WO2019239850A1 - Module de conversion de longueur d'onde et élément de conversion de longueur d'onde, et procédé de fabrication associé, et dispositif electroluminescent - Google Patents

Module de conversion de longueur d'onde et élément de conversion de longueur d'onde, et procédé de fabrication associé, et dispositif electroluminescent Download PDF

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Publication number
WO2019239850A1
WO2019239850A1 PCT/JP2019/020654 JP2019020654W WO2019239850A1 WO 2019239850 A1 WO2019239850 A1 WO 2019239850A1 JP 2019020654 W JP2019020654 W JP 2019020654W WO 2019239850 A1 WO2019239850 A1 WO 2019239850A1
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WIPO (PCT)
Prior art keywords
wavelength conversion
conversion member
skeleton
inorganic material
phosphor particles
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PCT/JP2019/020654
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English (en)
Japanese (ja)
Inventor
彰太郎 福本
忠仁 古山
俊輔 藤田
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日本電気硝子株式会社
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Priority claimed from JP2019057862A external-priority patent/JP2020095233A/ja
Application filed by 日本電気硝子株式会社 filed Critical 日本電気硝子株式会社
Priority to CN201980033998.6A priority Critical patent/CN112154358A/zh
Priority to DE112019002989.4T priority patent/DE112019002989T5/de
Priority to US17/052,822 priority patent/US20210231294A1/en
Publication of WO2019239850A1 publication Critical patent/WO2019239850A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/02—Structural details or components not essential to laser action

Definitions

  • the present invention relates to a wavelength conversion member and a wavelength conversion element that convert the wavelength of light emitted from a light emitting diode (LED: Light Emitting Diode), a laser diode (LD: Laser Diode), and the like, and a method for manufacturing the same, and The present invention relates to a light emitting device.
  • LED Light Emitting Diode
  • LD Laser Diode
  • next-generation light-emitting device that replaces fluorescent lamps and incandescent lamps
  • attention has been focused on light-emitting devices using LEDs and LDs from the viewpoint of low power consumption, small size and light weight, and easy light quantity adjustment.
  • a wavelength conversion member that absorbs part of light from the LED and converts it into yellow light is disposed on the LED that emits blue light.
  • a light emitting device is disclosed. This light emitting device emits white light that is a combined light of blue light emitted from the LED and yellow light emitted from the wavelength conversion member.
  • a wavelength conversion member in which phosphor particles are dispersed in a resin matrix has been used.
  • a wavelength conversion member using such a resin matrix is discolored and deformed by receiving heat or irradiation light emitted from an LED or LD, and this is a cause of reducing the performance of the wavelength conversion member. It was.
  • the wavelength conversion member has a feature that a glass matrix as a base material is not easily deteriorated by heat or irradiation light from an LED, and problems such as discoloration and deformation hardly occur.
  • the present invention provides a wavelength conversion member and a wavelength conversion element capable of suppressing a decrease in light emission intensity over time and dissolution of constituent materials when irradiated with light from a high-power LED or LD, and those
  • An object of the present invention is to provide a manufacturing method and a light emitting device.
  • the wavelength conversion member of the present invention is a wavelength conversion member including a matrix and phosphor particles dispersed in the matrix, and the matrix is filled in a skeleton made of an inorganic material and a hole formed by the skeleton.
  • a transparent material, and the inorganic material has a higher thermal conductivity than the transparent material.
  • the skeleton made of an inorganic material has higher thermal conductivity than glass or resin, and as a heat conduction path, when the wavelength conversion member is irradiated with heat from the light source or excitation light, Since the generated heat is efficiently released to the outside, an increase in the temperature of the wavelength conversion member can be suppressed.
  • a difference in refractive index between the skeleton and the hole can be reduced, and light scattering can be suppressed.
  • the translucency of the wavelength conversion member is increased, excitation light and fluorescence emitted from the phosphor particles can be efficiently extracted.
  • the skeleton is preferably made of a sintered body. This makes it easy to increase the thermal conductivity of the skeleton.
  • the phosphor particles are preferably dispersed in the pores.
  • the phosphor particles are preferably dispersed inside the skeleton.
  • the phosphor particles are in contact with both the skeleton and the pores.
  • the volume ratio of the transparent material to the entire wavelength conversion member is preferably 10 to 80%. If it does in this way, both translucency and heat dissipation can be made compatible.
  • the refractive index difference between the inorganic material and the transparent material is preferably 0.3 or less. In this way, excessive scattering occurring at the interface between the skeleton made of an inorganic material and the transparent material can be suppressed, and the scattering state can be controlled so that the fluorescence emitted from the phosphor particles can be efficiently extracted.
  • the skeleton is preferably formed by three-dimensionally connecting the inorganic material powder.
  • the pores are not substantially independent. If it does in this way, a transparent material can fully be filled, and extra scattering can be suppressed.
  • the inorganic material preferably contains at least one selected from aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, and boron nitride. Since the above inorganic materials have higher thermal conductivity than transparent materials such as glass and resin, the thermal conductivity of the skeleton made of inorganic materials is increased, and the heat generated by the phosphor particles is effectively released to the outside. be able to.
  • the transparent material is preferably glass.
  • the transparent material is preferably a resin.
  • the wavelength conversion member of the present invention preferably has a thickness of 1000 ⁇ m or less. If it does in this way, excessive scattering of a wavelength conversion member can be reduced and luminous efficiency can be raised.
  • the wavelength conversion member of the present invention preferably has a thermal diffusivity of 1 ⁇ 10 ⁇ 6 m 2 / s or more. If it does in this way, excessive heat_generation
  • the wavelength conversion member of the present invention preferably has a quantum efficiency of 20% or more.
  • the method for producing a wavelength conversion member according to the present invention is a method for producing the above-described wavelength conversion member, the step of firing inorganic material powder to produce a skeleton made of an inorganic material, and preparing a mixture of phosphor particles and a transparent material And a step of impregnating the pores formed by the skeleton with the step of performing the step.
  • the maximum temperature when firing the inorganic material powder is 1600 ° C. or less.
  • the maximum temperature when the skeleton is impregnated with a mixture of phosphor particles and a transparent material is 1000 ° C. or less.
  • the wavelength conversion member manufacturing method of the present invention is the above-described wavelength conversion member manufacturing method, comprising a step of preparing a mixture of phosphor particles and inorganic material powder, firing the mixture, and having a skeleton made of an inorganic material. And a step of producing a sintered body in which phosphor particles are dispersed inside the skeleton, and a step of impregnating pores formed by the skeleton with a transparent material.
  • the maximum temperature when firing a mixture of phosphor particles and inorganic material powder is 1600 ° C. or lower.
  • the maximum temperature when the transparent material is impregnated in the skeleton is 1000 ° C. or less.
  • the average particle size of the inorganic material powder is preferably 3 ⁇ m or more.
  • the wavelength conversion element of the present invention is characterized by comprising the above-described wavelength conversion member and a substrate bonded to the wavelength conversion member.
  • the substrate is preferably bonded to the wavelength conversion member with a transparent material exposed from the surface of the wavelength conversion member.
  • the method for producing a wavelength conversion element of the present invention includes a step of firing inorganic material powder to prepare a skeleton made of an inorganic material, a step of preparing a mixture of phosphor particles and a transparent material, and a pore formed by the skeleton. A step of impregnating the substrate, a step of bringing the substrate and the skeleton into close contact before the mixture is cured, and a step of integrating the skeleton and the substrate with the mixture exposed from the pores.
  • the method for producing a wavelength conversion element of the present invention includes a step of preparing a mixture of phosphor particles and an inorganic material powder, firing the mixture, having a skeleton made of an inorganic material, and phosphor particles dispersed within the skeleton
  • the step of producing a sintered body, the step of impregnating the pores formed by the skeleton with a transparent material, the substrate and the sintered body are brought into close contact before the transparent material is cured, and the transparent material exposed from the pores, A step of integrating the sintered body and the substrate.
  • a light-emitting device of the present invention is characterized by comprising the above-described wavelength conversion member and a light source that irradiates the wavelength conversion member with excitation light.
  • the light-emitting device of the present invention is characterized by comprising the above-described wavelength conversion element and a light source that irradiates the wavelength conversion element with excitation light.
  • the light source is preferably a laser diode.
  • a wavelength conversion member and a wavelength conversion element capable of suppressing a decrease in light emission intensity over time and dissolution of constituent materials even when irradiated with light of a high-power LED or LD, and their A manufacturing method and a light-emitting device can be provided.
  • FIG. 2 is a partial cross-sectional photograph of the wavelength conversion member of Example 1.
  • FIG. It is typical sectional drawing which shows one Embodiment of the wavelength conversion element of this invention. It is typical sectional drawing which shows the light-emitting device using the wavelength conversion member which concerns on one Embodiment of this invention. It is typical sectional drawing which shows the light-emitting device using the wavelength conversion element which concerns on one Embodiment of this invention.
  • FIG. 1 is a schematic cross-sectional view showing a wavelength conversion member according to an embodiment of the present invention.
  • the wavelength conversion member 10 contains phosphor particles 2 inside the matrix 1.
  • the matrix 1 is formed of a skeleton made of the inorganic material 3 and a transparent material 4 filled in the pores of the skeleton made of the inorganic material 3, and the phosphor particles 2 are either the inorganic material 3 or the transparent material 4. , Or both in contact with both.
  • hole part is filled with the transparent material 4, a part of void
  • FIG. each component will be described in detail.
  • the phosphor particles in the present invention are not particularly limited as long as the phosphor particles emit fluorescence upon incidence of excitation light. Specific examples include, for example, oxide phosphors, nitride phosphors, oxynitride phosphors, chlorides. Product phosphor, acid chloride phosphor, sulfide phosphor, oxysulfide phosphor, halide phosphor, chalcogenide phosphor, aluminate phosphor, halophosphate chloride phosphor and the like. These can be used individually or in mixture of 2 or more types.
  • a step of firing inorganic material powder to produce a skeleton made of inorganic material, phosphor particles and transparent A step of preparing a mixture of materials, a manufacturing method including a step of impregnating the mixture into pores formed by a skeleton, or (ii) a step of preparing a mixture of phosphor particles and inorganic material powder, and baking the mixture
  • a manufacturing method including a step of producing a sintered body having a skeleton made of an inorganic material, and phosphor particles dispersed in the skeleton, and a step of impregnating a void portion formed by the skeleton with a transparent material.
  • the wavelength conversion member is obtained by the production method (ii) or when glass is used as the transparent material, it is preferable to use a phosphor particle that is less susceptible to thermal deterioration during firing or impregnation.
  • the phosphor particles are oxide phosphors, particularly oxide phosphors having a garnet structure (Y 3 Al 5 O 12 : Ce 3+ , Lu 3 Al 5 O 12 : Ce 3+ etc.). It is preferable.
  • the average particle diameter (D 50 ) of the phosphor particles is preferably 1 to 50 ⁇ m, more preferably 3 to 30 ⁇ m, and particularly preferably 5 to 30 ⁇ m. If the average particle size of the phosphor particles is too small, the emission intensity tends to decrease. On the other hand, if the average particle size is too large, it is difficult to uniformly disperse the phosphor particles in the matrix, and the luminescent color may become non-uniform.
  • the average particle diameter means a value measured by the laser diffraction method, and in the volume-based cumulative particle size distribution curve measured by the laser diffraction method, the cumulative amount is accumulated from the smaller particle. The particle size is 50%.
  • the volume percentage of the phosphor particles in the total amount of the phosphor particles and the inorganic material is preferably 0.01 to 90% in any of the above methods (i) and (ii), and 0.01 to 70%. Is more preferable, and 0.01 to 50% is particularly preferable.
  • the volume percentage of the phosphor particles in the total amount of the phosphor particles and the inorganic material is described as the phosphor particle content. If the content of the phosphor particles is too large, the content of the inorganic material in the mixture of the phosphor particles and the inorganic material is relatively reduced, and the thermal conductivity of the matrix may be lowered. Moreover, when there is too little phosphor particle content, it becomes difficult to obtain sufficient light emission intensity.
  • the phosphor particle content is preferably 0.01 to 50%, more preferably 0.1 to 35%, and particularly preferably 1 to 20%.
  • the dispersed state include (1) a state where the phosphor particles are dispersed in the pores, and (2) a state where the phosphor particles are dispersed inside the skeleton.
  • State (1) is preferable because it can be relatively easily produced by the above-described production method (i).
  • the state (2) can be manufactured by the above-described manufacturing method (ii), and since the skeleton having high thermal conductivity and the phosphor particles are bound, the heat generated by the phosphor particles is particularly effectively released to the outside. It becomes easy and preferable.
  • the phosphor particles may be in contact with both the skeleton and the pores.
  • the inorganic material is preferably a ceramic powder. Specifically, it is preferable to contain at least one selected from aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, and boron nitride.
  • the inorganic material powder as a raw material, in addition to the above inorganic material, a raw material from which at least one selected from aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride and boron nitride can be obtained by firing.
  • hydroxide, carbonate, fluoride, chloride and the like can be used. These may be used alone or in combination of two or more.
  • the inorganic material has a higher thermal conductivity than transparent materials such as glass and resin, the heat generated by the phosphor particles can be effectively released to the outside.
  • aluminum oxide and magnesium oxide are preferable because of their relatively high thermal conductivity.
  • magnesium oxide is more preferable because of high heat conductivity and low light absorption.
  • Inorganic materials have a higher thermal conductivity than transparent materials.
  • the thermal conductivity of the inorganic material is preferably 5 W ⁇ m ⁇ 1 ⁇ K ⁇ 1 or more, more preferably 10 W ⁇ m ⁇ 1 ⁇ K ⁇ 1 or more, and 25 W ⁇ m ⁇ . It is particularly preferred that it is 1 ⁇ K ⁇ 1 or more. If it does in this way, it will become easy to discharge
  • the thermal conductivity of magnesium oxide is about 45 to 60 W ⁇ m ⁇ 1 ⁇ K ⁇ 1 .
  • the skeleton made of the inorganic material is preferably formed by three-dimensionally connecting the inorganic material powder.
  • a bicontinuous porous body (a porous body in which the skeleton and the pores are three-dimensionally continuous) is formed. It is preferable to form. With such a structure, the transparent material can be more easily impregnated into the matrix. Moreover, it becomes easy to discharge
  • the fact that the inorganic material powder is three-dimensionally connected can be confirmed from a three-dimensional image captured using a micro X-ray CT scanner.
  • the skeleton made of an inorganic material is preferably made of a sintered body (powder sintered body). If it does in this way, it will become easy to fully bind inorganic material powder, and it will become easy to make thermal conductivity of skeleton high.
  • a mixed sintered body in which phosphor particles are dispersed inside a skeleton made of an inorganic material can be obtained.
  • the skeleton made of an inorganic material is a sintered body, and the phosphor particles are dispersed inside the skeleton, or the phosphor particles are separated from the skeleton.
  • a wavelength conversion member in contact with both of the holes can be obtained.
  • the mixed sintered body is preferable because the phosphor particles and the skeleton are bonded to each other by firing, and thus heat generated by the phosphor particles can be more effectively released to the outside.
  • the pores formed by the skeleton are not substantially independent. If it does in this way, a transparent material can fully be filled and unnecessary scattering can be suppressed.
  • substantially not independent means that, in a three-dimensional image picked up using a micro X-ray CT scanner, the volume of independent holes is 1% of the total holes. It means the following cases.
  • the central pore diameter of the pore is preferably 0.05 ⁇ m to 50 ⁇ m, more preferably 0.1 ⁇ m to 40 ⁇ m, and particularly preferably 0.5 ⁇ m to 30 ⁇ m. If the central pore diameter is too small, the transparent material is not sufficiently filled and voids remain, resulting in excessive scattering. On the other hand, if the pore diameter is too large, when the phosphor particles are dispersed in the pores, the phosphor particles and the skeleton made of an inorganic substance are not sufficiently in contact with each other, and the heat generated by the phosphor particles cannot be sufficiently dissipated.
  • the center pore diameter means a value measured using a mercury intrusion method, and indicates a pore diameter having a larger peak value in the pore diameter distribution measured by the mercury intrusion method.
  • the glass used as the transparent material preferably has a softening point of 250 to 1000 ° C., more preferably 300 to 950 ° C., and particularly preferably 350 to 900 ° C. in consideration of thermal deterioration of the phosphor particles. preferable. Since glass is superior in heat resistance as compared with a resin that is an organic matrix, a wavelength conversion member that is more excellent in heat resistance can be produced. If the softening point of the glass is too low, softening deformation may occur due to heat generated from the phosphor particles. On the other hand, if the softening point of the glass is too high, an impregnation treatment at a higher temperature is required. Therefore, when using phosphor particles with low heat resistance, the softening point of glass is preferably 600 ° C. or lower.
  • the resin used as the transparent material examples include general resins such as a thermoplastic resin such as silicone and a thermosetting resin such as epoxy resin. Since the resin has a lower softening point than glass and can be impregnated at a lower temperature, it is particularly useful when using phosphor particles with low heat resistance, resulting in a reduction in manufacturing cost. it can. Moreover, since specific gravity is small compared with glass, a lighter wavelength conversion member can be produced.
  • an optimal transparent material can be used in consideration of the heat resistance and manufacturing cost of the phosphor particles.
  • the volume ratio of the transparent material in the entire wavelength conversion member is preferably 10 to 80%, more preferably 20 to 60%, and particularly preferably 30 to 50%.
  • the ratio of the transparent material is too large, the inorganic material forming the skeleton becomes too small, and it becomes difficult to obtain a desired heat dissipation effect.
  • the ratio of the transparent material is too small, the number of holes that are not filled with the transparent material increases, and air remains inside. As a result, it becomes difficult to reduce light scattering due to the difference in refractive index (nd) between air and the matrix, and the light transmissivity of the wavelength conversion member is lowered, so that the light extraction efficiency is lowered.
  • the difference in refractive index (nd) between the inorganic material and the transparent material constituting the matrix is preferably 0.3 or less, more preferably 0.2 or less, and particularly preferably 0.1 or less. In this way, excessive scattering occurring at the interface between the skeleton made of an inorganic material and the transparent material can be suppressed, and the scattering state can be adjusted so that the fluorescence emitted from the phosphor particles can be efficiently extracted.
  • the refractive index difference is not limited to the above.
  • the shape of a wavelength conversion member is not specifically limited, Usually, it is plate shape (rectangular plate shape, disk shape, etc.).
  • the thickness of the wavelength conversion member can be appropriately selected so as to obtain the light of the target color. Specifically, the thickness is preferably 1000 ⁇ m or less, more preferably 800 ⁇ m or less, and particularly preferably 500 ⁇ m or less. When the thickness of the wavelength conversion member is too large, light scattering and absorption in the wavelength conversion member become too large, and the emission efficiency of excitation light and fluorescence tends to decrease.
  • the thickness of the wavelength conversion member is preferably 30 ⁇ m or more, more preferably 50 ⁇ m or more, and particularly preferably 80 ⁇ m or more.
  • the thickness of the wavelength conversion member is too small, the mechanical strength tends to decrease. Moreover, since it is necessary to increase the content of the phosphor particles in order to obtain a desired emission intensity, the skeleton and the transparent material made of an inorganic material are relatively reduced, and the thermal conductivity and light transmittance are reduced. There is a tendency to decrease.
  • the wavelength conversion member of the present invention is composed of phosphor particles and a matrix having excellent thermal conductivity, it tends to have a high thermal diffusivity.
  • the thermal diffusivity of the wavelength conversion member is preferably 1 ⁇ 10 ⁇ 6 m 2 / s or more, preferably 1.5 ⁇ 10 ⁇ 6 m 2 / s or more, and 2 ⁇ 10. Particularly preferably, it is ⁇ 6 m 2 / s or more.
  • the quantum efficiency of the wavelength conversion member is preferably 20% or more, more preferably 30% or more, further preferably 50% or more, and particularly preferably 60% or more. If the quantum efficiency is too low, the energy that becomes heat loss in the light absorbed during wavelength conversion increases, and the temperature of the phosphor tends to rise. As a result, a decrease in brightness tends to be caused by temperature quenching.
  • quantum efficiency points out the value calculated by a following formula, and can be measured using an absolute PL quantum yield apparatus.
  • Quantum efficiency ⁇ (number of photons emitted from the sample as fluorescence) / (number of photons absorbed by the sample) ⁇ ⁇ 100 (%)
  • the wavelength conversion member includes (i) a step of firing inorganic material powder to prepare a skeleton made of inorganic material, a step of preparing a mixture of phosphor particles and a transparent material, and impregnating the pores formed by the skeleton with the mixture Or (ii) preparing a mixture of phosphor particles and inorganic material powder, firing the mixture, having a skeleton made of an inorganic material, and phosphor particles dispersed inside the skeleton It can be produced by any one of a production method including a step of producing a sintered body and a step of impregnating a pore portion formed of a transparent material with a transparent material.
  • a sintered body having a skeleton made of an inorganic material is prepared by pressing an inorganic material powder with a mold and firing the obtained preform.
  • the sintered body can be obtained by adding an organic component such as a binder or a solvent to the inorganic material powder to form a paste, and then firing the paste. If it does in this way, it will become easy to form the preforming body of a desired shape using methods, such as green sheet fabrication.
  • after removing the organic component in the degreasing step (about 600 ° C.), it can be fired at the sintering temperature of the inorganic material powder.
  • polypropylene carbonate, polybutyl methacrylate, polyvinyl butyral, polymethyl methacrylate, polyethyl methacrylate, ethyl cellulose, nitrocellulose, polyester carbonate and the like can be used, and these can be used alone or in combination.
  • terpineol isoamyl acetate, toluene, methyl ethyl ketone, diethylene glycol monobutyl ether acetate, 2,2,4-trimethyl-1,3-pentadiol monoisobutyrate or the like can be used alone or in combination.
  • the paste may contain a sintering aid.
  • a sintering aid By adding a sintering aid, fusion between particles is promoted, and the thermal conductivity of a skeleton made of an inorganic material is easily improved. In addition, the firing temperature can be lowered, and the thermal deterioration of the phosphor can be easily suppressed.
  • the sintering aid include crystalline powders such as magnesium phosphate, zirconium phosphate, manganese oxide, barium oxide, yttrium oxide, aluminum oxide, silicon oxide, calcium fluoride, magnesium fluoride, and barium fluoride. Silicic acid-based and phosphoric acid-based oxide amorphous powders can be used.
  • a sintering aid containing the same metal cation as the metal cation contained in the inorganic material powder it is preferable to use magnesium phosphate and / or magnesium fluoride as a sintering aid.
  • the main component of the skeleton made of an inorganic material can be magnesium oxide, and it is easy to suppress unintentional crystal formation due to different cations.
  • the average particle diameter (D 50 ) of the sintering aid is preferably 10 ⁇ m or less, more preferably 7 ⁇ m or less, and particularly preferably 5 ⁇ m or less.
  • the sintering aid can easily enter between the inorganic material powders.
  • the reactivity of the sintering aid is increased and it becomes easy to soften at a low temperature, so that the inorganic material powder is easily fused by sintering. As a result, the thermal diffusivity of the wavelength conversion member is easily improved. If the particle size of the sintering aid is too large, the above effect is difficult to obtain.
  • the lower limit value of the average particle diameter is not particularly limited, but is generally 0.001 ⁇ m or more.
  • the sintering aid is preferably contained in an amount of 0.01 to 30%, more preferably 0.1 to 20% by volume with respect to the mixture of the inorganic material powder and the sintering aid.
  • the content is particularly preferably 0.5 to 10%.
  • the raw material powder having a small particle size can be regarded as the sintering aid. In this case, since the raw material powder having a smaller particle size has higher reactivity and is easily softened at a low temperature, it functions as a sintering aid.
  • the inorganic material powder a raw material from which at least one selected from aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, and boron nitride can be obtained by firing can be used.
  • oxides, nitrides, hydroxides, fluorides, chlorides, carbonates can be used.
  • aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, magnesium hydroxide It is preferable to use aluminum hydroxide, boron fluoride, magnesium fluoride, aluminum fluoride, magnesium chloride, aluminum chloride, magnesium carbonate, or the like. These can be used alone or in combination. In particular, it is preferable to use magnesium fluoride (MgF 2 ).
  • Magnesium fluoride is easy to sinter at low temperatures, and in particular in the production method (ii) described later, it is possible to suppress the thermal deterioration of the phosphor particles due to sintering and to suppress the decrease in the luminous efficiency of the wavelength conversion member. it can. In this case, at least a part of the fluorine component (F 2 ) is eliminated by sintering, and a skeleton containing magnesium oxide (MgO) can be obtained.
  • the maximum temperature when firing the inorganic material powder is preferably 1600 ° C. or less, more preferably 1400 ° C. or less, and particularly preferably 1200 ° C. or less.
  • the lower limit of the firing temperature is preferably 700 ° C. or higher, more preferably 800 ° C. or higher, and particularly preferably 900 ° C. or higher.
  • the average particle size (D 50 ) of the inorganic material powder is preferably 3 ⁇ m to 50 ⁇ m, more preferably 3 ⁇ m to 30 ⁇ m, and particularly preferably 3 ⁇ m to 10 ⁇ m. If the particle size of the inorganic material powder is too small, pores are not sufficiently formed, and impregnation of the transparent material becomes difficult. In addition, if the particle size of the inorganic material powder is too large, the particles are difficult to fuse with each other, making it difficult to form a three-dimensional continuous skeleton.
  • a mixture of phosphor particles and a transparent material is prepared.
  • the mixing method is not particularly limited.
  • phosphor particles can be introduced into a liquid resin main liquid and a curing agent at room temperature to form a mixture.
  • a fluorescent substance particle can be added to the glass melt
  • the impregnation temperature is preferably 1000 ° C. or lower, more preferably 950 ° C. or lower, and particularly preferably 900 ° C. or lower. If the impregnation temperature is too high, the phosphor particles are likely to be thermally deteriorated. When glass is used for the transparent material, if the impregnation temperature is too low, the softening flow of the glass becomes insufficient and the pores are not sufficiently filled. Therefore, the lower limit of the impregnation temperature is preferably 200 ° C.
  • the impregnation temperature of resin before hardening is 100 degrees C or less, It is more preferable that it is 50 degrees C or less, It is especially preferable that it is normal temperature.
  • the heating temperature is preferably 350 ° C. or lower, preferably 250 ° C. or lower, and preferably 150 ° C. or lower. If the heating temperature is too high, the resin may be thermally decomposed.
  • the phosphor particles are present in the pores of the skeleton by being dispersed in the transparent material.
  • the phosphor particles may be in contact with the skeleton. That is, the phosphor particles may be in contact with both the skeleton and the pores.
  • a mixture of phosphor particles and inorganic material powder is prepared, and the mixture is fired to produce a sintered body including the phosphor particles.
  • the maximum temperature when firing the mixture of the phosphor particles and the inorganic material powder is preferably 1600 ° C. or less, more preferably 1400 ° C. or less, and particularly preferably 1200 ° C. or less. preferable.
  • the valence of the luminescent center ion in the phosphor particles may change, and the quantum yield of the phosphor particles may decrease. Therefore, when firing the mixture of phosphor particles and inorganic material powder, it is preferable to fire in a reducing atmosphere or an inert atmosphere. By doing so, it is possible to suppress a change in the valence of the luminescent center ion.
  • the reducing atmosphere is preferably an atmosphere containing hydrogen.
  • the inert atmosphere is preferably a nitrogen atmosphere or an argon atmosphere.
  • baking can be performed in a reducing atmosphere or an inert atmosphere.
  • the average particle size (D 50 ) of the inorganic material powder is preferably 3 ⁇ m to 50 ⁇ m, more preferably 3 ⁇ m to 30 ⁇ m, and particularly preferably 3 ⁇ m to 10 ⁇ m. If the particle size of the inorganic material powder is too small, pores are not sufficiently formed, and impregnation of the transparent material becomes difficult. In addition, if the particle size of the inorganic material powder is too large, the particles are difficult to fuse with each other, making it difficult to form a three-dimensional continuous skeleton.
  • the pores formed by the skeleton are impregnated with the transparent material.
  • the same method as the production method (i) can be applied.
  • the phosphor particles are dispersed inside the skeleton made of an inorganic material.
  • the phosphor particles may protrude from the skeleton. That is, the phosphor particles may be in contact with both the skeleton and the pores.
  • the phosphor particles present in the skeleton and the phosphor particles present in the transparent material may be the same or different.
  • FIG. 3 is a schematic cross-sectional view showing a wavelength conversion element according to an embodiment of the present invention.
  • the wavelength conversion element 30 includes a wavelength conversion member 10 and a substrate 6 bonded to the wavelength conversion member 10.
  • the wavelength conversion member 10 and the substrate 6 are joined to each other by the transparent material 4 exposed from the surface of the wavelength conversion member 10, that is, a skeleton made of the inorganic material 3 is formed by the skeleton.
  • the substrate 6 is joined with the same material as the transparent material 4 filling the hole.
  • the wavelength conversion member and the substrate are joined to each other by the transparent material exposed from the surface of the wavelength conversion member.
  • the present invention is not limited to this, and the transparent material newly applied to the surface of the wavelength conversion member May be joined together.
  • an arbitrary adhesive different from the transparent material may be used.
  • the substrate has a rectangular plate shape and is bonded to one surface of the wavelength conversion member, but is not limited thereto, and may have any shape.
  • the shape which covers the side surface of a wavelength conversion member may be sufficient.
  • the substrate is preferably made of an inorganic material, and specifically includes glass, ceramics, metal, and the like.
  • ceramics or metal when used in applications where the wavelength conversion member has a high temperature, it is preferable to use ceramics or metal with high heat dissipation.
  • a metal when used as a reflection type light emitting device to be described later, it is preferable to use a metal.
  • the ceramic is preferably at least one selected from aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, and boron nitride.
  • the metal is preferably at least one selected from copper, aluminum, and iron.
  • the wavelength conversion element is preferably manufactured by closely integrating a skeleton made of an inorganic material of the wavelength conversion member and the substrate before the transparent material is cured when the wavelength conversion member is produced. Specifically, (i) a skeleton made of an inorganic material is impregnated with a mixture of phosphor particles and a transparent material, and the substrate and the skeleton are brought into close contact before the mixture is cured. Or (ii) before a transparent material is cured by impregnating a transparent material into a sintered body having a skeleton made of an inorganic material and phosphor particles dispersed in the skeleton.
  • the substrate and the sintered body are preferably adhered to each other, and the sintered body and the substrate are preferably integrated by a transparent material exposed from the pores.
  • an arbitrary adhesive different from the transparent material may be used.
  • the production method (i) for example, by immersing a skeleton made of an inorganic material in a mixture of phosphor particles and a transparent material, impregnating the mixture, and then taking out the skeleton before the mixture is cured, The mixture can be exposed from the pores.
  • the skeleton and the substrate are brought into close contact with each other in the atmosphere, whereby the skeleton and the substrate are brought into close contact with each other to obtain a wavelength conversion element.
  • both the skeleton and the substrate may be in close contact with each other in a mixture, that is, the mixture may be impregnated into the skeleton and the skeleton and the substrate may be integrated at the same time.
  • conditions, such as an impregnation temperature can apply the same conditions as the manufacturing method of the wavelength conversion member mentioned above.
  • a sintered body of an inorganic material and phosphor particles is immersed in a transparent material, impregnated with the transparent material, and then the sintered body is taken out before the transparent material is cured. Thereby, a transparent material can be exposed from the void
  • the sintered body and the substrate are brought into close contact with each other in the air, whereby the sintered body and the substrate are integrated to obtain a wavelength conversion element.
  • both the sintered body and the substrate may be immersed in a transparent material so that they are in close contact, that is, the sintered body may be impregnated with the transparent material and the sintered body and the substrate may be integrated at the same time.
  • conditions, such as an impregnation temperature can apply the same conditions as the manufacturing method of the wavelength conversion member mentioned above.
  • the substrate and the skeleton or the sintered body are brought into contact with each other and the mixture or the transparent material is cured in that state. If it does in this way, the impregnation of a mixture or a transparent material and joining of a frame
  • FIG. 4 is a schematic side view showing a light emitting device using the wavelength conversion member of the present invention according to the embodiment described above.
  • the light emitting device according to the present embodiment is a light emitting device using a transmission type wavelength conversion member.
  • the light emitting device 20 includes a wavelength conversion member 10 and a light source 5.
  • the excitation light L 0 emitted from the light source 5 is wavelength-converted by the wavelength conversion member 10 into fluorescence L 1 having a longer wavelength than the excitation light L 0 .
  • a part of the excitation light L 0 is transmitted through the wavelength conversion member 10.
  • the combined light L 2 of the excitation light L 0 and the fluorescence L 1 is emitted from the wavelength conversion member 10.
  • white synthetic light L 2 can be obtained.
  • FIG. 5 is a schematic side view showing a light-emitting device using the wavelength conversion element of the present invention according to the above-described embodiment.
  • the light emitting device according to this embodiment is a reflective light emitting device.
  • the light emitting device 40 includes a wavelength conversion element 30 and a light source 5.
  • the excitation light L 0 emitted from the light source 5 is wavelength-converted by the wavelength conversion member 10 into fluorescence L 1 having a longer wavelength than the excitation light L 0 .
  • a part of the fluorescence L 1 and the excitation light L 0 is reflected by the substrate 6.
  • the combined light L 2 of the excitation light L 0 and the fluorescence L 1 is emitted from the wavelength conversion element 30 from the side that irradiates the excitation light L 0 side.
  • the excitation light L 0 is blue light and the fluorescence L 1 is yellow light
  • white synthetic light L 2 can be obtained.
  • Examples of the light source include LEDs and LDs. From the viewpoint of increasing the light emission intensity of the light emitting device, it is preferable to use an LD capable of emitting high intensity light.
  • Tables 1 to 7 show Examples (Nos. 1 to 12, 14 to 50) and Comparative Examples (No. 13) of the present invention.
  • Examples (Nos. 1 to 12, 14 to 50) were produced as follows. First, phosphor particles and an inorganic material were mixed so as to have the contents shown in Tables 1 to 7 to obtain a mixture. The following materials were used for each material. In Tables 1 to 7, the phosphor particle content indicates the volume% of the mixture of the phosphor particles and the inorganic material.
  • the ratio of the total content of the phosphor particles and the inorganic material and the content of the immersed transparent material [phosphor particles + inorganic material]: [transparent material]
  • the phosphor particles and the inorganic material For the ratio of the total content of the sintering aid and the content of the impregnated transparent material ([phosphor particles + inorganic material + sintering aid]: [transparent material]), the obtained wavelength conversion
  • the sectional view of the member was binarized and calculated from the area ratio occupied by each region.
  • Inorganic material MgO powder (thermal conductivity: about 42 W / m ⁇ K, average particle diameter D 50 : 8 ⁇ m, refractive index (nd): 1.74) Al 2 O 3 powder (thermal conductivity: about 20 W / m ⁇ K, average particle diameter D 50 : 10 ⁇ m, refractive index (nd): 1.77)
  • the mixture obtained above was put in a mold and pressed at a pressure of 0.45 MPa to produce a preform.
  • the obtained preform was heated to a predetermined temperature in the atmosphere shown in Tables 1 to 7, held for 4 hours, and then slowly cooled to room temperature, thereby having a skeleton made of an inorganic material, A sintered body having phosphor particles dispersed therein was prepared. Note that a heat treatment (firing) performed in an atmosphere containing hydrogen was defined as a reducing atmosphere, and a heat treatment (firing) performed in a nitrogen atmosphere was defined as an inert atmosphere.
  • the above-mentioned sintered body was impregnated with the following transparent material at the temperatures shown in Tables 1 to 7.
  • Transparent material Transparent material A thiourethane resin, refractive index (nd): 1.74) Transparent material B (vinyl resin, refractive index (nd): 1.70) Transparent material C (acrylic resin, refractive index (nd): 1.72) Transparent material D (bismuth phosphate glass, refractive index (nd): 1.77) Transparent material E (tin phosphate glass, refractive index (nd): 1.75) Transparent material F (sulfide resin, refractive index (nd): 1.63) Transparent material G (silicone resin (Techne Glass, glass resin), refractive index (nd): 1.58) Transparent material H (borosilicate glass, refractive index (nd): 1.46)
  • the resin was impregnated into the sintered body at room temperature.
  • the thiourethane resin and the vinyl resin were used in the form of a mixture of a liquid resin main liquid and a curing agent. After the resin was cured by heat treatment, a rectangular plate-shaped wavelength conversion member was obtained by grinding and polishing.
  • the glass was heated to the temperatures shown in Tables 1 to 7, melted, and then impregnated into the sintered body. After the glass was cured, a rectangular plate-shaped wavelength conversion member was obtained by grinding and polishing.
  • Example No. A sample was prepared in the same manner as in Example 1. It was set to 13.
  • This comparative example is a sintered body having a skeleton made of an inorganic material and phosphor particles dispersed in the skeleton, but does not contain a transparent material.
  • the obtained wavelength conversion member was evaluated for thermal diffusivity, quantum efficiency, and translucency by the following methods. The results are shown in Tables 1-7. Moreover, the partial cross section photograph of the wavelength conversion member of Example 1 is shown in FIG.
  • the thermal diffusivity was measured by a thermal diffusivity measuring device ai-phase manufactured by Eye Phase.
  • the measurement of the thermal diffusivity was performed 11 times in a temperature range of 105 ° C. ⁇ 5 ° C., and the value obtained by averaging the results of 11 times was used as the thermal diffusivity of the sample.
  • Quantum efficiency refers to a value calculated by the following equation, and was measured using an absolute PL quantum yield device (Hamamatsu Photonics).
  • Quantum efficiency ⁇ (number of photons emitted from the sample as fluorescence) / (number of photons absorbed by the sample) ⁇ ⁇ 100 (%)
  • the translucency was judged by placing the obtained wavelength conversion member on a paper surface on which letters were written under a 1000 lux fluorescent lamp, and determining whether or not the shadow of the letters could be confirmed.
  • the thickness of the wavelength converting member was 500 ⁇ m. “ ⁇ ” indicates that the shadow of the character was confirmed, and “ ⁇ ” indicates that the shadow was not confirmed even when the thickness was 200 ⁇ m. Moreover, although the shadow of the character could not be confirmed at a thickness of 500 ⁇ m, the case where the shadow of the character was confirmed at a thickness of 200 ⁇ m was indicated as “ ⁇ ”.
  • the wavelength conversion members of Examples had a high thermal diffusivity of 1.23 ⁇ 10 ⁇ 6 m 2 / s or more. Moreover, all the examples were excellent in translucency. In particular, in Examples where the phosphor particle content was low, there was a tendency for thermal diffusivity and translucency to improve. Furthermore, in the examples where baking was performed in an inert atmosphere or a reducing atmosphere or in examples where the baking temperature was low, there was a tendency for the quantum efficiency to increase. On the other hand, since the wavelength conversion member of the comparative example (No.

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Abstract

L'objectif de la présente invention est de réaliser un module de conversion de longueur d'onde et un élément de conversion de longueur d'onde au moyen desquels la fusion d'un matériau constitutif ou une diminution de l'intensité d'émission de lumière au fil du temps peut être supprimée lorsque le module de conversion de longueur d'onde et l'élément de conversion de longueur d'onde sont irradiés par la lumière d'une DEL ou diode laser (LD) haute puissance, et de réaliser un procédé de fabrication du module de conversion de longueur d'onde et de l'élément de conversion de longueur d'onde, et un dispositif électroluminescent. Un module de conversion de longueur d'onde (10) comprend une matrice (1) et des particules luminescentes (2) dispersées dans la matrice (1), le module de conversion de longueur d'onde (10) étant caractérisé en ce que la matrice (1) est pourvue d'un squelette comprenant un matériau inorganique (3), et d'un matériau transparent (4) qui remplit les trous formés par le squelette, et le matériau inorganique (3) présente une conductivité thermique supérieure à celle du matériau transparent (4).
PCT/JP2019/020654 2018-06-12 2019-05-24 Module de conversion de longueur d'onde et élément de conversion de longueur d'onde, et procédé de fabrication associé, et dispositif electroluminescent WO2019239850A1 (fr)

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CN201980033998.6A CN112154358A (zh) 2018-06-12 2019-05-24 波长转换材料和波长转换元件、以及它们的制造方法和发光装置
DE112019002989.4T DE112019002989T5 (de) 2018-06-12 2019-05-24 Wellenlängen-Umwandlungsteil und Wellenlängen-Umwandlungselement, Verfahren zur Herstellung derselben und Licht emittierende Vorrichtung
US17/052,822 US20210231294A1 (en) 2018-06-12 2019-05-24 Wavelength conversion member and wavelength conversion element, method for manufacturing same, and light-emitting device

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JP2019057862A JP2020095233A (ja) 2018-06-12 2019-03-26 波長変換部材及び波長変換素子、並びにそれらの製造方法、並びに発光装置
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WO2022075293A1 (fr) * 2020-10-06 2022-04-14 シャープ株式会社 Élément de conversion de longueur d'onde, équipement optique et procédé de fabrication d'élément de conversion de longueur d'onde

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