WO2020235297A1 - SUBSTANCE FLUORESCENTE À BASE DE α-SIALON, ÉLÉMENT ÉLECTROLUMINESCENT ET DISPOSITIF ÉLECTROLUMINESCENT - Google Patents

SUBSTANCE FLUORESCENTE À BASE DE α-SIALON, ÉLÉMENT ÉLECTROLUMINESCENT ET DISPOSITIF ÉLECTROLUMINESCENT Download PDF

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WO2020235297A1
WO2020235297A1 PCT/JP2020/017774 JP2020017774W WO2020235297A1 WO 2020235297 A1 WO2020235297 A1 WO 2020235297A1 JP 2020017774 W JP2020017774 W JP 2020017774W WO 2020235297 A1 WO2020235297 A1 WO 2020235297A1
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light
type
phosphor
light emitting
wavelength
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PCT/JP2020/017774
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English (en)
Japanese (ja)
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慶太 小林
雄介 武田
駿介 三谷
将 浦
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デンカ株式会社
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Priority to KR1020217041700A priority Critical patent/KR20220013389A/ko
Priority to CN202080037362.1A priority patent/CN113874468A/zh
Priority to JP2021520671A priority patent/JPWO2020235297A1/ja
Publication of WO2020235297A1 publication Critical patent/WO2020235297A1/fr

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    • 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
    • C09K11/646—Silicates
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder

Definitions

  • the present invention relates to an ⁇ -type sialone phosphor, a light emitting member, and a light emitting device.
  • Patent Document 1 describes a technique for adjusting the composition component of an ⁇ -type sialon phosphor (claim 1 of Patent Document 1).
  • the present inventor focused on the particle size and examined it, by appropriately removing the fine powder contained in the ⁇ -type sialon particles having an appropriately small particle size, the ⁇ -type sialon fluorescence containing such ⁇ -type sialon particles We have found that the external quantum efficiency of the body can be improved. Further, the external quantum efficiency can be further improved by using an ⁇ -type sialone phosphor having an internal quantum efficiency of 75% or more for excitation light having a wavelength of 455 nm.
  • the particle size at which the cumulative value is 5% is D5
  • the particle size at which the cumulative value is 50% is D5
  • an ⁇ -type sialon phosphor containing ⁇ -type sialon particles can be used.
  • an ⁇ -type sialon phosphor containing ⁇ -type sialon particles In the volume frequency particle size distribution of the ⁇ -type Sialon phosphor measured by the laser diffraction / scattering method, the particle size having a cumulative value of 5% is D5, the particle size having a cumulative value of 50% is D50, and the particle size having a 98% value is D98.
  • D5 the particle size having a cumulative value of 5%
  • D50 the particle size having a cumulative value of 50%
  • D50 the particle size having a 98% value
  • D98 When ((D98-D5) / D50) is 1.00 or more and 8.00 or less.
  • D50 is 10 ⁇ m or less, and
  • the internal quantum efficiency for excitation light with a wavelength of 455 nm measured according to the procedure below is 75% or more.
  • An ⁇ -type sialone fluorophore is provided.
  • the ⁇ -type sialon phosphor is used as a sample, and the sample is filled in a concave cell so that the surface is smooth. After the concave cell is attached to the opening of the integrating sphere, monochromatic light having a predetermined wavelength is introduced into the integrating sphere as excitation light from a light emitting source. At 25 ° C., the sample in the concave cell is irradiated with excitation light, and the spectrum from the sample is measured with a spectrophotometer. From the obtained spectral data, the number of excited reflected light photons (Qref) and the number of fluorescent photons (Qem) are calculated.
  • Qref excited reflected light photons
  • Qem the number of fluorescent photons
  • the standard reflector is attached to the opening of the integrating sphere in the same manner as in (1) above, except that a standard reflector having a reflectance of 99% is used instead of the concave cell, and the excitation light is reflected as standard.
  • the plate is irradiated, the spectrum of the excitation light having a wavelength of 455 nm is measured, and the number of excitation light photons (Qex) is calculated from the obtained spectrum data.
  • Light emitting element and A wavelength converter that converts the light emitted from the light emitting element and emits light Is a light emitting member
  • the wavelength converter has the above-mentioned ⁇ -sialon phosphor.
  • a light emitting member is provided.
  • a light emitting device including the above light emitting member is provided.
  • an ⁇ -type sialone phosphor having excellent external quantum efficiency, a light emitting member using the same, and a light emitting device are provided.
  • the ⁇ -type sialone phosphor of the present embodiment will be described.
  • the ⁇ -type sialon phosphor of the present embodiment contains ⁇ -type sialon particles, and has a particle diameter of D5 in which the cumulative value is 5% in the volume frequency particle size distribution of the ⁇ -type sialon phosphor measured by the laser diffraction scattering method.
  • D5 particle diameter
  • D98 particle size of 50%
  • D98-D5 / D50 particle size of 98%
  • D50 is 10 ⁇ m or less.
  • the internal quantum efficiency with respect to the excitation light having a wavelength of 455 nm measured according to the following procedure satisfies 75% or more.
  • the ⁇ -type sialon phosphor is used as a sample, and the sample is filled in a concave cell so that the surface is smooth. After the concave cell is attached to the opening of the integrating sphere, monochromatic light having a predetermined wavelength is introduced into the integrating sphere as excitation light from a light emitting source. At 25 ° C., the sample in the concave cell is irradiated with excitation light, and the spectrum from the sample is measured with a spectrophotometer. From the obtained spectral data, the number of excited reflected light photons (Qref) and the number of fluorescent photons (Qem) are calculated.
  • Qref excited reflected light photons
  • Qem the number of fluorescent photons
  • the standard reflector is attached to the opening of the integrating sphere in the same manner as in (1) above, except that a standard reflector having a reflectance of 99% is used instead of the concave cell, and the excitation light is reflected as standard.
  • the plate is irradiated, the spectrum of the excitation light having a wavelength of 455 nm is measured, and the number of excitation light photons (Qex) is calculated from the obtained spectrum data.
  • the external quantum efficiency of the ⁇ -type sialon phosphor containing such ⁇ -type sialon particles is obtained by appropriately removing the fine powder contained in the ⁇ -type sialon particles having an appropriately small particle size.
  • ((D98-D5) / D50) as an index, the properties of the ⁇ -type sialon particles from which fine powder has been removed can be stably evaluated, and the index ((D98-D5) / D50) can be evaluated stably. It was found that the external quantum efficiency of the ⁇ -type sialon phosphor containing the ⁇ -type sialon particles can be improved by setting) in an appropriate numerical range.
  • fine powder generated by particle miniaturization treatment has a relatively large specific surface area, a large amount of reflection, and a relatively large amount of crystal defects, so such fine powder is removed. It is considered that this can improve the internal quantum efficiency and reflectance of 455 nm, and thus the external quantum efficiency of 455 nm.
  • the upper limit of ((D98-D5) / D50) is 8.00 or less, preferably 7.70 or less, and more preferably 7.30 or less. This makes it possible to improve the external quantum efficiency in the ⁇ -type sialon phosphor containing the ⁇ -type sialon particles from which fine particles have been appropriately removed.
  • the lower limit of ((D98-D5) / D50) is, for example, 1.00 or more, preferably 3.00 or more, and more preferably 4.00 or more. This makes it possible to reduce the absorptivity at 700 nm in the ⁇ -type sialon phosphor containing the ⁇ -type sialon particles that are appropriately reduced in size.
  • D50 is, for example, 1.0 ⁇ m to 10.0 ⁇ m, preferably 2.5 ⁇ m to 9.0 ⁇ m, and more preferably 3.0 ⁇ m to 9.0 ⁇ m.
  • an ⁇ -type sialon phosphor containing ⁇ -type sialon particles having appropriately reduced particles can be realized.
  • D50 By setting D50 to the above lower limit value or more, the fluorescence intensity at 455 nm can be improved.
  • the particle size at which the cumulative value is 90% is defined as D90.
  • the D90 is, for example, 5.5 ⁇ m to 35.0 ⁇ m, preferably 8.5 ⁇ m to 27.0 ⁇ m, and more preferably 10.0 ⁇ m to 25.0 ⁇ m.
  • the measured values of D5, D50, D90, D98, Dmax, etc. by the laser diffraction / scattering method of the ⁇ -type sialon phosphor of the present invention are JIS R1622 and R1629.
  • 0.5 g of the phosphor to be measured was put into 100 ml of an ion exchange aqueous solution mixed with 0.05 wt% of sodium hexametaphosphate, and this was put into 100 ml of an ion exchange aqueous solution having a transmission frequency of 19.5 ⁇ 1 kHz, a chip size of 20 ⁇ , and an amplitude of 31 ⁇ 5 ⁇ m.
  • the chip is placed in the center of the liquid and dispersed for 3 minutes.
  • the notation of 19.5 ⁇ 1 indicates that the range is 18.5 or more and 20.5 or less
  • 31 ⁇ 5 indicates that the range is 26 or more and 36 or less.
  • the internal quantum efficiency for excitation light having a wavelength of 455 nm can be improved by appropriately removing fine particles contained in ⁇ -type sialone particles having an appropriately small particle diameter. ..
  • the lower limit of the internal quantum efficiency with respect to the excitation light having a wavelength of 455 nm is 75% or more, preferably 76% or more, and more preferably 77% or more.
  • the upper limit of the internal quantum efficiency of 455 nm is not particularly limited, but may be, for example, 100% or less or 99% or less.
  • the external quantum efficiency can be improved by using an ⁇ -type sialone phosphor in which ((D98-D5) / D50) is within a predetermined range and the internal quantum efficiency at 455 nm is equal to or higher than a predetermined value.
  • a light emitting device having excellent brightness can be realized.
  • the upper limit of the light absorption rate for excitation light having a wavelength of 700 nm is, for example, 10% or less, preferably 9% or less, more preferably 7% or less, and further preferably 5% or less.
  • the lower limit of the light absorption rate at 700 nm is not particularly limited and may be 0% or more.
  • the lower limit of the diffuse reflectance for excitation light having a wavelength of 800 nm is, for example, 90% or more, preferably 92% or more, and more preferably 93% or more.
  • the upper limit of the diffuse reflectance at 800 nm is not particularly limited and may be 100% or less.
  • the ⁇ -type sialone phosphor of the present embodiment may contain ⁇ -type sialon containing an Eu element represented by the following general formula (1).
  • General formula (1) (M) m (1-x) / p (Eu) mx / 2 (Si) 12- (m + n) (Al) m + n (O) n (N) 16-n ...
  • M represents one or more elements selected from the group consisting of Li, Mg, Ca, Y and lanthanide elements (excluding La and Ce), and p is the valence of the M element, 0. ⁇ X ⁇ 0.5, 1.5 ⁇ m ⁇ 4.0, 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 ⁇ -type sialon is such that m Si—N bonds of ⁇ -type silicon nitride unit cells (Si 12 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
  • ⁇ -type sialone is stabilized in a wide composition range, and by substituting a part of it with Eu, it is excited by light in a wide wavelength range from ultraviolet to blue, and from yellow. A phosphor exhibiting orange visible light is obtained.
  • the solid solution composition cannot be strictly defined by composition analysis or the like.
  • the crystal phase of alpha-SiAlON, alpha-sialon single-phase is preferred, beta-sialon as other crystal phases, aluminum nitride or its polytypoid may include Ca 2 Si 5 N 8, CaAlSiN 3 and the like.
  • a method for producing an ⁇ -type sialon phosphor there is a method in which a mixed powder composed of a compound of silicon nitride, aluminum nitride and an infiltrated solid solution element is heated and reacted in a high temperature nitrogen atmosphere.
  • a known method may be used for the step of producing the ⁇ -type sialon particles. For example, a firing step of calcining the raw material mixed powder to obtain a calcined product and a calcined product after the firing step are further crushed and pulverized. It may have post-treatment steps such as treatment, classification treatment, annealing treatment and acid treatment. Further, in the post-treatment step, ball mill pulverization and / or decanter treatment can be further performed.
  • the method for preparing the ⁇ -type sialon phosphor by appropriately selecting the type and blending amount of each component contained in the ⁇ -type sialone phosphor, the method for preparing the ⁇ -type sialon phosphor, and the like, the above ((D98-D5) / D50) , D5, D50, D90, D98, 455 nm internal quantum efficiency, 700 nm light absorption, and 800 nm diffuse reflectance can be controlled.
  • the post-treatment step, ball mill pulverization, decanter treatment, or classification utilizing centrifugal force are appropriately performed as described above ((D98-D5) / D50), D5, D50, D90, D98, 455 nm.
  • the internal quantum efficiency of the above, the light absorption rate of 700 nm, and the diffuse reflectance of 800 nm are mentioned as factors for setting the desired numerical range.
  • the wavelength converter of the present embodiment converts the light emitted from the light emitting element and emits light, and has the ⁇ -type sialone phosphor.
  • the wavelength converter may be composed only of the ⁇ -type sialone phosphor, or may contain a base material in which the ⁇ -type sialon phosphor is dispersed.
  • the base material known materials can be used, and examples thereof include glass, resin, and inorganic materials.
  • the shape of the wavelength converter is not particularly limited, and the wavelength converter may be configured in a plate shape, or may be configured to seal a part of the light emitting element or the entire light emitting surface.
  • the light emitting device of this embodiment includes a light emitting member including a light emitting light source (light emitting element) and the wavelength converter. By combining a light emitting light source and a wavelength converter, light having high light emission intensity can be emitted.
  • FIG. 1 is a cross-sectional view schematically showing an example of the structure of the light emitting device of the present embodiment.
  • the light emitting device 100 of FIG. 1 includes, for example, a light emitting element 120, a heat sink 130, a case 140, a first lead frame 150, a second lead frame 160, a bonding wire 170, a bonding wire 172, and a composite 40.
  • the light emitting element 120 is a semiconductor element that emits excitation light.
  • an LED chip that generates light having a wavelength of 300 nm or more and 500 nm or less, which corresponds to blue light from near-ultraviolet light, can be used.
  • a group III nitride semiconductor light emitting device may be used.
  • the group III nitride semiconductor light emitting device includes, for example, an n layer, a light emitting layer, and a p layer composed 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.
  • One electrode (not shown) arranged on the upper surface side of the light emitting element 120 is connected to the surface of the first lead frame 150 via a bonding wire 170 such as a gold wire. Further, the other electrode (not shown) formed on the upper surface of the light emitting element 120 is connected to the surface of the second lead frame 160 via a bonding wire 172 such as a gold wire.
  • the light emitting element 120 is mounted on the upper surface of the heat sink 130.
  • the heat dissipation of the light emitting element 120 can be improved via the heat sink 130.
  • a packaging substrate may be used instead of the heat sink 130.
  • the case 140 is formed with a substantially funnel-shaped recess whose hole diameter gradually expands from the bottom surface upward.
  • the light emitting element 120 is provided on the bottom surface of the recess.
  • the wall surface of the recess surrounding the light emitting element 120 serves as a reflector.
  • the composite 40 is filled in the recess where the wall surface is formed by the case 140.
  • a wavelength converter that lengthens the wavelength of the excitation light emitted from the light emitting element 120 is used.
  • a wavelength converter in which phosphor particles 1 containing an ⁇ -type sialon phosphor are dispersed in a sealing material 30 such as a resin may be used.
  • the light emitting device 100 emits light generated from the phosphor particles 1 that are excited by absorbing the light emitted from the light emitting element 120, or mixed light with the light from the light emitting element 120.
  • the light emitting device 100 may emit white light by mixing the light of the light emitting element 120 and the light generated from the phosphor particles 1.
  • the light emitting device is not limited to the surface mount type, and may be a bullet type or a COB (chip on board) type.
  • This raw material mixed powder was heat-treated at 1800 ° C. for 16 hours in an atmospheric pressure nitrogen atmosphere in an electric furnace of a carbon heater together with the container. Since calcium nitride contained in the raw material mixed powder is easily hydrolyzed in the air, the boron nitride container filled with the raw material mixed powder is immediately installed in the electric furnace after being taken out from the glove box and immediately installed. Vacuum exhaust was performed to prevent the reaction of calcium nitride. The orange mass collected from the container was lightly crushed in a mortar and passed through a sieve having a mesh size of 150 ⁇ m to obtain a powder.
  • the obtained fluorescent powder was used as the ⁇ -sialon type fluorescent substance A.
  • Comparative Example 2 56.56 g of ⁇ -type silicon nitride powder (Si 3 N 4 , SN-E10 grade, manufactured by Ube Kosan Co., Ltd.) in a glove box maintained in a nitrogen atmosphere having a water content of 1 mass ppm or less and an oxygen content of 1 mass ppm or less.
  • ⁇ -type silicon nitride powder Si 3 N 4 , SN-E10 grade, manufactured by Ube Kosan Co., Ltd.
  • a phosphor powder was obtained in the same manner as in Comparative Example 1 except that 1.00 g and 10.00 g of the phosphor powder of Comparative Example 1 were mixed to obtain a raw material mixed powder.
  • the obtained fluorescent powder was used as the ⁇ -sialon type fluorescent substance B.
  • Example 1 The fluorescent powder obtained in Comparative Example 1 was subjected to a ball mill and a decanter in this order according to the following conditions to obtain a fluorescent powder.
  • the obtained fluorescent powder was used as the ⁇ -sialon type fluorescent substance C.
  • 0.8 L of ball mill ion-exchanged water and 50 g of the fluorescent powder (sample) obtained in Comparative Example 1 were placed in an alumina pot having a pot capacity of 2 L.
  • the alumina pot containing this sample was pulverized by a ball mill for 8 hours under the conditions of a silicon nitride ball ⁇ 5 mm, a ball amount of 1000 g, and a rotation speed of about 150 rpm. Then, it was filtered, dried at 120 ° C.
  • the decanter ball milled sample was dispersed in a 0.05 wt% Na hexametaphosphate aqueous solution and allowed to stand for 2 hours to remove fine powder by removing the supernatant at a depth of 4 cm from the water surface. After removal, the mixture was filtered, dried at 120 ° C. for 5 hours, and passed through a 150 ⁇ m sieve to obtain a fluorescent powder.
  • Example 2 56.56 g of ⁇ -type silicon nitride powder (Si 3 N 4 , SN-E10 grade, manufactured by Ube Kosan Co., Ltd.) in a glove box maintained in a nitrogen atmosphere having a water content of 1 mass ppm or less and an oxygen content of 1 mass ppm or less.
  • ⁇ -type silicon nitride powder Si 3 N 4 , SN-E10 grade, manufactured by Ube Kosan Co., Ltd.
  • Example 1 Calcium nitride powder (Ca 3 N 2 , manufactured by Materion) 12.02 g, Aluminum nitride powder (AlN, E grade, manufactured by Tokuyama) 20.41 g, Europium oxide powder (Eu 2 O 3 , RU grade, Shin-Etsu Chemical Industry)
  • a phosphor powder was obtained in the same manner as in Example 1 except that 1.00 g and 10.00 g of the phosphor powder of Comparative Example 1 were mixed to obtain a raw material mixed powder.
  • the obtained fluorescent powder was used as the ⁇ -sialon type fluorescent substance D.
  • Example 3 A phosphor powder was obtained in the same manner as in Example 1 except that the firing temperature was changed to 1900 ° C. The obtained fluorescent powder was used as the ⁇ -sialon type fluorescent E.
  • the particle size distribution of the ⁇ -sialon type phosphor was measured by Microtrac MT3300EXII (Microtrac Bell Co., Ltd.), which is a particle size measuring device of a laser diffraction / scattering method.
  • the particle size ( ⁇ m) at which the cumulative value is 5% is D5
  • the particle size ( ⁇ m) at which the cumulative value is 50% is D50.
  • the particle size ( ⁇ m) of 90% was defined as D90
  • the particle size ( ⁇ m) of 98% was defined as D98.
  • the 455 nm internal quantum efficiency, external quantum efficiency, fluorescence intensity, light absorption rate of the ⁇ -type Sialon phosphor were calculated by the following procedure.
  • An ⁇ -type Sialon phosphor was used as a sample, and the sample was filled in a concave cell so that the surface was smooth.
  • the concave cell was attached to the opening of the integrating sphere.
  • Monochromatic light separated into a wavelength of 455 nm from a light emitting light source (Xe lamp) was introduced into the integrating sphere as excitation light of a phosphor using an optical fiber.
  • the phosphor sample was irradiated with this monochromatic light, and the fluorescence spectrum of the sample was measured using a spectrophotometer (MCPD-7000 manufactured by Otsuka Electronics Co., Ltd.). From the obtained spectral data, the number of excited reflected light photons (Qref) and the number of fluorescent photons (Qem) were calculated. The number of excited reflected photons was calculated in the same wavelength range as the number of excited light photons, and the number of fluorescent photons was calculated in the range of 465 to 800 nm.
  • a standard reflector (Spectralon (registered trademark) manufactured by Labsphere) with a reflectance of 99% was attached to the opening of the integrating sphere instead of the concave cell, and the spectrum of excitation light with a wavelength of 455 nm was obtained. It was measured. At that time, the number of excited photons (Qex) was calculated from the spectrum in the wavelength range of 450 to 465 nm.
  • Qex the number of excited photons
  • the external quantum efficiency is calculated by the formula shown below.
  • External quantum efficiency (%) (Qem / Qex) x 100 Therefore, from the above equation, the external quantum efficiency has the following relationship.
  • External quantum efficiency 455 nm Light absorption rate ⁇ Internal quantum efficiency When a standard sample of ⁇ -type Sialon phosphor (NIMS Standard Green lot No. NSG1301, manufactured by Sialon) was measured by the above measurement method, the external quantum efficiency was 55.
  • the light absorption rate was 6%, the light absorption rate was 74.4%, and the internal quantum efficiency was 74.8%. Quantum efficiency and light absorption rate may fluctuate when the manufacturer of the measuring device, manufacturing lot number, etc. change. Therefore, if the manufacturer of the measuring device, manufacturing lot number, etc. change, the ⁇ -type sialon phosphor The measurement data is corrected using the standard sample of.
  • ⁇ 700 nm light absorption rate> Except that the wavelength of the excitation light was changed from 455 nm to 700 nm, and the number of excitation light photons (Qex) and the number of excitation reflected light photons (Qref) were calculated from the spectrum in the wavelength range of 695 to 710 nm, the light absorption rate of ⁇ 455 nm light absorption rate>.
  • the diffuse reflectance of the ⁇ -type Sialon phosphor was measured by attaching an integrating sphere device (ISV-469) to an ultraviolet-visible spectrophotometer (V-550) manufactured by JASCO Corporation. Baseline correction is performed with a standard reflector (Spectralon (registered trademark)), a solid sample holder filled with ⁇ -type Sialon phosphor (fluorescent material powder) is attached, and diffuse reflectance is measured in the wavelength range of 500 to 850 nm. did.
  • the 800 nm diffuse reflectance (%) referred to in the present invention is a value of the diffuse reflectance particularly at 800 nm.
  • the 800 nm diffuse reflectance was 95.7%.
  • the value of 800 nm diffuse reflectance may fluctuate when the manufacturer of the measuring device, manufacturing lot number, etc. change. Therefore, if the manufacturer of the measuring device, manufacturing lot number, etc. change, the standard sample of ⁇ -type sialon phosphor is used. Is used as the reference value to correct the measurement data.
  • ⁇ Saturation x, y> The chromaticity x and y are the values of CIE1931, and were measured by a spectrophotometer (MCPD-7000 manufactured by Otsuka Electronics Co., Ltd.). In the same manner as above, monochromatic light having a wavelength of 455 nm was irradiated, the excitation reflected light spectrum was measured in the range of 465 to 800 nm, and the chromaticities x and y were calculated. When a standard sample of ⁇ -type Sialon phosphor (NIMS Standard Green lot No. NSG1301, manufactured by Sialon) was measured by the above measurement method, the chromaticity x was 0.356.
  • the value of chromaticity x may fluctuate when the manufacturer of the measuring device, manufacturing lot number, etc. change. Therefore, if the manufacturer of the measuring device, manufacturing lot number, etc. change, use a standard sample of ⁇ -type sialon phosphor. Correct the measurement data as a reference value.
  • ⁇ Peak wavelength, half width> The peak wavelength and full width at half maximum were measured by a spectrophotometer (MCPD-7000 manufactured by Otsuka Electronics Co., Ltd.). In the same manner as above, monochromatic light having a wavelength of 455 nm was irradiated, the excitation reflected light spectrum was measured in the range of 465 to 800 nm, and the peak wavelength (nm) and half width of fluorescence were calculated. The full width at half maximum indicates the width (nm) of the intensity spectrum which is half the intensity of the peak wavelength.
  • NSG1301, manufactured by Sialon was measured by the above measurement method, the peak wavelength was 543.3 nm and the half width was 53.3 nm.
  • the peak wavelength and half-price range may fluctuate when the manufacturer of the measuring device, manufacturing lot number, etc. change, so if the manufacturer of the measuring device, manufacturing lot number, etc. change, the standard for ⁇ -type sialon phosphors The measurement data is corrected using the sample as a reference value.
  • Fluorescent particle 30 Encapsulant 40 Composite 100 Light emitting device 120 Light emitting element 130 Heat sink 140 Case 150 First lead frame 160 Second lead frame 170 Bonding wire 172 Bonding wire

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  • Led Device Packages (AREA)

Abstract

L'invention concerne une substance fluorescente à base de α-Sialon comprenant des particules α-Sialon. Lorsqu'elle est examinée par le procédé de diffraction/diffusion laser, la substance fluorescente à base de α-Sialon donne une répartition volume-fréquence de la taille des particules dans laquelle (D98-D5)/D50 est 1,00 à 10,00, où D5, D50 et D98 sont les diamètres de particule au niveau des volumes cumulés de 5 %, 50 % et 98 %, respectivement. La substance fluorescente à base de α-Sialon présente un rendement quantique interne de 75 % ou plus pour une lumière d'excitation ayant une longueur d'onde de 455 nm.
PCT/JP2020/017774 2019-05-23 2020-04-24 SUBSTANCE FLUORESCENTE À BASE DE α-SIALON, ÉLÉMENT ÉLECTROLUMINESCENT ET DISPOSITIF ÉLECTROLUMINESCENT WO2020235297A1 (fr)

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CN202080037362.1A CN113874468A (zh) 2019-05-23 2020-04-24 α型塞隆荧光体、发光构件和发光装置
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