WO2012023424A1 - 発光装置の製造方法 - Google Patents

発光装置の製造方法 Download PDF

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Publication number
WO2012023424A1
WO2012023424A1 PCT/JP2011/067634 JP2011067634W WO2012023424A1 WO 2012023424 A1 WO2012023424 A1 WO 2012023424A1 JP 2011067634 W JP2011067634 W JP 2011067634W WO 2012023424 A1 WO2012023424 A1 WO 2012023424A1
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Prior art keywords
light
nozzle
light emitting
emitting device
manufacturing
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Ceased
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PCT/JP2011/067634
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English (en)
French (fr)
Japanese (ja)
Inventor
小嶋　健
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Konica Minolta Opto Inc
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Konica Minolta Opto Inc
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Priority to JP2012529551A priority Critical patent/JP5870923B2/ja
Priority to US13/817,320 priority patent/US9153752B2/en
Publication of WO2012023424A1 publication Critical patent/WO2012023424A1/ja
Anticipated expiration legal-status Critical
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/851—Wavelength conversion means
    • H10H20/8511—Wavelength conversion means characterised by their material, e.g. binder
    • H10H20/8512—Wavelength conversion materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H10H20/011—Manufacture or treatment of bodies, e.g. forming semiconductor layers
    • H10H20/013—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials
    • H10H20/0137—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials the light-emitting regions comprising nitride materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/851—Wavelength conversion means
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/851—Wavelength conversion means
    • H10H20/8511—Wavelength conversion means characterised by their material, e.g. binder
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/852—Encapsulations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/852—Encapsulations
    • H10H20/854—Encapsulations characterised by their material, e.g. epoxy or silicone resins
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P74/00—Testing or measuring during manufacture or treatment of wafers, substrates or devices
    • H10P74/20—Testing or measuring during manufacture or treatment of wafers, substrates or devices characterised by the properties tested or measured, e.g. structural or electrical properties
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H10H20/036—Manufacture or treatment of packages
    • H10H20/0361—Manufacture or treatment of packages of wavelength conversion means

Definitions

  • the present invention relates to a method for manufacturing a light emitting device.
  • phosphors such as YAG phosphors are arranged in the vicinity of a gallium nitride (GaN) -based blue LED (Light Emitting Diode) chip, and the blue light emitted from the blue LED chip and the phosphor is blue light.
  • GaN gallium nitride
  • a technique for obtaining a white LED by mixing with yellow light emitted by secondary light emission in response to the light is widely used.
  • a method of sealing an LED chip or a mounting portion using a transparent resin in which a phosphor is dispersed is generally used.
  • the specific gravity of the phosphor is larger than that of the transparent resin, the phosphor settles before the resin is cured, causing color unevenness during light emission.
  • Patent Document 1 uses a silicone resin having a viscosity of 100 cP to 10,000 cP when cured as a sealing body. Thus, it is described that the sedimentation and segregation of the phosphor is suppressed.
  • Patent Document 2 an LED element is disposed between an upper end opening and a lower end opening of a cylindrical container, and the upper end opening to the lower end opening are filled with a translucent resin.
  • a chip component type LED in which an inner wall surface of a container is formed so as to be reflected toward the opening side is disclosed.
  • Patent Document 3 discloses a light emitting device in which a liquid translucent sealing material is added with a lipophilic compound obtained by adding an organic cation to a layered compound mainly composed of clay mineral as an anti-settling agent for a phosphor, and The manufacturing method is disclosed.
  • Patent Document 1 since the LED chip is sealed with a silicone resin, deterioration such as coloring of the sealing material easily proceeds due to light emission from the LED chip or heat generation of the LED chip and the phosphor. It was difficult to obtain durability sufficient to withstand the use of In addition, the configuration of Patent Document 2 has a problem in that the configuration of the LED is complicated, leading to an increase in cost. Furthermore, in Patent Documents 2 and 3, resin materials such as epoxy resin, silicone resin, and polyimide resin are listed as specific examples of the light-transmitting sealing material. Was not enough.
  • a main object of the present invention is to provide a method of manufacturing a light emitting device including a wavelength conversion unit in which a phosphor is uniformly dispersed in a light-transmissive member having high heat resistance.
  • a light emitting element that emits light of a predetermined wavelength
  • a method for manufacturing a light emitting device having: While the nozzle for injecting the mixed liquid containing the phosphor, the layered silicate mineral, and the translucent ceramic precursor is moved relative to the light emitting element, the mixed liquid is emitted from the nozzle.
  • a method for manufacturing a light-emitting device is provided.
  • the phosphor since the liquid mixture containing the phosphor, the layered silicate mineral, and the ceramic precursor is sprayed and applied to the light emitting element, the phosphor can be applied to the light emitting element in a dispersed state. In addition, it is possible to form a wavelength conversion part in which a phosphor is uniformly dispersed in a light-transmissive member having high heat resistance.
  • the light emitting device 100 includes an LED substrate 1 having a concave cross section.
  • a metal part 2 is provided in a recess (bottom part) of the LED substrate 1, and a rectangular parallelepiped LED element 3 is disposed on the metal part 2.
  • the LED element 3 is an example of a light emitting element that emits light of a predetermined wavelength.
  • a protruding electrode 4 is provided on the surface of the LED element 3 facing the metal part 2, and the metal part 2 and the LED element 3 are connected via the protruding electrode 4 (flip chip type).
  • a configuration in which one LED element 3 is provided for one LED substrate 1 is illustrated, but a plurality of LED elements 3 may be provided in a concave portion of one LED substrate 1.
  • a blue LED element is used as the LED element 3.
  • a blue LED element is formed by laminating an n-GaN-based cladding layer, an InGaN light-emitting layer, a p-GaN-based cladding layer, and a transparent electrode on a sapphire substrate.
  • a wavelength converter 6 is formed in the recess of the LED substrate 1 so as to seal the periphery of the LED element 3.
  • the wavelength conversion unit 6 is a part that converts light having a predetermined wavelength emitted from the LED element 3 into light having a different wavelength, and is excited by the wavelength from the LED element 3 in the translucent ceramic layer.
  • a phosphor that emits fluorescence having a wavelength different from the excitation wavelength is added.
  • the wavelength conversion unit 6 is formed so as to seal the periphery of the LED element 3, but the wavelength conversion unit 6 may be provided only on the periphery (upper surface and side surface) of the LED element 3, and the LED substrate.
  • the wavelength conversion unit 6 may not be provided in the concave portion 1.
  • a method of providing the wavelength conversion unit 6 only around the LED element 3 a method of installing a mask or the like is used when forming the wavelength conversion unit 6.
  • the wavelength conversion unit 6 is a transparent ceramic layer (glass body) formed by a so-called sol-gel method in which a sol-like mixed liquid in which an organic metal compound is mixed with an organic solvent is heated to be in a gel state and then fired.
  • the transparent ceramic layer contains a phosphor, a layered silicate mineral, and inorganic fine particles.
  • the organometallic compound serves as a binder for sealing the phosphor, the layered silicate mineral, and the inorganic fine particles.
  • organometallic compound used in the present invention include metal alkoxides, metal acetylacetonates, metal carboxylates, and the like, but metal alkoxides that are easily gelled by hydrolysis and polymerization reaction are preferable.
  • the metal alkoxide may be a single molecule such as tetraethoxysilane, or may be a polysiloxane in which an organic siloxane compound is linked in a chain or a ring, but a polysiloxane that increases the viscosity of the mixed solution is preferable.
  • a translucent glass body can be formed, but it is preferable to contain a silicon
  • the content of the organometallic compound in the ceramic layer is less than 2% by weight, the organometallic compound as the binder is too small, and the strength of the ceramic layer after heating and firing is lowered.
  • the content of the organometallic compound exceeds 50% by weight, the content of the layered silicate mineral is relatively lowered, so that the viscosity of the mixed solution before heating is lowered and the phosphor is easily precipitated. .
  • the content of the inorganic fine particles is relatively lowered, the strength of the ceramic layer is also lowered. Therefore, the content of the organometallic compound in the ceramic layer is preferably 2% by weight to 50% by weight, and more preferably 2.5% by weight to 30% by weight.
  • Polysilazane can also be used as the organometallic compound.
  • the polysilazane used in the present invention is represented by the following general formula (1).
  • R 1, R 2 and R 3 each independently represent a hydrogen atom or an alkyl group, an aryl group, a vinyl group or a cycloalkyl group, and at least one of R 1, R 2 and R 3 is a hydrogen atom, All are preferably hydrogen atoms, and n represents an integer of 1 to 60.
  • the molecular shape of polysilazane may be any shape, for example, linear or cyclic.
  • the polysilazane represented by the above formula (1) and a reaction accelerator as required are dissolved in an appropriate solvent and then cured by heating, excimer light treatment, UV light treatment, and excellent heat resistance and light resistance.
  • a ceramic film can be made.
  • the effect of preventing penetration of moisture can be further improved by heat curing after irradiation with UVU radiation (eg, excimer light) containing a wavelength component in the range of 170 to 230 nm.
  • UVU radiation eg, excimer light
  • an acid, a base, or the like is preferably used, but it may not be used.
  • reaction accelerators include triethylamine, diethylamine, N, N-diethylethanolamine, N, N-dimethylethanolamine, triethanolamine, triethylamine, hydrochloric acid, oxalic acid, fumaric acid, sulfonic acid, acetic acid, nickel, iron, palladium , Metal carboxylates including iridium, platinum, titanium, and aluminum, but are not limited thereto. Particularly preferred when a reaction accelerator is used is a metal carboxylate, and the addition amount is preferably 0.01 to 5 mol% based on polysilazane.
  • the solvent aliphatic hydrocarbons, aromatic hydrocarbons, halogen hydrocarbons, ethers, and esters can be used.
  • methyl ethyl ketone Preferred are methyl ethyl ketone, tetrahydrofuran, benzene, toluene, xylene, dimethyl fluoride, chloroform, carbon tetrachloride, ethyl ether, isopropyl ether, dibutyl ether, and ethyl butyl ether.
  • the polysilazane concentration is preferably high, but the increase in concentration leads to a shortening of the polysilazane storage period. Therefore, the polysilazane is preferably dissolved in the solvent at 5 to 50 wt% (wt%) or less.
  • the heating temperature during firing is preferably 150 ° C. to 500 ° C., and preferably 150 ° C. to 350 ° C. from the viewpoint of suppressing the deterioration of the glass material used as the substrate. More preferably.
  • the phosphor is excited by the wavelength of the light emitted from the LED element 3 (excitation wavelength) and emits fluorescence having a wavelength different from the excitation wavelength.
  • a YAG (yttrium, aluminum, garnet) phosphor that converts blue light (wavelength 420 nm to 485 nm) emitted from the blue LED element into yellow light (wavelength 550 nm to 650 nm) is used.
  • Such phosphors use oxides of Y, Gd, Ce, Sm, Al, La, and Ga, or compounds that easily become oxides at high temperatures, and are mixed well in a stoichiometric ratio.
  • a mixed raw material is obtained.
  • a coprecipitated oxide obtained by calcining a solution obtained by coprecipitation of a solution obtained by dissolving a rare earth element of Y, Gd, Ce, or Sm in an acid with a stoichiometric ratio with oxalic acid, and aluminum oxide or gallium oxide.
  • an appropriate amount of fluoride such as ammonium fluoride is mixed with the obtained mixed raw material as a flux and pressed to obtain a molded body.
  • the obtained molded body is 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 sintered body having the light emission characteristics of a phosphor.
  • the YAG phosphor is used.
  • the type of the phosphor is not limited to this.
  • other phosphors such as non-garnet phosphors containing no Ce are used. You can also.
  • the larger the particle size of the phosphor the higher the light emission efficiency (wavelength conversion efficiency).
  • the gap formed at the interface with the organometallic compound is increased, and the film strength of the formed ceramic layer is lowered. Accordingly, in consideration of the size of the gap generated at the interface between the light emission efficiency and the organometallic compound, it is preferable to use one having an average particle diameter of 1 ⁇ m or more and 50 ⁇ m or less.
  • the average particle diameter of the phosphor can be measured, for example, by a Coulter counter method.
  • the layered silicate mineral is preferably a swellable clay mineral having a structure such as a mica structure, a kaolinite structure, or a smectite structure, and particularly preferably a smectite structure rich in swellability. This is because, as will be described later, by adding water to the mixed solution, water enters the interlayer of the smectite structure and swells to form a card house structure, which has the effect of greatly increasing the viscosity of the mixed solution in a small amount. Because there is. Since the layered silicate mineral has a flat plate shape in the ceramic layer, the film strength of the ceramic layer can be improved.
  • the content of the layered silicate mineral in the ceramic layer is less than 0.5% by weight, the effect of increasing the viscosity of the mixed solution cannot be obtained sufficiently.
  • the content of the layered silicate mineral exceeds 20% by weight, the strength of the ceramic layer after heating is lowered. Therefore, the content of the layered silicate mineral is preferably 0.5% by weight or more and 20% by weight or less, and more preferably 0.5% by weight or more and 10% by weight or less.
  • a layered silicate mineral whose surface is modified (surface treatment) with an ammonium salt or the like can be used as appropriate.
  • Inorganic fine particles include a filling effect that fills gaps formed at the interface between the organometallic compound, the phosphor and the layered silicate mineral, a thickening effect that increases the viscosity of the mixed solution before heating, and a ceramic layer film after heating. It has a film strengthening effect that improves strength.
  • Examples of the inorganic fine particles used in the present invention include oxide fine particles such as silicon oxide, titanium oxide and zinc oxide, and fluoride fine particles such as magnesium fluoride.
  • silicon oxide fine particles such as silicon oxide, titanium oxide and zinc oxide
  • fluoride fine particles such as magnesium fluoride.
  • silicon oxide fine particles such as silicon oxide, titanium oxide and zinc oxide
  • fluoride fine particles such as magnesium fluoride.
  • silicon oxide fine particles such as silicon-containing organic compound such as polysiloxane
  • the content of the inorganic fine particles in the ceramic layer is less than 0.5% by weight, the above-described effects cannot be sufficiently obtained.
  • the content of the inorganic fine particles exceeds 50% by weight, the strength of the ceramic layer after heating is lowered. Therefore, the content of the inorganic fine particles in the ceramic layer is 0.5 wt% or more and 50 wt% or less.
  • the content of the inorganic fine particles in the ceramic layer is preferably 0.5% by weight or more and 40% by weight or less.
  • the average particle diameter of the inorganic fine particles is preferably 0.001 ⁇ m or more and 50 ⁇ m or less, more preferably 0.005 ⁇ m or more and 20 ⁇ m or less in consideration of the above-described effects.
  • the average particle diameter of the inorganic fine particles can be measured, for example, by a Coulter counter method.
  • a material obtained by treating the surface of inorganic fine particles with a silane coupling agent or a titanium coupling agent can be used as appropriate.
  • the precursor solution is a mixture of an organometallic compound in an organic solvent, and a translucent ceramic layer can be obtained by heating the precursor solution.
  • the wavelength conversion part 6 is formed by heating the liquid mixture which mixed fluorescent substance, a layered silicate mineral, and inorganic fine particles with this precursor solution. Furthermore, when water is added to the mixed solution, water enters between the layers of the layered silicate mineral and the viscosity of the mixed solution increases, so that sedimentation of the phosphor can be suppressed. In addition, since there exists a possibility of inhibiting a polymerization reaction when the impurity is contained in water, it is necessary to use the pure water which does not contain an impurity for the water to add.
  • the organic solvent alcohols such as methanol, ethanol, propanol and butanol having excellent compatibility with added water are preferable. Further, when the amount of the organometallic compound mixed with the organic solvent is less than 5% by weight, it becomes difficult to increase the viscosity of the mixed solution, and when the amount of the organometallic compound exceeds 50% by weight, the polymerization reaction is faster than necessary. Proceed. Therefore, the amount of the organometallic compound mixed with the organic solvent is preferably 5% by weight or more and 50% by weight or less, and more preferably 8% by weight or more and 40% by weight or less.
  • the layered silicate mineral when using a surface-treated lipophilic layered silicate mineral, the layered silicate mineral is first added to a solution (precursor solution) in which an organometallic compound is mixed in an organic solvent. Premixing is performed, and then phosphor, inorganic fine particles, and water are mixed.
  • a hydrophilic layered silicate mineral that has not been surface-treated is used, first the layered silicate mineral and water are premixed, and then the phosphor, inorganic fine particles, and precursor solution are mixed. Thereby, a layered silicate mineral can be mixed uniformly and the thickening effect can be heightened more.
  • the preferred viscosity of the mixed solution is 25 to 800 cP, and the most preferred viscosity is 30 to 500 cP.
  • the ratio of the water with respect to the total amount of solvent shall be 5% or more.
  • the ratio of water is preferably 5% by weight or more and 60% by weight or less, and more preferably 7% by weight or more and 55% by weight or less with respect to the total amount of solvent.
  • the most preferred composition of the mixed solution is one using polysiloxane as the organometallic compound, and the most preferred composition range of each of the above components contained in the mixed solution is 35 to 65% by weight of the polysiloxane dispersion and layered silica.
  • the acid salt mineral is 0.1 to 5% by weight
  • the inorganic fine particles are 1 to 40% by weight
  • the water is 5 to 50% by weight.
  • the manufacturing method of the light-emitting device 100 (wavelength conversion part 6) is demonstrated.
  • the manufacturing apparatus 10 When manufacturing the wavelength conversion part 6 of the light-emitting device 100, the manufacturing apparatus 10 of FIG. 2, for example is used.
  • the manufacturing apparatus 10 mainly includes a movable table 20 that can move up and down, left and right, and back and forth, a spray device 30 that can spray the mixed liquid (40) described above, and the chromaticity and luminance of the wavelength conversion unit 6. And an inspection device 50 capable of inspecting.
  • the spray device 30 is disposed above the movable table 20.
  • the spray device 30 has a nozzle 32 into which air is sent.
  • the structure which sprays the liquid mixture 40 toward the upper direction in which the spray apparatus 30 is installed below the movable stand 20 may be sufficient.
  • the hole diameter at the tip of the nozzle 32 is 20 ⁇ m to 2 mm, preferably 0.1 to 0.3 mm.
  • the nozzle 32 is movable up and down, left and right, and front and rear, like the moving table 20. In particular, the angle of the nozzle 32 can be adjusted, and the nozzle 32 can be inclined with respect to the movable table 20 (or the LED substrate 1 installed on the moving table 20).
  • the nozzle 32 has a built-in temperature adjustment mechanism, and can adjust the temperature of the ejected matter.
  • a tank 36 is connected to the nozzle 32 via a connecting pipe 34.
  • a mixed liquid 40 is stored in the tank 36.
  • the tank 36 contains a stirring bar, and the mixed solution 40 is constantly stirred. If the liquid mixture 40 is stirred, sedimentation of the phosphor having a large specific gravity can be suppressed, and the state in which the phosphor is dispersed in the liquid mixture 40 can be maintained.
  • a pressure is applied to the liquid mixture 40 itself of the tank 36 using a motor or the like as a drive source, or the liquid mixture 40 is injected from the nozzle 32, or It is good also as a mechanism which extrudes.
  • the pressure variation with respect to the mixed liquid 40 is set to be within 10%.
  • the inspection device 50 includes an LED element 52 and a color luminance meter 54.
  • the LED element 52 is an element that emits light similar to the LED element 3.
  • the color luminance meter 54 is a measuring instrument that measures the chromaticity and luminance of received light.
  • the liquid mixture 40 is sprayed and applied in advance to a glass plate 60 for chromaticity / luminance adjustment (for testing), so that the chromaticity of white light is increased. And brightness are measured in advance (preliminary spraying / coating process).
  • the glass plate 60 is installed on the moving table 20, and the moving table 20 and the nozzle 32 of the spray device 30 are controlled so that the glass plate 60 and the tip of the nozzle 32 are arranged to face each other.
  • the liquid mixture 40 is sprayed and applied from the nozzle 32 to the glass plate 60, the glass plate 60 coated with the liquid mixture 40 is transferred to the vicinity of the inspection device 50, and the light emitting element 52 emits light.
  • the chromaticity and luminance of the white light are measured by the color luminance meter 54, and it is confirmed whether or not the chromaticity and luminance of the white light have a desired value (range).
  • the pre-spraying / coating process is repeated until the chromaticity and brightness of white light are stabilized.
  • the spraying pressure of the spray or the concentration of the phosphor in the liquid mixture 40 should be adjusted to a desired value. Can do.
  • the adjustment at this time is preferably automatically performed according to the measurement value, but may be manually adjusted according to the measurement value.
  • a plurality of LED substrates 1 (on which the LED elements 3 are mounted in advance) are installed on the moving base 20, and the positional relationship between the LED substrate 1 and the nozzle 32 of the spray device 30 is adjusted (position) Adjustment process).
  • the LED substrate 1 is installed on the moving table 20 in the same manner as when the glass plate 60 is installed, and the LED substrate 1 and the tip of the nozzle 32 are arranged to face each other.
  • the distance between the LED substrate 1 and the tip of the nozzle 32 is 5 to 30 cm.
  • the mixed solution 40 is sprayed from the nozzle 32 to apply the mixed solution 40 to the LED substrate 1 (spraying / coating step).
  • the moving base 20 and the nozzle 32 are moved to move the LED substrate 1 and the nozzle 32 back and forth and right and left.
  • Either one of the moving table 20 and the nozzle 32 may be fixed, and the other may be moved back and forth and left and right.
  • a method of applying a plurality of LED elements 3 in a direction orthogonal to the moving direction of the moving table 20 and moving the nozzle 32 in a direction orthogonal to the moving direction of the moving table 20 is also preferably used.
  • air is fed into the nozzle 32 and the mixed liquid 40 is sprayed from the tip of the nozzle 32 toward the LED substrate 1.
  • the tip end portion of the nozzle 32 is disposed immediately above the LED substrate 1 and the mixed liquid 40 is sprayed from directly above the LED element 3.
  • the LED element 3 has a rectangular parallelepiped shape, in addition to or instead of injecting the mixed liquid 40 from directly above the LED element 3, for example, the nozzle 32 is inclined to form four corners of the LED element 3. You may inject the liquid mixture 40 from the diagonal direction.
  • the mixed liquid 40 is sprayed from four directions by reducing the spray angle of the nozzle 32, the mixed liquid 40 can be uniformly applied also to the side surface of the LED element 3.
  • the injection angle of the nozzle 32 can be set as appropriate, and is preferably 45 °.
  • the injection amount of the mixed liquid 40 is constant, and the phosphor amount per unit area is constant.
  • the variation with time of the injection amount of the mixed liquid 40 is within 10%, preferably within 1%.
  • the temperature of the nozzle 32 is adjusted to adjust the viscosity when the mixed liquid 40 is jetted.
  • the temperature of the mixed solution 40 is adjusted to 40 ° C. or lower, or adjusted according to the viscosity of the mixed solution 40.
  • the LED substrate 1 may be in a room temperature environment, or a temperature adjustment mechanism may be provided on the moving base 20 to control the temperature of the LED substrate 1. If the temperature of the LED substrate 1 is set high at 30 to 100 ° C., the organic solvent in the mixed solution 40 sprayed onto the LED substrate 1 can be volatilized quickly, and the mixed solution 40 drips from the LED substrate 1. Can be prevented.
  • the solvent can be volatilized slowly, and the mixed solution 40 can be uniformly applied along the outer wall of the LED element 3.
  • the film density, film strength, and the like of the conversion unit 6 can be increased, and a dense film can be formed.
  • the environmental atmosphere (temperature / humidity) of the manufacturing apparatus 10 is made constant, and the injection of the mixed liquid 40 is stabilized.
  • the humidity is preferably lowered when the mixed solution 40 is sprayed.
  • a mask corresponding to the shape of the LED element 3 is arranged between the spray device 30 and the LED substrate 1, and the mixed liquid 40 is sprayed through the mask.
  • the mask it is necessary to use a material that does not dissolve in the organic solvent that constitutes the mixed solution 40, but a flammable material is preferably used from the viewpoint of recovery of a material such as a phosphor attached to the mask.
  • the chromaticity and luminance of white light by the mixed liquid 40 are measured by the color luminance meter 54, and the injection amount, the injection pressure, the injection temperature (the temperature of the nozzle 32), etc. of the mixed liquid 40 are changed based on the measurement result. Also good.
  • the mixed liquid 40 may be sprayed / coated on the glass plate 60, and this may be used as an inspection target for chromaticity or luminance of white light.
  • the LED element 52 is allowed to emit light and the chromaticity and luminance of white light can be measured.
  • the nozzle 32 may be cleaned during the spraying / coating process.
  • a cleaning tank storing the cleaning liquid is installed in the vicinity of the spray device 30, and the tip of the nozzle 32 is placed in the cleaning tank during the suspension of the jetting of the mixed liquid 40 or the inspection of the chromaticity / luminance of white light. It is soaked in that the tip of the nozzle 32 is prevented from drying.
  • a liquid that can dissolve the mixed liquid 40 can be used as the cleaning liquid.
  • the liquid mixture 40 may harden and the spray holes of the nozzle 32 may become clogged. Therefore, the nozzle 32 may be immersed in the cleaning tank, or the nozzle at the start of the spraying / coating process. It is preferable to perform 32 cleaning.
  • the cleaning of the nozzle 32 may be performed before executing the spraying / coating process itself.
  • the liquid mixture 40 is sprayed in the form of a mist. Therefore, when the organic solvent in the liquid mixture 40 volatilizes, powders such as phosphors and inorganic fine particles may be scattered.
  • the entire manufacturing apparatus 10 is covered with a housing or the like, and the processes of the spraying / coating process and the inspection process are performed while collecting / exhausting the dust through the filter. If the phosphor is collected by a filter, the expensive phosphor can be reused.
  • the LED substrate 1 coated with the mixed solution 40 is transferred to a sintering furnace, and the mixed solution 40 is baked (baking step).
  • the processing temperature sintering temperature
  • the processing temperature is set to such an extent that the LED element 3 is not damaged, and is 100 to 300 ° C., preferably 130 to 170 ° C., more preferably 140 to 160 ° C., and most preferably 150 It should be around °C.
  • the mixed liquid 40 is sintered and the wavelength conversion unit 6 is manufactured (formed).
  • the liquid mixture 40 containing the phosphor since the liquid mixture 40 containing the phosphor is sprayed and applied to the LED element 3, it can be applied to the LED element 3 in a state where the phosphor is dispersed, and has high heat resistance.
  • the wavelength conversion unit 6 in which the phosphor is uniformly dispersed in the ceramic layer can be formed.
  • the obtained fired product was pulverized, washed, separated, and dried to obtain yellow phosphor particles having an average particle diameter of about 10 ⁇ m.
  • the emission wavelength of excitation light having a wavelength of 465 nm of the phosphor particles was measured, it had a peak wavelength at a wavelength of approximately 570 nm.
  • the mixing amount of the polysiloxane, smectite, phosphor, and silicon oxide fine particles was determined so that the sum of the weight% in the ceramic layer after the heat polymerization was 100% by weight (the following mixed liquids 1-2 to 1). The same applies to ⁇ 3, 2-1 to 2-2).
  • liquid mixture 1-2 Lipophilic smectite (Lucentite SPN, manufactured by Coop Chemical Co., Ltd.) surface-treated in 1 g of polysiloxane dispersion (polysiloxane 14% by weight, isopropyl alcohol 86% by weight) ) 0.01 g was mixed and dispersed. In this dispersion, 0.7 g of the phosphor particles prepared above, 0.03 g of silicon oxide fine particles (Hisilica F3, manufactured by Nichetsu) having a particle size distribution of 1 to 24 ⁇ m, a median diameter (D50) of 3 ⁇ m, and 0.07 g of pure water were added. By mixing, “mixed liquid 1-2” was prepared.
  • liquid mixture 2-1 0.3 g of the phosphor particles prepared above were mixed in 1 g of a polysiloxane dispersion (polysiloxane 14 wt%, isopropyl alcohol 86 wt%). Liquid 2-1 ” was prepared.
  • Table 1 shows component data of the mixed liquids 1-1 to 1-3 and 2-1 to 2-2.
  • “*” represents the ratio of water to the total amount of solvent (the total amount of the solvent obtained by adding the organic solvent and water).
  • Viscosity of mixed liquids 1-1 to 1-3 and 2-1 to 2-2 was measured using a vibration viscometer (VM-10A-L, manufactured by CBC). did.
  • the mixed liquid 1-1 has a film thickness of 35 ⁇ m after firing, and the mixed liquid 1-2 and the mixed liquid 2-2 have a film thickness of 40 ⁇ m after firing.
  • the mixed solution 1-3 and the mixed solution 2-1 were applied by a spray device onto an LED substrate provided with 20 blue LED chips, so that the thickness of the fired ceramic layer was 45 ⁇ m.
  • the ceramic layer (wavelength conversion part) was produced by heating at 60 ° C. for 60 minutes.
  • the light emitting device in which the wavelength conversion unit is prepared using the mixed liquids 1-1 to 1-3 is used as a sample of “Examples 1 to 3,” and the wavelength conversion is performed using the mixed liquids 2-1 to 2-2.
  • the light emitting device in which the part was manufactured was used as a sample of “Comparative Examples 1 and 2”.
  • the average value of the film thickness on each LED chip of one sample applied first was set as a reference value (100%), and the remaining four units When the variation of the average value of the film thickness on each LED chip of the sample with respect to the reference value is within a range of ⁇ 10%, “ ⁇ ”, when the variation is within a range of ⁇ 20%, “ ⁇ ”, ⁇ 30 % When it was within the range of%, and “x” when the variation in film thickness exceeded ⁇ 40%.
  • the chromaticity of white light is (0.33, 0.33). The closer the chromaticity is to this value, the closer to white light.
  • the five chromaticities in Table 2 are the chromaticities of each of the five samples, and the value of each sample is the chromaticity measured by emitting any three LED chips out of the plurality of LED chips in the LED substrate. Is the average value.
  • the present invention can be suitably used to uniformly disperse phosphors in a light-transmissive member having high heat resistance in a method for manufacturing a light-emitting device.

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US20140349419A1 (en) 2014-11-27
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US8835192B2 (en) 2014-09-16
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US9306130B2 (en) 2016-04-05
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US20130143343A1 (en) 2013-06-06
EP2608284A1 (en) 2013-06-26
US20130149801A1 (en) 2013-06-13
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US9153752B2 (en) 2015-10-06
JP2013229621A (ja) 2013-11-07

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