WO2010140411A1 - Procédé de production de dispositif électroluminescent, et dispositif électroluminescent - Google Patents

Procédé de production de dispositif électroluminescent, et dispositif électroluminescent Download PDF

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WO2010140411A1
WO2010140411A1 PCT/JP2010/053980 JP2010053980W WO2010140411A1 WO 2010140411 A1 WO2010140411 A1 WO 2010140411A1 JP 2010053980 W JP2010053980 W JP 2010053980W WO 2010140411 A1 WO2010140411 A1 WO 2010140411A1
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emitting device
light emitting
phosphor layer
light
led chip
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PCT/JP2010/053980
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English (en)
Japanese (ja)
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仁 安達
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コニカミノルタオプト株式会社
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Priority to JP2011518336A priority Critical patent/JPWO2010140411A1/ja
Publication of WO2010140411A1 publication Critical patent/WO2010140411A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/507—Wavelength conversion elements the elements being in intimate contact with parts other than the semiconductor body or integrated with parts other than the semiconductor body
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
    • H01L2224/13—Structure, shape, material or disposition of the bump connectors prior to the connecting process of an individual bump connector
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
    • H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
    • H01L2224/161—Disposition
    • H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/16225—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/00011—Not relevant to the scope of the group, the symbol of which is combined with the symbol of this group
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/00014—Technical content checked by a classifier the subject-matter covered by the group, the symbol of which is combined with the symbol of this group, being disclosed without further technical details
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
    • H01L2924/181—Encapsulation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/44—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the coatings, e.g. passivation layer or anti-reflective coating

Definitions

  • the present invention relates to a method for manufacturing a light emitting device and a light emitting device.
  • the present invention relates to a method for manufacturing a light-emitting device and a light-emitting device that are excellent in durability and color rendering while having high emission intensity.
  • white light emitting devices using LEDs have recently attracted attention as highly efficient and highly reliable white illumination light sources, and some of them have already been put into practical use as small power small light sources.
  • This type of white light emitting device is generally a blue LED element (also referred to as an LED chip) covered with a mixture of a phosphor that is excited by blue light and emits yellow light and a transparent resin.
  • a method of combining an ultraviolet LED element with a blue phosphor, a green phosphor, a red phosphor and the like has been developed, and white light emitting devices of these various methods are disclosed.
  • the phosphor layer is formed by dispersing the phosphor in the glass material
  • the phosphor particles are dispersed in the glass melted at a high temperature when the phosphor particles are dispersed in the glass.
  • the phosphor is deactivated by heat, the brightness at the beginning of use is lowered, or the color tone changes when used for a long time.
  • a method for obtaining a phosphor without a binder a method for obtaining a phosphor film having a filling rate of 60 to 97% by an aerosol deposition method is known (for example, see Patent Document 2). Since this method does not require a high vacuum, it is excellent in that the apparatus cost is relatively low and the phosphor can be recovered and reused.
  • the phosphor particles are subjected to a strong impact when colliding with the surface on which the phosphor layer is formed, so that defects are not introduced into the crystal lattice, and the phosphor emits light. There was a problem that efficiency decreased.
  • An object of the present invention is to provide a light-emitting device having excellent durability, little deterioration with time, and preventing a decrease in light emission efficiency to provide a high luminance, and a method for manufacturing the light-emitting device.
  • an LED chip a phosphor layer that absorbs at least a portion of light emitted from the LED chip, emits light after wavelength conversion, and the phosphor layer on the surface of the phosphor layer.
  • a method for manufacturing a light emitting device comprising at least one inorganic layer provided so as to cover The phosphor is produced by colliding and depositing phosphor particles against the light emitting surface of the LED chip or the surface of the base material provided separately from the LED chip and facing the light emitting surface of the LED chip.
  • a method for manufacturing a light emitting device wherein a layer is formed, and then at least one inorganic layer is provided on the surface of the phosphor layer so as to cover the phosphor layer.
  • an LED chip a phosphor layer that absorbs at least a part of light emitted from the LED chip, emits light after wavelength conversion, and the phosphor on the surface of the phosphor layer.
  • a light emitting device comprising: at least one inorganic layer provided to cover the layer.
  • the phosphor particles are placed on the surface on which the phosphor layer is formed at a low speed. Even when the phosphor layer is formed by colliding, the phosphor layer is covered with the inorganic layer, so that the adhesion strength of the phosphor layer to the substrate can be increased.
  • the phosphor layer is formed by colliding and depositing the phosphor particles on the surface on which the phosphor layer is formed, and further provided with an inorganic layer. Deterioration can be suppressed even when the light source has high luminance.
  • the light emitting device 100 of the present invention is provided on the LED chip 1, the base material 2, and one surface 2 a of the base material 2, and converts part of the light emission of the LED chip 1 to a different wavelength.
  • a phosphor layer 3 and a lens 4 that is provided on the other surface 2b of the substrate 2 and collects light emitted from the LED chip 1 and the phosphor layer 3 and emits the light in a desired direction are provided.
  • the phosphor layer 3 is provided on the base 2 provided separately from the LED chip 1, but the same effect can be obtained even if the phosphor layer 3 is provided on the light emitting surface of the LED chip 1. It is done.
  • the configuration in which the phosphor layer 3 is provided on the base 2 provided separately from the LED chip 1 suppresses heat generated in the LED chip 1 from being transmitted to the phosphor. And higher durability can be obtained.
  • the substrate 2 has a flat plate shape and is disposed to face the LED chip 1.
  • a material of the base material 2 The resin material, glass material, translucent ceramic (translucent alumina etc.) which consists of oxide particles, etc. are mentioned. From the viewpoint of preventing deterioration of the light source due to heat or light, the substrate preferably has high heat resistance and light resistance, and a glass material or a translucent ceramic material is preferably used.
  • resin it is preferable to use curable resin with high heat resistance.
  • the substrate 2 is fixed to the support 5. Instead of using the support 5, a material having the same composition as that of the substrate 2 may be used to form an integral structure.
  • the support 5 is fixed to the top of the mount 6.
  • the phosphor layer 3 is provided on the surface 2a (the lower surface in FIG. 1) 2a of the base material 2 through the base layer 7, and the surface opposite to the phosphor layer 3 is provided.
  • a lens 4 is provided on the upper surface 2b (in FIG. 1).
  • the lens 4 has a dome shape that is convex upward, and is made of a known resin material. Further, the lens 4 and the base material 2 may be integrated with the base material 2 using a material having the same composition as the lens 4.
  • An inorganic layer 8 is provided on the surface of the phosphor layer 3 so as to cover the phosphor layer 3, and the inorganic layer 8 has a function of protecting the phosphor layer 3 and increasing the adhesive strength of the phosphor layer 3. is doing.
  • the LED chip 1 has the transparent substrate 9 side facing the phosphor layer 3, and the LED chip 1 receives a signal from the lead wire 11 via the bump electrode 10 on the surface of the semiconductor layer.
  • the LED chip 1 is fixed by a transparent mold resin 12, and the outside is protected by a mount 6.
  • the phosphor layer 3, the inorganic layer 8, the base layer 7, and the LED chip 1 will be described in detail.
  • a phosphor that is a raw material of the phosphor layer an oxide or a compound that easily becomes an oxide at a high temperature is used as a raw material of Y, Gd, Ce, Sm, Al, La, and Ga, and these are stoichiometrically. The raw materials are obtained by thoroughly mixing in the ratio.
  • a coprecipitated oxide obtained by firing a solution obtained by coprecipitation of a solution obtained by dissolving a rare earth element of Y, Gd, Ce, or Sm in an acid at a stoichiometric ratio with oxalic acid, and aluminum oxide or gallium oxide.
  • An appropriate amount of fluoride such as ammonium fluoride is mixed with this as a flux and packed in a crucible and fired in air at a temperature range of 1350 to 1450 ° C. for 2 to 5 hours to obtain a fired product.
  • the desired phosphor can be obtained by ball-milling the fired product in water, washing, separating, drying, and finally passing through a sieve.
  • the phosphor particles are collided with the substrate to form a film.
  • the aerosol deposition method is preferably used.
  • FIG. 2 is a schematic configuration diagram of an aerosol deposition film forming apparatus 200 used in the present invention.
  • the aerosol deposition film forming apparatus 200 includes a holder 21 for holding a substrate 20, an XYZ ⁇ stage 22 for operating the holder 21 in three dimensions with XYZ ⁇ , a nozzle 23 having a narrow opening for ejecting a raw material onto the substrate 20, and a nozzle 23.
  • the chamber 26 includes a pipe 25 connected to the aerosol generation chamber 24, a high-pressure gas cylinder 27 for storing the carrier gas, an aerosol generation chamber 24 in which the fine particle raw material and the carrier gas are stirred and mixed, and a pipe 28 connecting these.
  • a temperature control mechanism using a Peltier element is installed on the back surface of the stage 22 so that the substrate 20 can be maintained at an optimum temperature.
  • the phosphor fine particle raw material in the aerosolization chamber is formed on the substrate surface by the following procedure.
  • the aerosolized particulate material passes through the pipe and is sprayed with a carrier gas from a nozzle having a narrow opening in the chamber together with a carrier gas to form a coating film.
  • the chamber is evacuated by a vacuum pump or the like, and the degree of vacuum in the chamber is adjusted as necessary.
  • the degree of vacuum is preferably 0.01 to 10000 Pa, more preferably 0.1 to 1000 Pa.
  • the substrate holder can be moved three-dimensionally by the XYZ ⁇ stage, a phosphor layer having a necessary thickness can be formed on a predetermined portion of the substrate.
  • the aerosolized raw material particles are preferably transported by a carrier gas having a flow rate of 50 to 400 m / sec and can be deposited by colliding with the substrate.
  • the particles transported by the carrier gas are bonded to each other by impact of collision to form a film.
  • the nitrogen gas is preferably an inert gas such as He gas.
  • nitrogen gas can be preferably used.
  • the specific function of the protective layer is not particularly limited as long as it has a function of increasing the adhesive strength of the phosphor layer, and preferably has a function of protecting the phosphor layer from damage such as scratching or chemical adhesion. Have.
  • the material constituting the inorganic layer is not particularly limited, but is preferably formed of an inorganic oxide film, and particularly preferably contains inorganic oxide particles.
  • the light from the LED chip is scattered by the inorganic oxide particles by forming the inorganic layer with an inorganic oxide film containing inorganic oxide particles.
  • the color shift between the scattered light of the LED chip and the light emitted from the phosphor excited by the scattered light is reduced, and the color mixing property is improved.
  • an inorganic layer can be firmly formed by containing an inorganic oxide particle.
  • the composition of the inorganic oxide particles according to the present invention is not particularly limited, but is preferably at least one of silicon oxide, aluminum oxide, zinc oxide, titanium oxide and zirconium oxide.
  • the average particle diameter of the inorganic oxide particles is from 100 nm to 1 ⁇ m, preferably from 200 to 800 nm, more preferably from 300 to 700 nm, from the viewpoint of the strength of the inorganic layer and the prevention of lowering the incident efficiency of light emitted from the LED chip.
  • a coating film obtained from a dispersion of inorganic oxide particles on the order of ⁇ m cannot be obtained simply by heat treatment, but the specific surface area is reduced because the inorganic oxide particles used are on the order of nm.
  • a robust inorganic oxide film can be formed by heat treatment.
  • the average particle diameters of the inorganic oxide particles and the phosphor fine particles in the present invention are the points at which the cumulative curve becomes 50% when the cumulative curve is obtained by setting the total volume of one group of particle bodies to 100%.
  • particle diameter cumulative average diameter
  • volume average particle diameter or median diameter means one that is generally used as one of parameters for evaluating particle size distribution.
  • the particle size of the inorganic oxide particles and phosphor particles used in the present invention can be measured using a general laser diffraction particle size measuring device, specifically, HELOS (manufactured by JEOL), MicrotracHRA (manufactured by Nikkiso Co., Ltd.), SALD-1100 (manufactured by Shimadzu Corp.), Coulter counter (manufactured by Coulter Corp.) and the like can be mentioned, and SALD-1100 (manufactured by Shimadzu Corp.) is particularly preferable.
  • HELOS manufactured by JEOL
  • MicrotracHRA manufactured by Nikkiso Co., Ltd.
  • SALD-1100 manufactured by Shimadzu Corp.
  • Coulter counter manufactured by Coulter Corp.
  • SALD-1100 manufactured by Shimadzu Corp.
  • the “inorganic oxide film” is a film containing an inorganic oxide, and includes at least the above-mentioned inorganic oxide particles and a compound having a polysiloxane structure for forming a silica-based film described later.
  • a film containing as a constituent element is preferably used.
  • the content of the inorganic oxide particles is preferably 30 to 99 vol%, more preferably 50 to 80 vol% of the inorganic oxide film.
  • the cross section of the film is observed with a transmission electron microscope, and the ratio of the total area of the inorganic fine particles contained in the total cross-sectional area of the inorganic oxide film Indicated. Since the original particle interface of the inorganic fine particles is observed in the film, the area where the inorganic fine particles are present can be quantified.
  • Inorganic oxide films can be formed by vapor deposition, dry processes, and wet processes such as sol-gel methods, but they all have crystal grain interfaces, so they do not have sufficient barrier properties against gases and water vapor.
  • the inclusion of inorganic oxide particles in the inorganic oxide film according to the present invention can minimize the occurrence of cracks that impair the barrier property, thereby improving the barrier property. Became possible.
  • Method for forming silica-based film As a method for forming a silica-based coating, first, a composition for forming a silica-based coating is applied on a substrate. As a method for applying the composition for forming a silica-based film on the substrate, for example, any method such as a spray method, a spin coating method, a dip coating method, a roll coating method can be used. Used.
  • the silica-based film forming composition applied on the substrate is heat-treated.
  • the means, temperature, time, etc. of the heat treatment are not particularly limited, but in general, it may be heated for about 1 to 6 minutes on a hot plate at about 80 to 300 ° C.
  • an acid or a base is generated by heating with a heat treatment. Hydrolysis is promoted by the generated acid or base, so that the alkoxy group becomes a hydroxyl group and alcohol is generated. Thereafter, a hydroxyl group is polycondensed between two molecules to form a Si—O—Si network, and thus a dense silica-based film can be obtained by heat treatment.
  • the heat treatment is preferably performed in three or more steps in a stepwise manner. Specifically, after the first heat treatment is performed for 30 seconds to 2 minutes on a hot plate of about 60 to 150 ° C. in an air or an inert gas atmosphere such as nitrogen, the temperature is about 100 to 220 ° C. The second heat treatment is performed for about 30 seconds to 2 minutes, and the third heat treatment is performed at about 150 to 300 ° C. for about 30 seconds to 2 minutes.
  • stepwise heat treatment of three or more steps preferably about 3 to 6 steps, a silica-based film can be formed at a lower temperature.
  • the above-described inorganic layer may be a single layer or a plurality of layers.
  • the underlayer is an inorganic oxide layer provided between the phosphor layer and the surface on which the phosphor layer is provided, and is an inorganic oxide film containing the same inorganic oxide particles as the inorganic layer. It is preferable.
  • the underlayer may be a single layer or a plurality of layers.
  • the adhesive strength of the phosphor layer to the surface on which the phosphor layer is provided can be increased. Further, the amount of light emitted from the phosphor layer can be increased by the underlayer.
  • LED chip Various known LED chips can be used as the LED chip. In particular, when obtaining white light, a blue LED chip or an ultraviolet LED chip can be preferably used. As the blue LED chip, any existing one including In x Ga 1-x N system can be used. The emission peak wavelength of the blue LED chip is preferably 440 to 480 nm. Any existing UV LED chip can be used. The emission peak wavelength of the ultraviolet LED chip is preferably 140 to 420 nm.
  • the LED chip can be mounted on a substrate and radiated upward or sideward, or a blue LED chip is mounted on a transparent substrate such as a sapphire substrate, and bumps are formed on the surface.
  • a blue LED chip is mounted on a transparent substrate such as a sapphire substrate, and bumps are formed on the surface.
  • it can be applied to any form of LED chip, such as flip chip connection type that flips over and connects to the electrode on the substrate, but it is suitable for manufacturing method of high brightness type or lens type Is more preferable.
  • the phosphor particles collide with the surface on which the phosphor layer is formed at a low speed. Even when the phosphor layer is formed by depositing, the phosphor layer is covered with an inorganic layer, so that the adhesive strength of the phosphor layer can be increased and it also functions as a protective layer. Therefore, a light-emitting device that has excellent durability and little deterioration with time can be obtained. Further, since it is not necessary to increase the collision speed of the phosphor particles to the surface on which the phosphor layer is formed, no defects occur in the crystal lattice due to the impact applied when the phosphor particles collide. As a result, a reduction in luminous efficiency of the phosphor can be prevented and high luminance can be achieved.
  • LED chip an In 0.2 Ga 0.8 N semiconductor having a main emission peak of 460 nm was used.
  • the LED chip is formed by flowing a TMG (trimethylgallium) gas, a TMI (trimethylindium) gas, a nitrogen gas and a dopant gas together with a carrier gas on a cleaned sapphire substrate, and forming a gallium nitride compound semiconductor film by MOCVD. Formed.
  • N-type conductivity gallium nitride semiconductor and P-type conductivity can be obtained.
  • a gallium nitride based semiconductor was formed, and a PN junction was formed.
  • the semiconductor light emitting device includes a contact layer that is a gallium nitride semiconductor having N-type conductivity, a cladding layer that is a gallium aluminum nitride semiconductor having P-type conductivity, and a contact layer that is a gallium nitride semiconductor having P-type conductivity. Formed.
  • a non-doped InGaN active layer having a single quantum well structure having a thickness of about 3 nm was formed between the contact layer having N-type conductivity and the cladding layer having P-type conductivity.
  • a gallium nitride semiconductor was formed on the sapphire substrate at a low temperature to form a buffer layer.
  • the semiconductor having P-type conductivity was annealed at 400 ° C. or higher after film formation.
  • each PN semiconductor on the sapphire substrate was exposed by etching. Further, there are a plurality of portions where the surface of each PN semiconductor is exposed for each LED chip to be finally formed. Further, the semiconductor layer is partially removed up to the sapphire substrate so that it can be divided into rectangles for each LED chip size and electrically separated.
  • a resist was formed in advance on the pad electrode forming surface for attaching a gold wire to be a conductive wire to form a semiconductor wafer. Thereafter, the resist was removed by lift-off.
  • a scribe line was formed with a scriber. Pressing with a roller along the scribe line from the side of the sapphire substrate, the LED chips were formed by dividing them individually.
  • a chip type LED package was formed using polycarbonate resin by insert molding.
  • the chip type LED package includes an opening in which the LED chip is disposed.
  • a silver-plated copper plate is disposed as an external electrode.
  • a gold wire as a conductive wire is wire-bonded and electrically connected to each electrode of the LED chip and each external electrode provided in the package.
  • 1000 blue light emitting LED chips were formed.
  • Method for producing phosphor A >> Phosphor A ...
  • the phosphor A was dispersed in an epoxy resin so as to be 10% by mass with respect to the resin, and coated on the surface of a flat glass having a thickness of 0.5 mm so that the dry film thickness was 7 ⁇ m. The coating surface was directed to the LED chip side, and was fixed and adhered to the upper part of the package to produce a white light emitting device of Comparative Example 1.
  • Comparative Example 3 A film was formed on the glass by the same method as Comparative Example 2 except that the flow rate of the carrier gas was changed to 100 m / s on the surface of a flat glass having a thickness of 0.5 mm. The surface on which the phosphor layer was formed was directed to the LED chip side, and was fixed and adhered to the upper part of the package to produce a white light emitting device of Comparative Example 3.
  • Example 1 In order to prepare a sol solution using an organometallic compound as a raw material, 0.04 mol of tetraethoxysilane (manufactured by Wako Pure Chemical Industries, Ltd.) was weighed in a polypropylene beaker. While stirring, 0.25 mol of ethyl alcohol was added and stirred for 10 minutes with a magnetic stirrer. Further, 0.24 mol of pure water was added and stirred for 10 minutes, and then 1 ml of 1 mol / L HCL was added to prepare sol solution-1.
  • tetraethoxysilane manufactured by Wako Pure Chemical Industries, Ltd.
  • Example 1 The sample of Example 1 was produced by coating with a spin coater and drying by heating in a dry oven at 150 ° C. for 30 minutes.
  • Example 2 400 g of pure water is put into a 1 L stainless steel pot, and 600 g of silicon oxide (trade name: SFP-20M average particle size: 300 nm) manufactured by Denki Kagaku Kogyo Co., Ltd. is used at 6000 rpm using an Ultra Turrax T25 Digital (IKA). It was added over 5 minutes and then dispersed for 30 minutes.
  • the acidic solution was neutralized with triethylamine ((C 2 H 5 ) 3 N) to obtain a neutralized solution.
  • the solvent of the neutralized solution was replaced with methyl ethyl ketone to obtain a resin solution-1 having a resin nonvolatile content concentration of 60% and a viscosity of 400 cp.
  • 30 g of Dispersion-1 and 70 g of Resin Solution-1 were mixed to obtain 100 g of inorganic oxide particle coating solution-1.
  • Example 3 Sample of Example 3 in the same manner as in Example 2 except that the silicon oxide was changed to trade name: SFP-30M manufactured by Denki Kagaku Kogyo Co., Ltd. (inorganic oxide particle coating solution-2). Was made.
  • Example 4 The sample of Example 4 was prepared in the same manner as in Example 3, except that the silicon oxide was changed to alumina particles (Nippon Light Metal Fine Alumina, trade name: A33F, average particle size 700 nm) (inorganic oxide particle coating solution-3). Was made.
  • Example 5 The sample of Example 5 was prepared in the same manner as in Example 3 except that the silicon oxide was changed to zirconia particles (zirconia powder product name: 3YB average particle size 700 nm, manufactured by Toray Industries, Inc.) (inorganic oxide particle coating solution-4). Produced.
  • Example 6 The surface of a flat glass having a thickness of 0.5 mm was coated with the inorganic oxide particle coating solution-3 so that the thickness after drying was 500 nm. Subsequently, phosphor A was formed on the coating surface by the same method as in Comparative Example 3. Further, the inorganic oxide particle coating solution-2 was coated on the phosphor layer in the same manner as in Example 3, and further dried by heating in a dry oven at 150 ° C. for 30 minutes to prepare a sample of Example 6. [Example 7] A sample of Example 7 was produced in the same manner as in Example 6 except that a dome-shaped glass lens was used instead of the flat glass having a thickness of 0.5 mm in Example 6.
  • White light can be emitted by supplying power to the obtained light-emitting device.
  • the emission intensity was measured from the front of the light emitting device. That is, by supplying power and performing continuous lighting, using a spectral radiance meter CS-1000 manufactured by Konica Minolta Sensing Co., Ltd., the integrated value in the wavelength region of 400 nm to 800 nm with respect to the emission luminance (cd / m 2 ) at the start of lighting.
  • Example 1 Expressed in (Relative value where the integral value of Example 1 is 100) Further, the emission peak intensities at 460 nm and 560 nm were measured at the same time, and expressed as relative values with the intensity at each wavelength in the white light emitting device of Example 1 as 100.
  • the color temperature and color rendering were measured from the front of the light emitting device, and the variation was measured as the area on the chromaticity coordinate. That is, the luminescent color of each light emitting device was measured at a viewing angle of 2 degrees using the spectral radiance meter CS-1000 (manufactured by Konica Minolta Sensing Co., Ltd.), and the color when this data was applied to chromaticity coordinates was determined as CIE1931. The X and Y chromaticity coordinates in the color system were obtained, and the variations of these 50 samples were plotted on the chromaticity coordinates to obtain the area on the chromaticity coordinates.
  • Example 1 was expressed as a relative value with 100 as the value.
  • Examples 1 to 7 provided with the inorganic layer have higher white light intensity than Comparative Examples 1 to 3 provided with no inorganic layer.
  • variations in color temperature and color rendering are small, and it is recognized that the environmental test evaluation and vibration test have high luminance, excellent durability, and little deterioration with time.

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Abstract

L'invention concerne un procédé de production de dispositif électroluminescent (100) qui met œuvre une puce DEL (1) ; une couche de phosphore (3) qui absorbe la lumière émise par la puce DEL (1), convertit la longueur d'onde et émet de la lumière ; et au moins une couche inorganique (8) placée sur la surface de la couche de phosphore (3) afin de recouvrir ladite couche (3). Dans ce procédé, les particules de phosphore sont constituées pour entrer en collision avec la surface de sortie de lumière de la puce DEL (1) ou avec la surface (2a) d'un matériau de base (2) disposé séparément sur la puce DEL, ladite surface (2a) étant opposée à la surface de sortie de lumière de la puce DEL (1), les particules sont accumulées sur la surface, et la couche de phosphore (3) est formée. Puis, sur la surface de la couche de phosphore (3), au moins une couche inorganique est formée afin de recouvrir la couche de phosphore. Le dispositif électroluminescent présente une force d'adhésion améliorée de la couche de phosphore (3) même lorsque la vitesse de collision des particules de phosphore avec la surface sur laquelle la couche de phosphore (3) doit être formée est réduite. Le dispositif électroluminescent présente également une excellente durabilité, moins de détérioration avec le temps, et une luminance élevée par suppression de la détérioration de l'efficacité électroluminescente.
PCT/JP2010/053980 2009-06-05 2010-03-10 Procédé de production de dispositif électroluminescent, et dispositif électroluminescent WO2010140411A1 (fr)

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WO2011125646A1 (fr) * 2010-03-31 2011-10-13 Jsr株式会社 Composition de résine durcissable et dispositif électroluminescent
WO2014029642A1 (fr) * 2012-08-23 2014-02-27 Osram Opto Semiconductors Gmbh Procédé de fabrication d'un composant semi-conducteur à émission de lumière et composant semi-conducteur à émission de lumière
JP2014138081A (ja) * 2013-01-17 2014-07-28 Konica Minolta Inc 発光装置、波長変換・光拡散素子及びそれらの製造方法、光拡散セラミック層形成用組成物
JP2016072471A (ja) * 2014-09-30 2016-05-09 日亜化学工業株式会社 透光部材及びその製造方法ならびに発光装置及びその製造方法
JP2019050432A (ja) * 2018-12-28 2019-03-28 日亜化学工業株式会社 透光部材及びその製造方法ならびに発光装置及びその製造方法

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JP2006313829A (ja) * 2005-05-09 2006-11-16 Konica Minolta Opto Inc 白色発光ダイオード及びその製造方法
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011125646A1 (fr) * 2010-03-31 2011-10-13 Jsr株式会社 Composition de résine durcissable et dispositif électroluminescent
WO2014029642A1 (fr) * 2012-08-23 2014-02-27 Osram Opto Semiconductors Gmbh Procédé de fabrication d'un composant semi-conducteur à émission de lumière et composant semi-conducteur à émission de lumière
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JP2016072471A (ja) * 2014-09-30 2016-05-09 日亜化学工業株式会社 透光部材及びその製造方法ならびに発光装置及びその製造方法
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JP2019050432A (ja) * 2018-12-28 2019-03-28 日亜化学工業株式会社 透光部材及びその製造方法ならびに発光装置及びその製造方法

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