WO2015011925A1 - Procédé de fabrication de dispositif à diode électroluminescente - Google Patents

Procédé de fabrication de dispositif à diode électroluminescente Download PDF

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Publication number
WO2015011925A1
WO2015011925A1 PCT/JP2014/003891 JP2014003891W WO2015011925A1 WO 2015011925 A1 WO2015011925 A1 WO 2015011925A1 JP 2014003891 W JP2014003891 W JP 2014003891W WO 2015011925 A1 WO2015011925 A1 WO 2015011925A1
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wavelength conversion
led device
conversion layer
led
layered clay
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PCT/JP2014/003891
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Japanese (ja)
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小嶋　健
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Konica Minolta Inc
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Konica Minolta Inc
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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
    • H10H20/852—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
    • 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]
    • H10H20/01—Manufacture or treatment
    • H10H20/036—Manufacture or treatment of packages
    • H10H20/0361—Manufacture or treatment of packages of wavelength conversion means
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W74/00—Encapsulations, e.g. protective coatings
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W74/00—Encapsulations, e.g. protective coatings
    • H10W74/10—Encapsulations, e.g. protective coatings characterised by their shape or disposition
    • H10W74/15—Encapsulations, e.g. protective coatings characterised by their shape or disposition on active surfaces of flip-chip devices, e.g. underfills

Definitions

  • the present invention relates to a method for manufacturing an LED device.
  • phosphors such as YAG phosphors have been placed in the vicinity of gallium nitride (GaN) -based blue LED (Light Emitting Diode) chips to receive blue light and blue light emitted from the blue LED elements.
  • GaN gallium nitride
  • An LED device that obtains white light by mixing yellow light emitted from a phosphor has been developed.
  • an LED device that obtains white light by arranging various phosphors in the vicinity of a blue LED element and mixing blue light emitted from the blue LED element with red light and green light emitted from the phosphor upon receiving blue light. has also been developed.
  • White LED devices are widely applied to various lighting devices; in order to reduce the cost of lighting devices, there is a demand for improved light extraction efficiency from LED devices and longer life of LED devices.
  • Patent Documents 2 and 3 propose that the LED element is covered with a wavelength conversion layer in which a phosphor is dispersed in ceramic.
  • a wavelength conversion layer is formed by applying a phosphor dispersion in which a phosphor is dispersed in a solvent.
  • a phosphor having a high specific gravity tends to settle. Therefore, in this technique, a swellable clay compound such as smectite is dispersed in the phosphor dispersion liquid to increase the viscosity of the phosphor dispersion liquid and enhance the dispersion stability of the phosphor.
  • JP 2005-136379 A International Publication No. 2011/129320 International Publication No. 2012/023425
  • Swellable clay compounds such as smectite contained in the wavelength conversion layer described above are easy to absorb moisture, and more easily conduct electricity.
  • smectite absorbs moisture, current leaks to the wavelength conversion layer when the LED device is used.
  • the metal reflective layer in contact with the wavelength conversion layer is corroded, and the light reflectivity of the metal reflective layer is lowered. That is, the light extraction efficiency from the LED device decreases with time.
  • the present invention has been made in view of the above-described problems. That is, the objective of this invention is providing the manufacturing method of the LED device which can maintain favorable light extraction efficiency over a long period of time.
  • this invention relates to the manufacturing method of the following LED devices.
  • a substrate, an LED element disposed on the substrate, a metal reflective layer disposed on the substrate and around the LED element, and a wavelength conversion layer covering the LED element and the metal reflective layer A method of preparing an LED device including an LED element and a metal reflective layer disposed on a substrate, and covering the LED element and the metal reflective layer of the LED package.
  • concentration of a clay compound is 2 mass% is a manufacturing method of the LED apparatus which is 500 microsiemens / cm or less.
  • the non-conductive layered clay compound is a compound in which the electric conductivity of an aqueous solution in which the concentration of the non-conductive layered clay compound is 2% by mass is 10 to 80 ⁇ S / cm. Of manufacturing the LED device.
  • the non-conductive layered clay compound is a compound in which the electric conductivity of an aqueous solution in which the concentration of the non-conductive layered clay compound is 2% by mass is 150 to 500 ⁇ S / cm. Of manufacturing the LED device.
  • the non-conductive layered clay compound is one or more compounds selected from the group consisting of muscovite, phlogopite, sericite, fluorine phlogopite, potassium tetrasilicon mica, and synthetic mica. 6] The manufacturing method of the LED device in any one of. [8] The method for manufacturing an LED device according to any one of [1] to [7], wherein the non-conductive layered clay compound has a water absorption rate of 0.2% by mass or more. [9] The method for manufacturing an LED device according to any one of [1] to [8], wherein the solvent includes alcohol.
  • the current hardly leaks in the wavelength conversion layer of the LED device obtained by the manufacturing method of the present invention. Therefore, the metal reflective layer hardly deteriorates with time, and high light extraction performance is realized over a long period of time.
  • the LED device 100 obtained by the manufacturing method of the present invention is disposed on the substrate 1, the LED element 3 disposed on the substrate 1, and on the substrate 1 and around the LED element 3.
  • a metal portion composed of the metal reflection layer 2 and the protruding electrode 4 and the wavelength conversion layer 5 covering the LED element 3 and the metal portion are included.
  • the LED device 100 includes a sealing layer 6 that covers the wavelength conversion layer 5 as necessary.
  • the wavelength conversion layer 5 of the present invention contains a layered clay compound.
  • the layered clay compound is a compound for enhancing the dispersion stability of the phosphor in the phosphor dispersion for preparing the wavelength conversion layer 5.
  • the conventional wavelength conversion layer contains a large amount of layered clay compounds having high hygroscopicity and high electrical conductivity. Therefore, when the layered clay compound absorbs moisture, current easily leaks to the wavelength conversion layer when the LED device is used. When the current leaks, there is a problem that the metal reflection layer and the metal electrode in contact with the wavelength conversion layer corrode, and the light extraction efficiency from the LED device decreases with time.
  • a non-conductive layered clay compound that hardly conducts electricity to the wavelength conversion layer 5 is included.
  • the non-conductive layered clay compound refers to a layered clay compound having an electric conductivity of 500 ⁇ S / cm or less when an aqueous solution having a concentration of 2% by mass is formed. That is, the nonconductive layered clay compound has low electrical conductivity even in a wet state. Therefore, even if the non-conductive layered clay compound absorbs moisture, current leakage to the wavelength conversion layer 5 is suppressed. As a result, corrosion of the metal part is suppressed over a long period of time, and high light extraction efficiency from the LED device 100 is maintained.
  • the electric conductivity of the aqueous solution of the non-conductive layered clay compound is preferably 250 ⁇ S / cm or less, more preferably 100 ⁇ S / cm or less.
  • the electrical conductivity is 10 to 80 ⁇ S / cm, corrosion of the metal part is easily suppressed, and high light extraction efficiency from the LED device 100 is easily maintained.
  • the electrical conductivity is 150 to 500 ⁇ S / cm, corrosion of the metal part is suppressed, and the dispersion stability of the phosphor in the phosphor dispersion liquid for preparing the wavelength conversion layer is likely to increase.
  • the electrical conductivity of the aqueous solution of the non-conductive layered clay compound is measured as follows.
  • the non-conductive layered clay compound and water are mixed so that the concentration of the non-conductive layered clay compound is 2% by mass. And the said liquid mixture is mixed for 5 minutes with an ultrasonic wave, and a nonelectroconductive layered clay compound is fully disperse
  • the electrical conductivity of the aqueous solution is measured with an electrical conductivity meter.
  • An example of the electrical conductivity meter is LAQUATwin B771 manufactured by Horiba, Ltd.
  • the substrate 1 may have a cavity (concave portion) as shown in FIG. 1 or may have a flat plate shape.
  • the shape of the cavity that the substrate 1 has is not particularly limited. For example, a truncated cone shape, a truncated pyramid shape, a cylindrical shape, a prismatic shape, or the like may be used.
  • the substrate 1 preferably has insulating properties and heat resistance, and is preferably made of a ceramic resin or a heat resistant resin.
  • the heat resistant resin include liquid crystal polymer, polyphenylene sulfide, aromatic nylon, epoxy resin, hard silicone resin, polyphthalic acid amide and the like.
  • the substrate 1 may contain an inorganic filler.
  • the inorganic filler can be titanium oxide, zinc oxide, alumina, silica, barium titanate, calcium phosphate, calcium carbonate, white carbon, talc, magnesium carbonate, boron nitride, glass fiber, and the like.
  • Metal wiring is usually formed on the surface of the substrate 1.
  • the metal wiring is a member that supplies electricity to the LED element 3 from a power source (not shown) arranged outside the substrate 1, and the metal reflection layer 2 described later may also serve as the metal wiring.
  • the metal reflection layer 2 also serves as a metal wiring.
  • the LED element 3 is electrically connected to a metal wiring formed on the surface of the substrate 1 and emits light of a specific wavelength.
  • the wavelength of the light emitted from the LED element 3 is not particularly limited.
  • the LED element 3 may be, for example, an element that emits blue light (light of about 420 nm to 485 nm) or an element that emits ultraviolet light.
  • the configuration of the LED element 3 is not particularly limited.
  • the LED element 3 is an element that emits blue light
  • the LED element 3 includes an n-GaN compound semiconductor layer (cladding layer), an InGaN compound semiconductor layer (light emitting layer), and a p-GaN compound semiconductor layer. It may be a laminate of (cladding layer) and a transparent electrode layer.
  • the LED element 3 may have a light emitting surface of 200 to 300 ⁇ m ⁇ 200 to 300 ⁇ m, for example.
  • the height of the LED element 3 is usually about 50 to 200 ⁇ m. In the LED device 100 shown in FIG. 1, only one LED element 3 is disposed on the substrate 1, but a plurality of LED elements 3 may be disposed on the substrate 1.
  • connection method between the LED element 3 and the metal wiring formed on the surface of the substrate 1 is not particularly limited.
  • the LED element 3 and the metal wiring (metal reflection layer) 2 may be connected via the protruding electrode 4.
  • the LED element 3 and the metal wiring 2 may be connected via a wire.
  • a mode in which the LED element 3 and the metal wiring 2 are connected via the protruding electrode 4 is referred to as a flip chip type.
  • a mode in which the LED element 3 and the metal wiring 2 are connected via a wire is called a wire bonding type.
  • a metal part means the metal members formed on the board
  • the metal part is covered with a wavelength conversion layer 5 described later.
  • the metal reflection layer 2 When the metal reflection layer 2 is included in the LED device 100, the light emitted from the LED element 3 and the fluorescence emitted from the phosphor in the wavelength conversion layer 5 are reflected to the light extraction surface side. As a result, the light extraction efficiency from the LED device 100 is increased.
  • the metal reflection layer 2 may also serve as a metal wiring for supplying electricity to the LED element 3; the pattern of the metal reflection layer 2 depends on the connection method between the LED element 3 and the metal wiring, and the like. Are appropriately selected.
  • the metal reflection layer 2 only needs to be formed at least around the LED element 3, and may be formed between the LED element 3 and the substrate 1 as shown in FIG. 1, for example. Further, when the substrate 1 has a cavity, the metal reflection layer 2 may be formed on the inner wall surface 7 of the cavity. When the metal reflection layer 2 is formed on the cavity inner wall surface 7, light traveling in the horizontal direction on the surface of the wavelength conversion layer 5 can be reflected by the metal reflection layer 2 and extracted.
  • the metal reflection layer 2 is not particularly limited as long as it is a layer made of a metal capable of reflecting light.
  • it may be a layer made of copper, aluminum, silver, palladium, or an alloy thereof.
  • the thickness of the metal reflective layer 2 is not particularly limited, and is preferably 100 to 1000 ⁇ m, more preferably 200 to 600 ⁇ m.
  • the metal reflective layer 2 whose surface is silver-plated is particularly easy to improve light reflectivity.
  • the wavelength conversion layer 5 is a layer that covers the LED element 3 and the metal part (the metal reflection layer 2, the protruding electrode 4, etc.), and is a layer that is formed by applying a phosphor dispersion described later. .
  • the wavelength conversion layer 5 includes a phosphor that emits fluorescence upon receiving light (excitation light) emitted from the LED element 3.
  • excitation light light
  • the color of the light from the LED device 100 becomes a desired color. For example, when the light from the LED element 3 is blue and the fluorescence emitted from the phosphor included in the wavelength conversion layer 5 is yellow, the light from the LED device 100 is white.
  • the wavelength conversion layer 5 contains a non-conductive layered clay compound and inorganic oxide fine particles in addition to the phosphor.
  • the wavelength conversion layer 5 contains a non-conductive layered clay compound or inorganic oxide fine particles, not only the dispersion stability of the phosphor is increased in the phosphor dispersion liquid when the wavelength conversion layer 5 is produced, but also the wavelength conversion layer 5 The film strength increases.
  • the wavelength conversion layer 5 may not include a binder or may include a binder.
  • the binder is contained in the wavelength conversion layer 5, the adhesion between the wavelength conversion layer 5 and the LED element 3 and the adhesion between the wavelength conversion layer 5 and the metal part (for example, the metal reflection layer 2) are enhanced.
  • the type of the binder contained in the wavelength conversion layer 5 is not particularly limited, but is preferably polysiloxane. When the wavelength conversion layer 5 contains a binder made of polysiloxane, the adhesion between the wavelength conversion layer 5 and the LED element 3 or the metal part is likely to increase.
  • the binder binds the phosphor, inorganic oxide fine particles, non-conductive layered clay compound, and the like, the strength of the wavelength conversion layer 5 tends to increase. Furthermore, when the wavelength conversion layer 5 includes a binder made of polysiloxane, it becomes difficult for the wavelength conversion layer 5 to transmit the hydrogen sulfide gas and the like included in the usage environment of the LED device 100. As a result, the metal part covered with the wavelength conversion layer 5 becomes more difficult to corrode.
  • the material of the sealing layer 6 to be described later enters a gap such as a phosphor constituting the wavelength conversion layer 5.
  • a gap such as a phosphor constituting the wavelength conversion layer 5.
  • the amount of polysiloxane contained in the wavelength conversion layer 5 is preferably 5 to 50% by mass, more preferably 10 to 30% by mass with respect to the total mass of the wavelength conversion layer 5. If the amount of polysiloxane is less than 5% by mass, the polysiloxane may not be able to bind particles such as phosphors sufficiently. On the other hand, when the amount of polysiloxane exceeds 50% by mass, the amount of the phosphor is relatively lowered, and the density of the phosphor in the wavelength conversion layer 5 is lowered, so that color unevenness may occur.
  • the thickness of the wavelength conversion layer 5 is preferably 5 to 200 ⁇ m, more preferably 10 to 200 ⁇ m, and still more preferably 10 to 100 ⁇ m.
  • the thickness of the wavelength conversion layer 5 is less than 5 ⁇ m, the amount of the phosphor is reduced and there is a possibility that sufficient fluorescence cannot be obtained.
  • the thickness of the wavelength conversion layer 5 exceeds 200 ⁇ m, the concentration of the phosphor in the wavelength conversion layer 5 becomes excessively low, so that the concentration of the phosphor may not be uniform.
  • the thickness of the wavelength conversion layer 5 means the maximum thickness of the wavelength conversion layer 5 formed on the light emitting surface of the LED element 3.
  • the thickness of the wavelength conversion layer 5 is measured with a laser holo gauge.
  • the LED device 100 may include a sealing layer 6.
  • the LED element 3 and the metal part are protected from external impact, gas, moisture, and the like. As a result, the metal part is less likely to corrode, and high light extraction from the LED device 100 is maintained over a long period of time.
  • the sealing layer 6 includes transparent resin or translucent ceramic.
  • the transparent resin include a silicone resin and an epoxy resin.
  • An example of the translucent ceramic includes polysiloxane.
  • the thickness of the sealing layer 6 is preferably 25 ⁇ m to 5 mm, and more preferably 1 to 3 mm. Generally, it is difficult to make the thickness of the sealing layer 6 containing the resin 25 ⁇ m or less. On the other hand, from the viewpoint of downsizing the LED device 100, the thickness of the sealing layer 6 is preferably 5 mm or less.
  • the thickness of the sealing layer 6 means the maximum thickness of the sealing layer 6 formed on the light emitting surface of the LED element 3. The thickness of the sealing layer 6 is measured with a laser holo gauge.
  • the thickness of the sealing layer 6 is preferably 0.5 to 10 ⁇ m, more preferably 0.8 to 5 ⁇ m, and still more preferably 1 ⁇ 2 ⁇ m.
  • the thickness of the sealing layer 6 is less than 0.5 ⁇ m, the gas barrier effect of the sealing layer 6 may not be sufficient.
  • the thickness of the sealing layer 6 exceeds 10 ⁇ m, cracks are likely to occur in the sealing layer 6, and in this case as well, there is a possibility that the gas barrier effect cannot be sufficiently obtained.
  • the thickness of the sealing layer 6 means the maximum thickness of the sealing layer 6 formed on the light emitting surface of the LED element 3. The thickness of the sealing layer 6 is measured with a laser holo gauge.
  • Phosphor dispersion liquid The wavelength conversion layer 5 described above is formed by applying a phosphor dispersion liquid containing at least a phosphor, a layered clay compound, inorganic oxide fine particles, and a solvent.
  • the phosphor contained in the phosphor dispersion liquid may be anything that is excited by light emitted from the LED element 3 and emits fluorescence having a wavelength different from that of the light emitted from the LED element 3.
  • examples of phosphors that emit yellow fluorescence include YAG (yttrium, aluminum, garnet) phosphors.
  • the YAG phosphor receives blue light (wavelength 420 nm to 485 nm) emitted from the blue LED element, and emits yellow fluorescence (wavelength 550 nm to 650 nm).
  • the phosphor is, for example, 1) An appropriate amount of flux (fluoride such as ammonium fluoride) is mixed with a mixed raw material having a predetermined composition and pressed to form a molded body. 2) 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.
  • flux fluoride such as ammonium fluoride
  • a mixed raw material having a predetermined composition is obtained by sufficiently mixing oxides such as Y, Gd, Ce, Sm, Al, La, and Ga, or compounds that easily become oxides at high temperatures in a stoichiometric ratio. .
  • the mixed raw material which has a predetermined composition mixes the solution which dissolved 1) the rare earth elements of Y, Gd, Ce, and Sm in the acid in stoichiometric ratio, and oxalic acid, and obtains a coprecipitation oxide. 2) It can also be obtained by mixing this coprecipitated oxide with aluminum oxide or gallium oxide.
  • the kind of the phosphor is not limited to the YAG phosphor, and may be another phosphor such as a non-garnet phosphor that does not contain Ce.
  • the average particle diameter of the phosphor is preferably 1 ⁇ m to 50 ⁇ m, more preferably 10 ⁇ m or less.
  • the average particle diameter of the phosphor refers to the value of D50 measured with a laser diffraction particle size distribution meter. Examples of the laser diffraction particle size distribution measuring device include a laser diffraction particle size distribution measuring device manufactured by Shimadzu Corporation.
  • the amount of the phosphor contained in the phosphor dispersion is preferably 10 to 99% by mass, more preferably 20 to 97% by mass with respect to the total mass of the solid content of the phosphor dispersion.
  • concentration of the phosphor is less than 10% by mass, there is a possibility that the fluorescence cannot be sufficiently obtained from the obtained wavelength conversion layer 5.
  • amount of the phosphor exceeds 99% by mass, the amount of the layered clay compound and the amount of the inorganic oxide fine particles are relatively decreased, and the dispersion stability of the phosphor in the phosphor dispersion liquid is lowered. There is a case.
  • the layered clay compound is mainly composed of a non-conductive layered clay compound having low conductivity. If the layered clay compound is a non-conductive layered clay compound, it becomes difficult for the current to leak into the wavelength conversion layer 5.
  • the non-conductive layered clay compound is not particularly limited as long as it is a layered clay compound satisfying the above electrical conductivity, but non-swelling such as muscovite, phlogopite, sericite, fluorine phlogopite, potassium tetrasilicon mica, synthetic mica, etc. It is preferable that it is a natural clay compound. In general, the non-swelling clay compound is less likely to take moisture into the molecular structure, so the electrical conductivity tends to be low.
  • the surface of the non-conductive layered clay compound may be modified (surface treatment) with an ammonium salt or the like.
  • the non-conductive layered clay compound is easily dispersed in the phosphor dispersion liquid.
  • the water absorption of the non-conductive layered clay compound is preferably 0.2% by mass or more, more preferably 0.5 to 5% by mass, and further preferably 1 to 2% by mass.
  • the water absorption rate of the non-conductive layered clay compound is preferably low to some extent from the viewpoint of suppressing the electrical conductivity, but if the water absorption rate is less than 0.2% by mass, the water absorption rate is dispersed in the phosphor dispersion. It becomes difficult. As a result, the viscosity of the phosphor dispersion liquid is difficult to increase, and sedimentation of the phosphor may not be sufficiently suppressed.
  • the water absorption of the non-conductive layered clay compound is measured with a moisture meter. Examples of the moisture meter include MOC-120H manufactured by Shimadzu Corporation.
  • the layered clay compound may contain a clay compound (other clay compound) other than the non-conductive layered clay compound.
  • other clay compounds include smectite clay minerals such as hectorite, saponite, stevensite, beidellite, montmorillonite, nontronite, or bentonite, and swellables such as sodium tetrasilicon fluorine mica and lithium tetrasilicon fluorine mica. Clay compounds and the like are included.
  • the average particle size of the layered clay compound is preferably from 0.1 to 100 ⁇ m, more preferably from 1 to 50 ⁇ m.
  • the size of the layered clay compound is 1 ⁇ m or more, the above-described viscosity improving effect is easily obtained.
  • the size of the layered clay compound is larger than 50 ⁇ m, the light transmittance of the obtained wavelength conversion layer 5 may be lowered.
  • the size of the layered clay compound is measured by a Coulter counter method or the like.
  • the amount of the non-conductive layered clay compound contained in the phosphor dispersion is preferably 0.3 to 20% by mass, more preferably 0.5 to 15% by mass with respect to the total mass of the solid content of the phosphor dispersion. %.
  • concentration of the non-conductive layered clay compound is less than 0.3% by mass, the viscosity of the phosphor dispersion liquid is not sufficiently increased. Further, the strength of the obtained wavelength conversion layer 5 is not sufficiently increased.
  • the concentration of the non-conductive layered clay compound exceeds 20% by mass, the amount of the phosphor is relatively reduced and sufficient fluorescence cannot be obtained.
  • the amount of the other clay compound is preferably 2% by mass or less with respect to the amount of the non-conductive layered clay compound contained in the phosphor dispersion liquid, and it is particularly preferable that no other clay compound is contained. .
  • the viscosity does not increase as the proportion of the layered clay compound in the phosphor dispersion increases. Viscosity is determined by the content ratio with other components such as the amount of solvent in the phosphor dispersion and the amount of phosphor.
  • Inorganic oxide fine particles When the inorganic oxide fine particles are contained in the phosphor dispersion liquid, the viscosity of the phosphor dispersion liquid is further increased.
  • examples of the inorganic oxide fine particles include silicon oxide, titanium oxide, zinc oxide, aluminum oxide, zirconium oxide and the like.
  • the surface of the inorganic oxide fine particles may be treated with a silane coupling agent or a titanium coupling agent.
  • the inorganic oxide fine particles may be porous particles, and the specific surface area is preferably 200 m 2 / g or more.
  • the solvent enters the porous voids, so that the viscosity of the phosphor dispersion liquid tends to increase.
  • the viscosity of the phosphor dispersion liquid is not simply determined by the amount of the inorganic oxide fine particles, but also varies depending on the ratio of the inorganic oxide fine particles and the solvent, the amount of the layered clay compound, and the like.
  • the average primary particle size of the inorganic oxide fine particles is preferably 5 to 100 nm, more preferably 5 to 80 nm, and still more preferably 5 to 50 nm. When the average primary particle size of the inorganic oxide fine particles is within such a range, the viscosity of the phosphor dispersion liquid tends to increase.
  • the average primary particle size of the inorganic oxide fine particles is measured by a Coulter counter method.
  • the amount of inorganic oxide fine particles contained in the phosphor dispersion is preferably 1 to 40% by mass, more preferably 1 to 20% by mass, and still more preferably 1%, based on the total solid content of the phosphor dispersion. ⁇ 10% by mass.
  • the amount of the inorganic oxide fine particles is too small, the viscosity of the phosphor dispersion liquid is not sufficiently increased.
  • the amount of the inorganic oxide fine particles is too large, the amount of the layered clay compound is relatively reduced, and in the phosphor dispersion liquid, the phosphor may settle or the dispersibility of the phosphor may be lowered. .
  • the phosphor dispersion liquid contains a solvent.
  • the solvent is not particularly limited as long as the phosphor, the layered clay compound, and the inorganic oxide fine particles can be uniformly dispersed, but a solvent having a boiling point of 250 ° C. or lower is preferable. When the boiling point of the solvent is 250 ° C. or less, the drying rate of the phosphor dispersion liquid tends to increase.
  • the solvent examples include monoalcohols such as methanol, ethanol, propanol, and butanol; ethylene glycol, propylene glycol, diethylene glycol, glycerin, 1,3-butanediol, 1,4-butanediol, and the like.
  • the phosphor dispersion liquid may contain only one kind of solvent, or two or more kinds.
  • the solvent may contain water.
  • water When water is contained in the phosphor dispersion liquid, water enters between layers of the layered clay compound, and the viscosity of the phosphor dispersion liquid is likely to increase.
  • the amount of water contained in the phosphor dispersion is preferably 5% by mass or less, and more preferably 2% by mass or less with respect to the entire phosphor dispersion.
  • the amount of water contained in the phosphor dispersion is preferably 5% by mass or less, and more preferably 2% by mass or less with respect to the entire phosphor dispersion.
  • the total amount of the solvent contained in the phosphor dispersion liquid is appropriately set according to the viscosity of the entire phosphor dispersion liquid.
  • the total amount of the solvent contained in the phosphor dispersion is preferably 30 to 90% by mass, more preferably 40 to 70% by mass with respect to the entire phosphor dispersion.
  • a phosphor dispersion liquid is prepared by mixing and stirring a phosphor, a layered clay compound, inorganic oxide fine particles, and a solvent.
  • the stirrer can be, for example, a magnetic stirrer, an ultrasonic dispersing device, a homogenizer, a stirring mill, a blade kneading stirrer, a thin-film swirling disperser, a high-pressure impact disperser, a rotation and revolution mixer, and the like.
  • stirrer examples include known Ultra Turrax (manufactured by IKA Japan), TK homomixer (manufactured by Primix), TK pipeline homomixer (manufactured by Primix), TK Philmix (manufactured by Primix), Claremix.
  • Nanomizer manufactured by Yoshida Kikai
  • SC Mill Mitsubishi Mining Co., Ltd.
  • Altimizer agitator Nanomizer
  • Nanomizer manufactured by Yoshida Kikai
  • a high-pressure impact type dispersing device etc., such as NANO 3000 (manufactured by Bitsubusha).
  • a rotating and rotating mixer such as Awatori Nertaro (manufactured by Shinky Corporation) and an ultrasonic dispersion device are also suitable for preparing the phosphor dispersion.
  • the phosphor is very hard particles, it is preferable to avoid wear at the portion where the stirrer and the phosphor dispersion liquid are in contact with each other, and mixing of wear powder associated therewith.
  • the material of the portion where the stirrer and the phosphor dispersion are in contact with each other may be ceramic such as titania, zirconia, alumina, or silicone carbide. It is also preferable to coat the wetted part with titanium-based oxide, chromium-based nitride, diamond-like carbon.
  • the viscosity of the obtained phosphor dispersion at 25 ° C. is preferably 10 to 1000 cP, more preferably 12 to 800 cP, and still more preferably 20 to 600 cP.
  • the viscosity of the phosphor dispersion is adjusted by the amount of the solvent, the amount of the layered clay compound, the amount of the inorganic oxide fine particles, and the like.
  • the viscosity of the phosphor dispersion is measured with a vibration viscometer.
  • Manufacturing method of LED device includes the following two steps. (1) Step of preparing an LED package in which the LED element 3 and the metal part are arranged on the substrate 1 (2) The wavelength conversion layer 5 is formed so as to cover the LED element 3 and the metal part arranged in the LED package. Forming process
  • the manufacturing method of the present invention may include (3) a step of forming the sealing layer 6 on the wavelength conversion layer 5 as necessary.
  • LED Package Preparation Step In the LED package preparation step, a substrate 1 on which a metal part (a metal reflection layer 2, a metal wiring, a protruding electrode 4, etc.) is formed on a substrate 1 is prepared, and an LED element 3 is mounted on the substrate 1. Deploy.
  • the substrate 1 on which the metal reflection layer 2 and the metal wiring are formed is produced by a known method.
  • the method for manufacturing the substrate 1 may be a method of integrally molding a resin and a metal plate (such as a copper plate) patterned into a desired shape. In order to improve the light reflectivity of the metal reflective layer 2, the surface of the metal plate may be further plated.
  • the LED element 3 is fixed on the substrate 1 on which the metal reflective layer 2 is formed, and the LED element 3 and the metal wiring are electrically connected.
  • the method for fixing the LED element 3 to the substrate 1 is not particularly limited, and may be a method for fixing the LED element 3 by, for example, die bonding. Further, the electrical connection between the LED element 3 and the metal wiring may be via a wire or via the protruding electrode 4.
  • Wavelength conversion layer forming step The wavelength conversion layer 5 is formed so as to cover the LED element 3 and the metal part of the LED package described above. As described above, the wavelength conversion layer 5 obtained by the method of the present invention does not leak a current even if it absorbs moisture. Therefore, the wavelength conversion layer 5 may not contain a binder, but a ceramic binder (polysiloxane) is used. Further, it may be included. Therefore, the film forming method of the wavelength conversion layer 5 can be the following three methods.
  • the phosphor dispersion liquid is applied so that the phosphor dispersion liquid covers the LED element 3 and the metal part (for example, the metal reflection layer 2).
  • the method for applying the phosphor dispersion liquid is not particularly limited, and may be a conventionally known method such as a bar coating method, a spin coating method, a spray coating method, a dispensing method, a jet dispensing method, and an ink jet method.
  • the spray coating method is preferable because a thin film can be formed.
  • the solvent contained in the coating film is dried to cure the coating film.
  • the temperature at which the solvent is dried is usually 20 to 200 ° C., preferably 25 to 150 ° C. There exists a possibility that a coating film may not fully dry that the temperature at the time of solvent drying is less than 20 degreeC. On the other hand, if the drying temperature exceeds 200 ° C., the LED element 3 may be affected.
  • Second Method a mixed liquid of the above-described phosphor dispersion liquid and a polysiloxane precursor is prepared, and the mixed liquid is coated on the LED element 3 and a metal part (for example, the metal reflection layer 2). As described above, the phosphor dispersion liquid is applied. You may mix a solvent with a liquid mixture as needed.
  • the mixing method of the phosphor dispersion and the polysiloxane precursor is not particularly limited, and may be a general mixing / stirring method.
  • the polysiloxane precursor mixed with the phosphor dispersion may be a bifunctional, trifunctional, or tetrafunctional silane compound (monomer); or an oligomer obtained by polymerizing these.
  • tetrafunctional silane compounds include tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, tetrapentyloxysilane, tetraphenyloxysilane, trimethoxymonoethoxysilane, dimethoxydiethoxysilane, triethoxymono Methoxysilane, trimethoxymonopropoxysilane, monomethoxytributoxysilane, monomethoxytripentyloxysilane, monomethoxytriphenyloxysilane, dimethoxydipropoxysilane, tripropoxymonomethoxysilane, trimethoxymonobutoxysilane, dimethoxydibutoxysilane , Triethoxymonopropoxysilane, diethoxydipropoxysilane, tributoxymonopropoxysilane, dimethoxymonoethoxy
  • trifunctional silane compounds include trimethoxysilane, triethoxysilane, tripropoxysilane, tripentyloxysilane, triphenyloxysilane, dimethoxymonoethoxysilane, diethoxymonomethoxysilane, dipropoxymonomethoxysilane, di Propoxymonoethoxysilane, dipentyloxylmonomethoxysilane, dipentyloxymonoethoxysilane, dipentyloxymonopropoxysilane, diphenyloxylmonomethoxysilane, diphenyloxymonoethoxysilane, diphenyloxymonopropoxysilane, methoxyethoxypropoxysilane, monopropoxydimethoxysilane Monopropoxydiethoxysilane, monobutoxydimethoxysilane, monopentyloxydiethoxysilane, monophenyl Monohydrosilane compounds such as ruoxydiethoxysi
  • bifunctional silane compounds include dimethoxysilane, diethoxysilane, dipropoxysilane, dipentyloxysilane, diphenyloxysilane, methoxyethoxysilane, methoxypropoxysilane, methoxypentyloxysilane, methoxyphenyloxysilane, ethoxypropoxysilane , Ethoxypentyloxysilane, ethoxyphenyloxysilane, methyldimethoxysilane, methylmethoxyethoxysilane, methyldiethoxysilane, methylmethoxypropoxysilane, methylmethoxypentyloxysilane, methylmethoxyphenyloxysilane, ethyldipropoxysilane, ethylmethoxypropoxy Silane, ethyldipentyloxysilane, ethyldiphenyloxysilane, propyldimethoxy
  • the oligomer of the silane compound is obtained by hydrolyzing one or more of the silane compounds in the presence of an acid catalyst, water, and an organic solvent, and then subjecting this to a condensation reaction.
  • the mass average molecular weight of the oligomer is preferably 1000 to 3000, more preferably 1200 to 2700, and further preferably 1500 to 2000.
  • the mass average molecular weight of the oligomer exceeds 3000, the viscosity of the mixed liquid of the phosphor dispersion liquid and the polysiloxane precursor becomes excessively high, and it may be difficult to form a uniform film.
  • the mass average molecular weight is a value (polystyrene conversion) measured by gel permeation chromatography. The mass average molecular weight of the oligomer is adjusted by the reaction conditions (particularly the reaction time) at the time of oligomer preparation.
  • the solvent that can be mixed with the phosphor dispersion and the polysiloxane precursor should be a solvent that can dissolve or uniformly disperse the polysiloxane precursor and has good compatibility with the phosphor dispersion.
  • the solvent for preparing the oligomer may be mixed, or different solvents may be mixed.
  • the solvent examples include monohydric alcohols such as methanol, ethanol, propanol and n-butanol; alkyl carboxylic acid esters such as methyl-3-methoxypropionate and ethyl-3-ethoxypropionate; ethylene glycol, diethylene glycol, Polyhydric alcohols such as propylene glycol, glycerin, trimethylolpropane, hexanetriol; ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol mono Propyl ether, diethylene glycol monobutyl ether, propylene glycol Monoethers of polyhydric alcohols such as methyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether
  • Ester ethers include the like; ketones such as acetone, methyl ethyl ketone and methyl isoamyl ketone.
  • ketones such as acetone, methyl ethyl ketone and methyl isoamyl ketone.
  • the mixed liquid of the phosphor dispersion liquid and the polysiloxane precursor only one kind of these solvents may be mixed, or two or more kinds may be mixed.
  • the method for applying the mixed liquid of the phosphor dispersion and the polysiloxane precursor is not particularly limited, and may be the same as the method for applying the phosphor dispersion in the first method described above.
  • the coating film After applying the above mixed solution, the coating film is heated to 100 ° C. or higher, preferably 150 to 300 ° C., and the coating film is dried and cured.
  • the heating temperature is less than 100 ° C., water generated during the dehydration condensation of the polysiloxane precursor and the solvent contained in the mixed solution cannot be sufficiently removed, and the light resistance of the coating film may be lowered.
  • the phosphor dispersion liquid described above is applied and cured on the LED element 3 and the metal part (for example, the metal reflection layer 2) to form a cured film of the phosphor dispersion liquid. And a step of separately applying a polysiloxane precursor on the cured film of the phosphor dispersion liquid.
  • the phosphor dispersion liquid is applied so as to cover the LED element 3 and the metal part.
  • the method for applying and curing the phosphor dispersion liquid may be the same as the method for applying the phosphor dispersion liquid in the first method described above.
  • a polysiloxane precursor is applied so as to cover the cured film.
  • a polysiloxane precursor is applied onto the cured film of the phosphor dispersion liquid, the polysiloxane precursor enters between the phosphor, the inorganic oxide fine particles, the layered clay compound, and the like.
  • the obtained wavelength conversion layer 5 phosphors, inorganic oxide fine particles, and layered clay compounds are bound by polysiloxane.
  • the polysiloxane precursor applied onto the cured film of the phosphor dispersion liquid may be the same as the polysiloxane precursor mixed with the phosphor dispersion liquid in the second method.
  • the polysiloxane precursor and a solvent may be mixed as necessary.
  • the method for applying the polysiloxane precursor is not particularly limited, and may be the same as the method for applying the phosphor dispersion.
  • the coating film is heated to 100 ° C. or more, preferably 150 to 300 ° C., and the coating film is dried and cured. If the heating temperature is less than 100 ° C., water generated during the dehydration condensation of the polysiloxane precursor cannot be sufficiently removed, and the light resistance of the coating film may be lowered.
  • the manufacturing method of the present invention may include a formation step of the sealing layer 6 that covers the wavelength conversion layer 5.
  • the formation method of the sealing layer 6 is appropriately selected according to the components contained in the sealing layer 6.
  • a resin composition containing the resin (silicone resin, epoxy resin, etc.) or a precursor thereof is prepared, and the composition is applied on the wavelength conversion layer 5 ⁇ Curing.
  • the resin composition may contain a solvent.
  • the solvent is not particularly limited as long as it can dissolve the resin or the precursor thereof, for example, hydrocarbons such as toluene and xylene; ketones such as acetone and methyl ethyl ketone; diethyl ether, tetrahydrofuran and the like And ethers such as propylene glycol monomethyl ether acetate and ethyl acetate.
  • the coating method of the resin composition is not particularly limited, and may be a coating method using a general coating apparatus such as a dispenser.
  • the curing method and curing conditions of the resin composition are appropriately selected depending on the type of resin.
  • An example of the curing method is heat curing.
  • a polysiloxane precursor-containing liquid containing a polysiloxane precursor is prepared, and the containing liquid is applied and cured on the wavelength conversion layer 5.
  • the polysiloxane precursor-containing liquid may contain a solvent.
  • the polysiloxane precursor and the solvent contained in the polysiloxane precursor-containing liquid can be the same as the polysiloxane precursor and the solvent applied in the film forming step (third method) of the wavelength conversion layer 5 described above.
  • coating method and hardening method of a polysiloxane precursor containing composition can also be the same method as the film-forming process (3rd method) of the above-mentioned wavelength conversion layer 5.
  • Polysiloxane precursor-containing liquid Polysiloxane precursor-containing liquid prepared by the following method (1) Polysiloxane precursor-containing liquid prepared by the following method (2)
  • the weight average molecular weight in terms of polystyrene was 1600.
  • the weight average molecular weight in terms of polystyrene was 1500.
  • phosphor dispersion liquid (1) 50 parts by mass of YAG phosphor, 2 parts by mass of layered clay compound (1), and inorganic oxide fine particles (silica product name) : RX300, manufactured by Nippon Aerosil Co., Ltd.) and 2 parts by mass of a mixed liquid of 1,3-butanediol and ethyl alcohol (weight ratio 3: 2) were mixed.
  • the obtained mixed liquid was dispersed for 5 minutes at 1000 rpm with a rotation and revolution mixer (Awatori Netaro ARE-310: manufactured by Sinky Corporation) to prepare a phosphor dispersion liquid (1).
  • LED device An aromatic polyamide circular substrate (opening diameter 3 mm, bottom surface diameter 2 mm, opening wall inclination angle 60 °) having a metal reflection layer 2 (silver plating) shown in FIG. 1 was prepared.
  • One blue LED element 3 (cuboid: 200 ⁇ m ⁇ 300 ⁇ m ⁇ 100 ⁇ m) was fixed to the center of the opening of the substrate 1 with a die-bonding adhesive.
  • the anode electrode and the cathode electrode of the LED element were respectively connected by wires to obtain an LED package.
  • the above-mentioned phosphor dispersion liquid (1) was applied by spraying so as to cover the LED element 3 of the LED package and the metal reflection layer 2.
  • the spray pressure at the time of spray application was 0.2 MPa.
  • the relative moving speed of the spray nozzle and the LED package was appropriately adjusted so that the thickness of the obtained wavelength conversion layer became a desired thickness.
  • the thickness of the wavelength conversion layer (relative movement speed between the spray nozzle and the LED package) was adjusted so that the chromaticity (x value) of white light emitted from the obtained LED element was 0.33.
  • heating was performed at 150 ° C. for 1 hour to form a wavelength conversion layer.
  • Examples 2 to 13, 16 to 17, and Comparative Examples 1 to 8> It implemented except having applied the fluorescent substance dispersion liquid (or liquid mixture of fluorescent substance dispersion liquid and polysiloxane precursor containing liquid) shown in the said Table 2 instead of the fluorescent substance dispersion liquid (1) in Example 1. As in Example 1, a wavelength conversion layer was formed.
  • Example 14> Instead of the phosphor dispersion liquid (1) in Example 1, as shown in Table 2 above, the phosphor dispersion liquid (6) was applied and cured in the same manner as in Example 1. Furthermore, the above-mentioned polysiloxane precursor containing liquid (2) was apply
  • Example 15 Instead of the phosphor dispersion liquid (1) in Example 1, the phosphor dispersion liquid (20) was applied as shown in Table 2 above. Then, it heated at 150 degreeC for 1 hour, and formed the wavelength conversion layer into a film. Furthermore, the above-mentioned polysiloxane precursor (2) was apply
  • Phenyl silicone manufactured by Shin-Etsu Chemical Co., Ltd .: KER-6000
  • a dispenser on the wavelength conversion layer of the sample prepared in each example and comparative example, and heated at 150 ° C. for 1 hour to form a sealing layer. did.
  • the obtained sealing layer had a thickness of 2 mm.
  • a current of 20 mA was passed through the LED device on which the sealing layer was formed; the chromaticity of the emission color and the total luminous flux of each LED device were measured.
  • the chromaticity and total luminous flux were measured with a spectral radiance meter CS-1000A manufactured by Konica Minolta Sensing. As described above, the chromaticity x value of each LED device is adjusted to 0.33.
  • the total luminous flux value of the LED device of Example 1 was used as a reference (100), and the total luminous flux value of each LED device was evaluated according to the following criteria.
  • Total luminous flux maintenance rate after wet heat environment test After the initial total luminous flux value was measured, the LED device was charged in a high-temperature and high-humidity tank (trade name: SH251 manufactured by Espec Co., Ltd.) at 85 ° C. and 85% Rh with a current of 20 mA flowing, and taken out after 1000 hours. And based on the following formula
  • Total luminous flux maintenance factor total luminous flux value after 1000 hours of wet heat environment test / initial total luminous flux value ⁇ 100 A: Total luminous flux maintenance factor was 97% or more. O: Total luminous flux maintenance factor was 95% or more and less than 97%. ⁇ : Total luminous flux maintenance factor was 90% or more and less than 95%. Luminous flux maintenance factor was less than 90%
  • the wavelength conversion layer containing the non-conductive layered clay compound did not leak electricity and the metal reflection layer was less deteriorated.
  • a clay mineral having an electric conductivity of 80 ⁇ S / cm or less is used, a good LED device having a very high total luminous flux maintenance factor and little deterioration in light emission characteristics can be obtained.
  • the heat shock test is performed. Even if I went there, it was hard to break. Since the silicone resin of the sealing layer enters the gap between the phosphors of the wavelength conversion layer and there is no clear interface between the wavelength conversion layer and the sealing layer, even if the temperature of the LED device changes, the wavelength conversion layer and the sealing layer It is presumed that there was little difference in expansion rate and contraction rate, and it was difficult to apply a load to the wire.
  • the phosphor dispersion containing the clay mineral having an electrical conductivity of 150 ⁇ S / cm or more showed very good sedimentation stability. It is considered that these clay minerals have an increased electrical affinity with the phosphor surface and suppress sedimentation of the phosphor.
  • the LED device of the present invention has high gas barrier properties and light extraction properties over a long period of time. Therefore, both can be applied to indoor and outdoor lighting devices.

Landscapes

  • Led Device Packages (AREA)
  • Luminescent Compositions (AREA)

Abstract

Cette invention concerne un procédé de fabrication d'un dispositif à DEL présentant un rendement satisfaisant d'extraction de lumière sur une durée prolongée. Plus précisément, l'invention concerne un procédé de fabrication d'un dispositif à DEL comprenant un substrat, un élément de DEL disposé sur le substrat, une pièce métallique disposée sur le substrat et une couche de conversion de longueur d'onde recouvrant l'élément de DEL et la pièce métallique. Ledit procédé comprend les étapes consistant à : préparer un boîtier de DEL comprenant un élément de DEL et une pièce métallique disposés sur un substrat ; et appliquer et solidifier une solution de dispersion à base d'une substance luminescente contenant une substance luminescente, un composé d'argile non conducteur en forme de couche, des microparticules d'oxyde inorganique et un solvant de façon à recouvrir l'élément de DEL et la pièce métallique du boîtier de DEL et former une couche de conversion de longueur d'onde. Ledit composé d'argile non conducteur en forme de couche est un composé tel qu'une solution aqueuse comprenant une concentration de 2% en masse dudit composé d'argile non conducteur en forme de couche présente une conductivité inférieure ou égale à 500 μS/cm.
PCT/JP2014/003891 2013-07-24 2014-07-24 Procédé de fabrication de dispositif à diode électroluminescente Ceased WO2015011925A1 (fr)

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WO2017206331A1 (fr) * 2016-06-02 2017-12-07 深圳朝伟达科技有限公司 Substrat de boîtier de del et son procédé de fabrication
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KR102872843B1 (ko) * 2018-12-27 2025-10-21 덴카 주식회사 형광체 기판, 발광 기판 및 조명 장치
CN114388554A (zh) * 2020-10-21 2022-04-22 夏普福山激光株式会社 半导体模块
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