WO2020070995A1 - 蛍光体プレートおよびそれを用いた発光装置 - Google Patents
蛍光体プレートおよびそれを用いた発光装置Info
- Publication number
- WO2020070995A1 WO2020070995A1 PCT/JP2019/032618 JP2019032618W WO2020070995A1 WO 2020070995 A1 WO2020070995 A1 WO 2020070995A1 JP 2019032618 W JP2019032618 W JP 2019032618W WO 2020070995 A1 WO2020070995 A1 WO 2020070995A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- phosphor plate
- phosphor
- sialon
- alumina
- less
- Prior art date
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 163
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims description 19
- 239000004065 semiconductor Substances 0.000 claims description 12
- 230000003746 surface roughness Effects 0.000 claims description 10
- 150000004767 nitrides Chemical class 0.000 claims description 9
- 238000002834 transmittance Methods 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 2
- 150000002602 lanthanoids Chemical class 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229910003564 SiAlON Inorganic materials 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 21
- 239000002994 raw material Substances 0.000 description 21
- 238000000034 method Methods 0.000 description 13
- 238000005245 sintering Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012071 phase Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000000295 emission spectrum Methods 0.000 description 7
- 239000011812 mixed powder Substances 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000006104 solid solution Substances 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 229910007991 Si-N Inorganic materials 0.000 description 2
- 229910006294 Si—N Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
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- 229920001778 nylon Polymers 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- 229910018509 Al—N Inorganic materials 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
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- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
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- 239000011261 inert gas Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/77344—Aluminosilicates
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Definitions
- the present invention relates to a phosphor plate and a light emitting device using the same.
- Patent Literature 1 describes a plate-shaped luminescent color conversion member in which an inorganic phosphor is dispersed in SiO 2 glass (FIG. 4 of Patent Literature 1, Claim 1).
- the present inventor further studied and found that a phosphor plate capable of obtaining stable luminous efficiency can be realized by combining and combining appropriate materials of ⁇ -sialon phosphor and alumina (Al 2 O 3 ). And completed the present invention.
- a phosphor plate comprising a composite including an ⁇ -sialon phosphor and a sintered body containing alumina is provided.
- a group III nitride semiconductor light emitting device comprising:
- a phosphor plate having excellent luminous efficiency and a light emitting device using the same are provided.
- FIG. 2A is a cross-sectional view schematically illustrating a configuration of a flip-chip type light emitting device
- FIG. 2B is a cross-sectional view schematically illustrating a configuration of a wire bonding type light emitting element.
- FIG. 2 is a schematic diagram of an apparatus for measuring an emission spectrum of a complex. 4 is an emission spectrum obtained from the composites of Examples 1 and 2 and Comparative Example 1.
- the outline of the phosphor plate of the present embodiment will be described.
- the phosphor plate of the present embodiment is composed of a plate-like member made of a composite including an ⁇ -sialon phosphor and a sintered body containing alumina.
- the phosphor plate can function as a wavelength converter that emits light by converting the irradiated blue light into orange light.
- a stable luminous efficiency can be obtained by combining an appropriate material of an ⁇ -sialon phosphor and alumina (Al 2 O 3 ) as components constituting a composite. It has been found that plates can be realized.
- the difference in refractive index between the ⁇ -sialon phosphor and alumina is appropriately reduced, and the ⁇ -sialon phosphor is compared with the composite of glass powder (SiO 2 ). It is considered that light emitted from the phosphor is easily taken out and the light conversion efficiency is increased. Further, as compared with the case where glass powder is used, the use of alumina can increase the thermal conductivity. This suppresses a decrease in light emission intensity due to heating, so that the phosphor plate of the present embodiment can be applied to a high-output light emitting element.
- the difference in refractive index is too small, as in the case of a combination of a YAG phosphor and alumina, light scattering becomes difficult, and it is necessary to increase the phosphor content in order to prevent transmission of blue light.
- the difference in the refractive index between the ⁇ -sialon phosphor and alumina is moderately large, promoting the scattering of blue light, efficiently suppressing the transmission of blue light with a low phosphor content, and increasing the orange color with high brightness. It is considered that light can be emitted.
- ⁇ -sialon phosphor about 2
- YAG phosphor about 1.8
- Al 2 O 3 about 1.7
- SiO 2 about 1.4
- the peak wavelength of the converted wavelength light emitted from the phosphor plate is preferably 585 nm or more and 605 nm or less. According to this, a light emitting device that emits orange light with high luminance can be obtained by combining a phosphor plate with a light emitting element that emits blue light.
- the mixed state means a state in which the ⁇ -sialon phosphor is dispersed in alumina serving as a base material (matrix phase). That is, the composite may have a structure in which ⁇ -sialon phosphor particles are dispersed between and / or within the crystal grains of the (poly) crystal constituting the base material.
- the ⁇ -sialon phosphor particles may be uniformly dispersed in a base material (alumina sintered body).
- the ⁇ -sialon phosphor of the present embodiment includes an ⁇ -sialon phosphor containing an Eu element represented by the following general formula (1).
- M represents at least one element selected from the group consisting of Li, Mg, Ca, Y and lanthanide elements (excluding La and Ce)
- p is the valence of the M element, 0 ⁇ X ⁇ 0.5, 1.5 ⁇ m ⁇ 4.0, and 0 ⁇ n ⁇ 2.0.
- n may be, for example, 2.0 or less, 1.0 or less, or 0.8 or less.
- the solid solution composition of ⁇ -sialon is such that m Si—N bonds in an ⁇ -type silicon nitride unit cell (Si1 2 N 16 ) are converted into Al—N bonds, and n Si—N bonds are converted into Al—O bonds.
- m / p cations M, Eu
- M, Eu m / p cations
- ⁇ -sialon is stabilized in a wide composition range, and a part of the sialon is replaced by Eu serving as an emission center, so that it is excited by light in a wide wavelength range from ultraviolet to blue, and from yellow to yellow.
- a phosphor that emits orange visible light is obtained.
- the solid solution composition cannot be strictly defined by composition analysis or the like.
- the crystal phase of the ⁇ -sialon an ⁇ -sialon single phase is preferable, and other crystal phases may include ⁇ -sialon, aluminum nitride or its polytypoid, Ca 2 Si 5 N 8 , CaAlSiN 3 and the like.
- a method for producing the ⁇ -type sialon phosphor there is a method in which a mixed powder composed of a compound of silicon nitride, aluminum nitride, and an interstitial solid solution element is heated and reacted in a high-temperature nitrogen atmosphere. In the heating step, a part of the components forms a liquid phase, and a substance is transferred to the liquid phase, whereby an ⁇ -sialon solid solution is generated.
- a plurality of equiaxed primary particles are sintered to form massive secondary particles.
- the primary particles in the present embodiment are the smallest particles that have the same crystal orientation in the particles and can exist alone.
- the lower limit of the average particle diameter of the ⁇ -sialon phosphor is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more.
- the upper limit of the average particle size of the ⁇ -sialon phosphor is preferably 30 ⁇ m or less, more preferably 20 ⁇ m or less.
- the average particle size of the ⁇ -sialon phosphor is the size of the secondary particles.
- the average particle size of the ⁇ -sialon phosphor is defined as a small particle size in a volume-based particle size distribution obtained by a laser diffraction / scattering type particle size distribution measuring method (LS13-320, manufactured by Beckman Coulter, Inc.). Means the particle diameter D50 of 50% of the integration of the passing amount (integrated passing ratio) from the sample.
- the lower limit of the content of the ⁇ -sialon phosphor is, for example, 5 vol% or more, preferably 10 vol% or more, more preferably 15 vol% or more, in terms of volume, with respect to the entire composite. This makes it possible to increase the light emission intensity of the thin phosphor plate. Further, the light conversion efficiency of the phosphor plate can be improved.
- the upper limit of the content of the ⁇ -sialon phosphor is, for example, 50% by volume or less, preferably 45% by volume or less, more preferably 40% by volume or less relative to the whole composite in terms of volume. A decrease in the thermal conductivity of the phosphor plate can be suppressed.
- Alumina in the sintered body absorbs less visible light, so that the emission intensity of the phosphor plate can be increased. Moreover, since alumina has high thermal conductivity, the heat resistance of the phosphor plate containing alumina can be improved. Furthermore, since alumina has excellent mechanical strength, the durability of the phosphor plate can be enhanced.
- Alumina in the sintered body desirably has few impurities from the viewpoint of light extraction efficiency.
- the purity of the Al 2 O 3 compound can be, for example, 98% or more, preferably 99% or more.
- ⁇ ⁇ ⁇ ⁇ Alumina in the sintered body can include at least one selected from the group consisting of ⁇ -alumina and ⁇ -alumina. Thereby, the light conversion efficiency of the phosphor plate can be improved.
- the lower limit of the content of the ⁇ -sialon phosphor and alumina is, for example, 95 vol% or more, preferably 98 vol% or more, more preferably 99 vol% or more, in terms of volume, with respect to the entire composite. That is, the composite constituting the phosphor plate includes the ⁇ -sialon phosphor and alumina as main components. Thereby, heat resistance and durability can be improved, and stable luminous efficiency can be realized.
- the upper limits of the contents of the ⁇ -sialon phosphor and alumina are not particularly limited, but may be, for example, 100 vol% or less in terms of volume with respect to the entire composite.
- the lower limit of the thermal conductivity of the phosphor plate is, for example, 10 W / m ⁇ K or more, preferably 15 W / m ⁇ K, more preferably 20 W / m ⁇ K or more. Thereby, a high thermal conductivity can be realized, and thus a phosphor plate having excellent heat resistance can be realized.
- the upper limit of the thermal conductivity of the phosphor plate is not particularly limited, but may be, for example, 40 W / m ⁇ K or less.
- the surface of at least the main surface or both the main surface and the back surface of the phosphor plate may be surface-treated.
- the surface treatment include grinding using a diamond grindstone, polishing such as lapping and polishing, and the like.
- the surface roughness Ra of the main surface of the phosphor plate is, for example, 0.1 ⁇ m or more and 2.0 ⁇ m or less, preferably 0.3 ⁇ m or more and 1.5 ⁇ m or less.
- the surface roughness Ra on the back surface of the phosphor plate is, for example, 0.1 ⁇ m or more and 2.0 ⁇ m or less, preferably 0.3 ⁇ m or more and 1.5 ⁇ m or less.
- the surface roughness By setting the surface roughness to be equal to or less than the upper limit, it is possible to suppress the light extraction efficiency and the variation of the light intensity in the in-plane direction. By setting the surface roughness to be equal to or more than the lower limit, it is expected that the adhesion to the adherend can be enhanced.
- the upper limit of the light transmittance for blue light of 450 nm is, for example, 10% or less, preferably 5% or less, more preferably 1% or less. This can suppress the transmission of blue light through the phosphor plate, and can emit orange light with high luminance.
- the light transmittance of 450 nm blue light can be reduced.
- the lower limit of the light transmittance of blue light of 450 nm is not particularly limited, but may be, for example, 0.01% or more.
- the method for manufacturing a phosphor plate according to the present embodiment includes a step (1) of mixing an alumina powder and an ⁇ -sialon phosphor powder containing at least an Eu element as a luminescent center; And heating the mixture at 1300 ° C. or higher and 1700 ° C. or lower to bake the dense composite.
- the alumina powder and the ⁇ -sialon phosphor powder used as the raw materials preferably have as high a purity as possible, and it is preferable that impurities of elements other than the constituent elements are 0.1% or less.
- finer alumina is preferably used because densification proceeds due to sintering of the alumina powder, and the average particle diameter of the alumina powder used as a raw material is preferably 1 ⁇ m or less. preferable.
- Various methods such as a dry method and a wet method can be applied to the mixing of the raw material powders. However, it is preferable to use a method in which the ⁇ -sialon phosphor particles used as the raw material are not ground as much as possible and impurities from the apparatus are not mixed as much as possible during mixing.
- step (2) a mixture of the alumina powder and the ⁇ -sialon phosphor powder is fired at 1300 ° C. or more and 1700 ° C. or less.
- the firing temperature is higher.
- the sintering method may be normal pressure sintering or pressure sintering.
- the sintering is more easily performed than normal pressure sintering. Sintering is preferred.
- the pressure sintering method examples include hot press sintering, spark plasma sintering (SPS), and hot isostatic pressing sintering (HIP).
- SPS spark plasma sintering
- HIP hot isostatic pressing sintering
- the pressure is preferably 10 MPa or more, preferably 30 MPa or more, and more preferably 100 MPa or less.
- the firing atmosphere is preferably a non-oxidizing inert gas such as nitrogen or argon, or a vacuum atmosphere for the purpose of preventing the oxidation of ⁇ -sialon.
- the light emitting device of the present embodiment includes a group III nitride semiconductor light emitting element (light emitting element 20) and the above-described phosphor plate 10 provided on one surface of the group III nitride semiconductor light emitting element.
- the group III nitride semiconductor light emitting device includes, for example, an n layer, a light emitting layer, and a p layer made of a group III nitride semiconductor such as an AlGaN, GaN, or InAlGaN-based material.
- a blue LED that emits blue light can be used as the group III nitride semiconductor light emitting device.
- the phosphor plate 10 may be disposed directly on one surface of the light emitting element 20, but may be disposed via a light transmitting member or a spacer.
- the disk-shaped phosphor plate 100 (phosphor wafer) shown in FIG. 1 may be used.
- FIG. 1 is a schematic diagram illustrating an example of the configuration of a phosphor plate.
- the thickness of the phosphor plate 100 shown in FIG. 1 may be, for example, 100 ⁇ m or more and 1 mm or less. After the thickness of the phosphor plate 100 is obtained in the above manufacturing process, it can be appropriately adjusted by grinding or the like. Note that the disk-shaped phosphor plate 100 is more excellent in durability and transportability than in the case of a square shape, since the occurrence of chipping or cracking at corners is suppressed.
- FIG. 2A is a cross-sectional view schematically illustrating a configuration of a flip-chip type light emitting device 110
- FIG. 2B is a cross-sectional view schematically illustrating a configuration of a wire bonding type light emitting device 120.
- the light emitting device 110 of FIG. 2A includes a substrate 30, a light emitting element 20 electrically connected to the substrate 30 via solder 40 (die bonding material), and a fluorescent light provided on a light emitting surface of the light emitting element 20. And a body plate 10.
- the flip-chip type light emitting device 110 may have either a face-up type or a face-down type structure.
- 2B is provided on the substrate 30, the light emitting element 20 electrically connected to the substrate 30 via the bonding wire 60 and the electrode 50, and on the light emitting surface of the light emitting element 20. Phosphor plate 10.
- FIG. 2A includes a substrate 30, a light emitting element 20 electrically connected to the substrate 30 via solder 40 (die bonding material), and a fluorescent light provided on a light emitting surface of the light emitting element 20.
- the flip-chip type light emitting device 110 may have either a face-up type or a face-down type structure.
- 2B is provided on the substrate 30, the
- the light emitting element 20 and the phosphor plate 10 are attached by a known method, and may be attached by, for example, a silicone adhesive or a thermal fusion method. Further, the light emitting device 110 and the light emitting device 120 may be entirely sealed with a transparent sealing material.
- the individualized phosphor plate 10 may be attached to the light emitting element 20 mounted on the substrate 30. After the plurality of light emitting elements 20 are attached to the large-area phosphor plate 100, the light emitting elements 20 with the phosphor plate 10 may be separated into individual pieces by dicing. Alternatively, a large-area phosphor plate 100 may be attached to a semiconductor wafer having a plurality of light emitting elements 20 formed on the surface, and then the semiconductor wafer and the phosphor plate 100 may be collectively divided into individual pieces.
- Example 1 As raw materials for the phosphor plate of Example 1, alumina powder (TM-DAR, manufactured by Daimei Chemical Co., Ltd.), Ca- ⁇ sialon phosphor (Aron Bright YL-600B, manufactured by Denka Co., Ltd., average particle size D50: 15 ⁇ m) ) was used. 7.857 g of alumina powder and 2.833 g of Ca- ⁇ sialon phosphor powder were weighed and dry-mixed in an agate mortar. The mixed raw material was passed through a nylon mesh sieve having a mesh size of 75 ⁇ m to dissolve aggregation, thereby obtaining a raw material mixed powder.
- a hot press jig filled with the raw material mixed powder was set in a multipurpose high-temperature furnace (Hi-Multi 5000, manufactured by Fuji Denpa Kogyo KK) of a carbon heater.
- the inside of the furnace was evacuated to 0.1 Pa or less, and the upper and lower punches were pressed with a pressing pressure of 55 MPa while maintaining the reduced pressure.
- the temperature was raised to 1600 ° C. at a rate of 5 ° C./min. After reaching 1600 ° C., heating was stopped, the temperature was gradually cooled to room temperature, and the pressure was released.
- the fired product having an outer diameter of 30 mm was collected, and the outer peripheral portion was ground using a surface grinder and a cylindrical grinder to obtain a disk-shaped phosphor plate having a diameter of 25 mm and a thickness of 1.5 mm.
- the bulk density of the phosphor plate of Example 1 was measured by a method based on JIS-R1634: 1998, and was found to be 3.729 g / cm 3 . Since the theoretical density of the mixture calculated from the true density of the raw materials and the mixing ratio was 3.781 g / cm 3 , the relative density of the phosphor plate of Example 1 was 98.6%.
- the surface roughness Ra of the main surface of the phosphor plate of Example 1 measured using a surface roughness measuring device is 1.0 ⁇ m
- the surface roughness Ra of the back surface opposite to the main surface was 1.0 ⁇ m.
- the method of manufacturing the phosphor plate of Example 2 is the same as the method of manufacturing the phosphor plate of Example 1, except that the mixing ratio of the alumina powder and the Ca- ⁇ sialon phosphor is different.
- the bulk density of the phosphor plate of Example 2 was measured in the same manner as in Example 1, and the result was 3.665 g / cm 3 . Since the theoretical density of the raw material mixture was 3.717 g / cm 3 , the relative density of the phosphor plate of Example 2 was 98.6%.
- the surface roughness Ra of the main surface of the phosphor plate of Example 2 was 1.0 ⁇ m, and the surface roughness Ra of the back surface opposite to the main surface was 1.1 ⁇ m.
- Example 2 About 7 g of the raw material mixed powder was filled in a carbon die for hot pressing in the same manner as in Example 1, and hot press sintering was performed in a multipurpose high temperature furnace.
- the inside of the furnace was evacuated to 0.1 Pa or less, and while maintaining the reduced pressure, the temperature was raised from room temperature at a rate of 20 ° C./minute, nitrogen gas was introduced into the furnace at 800 ° C., and the atmosphere pressure in the furnace was reduced to zero. .1 MPa ⁇ G. After the introduction of the nitrogen gas, the temperature was raised to 1375 ° C. at a rate of 5 ° C./min and maintained at 1375 ° C. for 15 minutes. Thereafter, the temperature was lowered to room temperature at a rate of 5 ° C.
- Example 2 a fired product having an outer diameter of 30 mm was collected and processed in the same manner as in Example 1 to obtain a disk having a diameter of 25 mm and a thickness of 1.5 mm. A phosphor plate was obtained.
- Thermal conductivity measurement The thermal conductivity of the plates of the phosphors of Examples 1 and 2 and Comparative Example 1 at room temperature (25 ° C.) was measured by a flash method in accordance with JIS 1611: 2010. -Thermal diffusivity: Measured using a xenon flash analyzer (LFA447, manufactured by Netch Japan KK). -Specific heat capacity: Determined using a DSC measurement device (DSC8000, manufactured by PerkinElmer) according to JIS K7123. -Bulk density: Measured by a method according to JIS-R1634: 1998.
- Thermal conductivity (W / m ⁇ K) bulk density (g / cm 3) ⁇ thermal diffusivity (m 2 / s) ⁇ specific heat capacity (J / (kg ⁇ K) )
- the thermal conductivity of the phosphor plate of Example 1 was 18 W / m ⁇ K
- the thermal conductivity of the phosphor plate of Example 2 was 15 W / m ⁇ K
- the thermal conductivity of the phosphor plate of Comparative Example 1 was 1. It was 9 W / m ⁇ K.
- Crystal structure analysis The phosphor plates of Examples 1 and 2 were pulverized in a mortar to prepare a powdery sample, and the diffraction pattern of the obtained sample was measured using an X-ray diffractometer (product name: Ultima IV, manufactured by Rigaku Corporation). As a result, it was confirmed that a crystalline phase was present in the alumina sintered body. It was found that this crystal phase contained ⁇ -alumina as the main phase and slightly contained ⁇ -alumina.
- FIG. 3 is a schematic diagram of an apparatus (LED package 130) for measuring the emission spectrum of phosphor plate 100.
- LED package 130 an apparatus for measuring the emission spectrum of phosphor plate 100.
- the thickness of the obtained disk-shaped phosphor plate 100 having a thickness of 1.5 mm was reduced to 0.25 mm.
- an aluminum substrate (substrate 30) on which the recess 70 was formed was prepared.
- the diameter ⁇ of the bottom surface of the recess 70 was 13.5 mm, and the diameter ⁇ of the opening of the recess 70 was 16 mm.
- a blue LED (light emitting element 20) was mounted as a blue light emitting light source inside the concave portion 70 of the substrate 30.
- a circular phosphor plate 100 is set on the blue LED so as to cover the opening of the concave portion 70 of the substrate 30, and the device shown in FIG. 3 (chip-on-board (COB type) LED package 130) was prepared.
- FIG. 4 shows emission spectra when the phosphor plates of Examples 1 and 2 and Comparative Example 1 were used.
- the emission intensity on the vertical axis in FIG. 4 is a relative value when the maximum emission intensity in Example 1 is set to 100.
- the maximum value of the emission intensity of orange light (Orange) having a wavelength of 595 nm to 605 nm is T O
- the maximum value of the emission intensity of blue light (Blue) having a wavelength of 445 nm to 465 nm is T B.
- the transmission amount of the blue light from the blue LED was defined as T B / T O.
- the peak wavelengths of the emission spectra of Examples 1 and 2 and Comparative Example 1 were about 600 nm. However, it was found that the emission intensity at the peak wavelength in Examples 1 and 2 showed a higher value than that in Comparative Example 1.
- a spectrum derived from the transmitted light of the blue LED was slightly observed at a wavelength of around 450 nm. However, it was found that the transmittances T B / T O of blue light from the blue LEDs in Examples 1 and 2 were comparable to those in Comparative Example 1.
- the light transmittance of blue light at a wavelength of 450 nm was 1.5%, indicating that the transmission of blue light was sufficiently suppressed. It was found that by using the phosphor plates of Examples 1 and 2, it was possible to realize a light emitting device having excellent fluorescence intensity of orange light and excellent luminous efficiency for converting blue light to orange light.
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Abstract
Description
α型サイアロン蛍光体と、アルミナを含む焼結体と、を含む複合体からなる蛍光体プレートが提供される。
III族窒化物半導体発光素子と、
前記III族窒化物半導体発光素子の一面上に設けられた上記の蛍光体プレートと、
を備える、発光装置が提供される。
本実施形態の蛍光体プレートは、α型サイアロン蛍光体と、アルミナを含む焼結体と、を含む複合体からなる板状部材で構成される。
本実施形態のα型サイアロン蛍光体は、下記一般式(1)で表されるEu元素を含有するα型サイアロン蛍光体を含むものである。
(M)m(1-x)/p(Eu)mx/2(Si)12-(m+n)(Al)m+n(O)n(N)16-n ・・一般式(1)
上記蛍光体プレートの主面における表面粗さRaは、例えば、0.1μm以上2.0μm以下、好ましくは0.3μm以上1.5μm以下である。
一方、上記蛍光体プレートの裏面における表面粗さRaは、例えば、0.1μm以上2.0μm以下、好ましくは0.3μm以上1.5μm以下である。
上記表面粗さを上記上限値以下とすることで、光の取り出し効率や、面内方向における光強度のバラツキを抑制できる。上記表面粗さを上記下限値以上とすることで、被着体との密着性を高められることが期待される。
なお、450nmの青色光における光線透過率の下限値は、特に限定されないが、例えば、0.01%以上としてもよい。
焼成雰囲気はαサイアロンの酸化を防ぐ目的のため、窒素やアルゴンなどの非酸化性の不活性ガス、もしくは真空雰囲気下が好ましい。
蛍光体プレート10は、発光素子20の一面上に直接配置されてもよいが、光透過性部材またはスペーサーを介して配置され得る。
図1は、蛍光体プレートの構成の一例を示す模式図である。図1に示す蛍光体プレート100の厚みとしては、例えば、100μm以上1mm以下としてもよい。蛍光体プレート100の厚みは、上記の製造工程で得られた後、研削などにより、適当に調整され得る。
なお、円板形状の蛍光体プレート100は、四角形状の場合と比べて、角部における欠けや割れの発生が抑制されるため、耐久性や搬送性に優れる。
また、図2(b)の発光装置120は、基板30と、ボンディングワイヤ60および電極50を介して基板30と電気的に接続された発光素子20と、発光素子20の発光面上に設けられた蛍光体プレート10と、を備える。
図2中、発光素子20と蛍光体プレート10とは、公知の方法で貼り付けられており、例えば、シリコーン系接着剤や熱融着等の方法で貼り合わされてもよい。
また、発光装置110、発光装置120は、全体を透明封止材で封止されていてもよい。
実施例1の蛍光体プレートの原料として、アルミナ粉末(TM-DAR、大明化学工業株式会社製)、Ca-αサイアロン蛍光体(アロンブライトYL-600B、デンカ株式会社製、平均粒径D50:15μm)を用いた。アルミナ粉末を7.857g、Ca-αサイアロン蛍光体粉末を2.833g秤量し、メノウ乳鉢により乾式混合した。混合後の原料を目開き75μmのナイロン製メッシュ篩を通して凝集を解き、原料混合粉末を得た。尚、原料の真密度(アルミナ:3.97g/cm3、Ca-αサイアロン蛍光体:3.34g/cm3)から算出した配合比は、アルミナ:Ca-αサイアロン蛍光体=70:30体積%である。
実施例1の蛍光体プレートのかさ密度をJIS-R1634:1998に準拠した方法により測定したところ、3.729g/cm3であった。原料の真密度と配合比から算出した混合物の理論密度が3.781g/cm3であるので、実施例1の蛍光体プレートの相対密度は98.6%であった。
実施例1の蛍光体プレートを研磨してSEM観察を実施した結果、アルミナマトリックス相の間にCa-αサイアロン蛍光体粒子が分散した状態が観察された。
なお、JIS B0601:1994に準拠し、表面粗さ測定器(ミツトヨ製、SJ-400)を用いて測定した実施例1の蛍光体プレートの主面の表面粗さRaが1.0μmであり、主面とは反対側の裏面の表面粗さRaが1.0μmであった。
実施例2の蛍光体プレートの原料として、実施例1と同じアルミナ粉末とCa-αサイアロン蛍光体を用いた。アルミナ粉末を6.701g、Ca-αサイアロン蛍光体を3.777g秤量し、メノウ乳鉢で乾式混合した。原料の真密度から算出した配合比は、アルミナ:Ca-αサイアロン蛍光体=60:40体積%である。
実施例2の蛍光体プレートの作製方法は、アルミナ粉末とCa-αサイアロン蛍光体の配合比が異なることを除いて、実施例1の蛍光体プレートの作製方法と同様である。
実施例2の蛍光体プレートのかさ密度を実施例1の測定方法と同様に測定した結果、3.665g/cm3であった。原料混合物の理論密度が3.717g/cm3であるので、実施例2の蛍光体プレートの相対密度は98.6%であった。
実施例2の蛍光体プレートの主面の表面粗さRaは1.0μmであり、主面とは反対側の裏面の表面粗さRaは1.1μmであった。
比較例1の蛍光体プレートの原料として、SiO2粉末(FB-9DCグレード、デンカ株式会社製)、Ca-αサイアロン蛍光体(アロンブライトYL-600B、デンカ株式会社製)を用いた。SiO2粉末を4.354g、Ca-αサイアロン蛍光体粉末を2.723g秤量し、メノウ乳鉢により乾式混合した。混合後の原料を目開き75μmのナイロン製メッシュの篩を通し、原料混合粉末を得た。原料の真密度から算出した配合比は、SiO2:Ca-αサイアロン蛍光体=70:30体積%である。
約7gの原料混合粉末を実施例1と同様にホットプレス用のカーボンダイスに充填し、多目的高温炉により、ホットプレス焼結を行った。炉内を0.1Pa以下まで真空排気し、減圧状態を保ったまま、室温から毎分20℃の速度で昇温し、800℃で窒素ガスを炉内
へ導入し、炉内雰囲気圧力を0.1MPa・Gとした。窒素ガス導入後は毎分5℃の速度で1375℃まで昇温し、1375℃で15分間保持した。その後、毎分5℃の速度で室温まで降温し、除圧した後、外径30mmの焼成物を回収し、実施例1と同様に加工して、直径25mm、厚さ1.5mmの円板状の蛍光体プレートを得た。
実施例1、2及び比較例1の蛍光体のプレートの室温(25℃)での熱伝導率は、JIS1611:2010に準拠し、フラッシュ法により、測定した。
・熱拡散率:キセノンフラッシュアナライザー(LFA447、ネッチ・ジャパン株式会社製)を用いて測定した。
・比熱容量:JIS K7123に準拠し、DSC測定装置(DSC8000、パーキンエルマー社製)を用いて求めた。
・かさ密度:JIS-R1634:1998に準拠した方法で測定した。
熱伝導率(W/m・K)=かさ密度(g/cm3)×熱拡散率(m2/s)×比熱容量(J/(kg・K))
実施例1の蛍光体プレートの熱伝導率が18W/m・K、実施例2の蛍光体プレートの熱伝導率が15W/m・K、比較例1の蛍光体プレートの熱伝導率が1.9W/m・Kであった。
実施例1、2の蛍光体プレートを乳鉢で粉砕して粉末状のサンプルを作成し、X線回折装置(製品名:UltimaIV、リガク社製)を用いて、得られたサンプルにおける回折パターンを測定した結果、アルミナ焼結体に結晶相が存在することを確認した。この結晶相には、主相としてαアルミナが含まれており、僅かにγアルミナが混在していることが分かった。
蛍光体プレートの光学特性は、チップオンボード型(COB型)のLEDパッケージ130を用いて測定した。図3は、蛍光体プレート100の発光スペクトルを測定するための装置(LEDパッケージ130)の概略図である。
まず、得られた厚さ1.5mmの円板状の蛍光体プレート100の厚みを0.25mmまで薄く加工し実施した。
次いで、凹部70が形成されたアルミ基板(基板30)を用意した。凹部70の底面の径φを13.5mmとし、凹部70の開口部の径φを16mmとした。基板30の凹部70の内部に、青色発光光源として青色LED(発光素子20)を実装した。
その後、基板30の凹部70の開口部を塞ぐように、青色LEDの上部に円形状の蛍光体プレート100を設置し、図3に示す装置(チップオンボード型(COB型)のLEDパッケージ130)を作製した。
また、実施例1、2および比較例1のいずれにおいても、波長450nm付近に、青色LEDの透過光に由来するスペクトルがわずかに観測された。しかしながら、実施例1、2における青色LEDからの青色光の透過率TB/TOは、比較例1と比べて、同程度の値を示すことが判明した。
なお、実施例1の蛍光体プレートにおいて、波長450nmにおける青色光の光線透過率が1.5%であったことから、十分に青色光の透過が抑制されたことが分かった。
実施例1、2の蛍光体プレートを使用することで、橙色光の蛍光強度に優れており、青色光を橙色光に変換する発光効率に優れた発光装置を実現できることが分かった。
Claims (11)
- α型サイアロン蛍光体と、アルミナを含む焼結体と、を含む複合体からなる蛍光体プレート。
- 請求項1に記載の蛍光体プレートであって、
当該蛍光体プレートの熱伝導率が、10W/m・K以上40W/m・K以下である、蛍光体プレート。 - 請求項1または2に記載の蛍光体プレートであって、
前記α型サイアロン蛍光体の含有量は、前記複合体全体に対して、体積換算で、5Vol%以上50Vol%以下である、蛍光体プレート。 - 請求項1~3のいずれか一項に記載の蛍光体プレートであって、
前記α型サイアロン蛍光体および前記アルミナの含有量の合計値は、前記複合体全体に対して、体積換算で、95Vol%以上100Vol%以下である、蛍光体プレート。 - 請求項1~4のいずれか一項に記載の蛍光体プレートであって、
前記α型サイアロン蛍光体は、下記一般式(1)で表されるEu元素を含有するα型サイアロン蛍光体を含む、蛍光体プレート。
(M)m(1-x)/p(Eu)mx/2(Si)12-(m+n)(Al)m+n(O)n(N)16-n ・・一般式(1)
(上記一般式(1)中、MはLi、Mg、Ca、Y及びランタニド元素(LaとCeを除く)からなる群から選ばれる1種以上の元素を表し、pはM元素の価数、0<x<0.5、1.5≦m≦4.0、0≦n≦2.0を表す。) - 請求項1~5のいずれか一項に記載の蛍光体プレートであって、
前記アルミナが、αアルミナおよびγアルミナからなる群から選択される一種以上を含む、蛍光体プレート。 - 請求項1~6のいずれか一項に記載の蛍光体プレートであって、
前記複合体中のα型サイアロン蛍光体の平均粒子径D50が、5μm以上30μm以下である、蛍光体プレート。 - 請求項1~7のいずれか一項に記載の蛍光体プレートであって、
当該蛍光体プレートの主面における表面粗さRaが、0.1μm以上2.0μm以下である、蛍光体プレート。 - 請求項1~8のいずれか一項に記載の蛍光体プレートであって、
照射された青色光を橙色光に変換して発光する波長変換体として用いる、蛍光体プレート。 - 請求項1~9のいずれか一項に記載の蛍光体プレートであって、
450nmの青色光における光線透過率が10%以下である、蛍光体プレート。 - III族窒化物半導体発光素子と、
前記III族窒化物半導体発光素子の一面上に設けられた請求項1~10のいずれか一項に記載の蛍光体プレートと、
を備える、発光装置。
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