the monomer and is compatible with these monomers.
  • a method of polymerizing after adding the fine particles according to the present invention to a monomer solution is preferable, and in particular, a highly viscous solution in which the monomer and the fine particles according to the present invention are mixed is given a share while cooling.
  • a highly viscous solution in which the monomer and the fine particles according to the present invention are mixed is given a share while cooling.
  • the method for adjusting the viscosity include adjustment of the particle diameter, surface state, and addition amount of the fine particles according to the present invention, addition of a solvent and a viscosity modifier, and the fine particles according to the present invention are surface-modified depending on the structure. Since it is easy, an optimal kneading state can be obtained.
  • the fine particles according to the present invention can be added in a powder or agglomerated state. Or it is also possible to add in the state disperse
  • the fine particles according to the present invention are preferably added in a surface-treated state.
  • a method such as an integral blend in which a surface treatment agent and fine particles are added at the same time to form a composite with a curable resin. Is possible.
  • the present invention provides a light-scattering filler having an average particle size of 0.1 ⁇ m or more and 0.7 ⁇ m or less in a composite material comprising oxide nanoparticles having a refractive index of 1.65 or more and 1.80 or less and a resin as a light scattering layer.
  • One of the characteristics is to contain.
  • a light-scattering filler is a filler that has the function of multiple scattering of light that has entered the light-scattering layer.
  • the light-scattering filler is particularly effective for light having different light distribution luminance characteristics depending on the emission wavelength.
  • the particle size is preferably 0.1 ⁇ m or more and 0.7 ⁇ m or less in view of general scattering. If it is less than 0.1 ⁇ m, the effect is small because the intensity of scattered light is low with respect to all wavelengths, and if it exceeds 0.7 ⁇ m, the scattering intensity increases with light of all wavelengths. The desired effect cannot be obtained because it cannot be utilized well.
  • the particle size of the light scattering filler is more preferably 0.2 ⁇ m or more and 0.5 ⁇ m or less.
  • the refractive index of the light scattering filler is preferably 0.01 or more so that the difference in refractive index from the composite material to be added is obtained, and is preferably 0.5 or less.
  • the refractive index difference with the composite material is 0.2 or more and 0.3 or less.
  • the light-scattering filler used in the present invention a known filler made of inorganic or polymer can be used.
  • inorganic compounds include silicon dioxide (silica), titanium dioxide, aluminum oxide, zirconium oxide, calcium carbonate, talc, clay, calcined kaolin, calcined calcium silicate, hydrated calcium silicate, aluminum silicate, magnesium silicate, And calcium phosphate.
  • the polymer include silicone resin, fluororesin, and acrylic resin.
  • the optical filler used in the present invention is preferably silica or acrylic resin from the viewpoint of the difference in refractive index from the composite material. Further, the addition amount of these light scattering fillers is preferably 1% by mass or more and 30% by mass or less, but may be adjusted according to the degree of light scattering.
  • the light scattering filler can be in any shape such as a sphere, needle shape, flat plate shape, etc., and further, the dispersibility in the resin can be improved by performing the same surface treatment as the above-mentioned inorganic nanoparticles. It is.
  • the film thickness of the light scattering layer of the present invention is preferably about 1 to 10 ⁇ m, more preferably 2 to 7 ⁇ m, as long as it can improve the light extraction efficiency by the light scattering filler and improve the angle dependency of chromaticity and luminance. preferable.
  • the light scattering layer of the present invention may be formed on at least one surface of the transparent substrate, and may be formed on the light incident side surface or the emission side surface with respect to the transparent substrate. It may be formed on both sides.
  • the light scattering layer is formed on both surfaces of the transparent substrate, it is preferable to appropriately adjust the addition amount of the light scattering filler so that the scattering intensity does not become too strong due to both light scattering layers.
  • a resin layer not containing a light scattering filler is formed on the opposite surface, and one surface is warped when handled as a transparent substrate. It is preferable not to cause so-called curling.
  • a layer having a function as a barrier coat layer or a hard coat layer can also be formed.
  • the resin layer not containing this light-scattering filler if the difference in refractive index with the transparent base material is large, deterioration of light extraction due to interface reflection occurs. Therefore, the refractive index is the same as or slightly higher than that of the transparent base material. Preferably it is low.
  • the light scattering layer of the present invention is formed on the surface on the light incident side with respect to the transparent substrate, a transparent conductive layer is formed thereon, so that a smoothing layer is formed on the light scattering layer. It is preferable to form.
  • the smoothing layer it is only necessary to obtain a smoothness that does not cause a short circuit when a transparent conductive layer or an organic light emitting layer is formed on the surface, and a general resin can be used. Therefore, it is preferable to use a matrix resin for the light scattering layer.
  • the light scattering layer used in the organic electroluminescence device of the present invention is formed on the transparent substrate by means such as coating.
  • a coating method it can coat by well-known methods, such as a gravure coater, a dip coater, a reverse coater, a wire bar coater, a die coater, and an inkjet method.
  • the light scattering layer can be produced by a method such as curing by ultraviolet rays and heat, film formation by drying, curing by chemical reaction, or the like.
  • a light source for curing by a photocuring reaction to form a cured film layer can be used without limitation as long as it is a light source that generates ultraviolet rays.
  • a low pressure mercury lamp, a medium pressure mercury lamp, a high pressure mercury lamp, an ultrahigh pressure mercury lamp, a carbon arc lamp, a metal halide lamp, a xenon lamp, or the like can be used.
  • the irradiation conditions vary depending on individual lamps, irradiation of active rays, usually 5 ⁇ 500mJ / cm 2, but preferably 5 ⁇ 150mJ / cm 2, particularly preferably 20 ⁇ 100mJ / cm 2.
  • One feature of the present invention is that an organic electroluminescence layer is formed on a transparent substrate having the light scattering layer having a high refractive index.
  • the organic electroluminescence layer as used herein refers to an anode buffer layer, a hole transport layer, a light emitting layer, a hole blocking layer, an electron transport layer, a cathode buffer layer, or a portion between a transparent conductive layer and a counter electrode. Refers to the layer formed.
  • the organic electroluminescence layer of the present invention varies depending on the constituent materials, its refractive index is usually about 1.7.
  • the film thickness of the organic electroluminescence layer is usually 0.05 ⁇ m or more and 0.5 ⁇ m or less, and preferably 0.1 ⁇ m or more and 0.2 ⁇ m or less in terms of light emission efficiency and stability.
  • the film thickness of the electron transport layer in the organic electroluminescence layer in the range of 40 nm or more and 200 nm or less in order to improve the light extraction efficiency.
  • the light emission luminance characteristics in the light emitting layer are changed by changing the thickness of the electron transport layer in the organic electroluminescence layer.
  • the emission luminance of each wavelength is adjusted by adjusting the film thickness of the electron transport layer,
  • the luminance of the emitted light can be changed according to the outgoing angle.
  • the luminance ratio in an appropriate angle direction from the normal direction of the substrate is preferably larger in blue than in red or green, and in order to obtain such light distribution luminance characteristics, the film of the electron transport layer is used.
  • the thickness is preferably 40 nm or more and 200 nm or less, and particularly preferably 50 nm or more and 100 nm or less.
  • the thickness of the electron transport layer is less than 40 nm, the light distribution of each color becomes uniform, and the extraction efficiency of blue light having a particularly low emission luminance is lowered, which is not preferable.
  • the thickness of the electron transport layer exceeds 200 nm, the light distribution of each wavelength is made uniform, and the luminous efficiency is lowered due to the increase in the distance between the transparent conductive layer and the light emitting point. It is not preferable.
  • the luminance or chromaticity of the emitted light varies depending on the angle at which it is observed. Can be confirmed.
  • the transparent conductive layer of the present invention refers to a layer made of a transparent and conductive compound and acting as an electrode.
  • the transparent conductive layer has a refractive index of 1.8 or more and 2.1 or less when a metal oxide material such as ITO is used by vapor deposition or sputtering.
  • the film thickness t2 of the transparent conductive layer is 0.05 ⁇ m or more and 0.15 ⁇ m or less and is formed by coating using metal nanowires or the like, the refractive index is 1.6 or more and 1.8 or less, and the film thickness t2 is Generally, it is 0.1 ⁇ m or more and 1 ⁇ m or less.
  • the refractive index of the transparent conductive layer is preferably close to 1.7. Therefore, the transparent conductive layer of the present invention is preferably formed by applying metal nanowires such as silver nanowires together with a conductive polymer material, and preferably has a refractive index of 1.6 or more and 1.8 or less.
  • the film thickness is preferably 0.1 ⁇ m or more and 0.5 ⁇ m or less.
  • a commonly used method can be used as a method for measuring the refractive index.
  • it can be obtained from the measurement result of the spectral reflectance of a spectrophotometer (such as U-4000 type manufactured by Hitachi, Ltd.) for a sample in which each layer is coated alone. After roughening the back surface, light absorption treatment is performed with a black spray to prevent light reflection on the back surface, and the reflectance in the visible light region (400 to 700 nm) is measured under the condition of regular reflection at 5 degrees. Can be obtained.
  • a commonly used method can be used as a method of measuring the film thickness of each layer constituting the organic EL element.
  • the cross section of the organic EL element produced by laminating each layer can be obtained by photographing with a scanning electron microscope and measuring the film thickness.
  • Transparent conductive layer As the transparent conductive layer in the organic EL device of the present invention, a material having a work function (4 eV or more) of a metal, an alloy, an electrically conductive compound and a mixture thereof as an electrode material for forming the transparent conductive layer is preferably used.
  • electrode substances include metals such as Au, and conductive light-transmitting materials such as CuI, indium tin oxide (ITO), SnO 2 , and ZnO.
  • a material such as IDIXO (In 2 O 3 —ZnO) that can form an amorphous light-transmitting conductive film may be used.
  • the transparent conductive layer is preferably used as an anode.
  • 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 photolithography method, or when the pattern accuracy is not required (about 100 ⁇ m or more) ), A pattern may be formed through a mask having a desired shape when the electrode material is deposited or sputtered. Or when using the substance which can be apply
  • the sheet resistance as the anode is preferably several hundred ⁇ / ⁇ or less. Further, although the film thickness depends on the material, it is usually selected in the range of 10 to 1000 nm, preferably 50 to 200 nm.
  • the transparent conductive layer can be used in combination with other resins having a relatively low refractive index while having high conductivity, and contains metal nanowires that can be expected to improve light extraction efficiency due to the light scattering effect. It is preferable. Furthermore, since the strength of the transparent conductive layer is increased by the network structure of the metal nanowire and the durability of the organic EL element is improved, it is preferable to use the metal nanowire for the transparent conductive layer.
  • the average length is preferably 3 ⁇ m or more. It is preferably 3 to 500 ⁇ m, particularly preferably 3 to 300 ⁇ m. In addition, the relative standard deviation of the length is preferably 40% or less. Moreover, it is preferable that an average diameter is small from a transparency viewpoint, On the other hand, the larger one is preferable from an electroconductive viewpoint.
  • the average diameter of the metal nanowire is preferably 10 to 300 nm, and more preferably 30 to 200 nm. In addition, the relative standard deviation of the diameter is preferably 20% or less.
  • a metal composition of the metal nanowire which concerns on this invention, although it can comprise from the 1 type or several metal of a noble metal element and a base metal element, noble metals (for example, gold, platinum, silver, palladium, rhodium, (Iridium, ruthenium, osmium, etc.) and at least one metal belonging to the group consisting of iron, cobalt, copper, and tin is preferable, and at least silver is more preferable from the viewpoint of conductivity.
  • noble metals for example, gold, platinum, silver, palladium, rhodium, (Iridium, ruthenium, osmium, etc.
  • at least one metal belonging to the group consisting of iron, cobalt, copper, and tin is preferable, and at least silver is more preferable from the viewpoint of conductivity.
  • the metal nanowire according to the present invention includes two or more kinds of metal elements, for example, the metal composition may be different between the inside and the surface of the metal nanowire, or the entire metal nanowire has the same metal composition. May be.
  • the metal nanowires come into contact with each other to form a three-dimensional conductive network, exhibiting high conductivity, and allowing light to pass through the window of the conductive network where no metal nanowire exists.
  • the light from the organic light emitting layer can be efficiently extracted by the scattering effect of the metal nanowires. If the metal nanowire is installed in the electrode part on the side close to the organic light emitting layer part, this scattering effect can be used more effectively, and this is a more preferable embodiment.
  • highly conductive electrodes can be completed by coating. Therefore, even if unevenness due to particles exists on the surface of the composite material layer, the unevenness can be relaxed, and the possibility of damaging the light emitting layer can be eliminated.
  • the refractive index of the transparent conductive layer is preferably 1.5 or more and 2.0 or less, more preferably 1.6 or more and 1.9 or less.
  • the present invention by optimizing the balance of the refractive index and thickness of the transparent conductive layer, organic electroluminescence layer, and transparent resin film, not only the conventionally known light extraction efficiency is improved.
  • the film physical properties of the organic electroluminescence device having a fine film structure can be greatly improved.
  • Organic electroluminescence device The preferable specific example of the layer structure of an organic electroluminescent element is shown below.
  • the light emitting layer preferably contains at least two kinds of light emitting materials having different emission colors, and a single layer or a light emitting layer comprising a plurality of light emitting layers A unit may be formed.
  • the hole transport layer also includes a hole injection layer and an electron blocking layer.
  • the light emitting layer according to the present invention is a layer that emits light by recombination of electrons and holes injected from the electrode, the electron transport layer, or the hole transport layer, and the light emitting portion is in the layer of the light emitting layer. May be the interface between the light emitting layer and the adjacent layer.
  • the structure of the light emitting layer according to the present invention is not particularly limited as long as the contained light emitting material satisfies the above requirements.
  • the total thickness of the light emitting layers is preferably in the range of 1 to 100 nm, and more preferably 30 nm or less because a lower driving voltage can be obtained.
  • the sum total of the film thickness of the light emitting layer as used in the field of this invention is a film thickness also including the said intermediate
  • each light emitting layer is preferably adjusted in the range of 1 to 50 nm, more preferably in the range of 1 to 20 nm. There is no particular limitation on the relationship between the film thicknesses of the blue, green and red light emitting layers.
  • a light emitting material or a host compound which will be described later, is formed by forming a film by a known thinning method such as a vacuum deposition method, a spin coating method, a casting method, an LB method, an ink jet method, or the like. it can.
  • a plurality of light emitting materials may be mixed in each light emitting layer, or a phosphorescent light emitting material and a fluorescent light emitting material may be mixed and used in the same light emitting layer.
  • the light emitting layer preferably contains a host compound and a light emitting material (also referred to as a light emitting dopant compound) and emits light from the light emitting material.
  • a light emitting material also referred to as a light emitting dopant compound
  • a compound having a phosphorescence quantum yield of phosphorescence emission at room temperature (25 ° C.) of less than 0.1 is preferable. More preferably, the phosphorescence quantum yield is less than 0.01. Moreover, it is preferable that the volume ratio in the layer is 50% or more among the compounds contained in a light emitting layer.
  • known host compounds may be used alone or in combination of two or more.
  • the organic EL element can be made highly efficient.
  • the host compound used in the present invention may be a conventionally known low molecular compound or a high molecular compound having a repeating unit, and a low molecular compound having a polymerizable group such as a vinyl group or an epoxy group (evaporation polymerizable light emitting host). )But it is good.
  • the known host compound a compound that has a hole transporting ability and an electron transporting ability, prevents the emission of light from being increased in wavelength, and has a high Tg (glass transition temperature) is preferable.
  • the glass transition point (Tg) is a value determined by a method based on JIS-K-7121 using DSC (Differential Scanning Colorimetry).
  • a fluorescent compound or a phosphorescent material (also referred to as a phosphorescent compound or a phosphorescent compound) is used.
  • a phosphorescent material is a compound in which light emission from an excited triplet is observed. Specifically, it is a compound that emits phosphorescence at room temperature (25 ° C.), and the phosphorescence quantum yield is 0 at 25 ° C. A preferred phosphorescence quantum yield is 0.1 or more, although it is defined as 0.01 or more compounds.
  • the phosphorescent quantum yield can be measured by the method described in Spectra II, page 398 (1992 version, Maruzen) of Experimental Chemistry Lecture 4 of the 4th edition.
  • the phosphorescence quantum yield in a solution can be measured using various solvents.
  • the phosphorescence quantum yield (0.01 or more) is achieved in any solvent. Just do it.
  • the carrier recombination occurs on the host compound to which the carrier is transported to generate an excited state of the host compound, and this energy is transferred to the phosphorescent material.
  • Energy transfer type to obtain light emission from the phosphorescent light emitting material, and another one is that the phosphorescent light emitting material becomes a carrier trap, and recombination of carriers occurs on the phosphorescent light emitting material, and light emission from the phosphorescent light emitting material is obtained.
  • the excited state energy of the phosphorescent material is required to be lower than the excited state energy of the host compound.
  • the phosphorescent light-emitting material can be appropriately selected from known materials used for the light-emitting layer of the organic EL element, and 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), or a rare earth complex, and most preferably an iridium compound.
  • Fluorescent light emitters can also be used for the organic electroluminescence device according to the present invention.
  • fluorescent emitters include coumarin dyes, pyran dyes, cyanine dyes, croconium dyes, squalium dyes, oxobenzanthracene dyes, fluorescein dyes, rhodamine dyes, and pyrylium dyes. Examples thereof include dyes, perylene dyes, stilbene dyes, polythiophene dyes, and rare earth complex phosphors.
  • dopants can also be used in the present invention.
  • International Publication No. 00/70655 pamphlet JP-A Nos. 2002-280178, 2001-181616, 2002-280179, 2001 -181617, 2002-280180, 2001-247859, 2002-299060, 2001-313178, 2002-302671, 2001-345183, 2002 No. 324679, International Publication No. 02/15645, JP 2002-332291, 2002-50484, 2002-332292, 2002-83684, JP 2002-540572, JP 002-117978, 2002-338588, 2002-170684, 2002-352960, WO01 / 93642, JP2002-50483, 2002-1000047 No. 2002-173684, No.
  • At least one light emitting layer may contain two or more kinds of light emitting materials, and the concentration ratio of the light emitting materials in the light emitting layer may vary in the thickness direction of the light emitting layer.
  • ⁇ Middle layer ⁇ In the present invention, a case where a non-light emitting intermediate layer (also referred to as an undoped region) is provided between the light emitting layers will be described.
  • the non-light emitting intermediate layer is a layer provided between the light emitting layers.
  • the film thickness of the non-light emitting intermediate layer is preferably in the range of 1 to 20 nm, and more preferably in the range of 3 to 10 nm to suppress interaction such as energy transfer between adjacent light emitting layers, and This is preferable because a large load is not applied to the voltage characteristics.
  • the material used for the non-light emitting intermediate layer may be the same as or different from the host compound of the light emitting layer, but may be the same as the host material of at least one of the adjacent light emitting layers. preferable.
  • the non-light-emitting intermediate layer may contain a non-light-emitting layer, a compound common to each light-emitting layer (for example, a host compound), and each common host material (where a common host material is used) Including the case where the physicochemical characteristics such as phosphorescence emission energy and glass transition point are the same, and the case where the molecular structure of the host compound is the same, etc.)
  • a compound common to each light-emitting layer for example, a host compound
  • each common host material where a common host material is used
  • the host material is responsible for carrier transportation, and therefore a material having carrier transportation ability is preferable.
  • Carrier mobility is used as a physical property representing carrier transport ability, but the carrier mobility of an organic material generally depends on the electric field strength. Since a material having a high electric field strength dependency easily breaks the balance between injection and transport of holes and electrons, it is preferable to use a material having a low electric field strength dependency of mobility for the intermediate layer material and the host material.
  • the non-light emitting intermediate layer functions as a blocking layer described later, that is, a hole blocking layer and an electron blocking layer. It is done.
  • Injection layer electron injection layer, hole injection layer >> The injection layer is provided as necessary, and there are an electron injection layer and a hole injection layer, and as described above, it exists between the anode and the light emitting layer or the hole transport layer and between the cathode and the light emitting layer or the electron transport layer. May be.
  • An injection layer is a layer provided between an electrode and an organic layer in order to reduce drive voltage and improve light emission luminance.
  • Organic EL element and its forefront of industrialization (issued by NTT Corporation on November 30, 1998) 2), Chapter 2, “Electrode Materials” (pages 123 to 166) in detail, and includes a hole injection layer (anode buffer layer) and an electron injection layer (cathode buffer layer).
  • anode buffer layer hole injection layer
  • copper phthalocyanine is used.
  • examples thereof include a phthalocyanine buffer layer represented by an oxide, an oxide buffer layer represented by vanadium oxide, an amorphous carbon buffer layer, and a polymer buffer layer using a conductive polymer such as polyaniline (emeraldine) or polythiophene.
  • cathode buffer layer (electron injection layer) The details of the cathode buffer layer (electron injection layer) are described in JP-A-6-325871, JP-A-9-17574, JP-A-10-74586, and the like. Specifically, strontium, aluminum, etc.
  • Metal buffer layer typified by lithium, alkali metal compound buffer layer typified by lithium fluoride, alkaline earth metal compound buffer layer typified by magnesium fluoride, oxide buffer layer typified by aluminum oxide, etc.
  • the buffer layer (injection layer) is preferably a very thin film, and the film thickness is preferably in the range of 0.1 nm to 5 ⁇ m, although it depends on the material.
  • ⁇ Blocking layer hole blocking layer, electron blocking layer>
  • the blocking layer is provided as necessary in addition to the basic constituent layer of the organic compound thin film as described above. For example, it is described in JP-A Nos. 11-204258 and 11-204359, and “Organic EL elements and their forefront of industrialization” (published by NTT Corporation on November 30, 1998). There is a hole blocking (hole blocking) layer.
  • the hole blocking layer has a function of an electron transport layer and is composed of a hole blocking material having a function of transporting electrons and having a remarkably small ability to transport holes, while transporting electrons. By blocking holes, the recombination probability of electrons and holes can be improved. Moreover, the structure of the electron carrying layer mentioned later can be used as a hole-blocking layer concerning this invention as needed.
  • the hole blocking layer is preferably provided adjacent to the light emitting layer.
  • the electron blocking layer in a broad sense, has a function of a hole transport layer, and is made of a material having a function of transporting holes while having a remarkably small ability to transport electrons, while transporting holes. By blocking electrons, the probability of recombination of electrons and holes can be improved. Moreover, 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 to 100 nm, and more preferably 5 to 30 nm.
  • the hole transport layer 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 a plurality of layers.
  • the hole transport material has either hole injection or transport or electron barrier properties, and may be either organic or inorganic.
  • triazole derivatives oxadiazole derivatives, imidazole derivatives, polyarylalkane derivatives, pyrazoline derivatives and pyrazolone derivatives, phenylenediamine derivatives, arylamine derivatives, amino-substituted chalcone derivatives, oxazole derivatives, styrylanthracene derivatives, fluorenone derivatives, hydrazone derivatives
  • Examples thereof include stilbene derivatives, silazane derivatives, aniline copolymers, and conductive polymer oligomers, particularly thiophene oligomers.
  • the above-mentioned materials can be used as the hole transport material, but it is preferable to use a porphyrin 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-4,4′-diaminophenyl; N, N′-diphenyl-N, N′— Bis (3-methylphenyl)-[1,1′-biphenyl] -4,4′-diamine (TPD); 2,2-bis (4-di-p-tolylaminophenyl) propane; 1,1-bis (4-di-p-tolylaminophenyl) cyclohexane; N, N, N ′, N′-tetra-p-tolyl-4,4′-diaminobiphenyl; 1,1-bis (4-di-p-tolyl) Aminophenyl) -4-phenylcyclohexane; bis (4-dimethylamino-2-methylphenyl) phenylmethane; bis (4-di-p-tolylaminoph
  • No. 5,061,569 Having a condensed aromatic ring of, for example, 4,4'-bis [N- (1-naphthyl) -N-phenylamino] biphenyl (NPD), JP-A-4-308 4,4 ′, 4 ′′ -tris [N- (3-methylphenyl) -N-phenylamino] triphenylamine in which three triphenylamine units described in Japanese Patent No. 88 are linked in a starburst type ( MTDATA) and the like.
  • NPD 4,4'-bis [N- (1-naphthyl) -N-phenylamino] biphenyl
  • JP-A-4-308 4,4 ′, 4 ′′ -tris [N- (3-methylphenyl) -N-phenylamino] triphenylamine in which three triphenylamine units described in Japanese Patent No. 88 are linked in a starburst type ( MTDATA) and the
  • 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 the hole injection material and the hole transport material.
  • JP-A-11-251067, J. Org. Huang et. al. A so-called p-type hole transport material described in a book (Applied Physics Letters 80 (2002), p. 139) can also be used. In the present invention, it is preferable to use these materials because a light-emitting element with higher efficiency can be obtained.
  • the hole transport layer can be formed by thinning the hole transport material by a known method such as a vacuum deposition method, a spin coating method, a casting method, a printing method including an ink jet method, or an LB method. it can.
  • the thickness of the hole transport layer is not particularly limited, but is usually about 5 nm to 5 ⁇ m, preferably 5 to 200 nm.
  • the hole transport layer may have a single layer structure composed of one or more of the above materials.
  • a hole transport layer having a high p property doped with impurities examples thereof include JP-A-4-297076, JP-A-2000-196140, 2001-102175, J.A. Appl. Phys. 95, 5773 (2004), and the like.
  • a hole transport layer having such a high p property because a device with lower power consumption can be produced.
  • the electron transport layer is made of a material having a function of transporting electrons, and in a broad sense, an electron injection layer and a hole blocking layer are also included in the electron transport layer.
  • the electron transport layer can be provided as a single layer or a plurality of layers.
  • an electron transport material also serving as a hole blocking material used for an electron transport layer adjacent to the light emitting layer on the cathode side is injected from the cathode.
  • any material can be selected and used from among conventionally known compounds. For example, nitro-substituted fluorene derivatives, diphenylquinone derivatives Thiopyrandioxide derivatives, carbodiimides, fluorenylidenemethane derivatives, anthraquinodimethane and anthrone derivatives, oxadiazole derivatives and the like.
  • a thiadiazole derivative in which the oxygen atom of the oxadiazole 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 3 ), tris (5,7-dichloro-8-quinolinol) aluminum, tris (5,7-dibromo-8-quinolinol) Aluminum, tris (2-methyl-8-quinolinol) aluminum, tris (5-methyl-8-quinolinol) aluminum, bis (8-quinolinol) zinc (Znq), etc.
  • Mg Metal complexes replaced with Cu, Ca, Sn, Ga, or Pb can also be used as electron transport materials.
  • metal-free or metal phthalocyanine or those having terminal ends substituted with an alkyl group or a sulfonic acid group can be preferably used as the electron transporting material.
  • the distyrylpyrazine derivatives exemplified as the material of the light emitting layer can also be used as the electron transport material, and inorganic semiconductors such as n-type-Si and n-type-SiC can be used as well as the hole injection layer and the hole transport layer. It can be used as an electron transport material.
  • the electron transport layer can be formed by thinning the electron transport material by a known method such as a vacuum deposition method, a spin coating method, a casting method, a printing method including an ink jet method, or an LB method.
  • 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 examples thereof include JP-A-4-297076, JP-A-10-270172, JP-A-2000-196140, 2001-102175, J.A. Appl. Phys. 95, 5773 (2004), and the like.
  • an electron transport layer having such a high n property because an element with lower power consumption can be produced.
  • the counter electrode of the present invention refers to an electrode facing the transparent conductive layer.
  • the transparent conductive layer is mainly used as an anode, the following cathode can be used as the counter electrode.
  • the cathode a material having a work function (4 eV or less) metal (referred to as an electron injecting metal), an alloy, an electrically conductive compound and a mixture thereof as an electrode material is used.
  • Electrode materials include sodium, sodium-potassium alloy, magnesium, lithium, magnesium / copper mixture, magnesium / silver mixture, magnesium / aluminum mixture, magnesium / indium mixture, aluminum / aluminum oxide (Al 2 O 3 ) Mixtures, indium, lithium / aluminum mixtures, rare earth metals and the like.
  • a mixture of an electron injecting metal and a second metal which is a stable metal having a larger work function than this for example, a magnesium / silver mixture, Magnesium / aluminum mixtures, magnesium / indium mixtures, aluminum / aluminum oxide (Al 2 O 3 ) mixtures, lithium / aluminum mixtures, aluminum and the like are preferred.
  • the cathode can be produced by forming a thin film of these electrode materials by a method such as vapor deposition or sputtering.
  • the sheet resistance as the cathode is preferably several hundred ⁇ / ⁇ or less, and the film thickness is usually selected in the range of 10 nm to 5 ⁇ m, preferably 50 nm to 200 nm.
  • the light emission luminance is improved, which is convenient.
  • a transparent or semi-transparent cathode can be produced by producing a conductive transparent material on the cathode after the metal is produced with a thickness of 1 nm to 20 nm on the cathode.
  • An element in which both the anode and the cathode are transmissive can be manufactured.
  • the organic electroluminescence element of the present invention can be produced by sequentially forming a composite material layer, a transparent conductive layer, an organic electroluminescence layer, and a counter electrode on a transparent substrate.
  • a transparent conductive layer can be formed using a desired electrode substance on a transparent substrate on which a light scattering layer is formed.
  • the transparent conductive layer can be formed by a method such as vapor deposition or sputtering.
  • a transparent conductive layer can be formed from a material containing metal nanowires, a conductive polymer, or a transparent conductive metal oxide by a liquid phase film forming method such as a coating method or a printing method.
  • a liquid conductive film forming method such as a coating method or a printing method is applied to a transparent conductive layer containing metal nanowires. It is preferable to form by.
  • coating methods roll coating method, bar coating method, dip coating method, spin coating method, casting method, die coating method, blade coating method, bar coating method, gravure coating method, curtain coating method, spray coating method, doctor coating method Etc. can be used.
  • a letterpress (letter) printing method a stencil (screen) printing method, a lithographic (offset) printing method, an intaglio (gravure) printing method, a spray printing method, an ink jet printing method, and the like can be used.
  • physical surface treatment such as corona discharge treatment or plasma discharge treatment can be applied to the surface of the releasable substrate as a preliminary treatment for improving the adhesion and coating properties.
  • an organic electroluminescence layer As an example of a method for producing this organic electroluminescence layer, a method for producing an organic electroluminescence layer comprising a hole injection layer / a hole transport layer / a light emitting layer / a hole blocking layer / an electron transport layer will be described.
  • An organic compound thin film of a hole injection layer, a hole transport layer, a light emitting layer, a hole blocking layer, and an electron transport layer, which are organic electroluminescence element materials, is formed on a transparent substrate on which a transparent conductive layer is formed.
  • a method for thinning the organic compound thin film there are a vapor deposition method and a wet process (spin coating method, casting method, ink jet method, printing method) as described above, but it is easy to obtain a uniform film and a pinhole. From the point of being difficult to form, a vacuum deposition method, a spin coating method, an ink jet method, and a printing method are particularly preferable. Further, different film forming methods may be applied for each layer.
  • the vapor deposition conditions vary depending on the type of compound used, but generally a boat heating temperature of 50 to 450 ° C., a degree of vacuum of 10 ⁇ 6 to 10 ⁇ 2 Pa, and a vapor deposition rate of 0.01 to It is desirable to select appropriately within the range of 50 nm / second, substrate temperature ⁇ 50 to 300 ° C., film thickness 0.1 nm to 5 ⁇ m, preferably 5 to 200 nm.
  • a thin film made of a cathode material is formed thereon by a method such as vapor deposition or sputtering so as to have a film thickness of 1 ⁇ m or less, preferably in the range of 50 to 200 nm. Is provided.
  • the desired organic electroluminescence element is obtained by the above steps.
  • the organic EL element is preferably produced from the hole injection layer to the cathode consistently by a single evacuation, but may be taken out halfway and subjected to different film forming methods. At that time, it is necessary to consider that the work is performed in a dry inert gas atmosphere.
  • a DC voltage is applied to the multicolor liquid crystal display device thus obtained, light emission can be observed by applying a voltage of about 2 to 40 V with the positive polarity of the anode and the negative polarity of the cathode.
  • An alternating voltage may be applied.
  • the alternating current waveform to be applied may be arbitrary.
  • the surface light emitter and the light emitting panel according to the present invention can be used as a display device, a display, and various light emitting sources.
  • light sources include home lighting, interior lighting, clock and liquid crystal backlights, billboard advertisements, traffic lights, light sources for optical storage media, light sources for electrophotographic copying machines, light sources for optical communication processors, and light sources for optical sensors.
  • it is not limited to this, it can be effectively used for a backlight of a liquid crystal display device combined with a color filter and a light source for illumination.
  • the organic electroluminescent material according to the present invention can also be applied to an organic EL element that emits substantially white light as a lighting device.
  • a plurality of light emitting colors are simultaneously emitted by a plurality of light emitting materials to obtain white light emission by color mixing.
  • the combination of a plurality of emission colors may include three emission maximum wavelengths of the three primary colors of blue, green, and blue, or two using the relationship of complementary colors such as blue and yellow, blue green and orange, etc. The thing containing the light emission maximum wavelength may be used.
  • a combination of light emitting materials for obtaining a plurality of emission colors includes a combination of a plurality of phosphorescent or fluorescent materials (light emitting dopants), a light emitting material that emits fluorescent or phosphorescent light, and the light emission. Any combination of a dye material that emits light from the material as excitation light may be used, but in the white organic EL device according to the present invention, a method of combining a plurality of light-emitting dopants is preferable.
  • a method of having a plurality of emission dopants in one emission layer, a plurality of emission layers, and an emission wavelength of each emission layer examples thereof include a method in which different dopants are present, and a method in which minute pixels emitting light of different wavelengths are formed in a matrix.
  • patterning may be performed by a metal mask, an ink jet printing method, or the like at the time of film formation, if necessary.
  • patterning only the electrode may be patterned, the electrode and the light emitting layer may be patterned, or the entire element layer may be patterned.
  • the light emitting material used for the light emitting layer is not particularly limited.
  • the platinum complex according to the present invention is known so as to be suitable for the wavelength range corresponding to the CF (color filter) characteristics. Any one of the light emitting materials may be selected and combined to be whitened.
  • the white light-emitting organic EL element is used as a liquid crystal display as a kind of lamp such as various light-emitting light sources and lighting devices, home lighting, interior lighting, and exposure light source. It is also useful for display devices such as device backlights.
  • backlights such as clocks, signboard advertisements, traffic lights, light sources such as optical storage media, light sources for electrophotographic copying machines, light sources for optical communication processing machines, light sources for optical sensors, etc.
  • Example 1 Production of Composite Material (Organic / Inorganic Composite Material) 1 >> (Preparation of zirconia particles) To a zirconium salt solution in which 2600 g of zirconium oxychloride octahydrate is dissolved in 40 l (liter) of pure water, 340 g of 28% ammonia water and 20 l of dilute ammonia water in pure water are added with stirring to obtain a zirconia precursor. A slurry was prepared.
  • this mixture was dried in the atmosphere at 120 ° C. for 24 hours using a dryer to obtain a solid.
  • the solid was pulverized with an automatic mortar or the like and then baked at 500 ° C. for 1 hour in the air using an electric furnace.
  • This fired product is put into pure water, stirred to form a slurry, washed using a centrifuge, sufficiently removed the added sodium sulfate, dried in a drier, and zirconia particles 1 was prepared.
  • the average particle size was 5 nm.
  • XRD confirmed that the particles were ZrO 2 crystals.
  • the obtained composite material 1 was applied onto a smooth glass substrate so as to have a dry film thickness of 1 ⁇ m, and cured by irradiating with ultraviolet rays to prepare a sample in which a thin film layer was formed.
  • a spectrophotometer such as U-4000 type manufactured by Hitachi, Ltd.
  • the refractive index was 1.75.
  • the thin film layer was observed with a scanning electron microscope, and the spherical equivalent particle diameter of each particle was obtained from the projected area of 200 particles of zirconia nanoparticles, and the average value was obtained.
  • the average particle diameter of the zirconia nanoparticles dispersed in the thin film was 6 nm.
  • the composite material 2 was produced by changing the addition amount of the dispersion liquid of the zirconia particles 1 to 10% by volume in the same manner as the production of the composite material 1.
  • the refractive index and the average particle diameter of the zirconia nanoparticles were measured by the same method as for the composite material 1. As a result, the refractive index was 1.65, and the average particle diameter of the zirconia nanoparticles was 6 nm.
  • a composite material 4 in which titania nanoparticles were dispersed was produced in the same manner as the production method of the composite material 1.
  • the obtained resin monomer solution in which titania nanoparticles were dispersed was applied on a smooth glass substrate so as to have a dry film thickness of 1 ⁇ m, cured by irradiation with ultraviolet rays, and evaluated in the same manner as in the composite material 1. .
  • the refractive index was 1.74
  • the average particle diameter of the dispersed titania nanoparticles was 18 nm.
  • Table 1 shows the evaluation results of the above thin film layers.
  • the composite material 1 is applied to one side of a 125 ⁇ m thick biaxially stretched PEN film (manufactured by Teijin DuPont; refractive index 1.75) so that the dry film thickness is 3 ⁇ m and cured by irradiating with ultraviolet rays. Let this side be the surface. Furthermore, after adding 20% by mass of silica particles KE-P30 (average particle size 0.3 ⁇ m) manufactured by Nippon Shokubai Co., Ltd. to the composite material 1, ultrasonic dispersion is performed to obtain a resin solution 1A containing a light scattering filler. It was prepared, applied to the back surface of the PEN film so that the dry film thickness was 3 ⁇ m, and cured by irradiation with ultraviolet rays.
  • silica particles KE-P30 average particle size 0.3 ⁇ m
  • ⁇ Preparation of transparent substrate 3 The above-mentioned composite material 2 is applied to one side of a 125 ⁇ m thick biaxially stretched PEN film (manufactured by Teijin DuPont; refractive index: 1.75) so as to have a dry film thickness of 3 ⁇ m and cured by irradiating with ultraviolet rays. Let this side be the surface. Furthermore, after adding 20% by mass of silica particles KE-P30 (average particle size 0.3 ⁇ m) manufactured by Nippon Shokubai Co., Ltd. to the composite material 2, ultrasonic dispersion is performed to obtain a resin solution 2A containing a light scattering filler. It was prepared, applied to the back surface of the PEN film so that the dry film thickness was 3 ⁇ m, and cured by irradiation with ultraviolet rays.
  • silica particles KE-P30 average particle size 0.3 ⁇ m
  • ⁇ Preparation of transparent substrate 4 The composite material 3 described above is applied to one side of a 125 ⁇ m thick biaxially stretched PEN film (manufactured by Teijin DuPont; refractive index 1.75) so that the dry film thickness is 3 ⁇ m and cured by irradiating with ultraviolet rays. Let this side be the surface. Furthermore, after adding 20% by mass of silica particles KE-P30 (average particle size 0.3 ⁇ m) manufactured by Nippon Shokubai Co., Ltd. to the composite material 3, ultrasonic dispersion is performed to obtain a resin solution 3A containing a light scattering filler. It was prepared, applied to the back surface of the PEN film so that the dry film thickness was 3 ⁇ m, and cured by irradiation with ultraviolet rays.
  • silica particles KE-P30 average particle size 0.3 ⁇ m
  • Preparation of transparent substrate 6 After adding 20% by mass of silica particles KE-P30 (average particle size 0.3 ⁇ m) manufactured by Nippon Shokubai Co., Ltd. to the composite material 4, ultrasonic dispersion is performed to prepare a resin solution 4A containing a light scattering filler. This was applied to one side of a 125 ⁇ m thick biaxially stretched PEN film (manufactured by Teijin DuPont; refractive index 1.75) so as to have a dry film thickness of 5 ⁇ m, and cured by irradiating with ultraviolet rays.
  • silica particles KE-P30 average particle size 0.3 ⁇ m
  • a light scattering filler This was applied to one side of a 125 ⁇ m thick biaxially stretched PEN film (manufactured by Teijin DuPont; refractive index 1.75) so as to have a dry film thickness of 5 ⁇ m, and cured by irradiating with ultraviolet rays.
  • the composite material 4 was further applied as a smoothing layer so that the dry film thickness was 4 ⁇ m, and cured by irradiating with ultraviolet rays. Thereafter, the composite material 4 was applied to the opposite surface of the PEN film so as to have a dry film thickness of 4 ⁇ m, and cured by irradiation with ultraviolet rays.
  • ⁇ Preparation of transparent substrate 11 After adding 20% by mass of alumina particles AO-802 (average particle size 0.7 ⁇ m) manufactured by Admatechs Co., Ltd. to composite material 2, ultrasonic dispersion is performed to prepare resin solution 2B containing a light scattering filler. This was applied to one side of a 125 ⁇ m thick biaxially stretched PEN film (manufactured by Teijin DuPont; refractive index 1.75) so as to have a dry film thickness of 5 ⁇ m, and cured by irradiating with ultraviolet rays. Further, the composite material 2 was further applied as a smoothing layer so that the dry film thickness was 4 ⁇ m, and cured by irradiating with ultraviolet rays. Thereafter, the composite material 2 was applied to the opposite surface of the PEN film so as to have a dry film thickness of 4 ⁇ m, and cured by irradiation with ultraviolet rays.
  • alumina particles AO-802 average particle size 0.7 ⁇ m
  • Preparation of transparent substrate 12 After adding 20% by mass of silica particles KE-P30 (average particle size 0.3 ⁇ m) to the composite material 5, ultrasonic dispersion is performed to prepare a resin solution 5A containing a light-scattering filler, which has a thickness of 125 ⁇ m.
  • a biaxially stretched PEN film (manufactured by Teijin DuPont Co., Ltd .; refractive index 1.75) was applied to a dry film thickness of 5 ⁇ m and cured by irradiating with ultraviolet rays. Further, the composite material 5 was further applied as a smoothing layer so that the dry film thickness was 4 ⁇ m, and cured by irradiating with ultraviolet rays. Thereafter, the composite material 5 was applied to the opposite surface of the PEN film so as to have a dry film thickness of 4 ⁇ m, and was cured by irradiation with ultraviolet rays.
  • This substrate was transferred to a glove box in accordance with JIS B 9920 under a nitrogen atmosphere, with a measured cleanliness of class 100, a dew point temperature of ⁇ 80 ° C. or lower, and an oxygen concentration of 0.8 ppm.
  • a coating solution for a hole transport layer was prepared as follows in a glove box, and applied with a spin coater under conditions of 1500 rpm and 30 seconds. This substrate was dried by heating at a substrate surface temperature of 150 ° C. for 30 minutes to provide a hole transport layer. The film thickness was 20 nm when it apply
  • the coating liquid for electron carrying layers was prepared as follows, and it apply
  • a resistance heating boat containing potassium fluoride was energized and heated to provide a 3 nm electron injection layer made of potassium fluoride on the substrate.
  • a resistance heating boat containing aluminum was energized and heated, and a cathode having a thickness of 100 nm made of aluminum was provided at a deposition rate of 1 to 2 nm / second.
  • the thickness of the organic electroluminescence layer was 0.12 ⁇ m, and the thickness of the transparent conductive layer was 0.1 ⁇ m.
  • the produced organic EL device is set in a spectral radiance meter CS-1000 (manufactured by Konica Minolta Sensing), and the organic EL device emits light and changes the angle with respect to the normal direction, and the luminance and spectral spectrum at each tilt angle.
  • the front luminances of red, green, and blue in the normal direction are each 1, the relative luminances of red, green, and blue in directions inclined by 30 degrees, 45 degrees, and 60 degrees with respect to the normal direction And is shown in Table 2.
  • the relative luminance value is in the range of 0.95 to 1.05, changes in luminance and chromaticity are not visually recognized, and it is favorable as white illumination.
  • the refractive index of the matrix resin is the refractive index of the cured film of the composite material used for each light scattering layer, to which no light scattering layer filler is added.
  • the refractive indexes of the used silica, PMMA, and alumina are 1.45, 1.49, and 1.76, respectively.
  • the organic electroluminescence device having the configuration of the present invention has a high external extraction quantum efficiency, a small luminance and color change depending on the observation angle, and is excellent as white illumination.
  • Example 2 The organic EL element 8 of the present invention produced in Example 1 was covered with a glass case to obtain a lighting device.
  • the glass cover was filled with nitrogen gas, and a water capturing agent was provided in the glass cover on the side opposite to the light emitting surface.
  • the lighting device according to the present invention has high luminous efficiency and can be used as a thin lighting device that emits white light with a long light emission lifetime.
  • Example 3 The organic EL element 8 of the present invention produced in Example 1 was covered with a transparent barrier film (transparent resin film coated with a silicon dioxide film) to obtain a flexible lighting device.
  • the illuminating device according to the present invention can be used as a thin illuminating device that emits white light having a long emission life while maintaining high luminous efficiency even with some bending motion.

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  • Electroluminescent Light Sources (AREA)

Abstract

L'invention concerne un élément électroluminescent organique et un dispositif d'éclairage, lequel élément électroluminescent est formé en empilant une couche électroluminescente organique comprenant une couche électroconductrice transparente et une couche de transport d'électrons, et une électrode opposée séquentiellement sur un substrat transparent. Le substrat transparent comprend des nanoparticules d'oxyde ayant un diamètre moyen de 1 nm-20 nm et un plastique sur un côté au moins du substrat transparent. Il comprend en outre une couche de diffusion de lumière dans laquelle un fluide d'application, pour lequel un matériau de charge diffusant la lumière et ayant des particules d'un diamètre moyen de 0,1 µm-0,7 µm est ajouté à un matériau composite, est appliqué, séché et durci, sa réfraction après durcissement allant de 1,65 à 1,80 compris, et l'épaisseur de la couche de transport d'électrons étant de 40-200 nm.
PCT/JP2011/050251 2010-01-26 2011-01-11 Élément électroluminescent organique et dispositif d'éclairage WO2011093120A1 (fr)

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JP2015514293A (ja) * 2012-03-23 2015-05-18 エルジー・ケム・リミテッド 有機発光素子
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WO2013088997A1 (fr) * 2011-12-15 2013-06-20 東レ株式会社 Corps à surface électroluminescente et film de surface avant
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JP2014089860A (ja) * 2012-10-30 2014-05-15 Mitsubishi Rayon Co Ltd 硬化物、有機ｅｌ素子用基板及びそれらの製造方法
JP2016518018A (ja) * 2013-05-16 2016-06-20 エルジー・ケム・リミテッド 有機発光素子およびその製造方法
JP2015022794A (ja) * 2013-07-16 2015-02-02 東洋インキＳｃホールディングス株式会社 光散乱層用樹脂組成物、光散乱層、および有機エレクトロルミネッセンス装置
JPWO2015083660A1 (ja) * 2013-12-06 2017-03-16 コニカミノルタ株式会社 有機エレクトロルミネッセンス素子
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WO2015166764A1 (fr) * 2014-04-28 2015-11-05 コニカミノルタ株式会社 Corps stratifié d'extraction de lumière, élément électroluminescent organique, et leur procédé de fabrication
JP2017516265A (ja) * 2014-05-15 2017-06-15 エルジー ディスプレイ カンパニー リミテッド 有機発光素子
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WO2016002310A1 (fr) * 2014-07-04 2016-01-07 Ｎｅｃライティング株式会社 Couche de résine transparente pour écran électroluminescent organique, écran électroluminescent organique, dispositif d'éclairage électroluminescent organique et dispositif d'affichage électroluminescent organique
JPWO2016002310A1 (ja) * 2014-07-04 2017-04-27 Ｎｅｃライティング株式会社 有機ｅｌパネル用透明樹脂層、有機ｅｌパネル、有機ｅｌ照明装置、および有機ｅｌディスプレイ
US10205127B2 (en) 2014-07-04 2019-02-12 Nec Lighting, Ltd. Organic EL panel-use transparent resin layer, organic EL panel, organic EL lighting device, and organic EL display
JP2020047611A (ja) * 2014-07-04 2020-03-26 株式会社ホタルクス 有機ｅｌパネル用透明樹脂層、有機ｅｌパネル、有機ｅｌ照明装置、および有機ｅｌディスプレイ
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