WO2020213456A1 - 波長変換部材及びその製造方法、並びに発光装置 - Google Patents

波長変換部材及びその製造方法、並びに発光装置 Download PDF

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Publication number
WO2020213456A1
WO2020213456A1 PCT/JP2020/015530 JP2020015530W WO2020213456A1 WO 2020213456 A1 WO2020213456 A1 WO 2020213456A1 JP 2020015530 W JP2020015530 W JP 2020015530W WO 2020213456 A1 WO2020213456 A1 WO 2020213456A1
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Prior art keywords
wavelength conversion
conversion member
conductive particles
particle size
particles
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PCT/JP2020/015530
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English (en)
French (fr)
Japanese (ja)
Inventor
彰太郎 福本
俊輔 藤田
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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Priority to JP2021514888A priority Critical patent/JPWO2020213456A1/ja
Priority to US17/593,713 priority patent/US12140785B2/en
Priority to DE112020001953.5T priority patent/DE112020001953T5/de
Priority to CN202080016901.3A priority patent/CN113474439A/zh
Publication of WO2020213456A1 publication Critical patent/WO2020213456A1/ja
Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/206—Filters comprising particles embedded in a solid matrix
    • 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
    • H01S5/022—Mountings; Housings
    • H01S5/0225—Out-coupling of light
    • 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
    • H01S5/024—Arrangements for thermal management
    • H01S5/02469—Passive cooling, e.g. where heat is removed by the housing as a whole or by a heat pipe without any active cooling element like a TEC
    • 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
    • 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
    • H01S5/005—Optical components external to the laser cavity, specially adapted therefor, e.g. for homogenisation or merging of the beams or for manipulating laser pulses, e.g. pulse shaping
    • H01S5/0087—Optical components external to the laser cavity, specially adapted therefor, e.g. for homogenisation or merging of the beams or for manipulating laser pulses, e.g. pulse shaping for illuminating phosphorescent or fluorescent materials, e.g. using optical arrangements specifically adapted for guiding or shaping laser beams illuminating these materials

Definitions

  • the present invention relates to a wavelength conversion member that converts the wavelength of light emitted by a light emitting diode (LED: Light Emitting Audio), a laser diode (LD: Laser Diode), or the like into another wavelength, a method for manufacturing the same, and a light emitting device.
  • LED Light Emitting Audio
  • LD Laser Diode
  • the excitation light for example, blue light
  • the conversion light for example, blue light
  • the wavelength conversion member for example, a member in which phosphor particles are dispersed and fixed in a resin matrix or a glass matrix is disclosed (Patent Documents 1 to 3).
  • the intensity of excitation light has been improving with the increase in power of light emitting devices.
  • the intensity of heat generated by the phosphor particles increases, and the wavelength conversion member tends to have excessive heat.
  • the conventional wavelength conversion member has a problem that the excessive heat tends to cause a decrease in emission intensity with time (temperature quenching), deformation of the constituent material, discoloration, and the like.
  • the present invention provides a wavelength conversion member and a method for manufacturing the same, and a light emitting device capable of suppressing a temperature rise of the wavelength conversion member and suppressing a decrease in emission intensity over time, deformation and discoloration of constituent materials.
  • the purpose is to provide.
  • the wavelength conversion member of the present invention is a wavelength conversion member including heat conductive particles and phosphor particles, and the heat conductive particles include two types of heat conductive particles having different average particle diameters from each other. It is a feature.
  • the thermally conductive particles are composed of two types having different average particle diameters from each other.
  • the presence of the thermally conductive particles having different particle diameters makes it easier for the thermally conductive particles to exist densely in the wavelength conversion member, and when the wavelength conversion member is irradiated with excitation light, the phosphor particles It becomes easy to efficiently release the generated heat to the outside. As a result, it becomes easy to suppress a decrease in emission intensity over time (temperature quenching), deformation of the constituent material, and discoloration.
  • the wavelength conversion member of the present invention is preferably a sintered body of thermally conductive particles and phosphor particles.
  • the heat conductive particles include large particle size heat conductive particles and small particle size heat conductive particles, and the average particle size D of the large particle size heat conductive particles and the small particle size. It is preferable that the average particle size d of the heat conductive particles satisfies the following conditions (A) and (B). (A) 0.5 ⁇ m ⁇ D ⁇ 50 ⁇ m (B) 0.0001 ⁇ d / D ⁇ 0.1
  • the average particle size D of the large particle size thermally conductive particles and the average particle size D P of the phosphor particles satisfy the following condition (C). (C) 0.1 ⁇ D P / D ⁇ 10
  • Wavelength conversion member of the present invention the content of V of the large diameter thermally conductive particles occupying in the wavelength conversion member, the content V P of the phosphor particles, it is preferable to satisfy the following condition (D). (D) 50% ⁇ VP + V ⁇ 90%
  • the heat conductive particles are composed of oxides.
  • the thermally conductive particles are magnesium oxide.
  • the content V P of the phosphor particles is preferably 0.01 to 80% by vol%.
  • the wavelength conversion member of the present invention is a wavelength conversion member for converting the wavelength of the excitation light emitted from the light source, and is the excitation light transmitted through the wavelength conversion member and the light emitted by converting the wavelength of the excitation light.
  • the sum of the variations of the chromaticity Cx and the chromaticity Cy in all the rays of the combined light is 0.03 or less.
  • the method for manufacturing a wavelength conversion member of the present invention is the above-mentioned method for manufacturing a wavelength conversion member, in which heat conductive particles containing two types of heat conductive particles having different average particle diameters are mixed with phosphor particles. It is characterized by comprising a step of baking.
  • firing is performed by a heating press.
  • the maximum temperature at the time of firing is 1300 ° C. or less.
  • the wavelength conversion member of the present invention it is preferable to perform firing in an inert atmosphere, a reducing atmosphere or a vacuum atmosphere.
  • the light emitting device of the present invention is characterized by including the above-mentioned wavelength conversion member and a light source for irradiating the wavelength conversion member with excitation light.
  • the light source is a laser diode.
  • a wavelength conversion member capable of suppressing a temperature rise of the wavelength conversion member, a decrease in emission intensity over time, deformation and discoloration of constituent materials, a method for manufacturing the same, and a light emitting device. can do.
  • FIG. 1 is a schematic cross-sectional view showing an embodiment of the wavelength conversion member of the present invention.
  • the wavelength conversion member 10 includes the heat conductive particles 1 and the phosphor particles 4.
  • the heat conductive particles 1 include two types of heat conductive particles having different average particle diameters, that is, a large particle size heat conductive particle 2 and a small particle size heat conductive particle 3.
  • the small particle size thermally conductive particles 3 are present between the large particle size thermally conductive particles 2 and between the large particle size thermally conductive particles 2 and the phosphor particles 4.
  • each component will be described in detail.
  • the thermally conductive particles 1 are preferably composed of oxides, and particularly preferably composed of metal oxides having high thermal conductivity. Specifically, aluminum oxide, magnesium oxide, and zinc oxide are preferable, and magnesium oxide is particularly preferable. Among them, magnesium oxide has a high thermal conductivity (45 to 60 W ⁇ m -1 ⁇ K -1 ), so that the heat generated by the phosphor particles 4 can be effectively released to the outside. Further, the light absorption in the excitation light wavelength region (for example, 300 to 500 nm) and the emission wavelength region (for example, 380 to 780 nm) of the phosphor particles 4 described later is small, and the light extraction efficiency of the wavelength conversion member 10 is unlikely to be lowered. These may be used alone or in combination of two or more.
  • the thermal conductivity of the thermally conductive particles 1 is preferably 15 W ⁇ m -1 ⁇ K -1 or more, more preferably 20 W ⁇ m -1 ⁇ K -1 or more, and 30 W ⁇ m -1 ⁇ . It is particularly preferable that it is K- 1 or higher. In this way, the heat generated by the phosphor particles 4 can be effectively released to the outside.
  • the heat conductive particles 1 include two types of heat conductive particles having different average particle diameters from each other. Specifically, it includes a large particle size thermally conductive particle 2 and a small particle size thermally conductive particle 3.
  • the large particle size thermally conductive particles 2 and the small particle size thermally conductive particles 3 are preferably composed of the same oxide.
  • the large particle size thermally conductive particles 2 are magnesium oxide
  • it is preferable that the small particle size thermally conductive particles 3 are also magnesium oxide. In this way, when the wavelength conversion member 10 is irradiated with excitation light, cracks due to the difference in thermal expansion are less likely to occur at the interface between the large particle size thermally conductive particles 2 and the small particle size thermally conductive particles 3. ..
  • the wavelength conversion member 10 is manufactured by firing, the two are bonded to each other, and it becomes easy to obtain the wavelength conversion member 10 made of a dense sintered body.
  • the content V of the large particle size thermally conductive particles 2 in the entire wavelength conversion member 10 is 0.01 to 80%, 0.1 to 75%, 1 to 70%, 5 to 60%, in particular, in volume%. It is preferably 10 to 50%. If the content V is too large, it becomes difficult for the small particle size thermally conductive particles 3 to enter between the large particle size thermally conductive particles 2 and the phosphor particles 4, and it becomes difficult to densify the particles. As a result, it becomes difficult to release the heat generated by the phosphor particles 4 to the outside. Even if the content V is too small, the heat conduction path by the large particle size heat conductive particles 2 is reduced, so that it becomes difficult to release the heat generated by the phosphor particles 4 to the outside.
  • the content V s of the small particle size thermally conductive particles 3 in the entire wavelength conversion member 10 is 0.01 to 50%, 0.1 to 40%, 1 to 30%, 5 to 30%, 10 by volume. It is particularly preferably about 30%. If the content V s is too large, the distance between the large particle size thermally conductive particles 2 and the phosphor particles 4 becomes large, so that it becomes difficult to release the heat generated by the phosphor particles 4 to the outside. If the content V s is too small, the small particle size thermally conductive particles 3 cannot sufficiently exist in the gaps between the large particle size thermally conductive particles 2 and the phosphor particles 4, and the heat generated by the phosphor particles 4 is externally generated. It becomes difficult to release to.
  • the average particle diameter D of the large particle size thermally conductive particles 2 and the average particle diameter d of the small particle size thermally conductive particles 3 satisfy the following conditions (A) and (B). By doing so, the large particle size thermally conductive particles 2 and the small particle size thermally conductive particles 3 are likely to be densely present in the wavelength conversion member 10, and the heat generated by the phosphor particles 4 is released to the outside. It will be easier to do.
  • the average particle size means a value measured by a laser diffraction method, and in the volume-based cumulative particle size distribution curve when measured by a laser diffraction method, the integrated amount is accumulated from the smaller particle. It shows a particle size of 50%.
  • the particle size distribution of each particle is considered to have a monomodal distribution shape in principle. That is, particles having a bimodal distribution shape are considered to be a mixture of two or more types of monomodal particle size distribution shapes, and after peak separation, the average particle size is calculated for each distribution.
  • the average particle size D of the large particle size thermally conductive particles 2 is preferably 0.5 ⁇ m ⁇ D ⁇ 50 ⁇ m, more preferably 1 ⁇ m ⁇ D ⁇ 40 ⁇ m, and further preferably 3 ⁇ m ⁇ D ⁇ 30 ⁇ m. It is preferable that 5 ⁇ m ⁇ D ⁇ 10 ⁇ m. If the average particle diameter D is too large, the phosphor particles 4 are likely to be unevenly distributed, and color unevenness is likely to occur. If the average particle size D is too small, the path of the heat path transmitted inside the large particle size heat conductive particles 2 becomes short, and it becomes difficult to form a sufficient heat path.
  • the particle size ratio d / D between the average particle size D of the large particle size thermally conductive particles 2 and the average particle size d of the small particle size thermally conductive particles 3 is 0.0001 ⁇ d / D ⁇ 0.1. It is preferable that 0.0005 ⁇ d / D ⁇ 0.05, and 0.001 ⁇ d / D ⁇ 0.01 is particularly preferable. If the particle size ratio d / D is too large, it becomes difficult for the small particle size thermally conductive particles 3 to sufficiently exist in the gaps composed of the large particle size thermally conductive particles 2 and the phosphor particles 4, and the phosphor particles 4 It becomes difficult to release the generated heat to the outside.
  • the particle size ratio d / D is too small, agglomeration of the small particle size heat conductive particles 3 tends to occur, and the small particle size heat conduction in the gaps composed of the large particle size heat conductive particles 2 and the phosphor particles 4. It becomes difficult for the sex particles 3 to sufficiently exist, and it becomes difficult for the heat generated by the phosphor particles 4 to be released to the outside.
  • the phosphor particle 4 is preferably an inorganic phosphor having an excitation band at a wavelength of 300 to 500 nm and an emission peak at a wavelength of 380 to 780 nm.
  • oxide phosphors, nitride phosphors, oxynitride phosphors, chloride phosphors, acidified phosphors, halide phosphors, aluminate phosphors and halophosphate phosphors can be used. it can.
  • oxide phosphors and oxynitride phosphors are preferable because they have high heat resistance and do not easily deteriorate during firing.
  • garnet-based ceramic phosphor particles containing YAG (yttrium aluminum garnet) phosphor particles it is preferable to use garnet-based ceramic phosphor particles containing YAG (yttrium aluminum garnet) phosphor particles.
  • a plurality of phosphor particles 4 may be mixed and used according to the wavelength range of excitation light or emission.
  • the average particle diameter D P of the phosphor particles 4 is preferably 0.1 ⁇ 50 [mu] m, more preferably 1 ⁇ 30 [mu] m, particularly preferably 3 ⁇ 20 [mu] m.
  • the average particle diameter D P is too small, the phosphor particles 4 are likely to agglomerate during production, the emission color of the wavelength conversion member 10 is likely to become uneven.
  • the luminous efficiency of the phosphor particles 4 itself becomes low, and the brightness of the wavelength conversion member 10 tends to decrease. Be an average particle diameter D P is too large, the emission color of the wavelength conversion member 10 is likely to become uneven.
  • the LD has a small spot size of excitation light and strong directivity
  • the excitation light does not hit the phosphor particles 4 and is transmitted. Is easy to occur. Therefore, when the wavelength conversion member 10 is used in a light emitting device using the LD as a light source, the average particle size of the phosphor particles 4 is preferably 15 ⁇ m or less, particularly preferably 10 ⁇ m or less.
  • the content V p of the phosphor particles 4 in the wavelength conversion member 10 of the transmission type preferably 0.01 to 50%, more preferably 0.1 to 35% 1-20% Is particularly preferable.
  • the average particle size D P of the phosphor particles 4 and the average particle size D of the large particle size thermally conductive particles 2 preferably satisfy 0.1 ⁇ D P / D ⁇ 10, and 0.5 ⁇ D P / it is more preferable to satisfy D ⁇ 5, 1 ⁇ D more preferably to satisfy the P / D ⁇ 3, it is particularly preferably 1 ⁇ D P / D ⁇ 3 .
  • the phosphor particles 4 and the large-particle heat conductive particles 2 are likely to be uniformly dispersed and exist in the wavelength conversion member 10, and when the wavelength conversion member 10 is irradiated with the excitation light, the excitation light is easily present.
  • the heat generated by the phosphor particles 4 can be efficiently released to the outside.
  • resulting an average particle diameter D P of the phosphor particles 4 is greater (1 ⁇ D P / D) is compared to the average particle diameter D of the large diameter thermally conductive particles 2, a dense wavelength converting member 10 It will be easier.
  • the content V P of the phosphor particles 4 in the entire wavelength converting member 10 preferably satisfies 50% ⁇ V P + V ⁇ 90%, 55% ⁇ it is more preferable to satisfy V P + V ⁇ 85%, and particularly preferably satisfies 60% ⁇ V P + V ⁇ 80%. In this way, when the wavelength conversion member 10 is irradiated with the excitation light, the heat generated by the phosphor particles 4 can be easily efficiently released to the outside.
  • the wavelength conversion member 10 is preferably a sintered body of the thermally conductive particles 1 and the phosphor particles 4. In this way, the heat conductive particles 1 and the phosphor particles 4 are bound to each other, and the heat generated by the phosphor particles 4 can be more effectively released to the outside. In addition, compared to a wavelength conversion member in which phosphor particles are dispersed and fixed in a translucent material such as a resin matrix or a glass matrix, discoloration or discoloration occurs even when high-power excitation light such as LD is irradiated. Dissolution is less likely to occur.
  • the thermal diffusivity of the wavelength conversion member 10 is 2 ⁇ 10 -6 m 2 / s or more, preferably 3 ⁇ 10 -6 m 2 / s or more, and 4 ⁇ 10 -6 m 2 / s or more. It is more preferably 5 ⁇ 10 -6 m 2 / s or more.
  • the quantum efficiency of the wavelength conversion member 10 is preferably 20% or more, more preferably 40% or more, further preferably 60% or more, and particularly preferably 80% or more. If the quantum efficiency is too low, the energy that causes heat loss becomes large, and the luminous efficiency of the wavelength conversion member 10 tends to decrease.
  • the quantum efficiency refers to a value calculated by the following formula, and can be measured using an absolute PL quantum yield device.
  • Quantum efficiency ⁇ (number of photons emitted from the sample as fluorescence) / (number of photons absorbed by the sample) ⁇ x 100 (%)
  • the shape of the wavelength conversion member 10 can be, for example, a plate shape (rectangular plate shape, disk shape, etc.).
  • the thickness of the wavelength conversion member 10 is preferably 1000 ⁇ m or less, more preferably 800 ⁇ m or less, and particularly preferably 500 ⁇ m or less. If the thickness is too large, it will be difficult to obtain the desired shade of light. In addition, the luminous efficiency tends to decrease.
  • the thickness of the wavelength conversion member 10 is preferably 30 ⁇ m or more, more preferably 50 ⁇ m or more, and particularly preferably 80 ⁇ m or more. If the thickness is too small, the mechanical strength of the wavelength conversion member 10 tends to decrease.
  • the porosity of the wavelength conversion member 10 is preferably 10% or less, more preferably 5% or less, and particularly preferably 1% or less, based on the total product of the wavelength conversion member 10. If the porosity is too high, it becomes difficult to release the heat generated by the phosphor particles 4 to the outside. In addition, the mechanical strength of the wavelength conversion member 10 tends to decrease. Further, the light extraction efficiency of the wavelength conversion member 10 tends to decrease.
  • the lower limit of the porosity is not particularly limited, but is actually 0.01% or more.
  • the wavelength conversion member 10 of the present invention has small color unevenness. Specifically, the sum of the variations of the chromaticity Cx and the chromaticity Cy in all the combined light of the excitation light transmitted through the wavelength conversion member 10 and the light emitted by converting the wavelength of the excitation light is 0.03 or less. It is particularly preferable that it is 0.025 or less, 0.02 or less, and 0.015 or less. In the present invention, the sum of the variations of the chromaticity Cx and the chromaticity Cy can be obtained by the following methods (i) and (ii).
  • the variation in chromaticity Cx is the difference (Cx max- Cx) between the maximum chromaticity Cx (Cx max ) among the four pieces and the smallest chromaticity Cx (Cx min ) among the four small pieces. min ).
  • the variation in chromaticity Cy is the difference (Cy max- ) between the maximum chromaticity Cy (Cy max ) among the four small pieces and the minimum chromaticity Cy (Cy min ) among the four small pieces. Cy min ). From these values, the sum of the variation in chromaticity Cx and the variation in chromaticity Cy ⁇ (Cx max- Cx min ) + (Cy max- Cy min ) ⁇ can be calculated.
  • two plates having a through hole of ⁇ (X-0.1) mm in the center are prepared, and the small pieces are sandwiched by aligning the centers.
  • the excitation light is irradiated from one surface, the light emitted from the other surface is taken into the integrating sphere, and the chromaticity of all the light rays is measured. This is measured for each of the four small pieces. From the obtained data, the variation in chromaticity Cx and the variation in chromaticity Cy are obtained.
  • the method of obtaining the sum of the variation in the chromaticity Cx and the variation in the chromaticity Cy is the same as in the above method (i).
  • the method for producing the wavelength conversion member 10 of the present invention preferably includes a step of mixing and firing the heat conductive particles 1 containing two types of heat conductive particles having different average particle diameters and the phosphor particles 4.
  • Baking is preferably performed by a heating press. By doing so, it becomes easy to obtain a dense sintered body, and it becomes easy to increase the thermal conductivity of the wavelength conversion member 10.
  • the press surface pressure can be appropriately adjusted according to the thickness of the target wavelength conversion member 10. For example, 1 MPa or more is preferable, 10 MPa or more is more preferable, and 20 MPa or more is particularly preferable.
  • the upper limit is not particularly limited, but in order to prevent damage to the press die, it is preferably 100 MPa or less, and particularly preferably 50 MPa or less.
  • the maximum temperature at the time of firing is preferably 1300 ° C. or lower, more preferably 1200 ° C. or lower, further preferably 1100 ° C. or lower, and particularly preferably 1000 ° C. or lower. If the maximum temperature at the time of firing is too high, the phosphor particles 4 are likely to be deteriorated by heat. If the maximum temperature at the time of firing is too low, it becomes difficult to obtain a dense sintered body. From such a viewpoint, the maximum temperature at the time of firing is preferably 600 ° C. or higher, more preferably 650 ° C. or higher, and particularly preferably 700 ° C. or higher.
  • the press time is preferably 0.1 to 300 minutes, more preferably 0.5 to 120 minutes, and particularly preferably 1 to 60 minutes.
  • the atmosphere at the time of firing is preferably an inert atmosphere, a reducing atmosphere or a vacuum atmosphere. By doing so, it becomes easy to suppress the deterioration of the phosphor particles 4 and the deterioration of the heat conductive particles 1. In addition, deterioration due to oxidation of the press die can be easily suppressed.
  • nitrogen or argon in the inert atmosphere. From the viewpoint of running cost, it is particularly preferable to use nitrogen.
  • the reducing atmosphere it is preferable to use hydrogen, and it is particularly preferable to use a mixed gas of hydrogen and an inert gas.
  • the inert gas refers to nitrogen or argon.
  • the mixed powder of the phosphor particles 4, the large particle size thermally conductive particles 2, and the small particle size thermally conductive particles 3 is pressed with a mold, and the obtained premolded body is fired. May produce a sintered body.
  • the preformed body may be encapsulated in a rubber mold to produce a sintered body by a hot isostatic pressing method.
  • FIG. 2 is a schematic cross-sectional view showing a light emitting device according to an embodiment of the present invention.
  • the light emitting device 50 includes a wavelength conversion member 10 and a light source 6.
  • the light source 6 is arranged so that the excitation light L 0 is incident on the wavelength conversion member 10.
  • the excitation light L 0 emitted from the light source 6 is wavelength-converted by the wavelength conversion member 10 into fluorescence L 1 having a wavelength longer than that of the excitation light L 0 .
  • a part of the excitation light L 0 passes through the wavelength conversion member 10. Therefore, the combined light L 2 of the excitation light L 0 and the fluorescence L 1 is emitted from the wavelength conversion member 10.
  • the excitation light L 0 is blue light and the fluorescence L 1 is yellow light
  • white synthetic light L 2 can be obtained.
  • the light source 6 is preferably an LED or an LD. From the viewpoint of increasing the light emission intensity of the light emitting device 50, it is particularly preferable to use an LD capable of emitting high intensity light.
  • Tables 1 and 2 show Examples (No. 1, 3 to 14) and Comparative Examples (No. 2) of the present invention.
  • Examples (No. 1, 3 to 14) were prepared as follows. First, the phosphor particles, the large particle size thermally conductive particles and the small particle size thermally conductive particles were mixed so as to have the contents shown in Tables 1 and 2 to obtain a mixture. The following materials were used for each material.
  • thermally conductive particles MgO particles (thermal conductivity: about 45 W / m ⁇ K, average particle diameter: 3 ⁇ m, 8 ⁇ m, 12 ⁇ m, 25 ⁇ m, 47 ⁇ m, refractive index (nd): 1.74)
  • the mixture obtained above was placed in a mold, heat-press fired under the conditions shown in Table 1, and then slowly cooled to room temperature to prepare a wavelength conversion member which is a sintered body.
  • Comparative example (No. 2) was prepared as follows. First, the phosphor particles and the large particle size thermally conductive particles were mixed so as to have the contents shown in Table 1 to obtain a mixture. The same material as in Example (No. 1) was used for each material.
  • the mixture obtained above was placed in a mold and pressed at 0.45 MPa to form a green compact, which was then calcined under the conditions shown in Table 1. After firing, the wavelength conversion member, which is a sintered body, was produced by slowly cooling to room temperature.
  • the obtained wavelength conversion member was evaluated for thermal diffusivity, quantum efficiency, and color unevenness by the following methods. The results are shown in Tables 1 and 2.
  • the thermal diffusivity was measured by a thermal diffusivity measuring device ai-phase manufactured by iPhase.
  • the thermal diffusivity was measured 11 times in total under the condition of 105 ⁇ 5 ° C., and the value obtained by averaging the results of the 11 times was taken as the thermal diffusivity of the sample.
  • Quantum efficiency refers to the value calculated by the following formula, and was measured using an absolute PL quantum yield device (manufactured by Hamamatsu Photonics).
  • Quantum efficiency ⁇ (number of photons emitted from the sample as fluorescence) / (number of photons absorbed by the sample) ⁇ x 100 (%)
  • Color unevenness was evaluated as follows. First, the obtained wavelength conversion member was mirror-polished to prepare a plate-shaped sample having a thickness of 200 ⁇ m. A part of the obtained plate-shaped sample was cut out to a size of 5 mm ⁇ 5 mm and divided into four to a size of 2.5 mm ⁇ 2.5 mm to obtain four small pieces. Next, two aluminum plates having a thickness of 1 mm and a 30 mm ⁇ 30 mm surface having a circular through hole of ⁇ 2.4 mm in the center and black alumite treatment were prepared, and one of the above small pieces was sandwiched between the two plates. This was used as a measurement sample.
  • the excitation light (wavelength 450 nm) was irradiated from one main surface of the measurement sample, and the light emitted from the other main surface of the measurement sample was taken into the integrating sphere to measure the chromaticity. Further, a measurement sample was prepared in the same manner using the remaining three small pieces, and the chromaticity was measured. From the obtained data, the maximum value Cx max and the minimum value Cx min of the chromaticity Cx, the maximum value Cy max and the minimum value Cy min of the chromaticity Cy are obtained, and the sum of the variation of the chromaticity Cx and the variation of the chromaticity Cy ⁇ (( Cx max- Cx min ) + (Cy max- Cy min ) ⁇ was calculated. When the sum of the variations of the obtained chromaticity Cx and the chromaticity Cy was 0.03 or less, it was evaluated as “ ⁇ ”, and when it was larger than 0.03, it was evaluated as “x”.
  • the wavelength conversion members of Examples had a high thermal diffusivity of 2.0 ⁇ 10-6 m 2 / s or more.
  • the quantum efficiency was as high as 80% or more.
  • the wavelength conversion member of Comparative Example had a low thermal diffusivity of 1.0 ⁇ 10-6 m 2 / s and a low quantum efficiency of 79%.
  • Thermally conductive particles 1 Thermally conductive particles 2 Large particle size thermally conductive particles 3 Small particle size thermally conductive particles 4 Phosphorescent particles 6 Light source 10 Wavelength conversion member 50 Light emitting device

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  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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PCT/JP2020/015530 2019-04-18 2020-04-06 波長変換部材及びその製造方法、並びに発光装置 Ceased WO2020213456A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2021514888A JPWO2020213456A1 (https=) 2019-04-18 2020-04-06
US17/593,713 US12140785B2 (en) 2019-04-18 2020-04-06 Wavelength conversion member, production method therefor, and light-emitting device
DE112020001953.5T DE112020001953T5 (de) 2019-04-18 2020-04-06 Wellenlängen-umwandlungselement, verfahren zu dessen herstellung und lichtemittierende vorrichtung
CN202080016901.3A CN113474439A (zh) 2019-04-18 2020-04-06 波长转换部件及其制造方法、以及发光装置

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