WO2011013505A1 - Verre à dispersion de phosphore et son procédé de production - Google Patents

Verre à dispersion de phosphore et son procédé de production Download PDF

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Publication number
WO2011013505A1
WO2011013505A1 PCT/JP2010/061763 JP2010061763W WO2011013505A1 WO 2011013505 A1 WO2011013505 A1 WO 2011013505A1 JP 2010061763 W JP2010061763 W JP 2010061763W WO 2011013505 A1 WO2011013505 A1 WO 2011013505A1
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Prior art keywords
glass
phosphor
dispersed
light
bao
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PCT/JP2010/061763
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English (en)
Japanese (ja)
Inventor
昭男 大垣
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コニカミノルタオプト株式会社
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Priority to JP2011524727A priority Critical patent/JP5757238B2/ja
Publication of WO2011013505A1 publication Critical patent/WO2011013505A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/14—Silica-free oxide glass compositions containing boron
    • C03C3/15—Silica-free oxide glass compositions containing boron containing rare earths
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/14—Silica-free oxide glass compositions containing boron
    • C03C3/15—Silica-free oxide glass compositions containing boron containing rare earths
    • C03C3/155—Silica-free oxide glass compositions containing boron containing rare earths containing zirconium, titanium, tantalum or niobium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/17—Silica-free oxide glass compositions containing phosphorus containing aluminium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/19—Silica-free oxide glass compositions containing phosphorus containing boron
    • 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
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder

Definitions

  • the present invention relates to a phosphor-dispersed glass used for converting light of an LED light-emitting element into light of another color and a method for manufacturing the same.
  • a light emitting diode light source including an LED light emitting element that emits light of a predetermined color and a glass in which a phosphor that converts a color emitted from the LED light emitting element into light of a desired color is dispersed is known.
  • a light emitting diode light source that emits white light by mixing the blue and yellow light can be produced.
  • phosphor light-emitting glass in which the phosphor is uniformly dispersed in a transparent resin (glass) is used, and light is emitted from the LED light emitting element in this glass body. It is important to uniformly mix blue and yellow emitted from the phosphor to uniformly emit white light, which is mixed color, outside the glass body.
  • the glass used for the blue LED light-emitting element can obtain a long-life white illumination light source that does not deteriorate due to blue light. Glass is preferred.
  • glass powder having a predetermined particle diameter and phosphor powder are mixed and sintered to synthesize blue light emitted from a blue light source and yellow converted by the phosphor to obtain white light and strong energy.
  • a luminescent color conversion member that improves reliability by using stable glass that does not change color with respect to blue light and has a small temperature rise (see, for example, Patent Document 1).
  • the LED light-emitting element in order for the LED light-emitting element to have a long life and exhibit a light emission color with a predetermined luminance, a method of manufacturing an LED light-emitting element that has weather resistance and does not deteriorate the LED is preferable, and a glass material that exhibits weather resistance is used. At the same time, it is important to lower the firing temperature of the glass so as not to adversely affect the LED thermally.
  • the luminescent color conversion member and the conventional phosphor composite member described in Patent Documents 1 and 3 corresponding to the phosphor-dispersed glass of the present invention are produced, for example, by the following production method.
  • a predetermined glass raw material is prepared, mixed uniformly, and then melted to produce a plate-like glass.
  • the plate-like glass is pulverized and classified to obtain a glass powder having a predetermined particle diameter.
  • the glass powder and the phosphor powder are mixed in the mixing step, and a resin binder is added thereto to produce a mixed material in which the glass powder and the phosphor powder are uniformly mixed.
  • a preform is produced by pressure molding using a mold having a predetermined shape. Then, it is fired at a predetermined temperature in a sintering process to produce a phosphor-dispersed glass that is a homogeneous scatterer.
  • generating a mixed material is removed by this sintering process.
  • the luminescent color conversion member (corresponding to the phosphor-dispersed glass) described in Patent Document 1 is a phosphor-dispersed glass that has a high reliability and can provide a long-life white illumination light source.
  • glass having a temperature higher than 500 ° C. is used, the mold temperature at the time of firing becomes higher than that, the surface composition of the mold tends to change, and the mold life is shortened. Arise.
  • the glass described in Patent Documents 2 and 3 because it contains a coloring tends components such as SnO and TeO 2 and Bi 2 O 3, the transmittance of the glass becomes too bad, 100% in the visible range It is difficult to obtain a glass having an internal transmittance close to. Therefore, there arises a problem that the transmission of the excitation light and the converted light emitted by the excitation light is deteriorated. In addition, since heat is generated due to light absorption, it is necessary to take measures against heat dissipation of the light-emitting diode light source. Further, when the luminescent color conversion member is sealed with a silicone resin or the like, there is also a problem that the sealing material is deteriorated due to heat generated by the luminescent color conversion member.
  • the present invention provides a glass that can be fired at a relatively low temperature and does not deteriorate the life of the mold and maintains a high transmittance, and a predetermined phosphor powder is dispersed and blended in the glass to uniformly produce a desired color light.
  • An object of the present invention is to provide a phosphor-dispersed glass that can be released into a glass.
  • a phosphor-dispersed glass that converts primary light emitted by an LED light-emitting element into secondary light of another color by a phosphor dispersed in glass, and generates light in which the primary light and the secondary light are mixed.
  • the glass is a P 2 O 5 —BaO-based glass substantially free of SnO, Bi 2 O 3 , TeO 2 and R 2 O (R is at least one selected from Li, Na, and K).
  • R is at least one selected from Li, Na, and K.
  • a phosphor-dispersed glass characterized by having a softening point of 300 to 500 ° C.
  • the glass is, by weight, P 2 O 5 : 30 to 58%, BaO: 1 to 41%, Li 2 O: 0 to 17%, Na 2 O: 0 to 18%, K 2 O: 0 to 20%, provided that (Li 2 O + Na 2 O + K 2 O) is 1 to 25%, Furthermore, Al 2 O 3 : 0 to 10%, B 2 O 3 : 0 to 20%, MgO 0 to 20%, CaO 0 to 20%, SrO 0 to 20%, ZnO 0 to 35%, La 2 O 3 : 0 to 10%, Y 2 O 3 : 0 to 10%, Gd 2 O 3 : 0 to 12%, ZrO 2 : 0 to 3%, Ta 2 O 5 : 0 to 12%, SiO 2 : 0 to 4%, GeO 2 : 0 to 4%, Nb 2 O 5 : 0 to 24%, TiO 2 : 0 to 8%, WO 3 : 0 to 10%, Sb 2 O 3
  • a phosphor-dispersed glass that converts primary light emitted by an LED light-emitting element into secondary light of another color by a phosphor dispersed in glass, and generates light in which the primary light and the secondary light are mixed.
  • the glass is a B 2 O 3 —La 2 O 3 glass substantially free of SnO, Bi 2 O 3 , TeO 2 , and R 2 O (R is selected from Li, Na, K).
  • R′O is at least one kind selected from Mg, Ca, Sr, Ba, Zn
  • the glass is, by weight, B 2 O 3 : 20 to 47%, La 2 O 3 : 3 to 35%, Li 2 O: 6-20%, Na 2 O: 0-5%, K 2 O: 0-5%, provided that (Li 2 O + Na 2 O + K 2 O) is 8-20%, MgO: 0 to 10%, CaO: 0 to 25%, SrO: 0 to 10%, BaO: 0 to 20%, ZnO: 0 to 31%, provided that (MgO + CaO + SrO + BaO + ZnO) is 5 to 32%, Further, Gd 2 O 3 : 0 to 30%, SiO 2 : 0 to 25%, Al 2 O 3 : 0 to 4%, Y 2 O 3 : 0 to 15%, ZrO 2 : 0 to 8%, Ta 2 O 5 : 0 to 8%, Nb 2 O 5 : 0 to 8%, TiO 2 : 0 to 3%, WO 3 : 0 to 4%, Sb
  • a phosphor-dispersed glass that converts primary light emitted by an LED light-emitting element into secondary light of another color by a phosphor dispersed in glass, and generates light in which the primary light and the secondary light are mixed.
  • the glass is SiO 2 —B 2 O 3 based glass substantially free of SnO, Bi 2 O 3 , TeO 2 , and R 2 O (R is at least one selected from Li, Na, and K). ) And Al 2 O 3 , and has a softening point of 300 to 500 ° C.
  • the glass is, by weight, SiO 2 : 20 to 50%, B 2 O 3 : 15 to 40%, Li 2 O: 7-22%, Na 2 O: 0-15%, K 2 O: 0-10%, provided that (Li 2 O + Na 2 O + K 2 O) is 12-27%, Al 2 O 3 : 5 to 20%, MgO: 0 to 10%, CaO: 0 to 25%, SrO: 0 to 10%, BaO: 0 to 25%, ZnO: 0 to 15%, La 2 O 3 : 0 to 3%, Y 2 O 3 : 0 to 3%, Gd 2 O 3 : 0 to 3%, ZrO 2 : 0 to 3%, Ta 2 O 5 : 0 to 3%, Nb 2 O 5 : 0 to 3%, TiO 2 : 0 to 3%, WO 3 : 0 to 3%, Sb 2 O 3 : 0 to 1%,
  • a method for producing a phosphor-dispersed glass which is a production method in which a doubled glass powder and a phosphor powder are mixed and sintered.
  • the present invention it is possible to obtain a glass that can be fired at a relatively low temperature and does not deteriorate the life of the mold without containing components that easily cause the glass to be colored. Can be blended to obtain a phosphor-dispersed glass capable of uniformly emitting desired colored light.
  • the phosphor-dispersed glass according to the present embodiment disperses a predetermined phosphor in the glass, and the phosphor converts the primary light emitted from the LED light emitting element into secondary light of another color, and the primary light and the A phosphor-dispersed glass that generates light mixed with secondary light, which is substantially free of SnO, Bi 2 O 3 , and TeO 2 , and contains P 2 O 5 —BaO-based glass with R 2 O (R is P 2 O 5 —BaO—R 2 O based glass to which at least one selected from Li, Na, and K) is added, or B 2 O 3 —La 2 O 3 based glass to R 2 O (R is Li , Na, K) and R′O (R ′ is at least one selected from Mg, Ca, Sr, Ba, Zn) and B 2 O 3 —La 2 O 3 —R 2 O-R'O glass of, or the SiO 2 -B 2 O 3 -based glass (The R Li, Na
  • the blending amount of R 2 O is set within a predetermined range, and the softening point of the glass is set to 300 to 500 ° C. Therefore, the glass can be fired at a relatively low temperature without deteriorating the life of the mold. Since the firing temperature is low, reactions (discoloration, etc.) with phosphors such as sulfides, aluminates and halophosphates having low heat resistance can be suppressed. Further, since the viscosity of the glass is low at the time of firing, the softened glass easily enters the gap between the phosphor, the adhesion between the glass and the phosphor is improved, and the pores in the phosphor-dispersed glass can be reduced.
  • the dispersion glass becomes a scatterer (phosphor dispersion glass) capable of uniformly emitting desired color light.
  • the phosphor-dispersed glass is obtained by mixing a glass powder having a predetermined particle diameter and a predetermined amount of phosphor powder, and heating and press-molding the mixed powder produced in the mixing step to obtain a phosphor-dispersed glass. It can manufacture using a manufacturing method provided with a heat press molding process.
  • the glass powder to be mixed preferably has a maximum particle size of 5 to 200 ⁇ m and a median diameter d50 of 0.1 to 15 times the particle size of the phosphor used.
  • the median diameter d50 is the particle diameter (cumulative average diameter) at which the cumulative curve becomes 50% when the cumulative curve is obtained with the total volume of one group of particles as 100%, and the maximum particle diameter is This is the particle size at which the cumulative curve becomes 100%.
  • These parameters are generally used as one of parameters for evaluating the particle size distribution.
  • the median diameter d50 and the maximum particle diameter can be measured using a general laser diffraction / scattering particle size measuring device.
  • HELOS manufactured by JEOL
  • Microtrac HRA manufactured by Nikkiso
  • SALD series manufactured by Shimadzu Corporation
  • SALD series manufactured by Shimadzu Corporation
  • the maximum particle diameter exceeds 200 ⁇ m, transparent glass portions are scattered on the scatterer, making it difficult to obtain a uniform scatterer.
  • the maximum particle diameter is less than 5 ⁇ m, the surface area of the glass in contact with the phosphor increases, and therefore, when a phosphor highly reactive with glass is dispersed, the phosphor is easily deactivated.
  • the radian diameter d50 exceeds 15 times the particle diameter of the phosphor, the phosphor is unevenly distributed in the glass powder and it becomes difficult to uniformly disperse.
  • the radian diameter d50 is less than 0.1 times the particle diameter of the phosphor, the incident blue light is excessively scattered and the transmitted light is reduced. More preferably, the particle diameter of the glass is close to the particle diameter of the phosphor.
  • the phosphor is preferably an inorganic phosphor. Further, it is desirable to emit light that is excited by light in the visible range (360 nm to 830 nm). Accordingly, oxides, nitrides, oxynitrides, sialon phosphors, YAG phosphors, silicate phosphors, and the like are preferable.
  • oxides or compounds that easily become oxides at high temperatures are used, and these are sufficiently mixed in a stoichiometric ratio to obtain raw materials.
  • a mixed raw material for example, as raw materials for Y, Gd, Ce, Sm, Al, La, and Ga.
  • fluoride such as ammonium fluoride
  • a flux is mixed with this as a flux and packed in a crucible and fired in air at a temperature range of 1350 to 1450 ° C. for 2 to 5 hours to obtain a fired product.
  • the fired product is ball milled in water, washed, separated and dried, and finally passed through a sieve to obtain a desired phosphor.
  • Y 2 O 3, Gd 2 O 3, CeO 2, Al 2 O 3 were appropriate amount prepared
  • a raw material mixture in which these are sufficiently mixed is filled in an aluminum crucible, and an appropriate amount of fluoride such as ammonium fluoride is mixed as a flux into the aluminum crucible, and 1350 to 1450 in a reducing atmosphere while flowing hydrogen-containing nitrogen gas.
  • Firing is performed for 2 to 5 hours in a temperature range of 0 ° C. to obtain a fired product.
  • the obtained baked product is pulverized, washed, separated, and dried to obtain a desired phosphor.
  • the composition of the obtained phosphor was examined to confirm that it was a desired phosphor, and the emission wavelength in the excitation light of 465 nm was examined. As a result, it was confirmed that the peak wavelength was approximately 570 nm. That is, it was possible to obtain a phosphor that emits yellow light when irradiated with blue light.
  • the content of the inorganic phosphor is preferably about 0.02 to 12% by volume. If the phosphor content is less than 0.02%, the amount of fluorescent light is too small, and if it exceeds 12%, the phosphor itself shields the light. A more preferable range is 0.05 to 5%.
  • the glass can be used as long as it does not precipitate crystals or does not precipitate in large quantities during firing. If a large amount of crystals are precipitated in the glass, the light transmittance may be lowered.
  • the atmosphere for firing glass may be in the air. Further, in order to reduce the reaction between the phosphor and the glass, it may be fired in a vacuum or in an inert gas atmosphere such as nitrogen or argon. Moreover, the form of the glass to produce is not specifically limited. The phosphor and glass powder can be pressure-molded into a desired shape. Moreover, the form of a green sheet may be sufficient.
  • a resin binder is added to a composite material made of phosphor powder and glass powder and subjected to pressure molding to produce a preform having a desired shape. Thereafter, the preform is fired to remove the resin binder and sinter to produce a phosphor-dispersed glass.
  • the phosphor-dispersed glass can be fixed to the LED substrate by the following method.
  • the phosphor-dispersed glass produced in a plate shape is set in parallel so as to cover the upper surface of the LED light emitting element, and is fixed by heating.
  • the glass can be melted at a relatively low temperature, and a uniform state can be maintained without deteriorating the degree of dispersion of the phosphor in the glass. If the adhesion of the glass is insufficient, it may be further pressurized and fixed.
  • a phosphor-dispersed glass having a shape covering the upper surface of the LED light-emitting element may be produced, and the phosphor-dispersed glass may be set on the LED light-emitting element, heated, and pressurized and fixed as necessary.
  • an adhesive may be applied and fixed to the surface of the phosphor-dispersed glass that does not contact the LED.
  • Example 1 Glass powder used in Example 1, P 2 O 5 (the R Li, Na, at least one selected from K) R 2 O in -BaO based glass P 2 O 5 -BaO-R 2 O system plus It is a glass powder made of glass.
  • the predetermined range the amount of the R 2 O, the softening point of the glass is set to 500 ° C. or less.
  • This glass is in mass%, P 2 O 5 : 30 to 58%, BaO: 1 to 41%, Li 2 O: 0 to 17%, Na 2 O: 0 to 18%, K 2 O: 0 to 20% However, (Li 2 O + Na 2 O + K 2 O) is 1 to 25%, and Al 2 O 3 : 0 to 10%, B 2 O 3 : 0 to 20%, MgO 0 to 20%, CaO: 0 to 20%, SrO: 0 to 20%, ZnO: 0 to 35%, La 2 O 3 : 0 to 10%, Y 2 O 3 : 0 to 10%, Gd 2 O 3 : 0 to 12% ZrO 2 : 0 to 3%, Ta 2 O 5 : 0 to 12%, SiO 2 : 0 to 4%, GeO 2 : 0 to 4%, Nb 2 O 5 : 0 to 24%, TiO 2 : 0 to It has a composition of 8%, WO 3 : 0 to 10%,
  • P 2 O 5 is essential as a glass forming component. If it is less than 30%, the glass tends to devitrify, and if it exceeds 58%, the weather resistance deteriorates. A preferred range is 32 to 58%. BaO has an effect of stabilizing the glass. If it is less than 1%, the effect is not sufficient, and if it exceeds 50%, it becomes difficult to make the softening point 500 ° C. or less. A preferred range is from 2 to 41%.
  • Li 2 O, Na 2 O, and K 2 O have an effect of lowering the softening point, but weather resistance is significantly deteriorated when the content exceeds 17%, 18%, and 20%, respectively.
  • a preferable range of Li 2 O is 0 to 16%
  • a preferable range of Na 2 O is 0 to 10%
  • a preferable range of K 2 O is 0 to 10%.
  • it becomes easy to a softening point 500 ° C. or less by the total amount of R 2 O Li 2 O + Na 2 O + K 2 O and 1% or more.
  • the preferable range of R 2 O is 1 to 25%, more preferably 1.5 to 22%.
  • Al 2 O 3 has the effect of increasing the weather resistance of the glass, but if it exceeds 10%, the glass tends to devitrify.
  • the preferred range is 0-5%.
  • Al 2 O 3 is more preferable to contain Al 2 O 3 in the range of 2% to 5%.
  • B 2 O 3 has the effect of stabilizing the glass. If it exceeds 20%, the weather resistance deteriorates. A preferred range is 0 to 15%. MgO has the effect of increasing the weather resistance, but if it exceeds 20%, the glass tends to devitrify. A preferred range is 0 to 14%. CaO also has an effect of improving weather resistance, but if it exceeds 20%, the glass tends to devitrify. A preferred range is 0 to 17%. SrO has the effect of stabilizing the glass, and may be substituted for BaO or the like, but if it exceeds 20%, it becomes difficult to make the softening point 500 ° C. or less. A preferred range is 0 to 16%. ZnO has the effect of lowering the softening point, but if it exceeds 35%, the glass tends to devitrify.
  • La 2 O 3 , Y 2 O 3 , Gd 2 O 3 , ZrO 2 , and Ta 2 O 5 have an effect of improving the weather resistance, but when La 2 O 3 exceeds 10%, the glass tends to devitrify.
  • a preferable range is 6% or less.
  • Y 2 O 3 also tends to devitrify glass exceeding 10%.
  • a preferred range is 5% or less.
  • Gd 2 O 3 exceeds 12%, it tends to devitrify.
  • a preferred range is 11% or less.
  • ZrO 2 exceeds 3%, it tends to devitrify.
  • Ta 2 O 5 exceeds 12%, it tends to devitrify.
  • a preferred range is 10% or less.
  • SiO 2 and GeO 2 can also be expected to have an effect of improving the weather resistance, but if they exceed 4% and 8%, respectively, they tend to remain as undissolved materials at the time of melting. In order to obtain a glass having a high transmittance at a softening point of 500 ° C. or lower, it is preferable to use only the above components.
  • Nb 2 O 5 , TiO 2 , and WO 3 also have an effect of improving the weather resistance, but since all of them are components that are easily colored, it should be limited to limited use. If it exceeds 25%, 8% and 10%, respectively, the glass tends to be colored.
  • Nb 2 O 5, 5 % or less for TiO 2 , and 8% or less for WO 3 are 21% or less for Nb 2 O 5, 5 % or less for TiO 2 , and 8% or less for WO 3 .
  • Nb 2 O 5, TiO 2 , WO 3 an amount of 0.5% or less of Sb 2 O 3 component when using the component may be used in the decoloring purposes.
  • the glass raw materials are prepared so that the target compositions shown in A1 to A17 in Tables 1 to 3 are obtained.
  • a blended raw material This was put into a melting furnace heated to 700 to 1200 ° C., melted, vitrified, and then poured into water to obtain a rough snow-like cullet. This cullet was classified by passing through a standard sieve of 420 ⁇ m, and a glass powder having a maximum particle diameter of 200 ⁇ m or less and a median diameter d50 of 15 times or less of the phosphor particle diameter was prepared.
  • These powders were mixed with a predetermined proportion of phosphor powder shown in the table to obtain a mixed powder.
  • a small amount of binder was added to and mixed with the mixed powder, and then pressure-molded with a mold to prepare a preform of about 23 mm square.
  • the firing atmosphere was set to the atmosphere, vacuum, N 2 filling, or Ar filling at the firing temperature shown in the table, and the preform was fired to produce a 20 mm square phosphor-dispersed glass.
  • the phosphor a cerium-added YAG phosphor having a particle size of 6.5 to 9.5 ⁇ m was used.
  • the softening point was measured by DTA by crushing a glass powder sample with a mortar to prepare a sample having a maximum particle size of about 35 ⁇ m.
  • the internal transmittance of the glass is mirror-polished so that the glass plate has a thickness of 2 mm, and the transmittance and reflectance at a wavelength of 588 nm are measured using a spectrophotometer. (The value obtained by adding the reflectance at). Further, processing and measurement were performed under the same conditions at a wavelength of 400 nm.
  • the weather resistance after baking at the baking temperature shown in the table, one surface of a 20 mm ⁇ 20 mm, 5 mm thick sample was mirror-polished. After holding this sample in a constant temperature and humidity chamber at 60 ° C. and 95% for 168 hours, the sample was taken out and the surface was observed with an optical microscope (40 times magnification). did.
  • Tables 1 to 3 show data of the phosphor dispersed glasses A1 to A17 using the obtained P 2 O 5 —BaO—R 2 O glass.
  • Table 4 shows data of comparative samples A18 to A22.
  • the glass used for the phosphor-dispersed glasses A1 to A17 has a softening point of all the glasses of 500 ° C. or less. Moreover, it became clear that the internal transmittances of the glass having a thickness of 2 mm at wavelengths of 588 nm and 400 nm are all 99% or more. For this reason, the P 2 O 5 —BaO—R 2 O glass according to the present embodiment is a glass that can be fired at a relatively low temperature without deteriorating the mold life and maintains a high transmittance. It has been found that by dispersing a predetermined phosphor, it is possible to produce a phosphor-dispersed glass capable of uniformly emitting desired colored light.
  • the blending ratio of R 2 O is 1.5% for phosphor-dispersed glass A14 and 22% for phosphor-dispersed glass A15. Is clearly 1.5-22%. However, even in this range, the internal transmitted light of the glass is 99, 9%, and there is a margin, so the mixing ratio of R 2 O (Li 2 O + Na 2 O + K 2 O) should be 1-25% by mass%. In this case, a sufficiently usable phosphor-dispersed glass is obtained.
  • A18 is an example which does not contain Li 2 O, Na 2 O, K 2 O, which are components that lower the softening point.
  • Glass A18 has a softening point of 520 ° C., and the mold temperature during firing becomes higher than that, which may shorten the mold life.
  • Glasses A19 and A20 are examples in which Bi 2 O 3 which is a component that is easily colored contains more than 1%.
  • Glass A19 has an internal transmittance of 86% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required.
  • the glass A20 has an internal transmittance of 97% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where a high transmittance close to 100% is required.
  • A21 is an example in which SnO, which is an easily colored component, contains more than 1%.
  • Glass A21 has an internal transmittance of 96% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required.
  • Glass A22 is an example in which TeO 2 which is an easily colored component contains more than 1%.
  • Glass A22 has an internal transmittance of 97% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required. Further, in the glasses A19 to A21, since light is absorbed, a problem of heat generation occurs.
  • Example 2 The glass powder used in Example 2 is substantially free of SnO, Bi 2 O 3 , and TeO 2 , and R 2 O (R is selected from Li, Na, and K) in the B 2 O 3 —La 2 O 3 system glass.
  • R′O R ′ is at least one selected from Mg, Ca, Sr, Ba, Zn
  • It is a glass powder made of glass.
  • the amount of the R 2 O as a predetermined range corresponding to the glass of this composition, the softening point of the glass is set to 500 ° C. or less.
  • This glass is in mass%, B 2 O 3 : 20 to 47%, La 2 O 3 : 3 to 35%, Li 2 O: 6 to 20%, Na 2 O: 0 to 5%, K 2 O: 0 -5%, provided that (Li 2 O + Na 2 O + K 2 O) is 8-20%, MgO: 0-10%, CaO: 0-25%, SrO: 0-10%, BaO: 0-20 %, ZnO: 0 to 31%, (MgO + CaO + SrO + BaO + ZnO) is 5 to 32%, Gd 2 O 3 : 0 to 30%, SiO 2 : 0 to 25%, Al 2 O 3 : 0 to 4 %, Y 2 O 3 : 0 to 15%, ZrO 2 : 0 to 8%, Ta 2 O 5 : 0 to 8%, Nb 2 O 5 : 0 to 8%, TiO 2 : 0 to 3%, WO 3 : 0 to 4%,
  • B 2 O 3 is a component constituting a glass skeleton, and when the content is less than 20%, the glass tends to devitrify. If it exceeds 47%, the weather resistance deteriorates. A preferred range is 22-45%. SiO 2 is B 2 O 3 and it becomes easy to obtain a component a and B 2 O 3 at the same time the inclusion devitrified hardly stable glass constituting the glass network similar, the softening point exceeds 25% 500 ° C. It will be difficult to: A preferred range is 5 to 23%.
  • Li 2 O is an effective component for lowering the softening point. If it is less than 6%, the effect is not sufficient, and if it exceeds 20%, the weather resistance deteriorates.
  • the preferred range is 7-18%.
  • Na 2 O and K 2 O have the effect of lowering the softening point, but if each exceeds 5%, the glass tends to devitrify significantly.
  • the preferred range is 10-18%.
  • La 2 O 3 has a good compatibility with B 2 O 3 , can provide a stable glass that is not easily devitrified, and is effective in improving weather resistance. If it is less than 3%, the effect is not sufficient, and if it exceeds 35%, it becomes difficult to make the softening point 500 ° C. or less. A preferred range is 3 to 31%.
  • the glass is more difficult to devitrify and can be stabilized.
  • Y 2 O 3 is used in the same manner as La 2 O 3 , the glass is stabilized, but when it exceeds 15%, it tends to devitrify.
  • a preferred range is 0-12%.
  • MgO, CaO, SrO, BaO and ZnO components have the effect of lowering the softening point of the glass, but the weather resistance of the glass deteriorates.
  • a preferred range is 6 to 31%.
  • Al 2 O 3 has the effect of increasing the weather resistance of the glass, but if it exceeds 4%, the glass tends to devitrify.
  • Ta 2 O 5 and ZrO 2 have the effect of improving the weather resistance of the glass, but are also components that raise the softening point, so 8% or less is preferable.
  • the preferred ranges are each 4% or less.
  • the Nb 2 O 5 component has an effect of improving weather resistance, but it is preferably 8% or less because the glass is easily colored.
  • a preferred range is 3% or less.
  • WO 3 and TiO 2 have the effect of preventing devitrification, but the glass tends to be colored, so 4% and 3% are preferable, respectively.
  • Preferable ranges are 2% or less and 1% or less, respectively.
  • Sb 2 O 3 may be used as a defoaming agent, but its effect is sufficient at 1% or less.
  • the phosphor-dispersed glasses B1 to B12 using the B 2 O 3 —La 2 O 3 —R 2 O—R′O glass have softening points of all the glasses. Is 500 ° C. or lower. Moreover, it became clear that the internal transmittance
  • R 2 O Li 2 O + Na 2 O + K 2 O
  • the mixing ratio of R 2 O is 7.9% for the phosphor-dispersed glass B11 and 19% for the phosphor-dispersed glass B2
  • R 2 O it is preferable to use R 2 O. It is clear that the mass% is 8-20%.
  • R 2 O Li The mixing ratio of 2 O + Na 2 O + K 2 O
  • the phosphor dispersion glass B2 is 6.6%
  • the internal transmittance is 99.9%
  • the phosphor dispersion glass B11 is 30.1%. Since the internal transmittance is 99.4% (wavelength 400 nm) as a blending ratio, if the blending ratio of R′O (MgO + CaO + SrO + BaO + ZnO) is 5 to 32%, the internal transmittance may be maintained at about 99%. .
  • B13 is an example in which the content of Li 2 O, Na 2 O, K 2 O, which is a component that lowers the softening point, is low.
  • Glass B13 has a softening point of 520 ° C., and the mold temperature during firing becomes higher than that, which may shorten the mold life.
  • Glass B14 is an example which contains SnO which is a component which is easy to color exceeding 1%.
  • Glass B14 has an internal transmittance of 63% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required.
  • Glass B15 is an example containing more than 1% of TeO2, which is an easily colored component.
  • Glass B15 has an internal transmittance of 97% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required.
  • B16 is an example containing more than 1% of Bi 2 O 3 which is an easily colored component.
  • Glass B16 has an internal transmittance of 97% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required. Further, since the glass B14 to B16 absorb light, a problem of heat generation occurs.
  • Example 3 The glass powder used in Example 3 is substantially free of SnO, Bi 2 O 3 , and TeO 2 , and is SiO 2 —B 2 O 3 based glass with R 2 O (R is selected from Li, Na, K) This is a glass powder made of SiO 2 —B 2 O 3 —R 2 O—Al 2 O 3 based glass to which 1 type) and Al 2 O 3 are added. Also the amount of the R 2 O as a predetermined range corresponding to the glass of this system, the softening point of the glass is set to 500 ° C. or less.
  • This glass is by mass, SiO 2 : 20 to 50%, B 2 O 3 : 15 to 40%, Li 2 O: 7 to 22%, Na 2 O: 0 to 15%, K 2 O: 0 to 10 %, Where (Li 2 O + Na 2 O + K 2 O) is 12 to 27%, Al 2 O 3 : 5 to 20%, MgO: 0 to 10%, CaO: 0 to 25%, SrO: 0 to 10%, BaO: 0 to 25%, ZnO: 0 to 15%, La 2 O 3 : 0 to 3%, Y 2 O 3 : 0 to 3%, Gd 2 O 3 : 0 to 3%, ZrO 2 : 0 to 3%, Ta 2 O 5 : 0 to 3%, Nb 2 O 5 : 0 to 3%, TiO 2 : 0 to 3%, WO 3 : 0 to 3%, Sb 2 O 3 : 0 to 1%
  • the glass having this composition has a high transmittance because it does not contain a component that makes the glass easily colored. Moreover, the softening point of glass becomes 500 degrees C or less, and the lifetime of a type
  • SiO 2 is a component that forms a glass skeleton, and if its amount is less than 20%, it is difficult to vitrify, and if it exceeds 50%, the glass tends to devitrify.
  • B 2 O 3 is a component that forms a glass skeleton as well as SiO 2 . When used simultaneously with SiO 2 , the glass is hardly devitrified and the glass is stabilized. If it is less than 15%, the effect is not sufficient, and if it exceeds 40%, the weather resistance is remarkably deteriorated. A preferred range is 15 to 34%.
  • Al 2 O 3 is effective in improving the weather resistance. If it is less than 5%, the effect is not sufficient, and if it exceeds 20%, the glass tends to devitrify. A preferred range is 5 to 13%.
  • MgO, CaO, SrO, BaO and ZnO components have the effect of lowering the softening point of the glass. However, if it exceeds 10%, 25%, 10%, 20% and 15%, the glass tends to devitrify. Preferred ranges are MgO 6% or less, CaO 17% or less, SrO 6% or less, BaO 18% or less, and ZnO 13% or less.
  • La 2 O 3 , Y 2 O 3 , Gd 2 O 3 , ZrO 2 , Ta 2 O 5 , Nb 2 O 5 are effective in improving weather resistance, but La 2 O 3 , Y 2 O 3 , If Gd 2 O 3 , ZrO 2 , and Ta 2 O 5 exceed 3%, the glass tends to devitrify. If Nb 2 O 5 exceeds 3%, the glass tends to be colored.
  • WO 3 and TiO 2 have an effect of suppressing devitrification of the glass, but since both are easily colored components, each of them is preferably used at 3% or less.
  • Example 1 phosphor-dispersed glasses C1 to C8 using glasses having the compositions shown in Tables 8 and 9 were produced.
  • the obtained SiO 2 —B 2 O 3 —R 2 O—Al 2 O 3 series phosphor-dispersed glasses C1 to C8 were evaluated in the same manner as in Example 1, and are also shown in Tables 8 and 9.
  • Table 10 shows the data of comparative samples C9 to C12.
  • the phosphor-dispersed glasses C1 to C8 using the SiO 2 —B 2 O 3 —R 2 O—Al 2 O 3 glass have softening points of all the glasses. It is 500 degrees C or less. Moreover, it became clear that the internal transmittance
  • the blending ratio of R 2 O (Li 2 O + Na 2 O + K 2 O) is preferably 12% to 27%, and more preferably 15% to 27%.
  • This is a blending ratio of phosphor dispersion glass C7 of 15.0%, softening point is 478 ° C., internal transmittance is 99.4%, phosphor dispersion glass C1 is blending ratio of 26.3%, This is reasonable because the softening point is 469 ° C. and the internal transmittance is 99.8%.
  • the preferable range of Al 2 O 3 is 5 to 13% means that the phosphor dispersion glass C5 has an internal transmittance of 99.4% in the case where the blending ratio of the phosphor dispersion glass C7 is 5.1% and the phosphor dispersion glass C5. In the example where the blending ratio of C6 is 12.0%, the internal transmittance is 99.8% or more.
  • C9 is an example in which the content of Li 2 O, Na 2 O, K 2 O, which is a component that lowers the softening point, is low.
  • Glass C9 has a softening point of 560 ° C., and the mold temperature during firing becomes higher than that, which may shorten the mold life.
  • Glass C10 is an example containing more than 1% of Bi2O3, which is a component that is easily colored.
  • Glass C10 has an internal transmittance of 96% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where a high transmittance close to 100% is required.
  • Glass C11 is an example which contains SnO which is a component which is easy to color exceeding 1%.
  • Glass C11 has an internal transmittance of 92% at a wavelength of 400 nm, which is 99% or less, and is limited to use in fields where high transmittance close to 100% is required.
  • C12 is an example containing more than 1% of TeO2, which is an easily colored component.
  • Glass C12 has an internal transmittance of 97% at a wavelength of 400 nm, which is 99% or less, and is restricted to use in fields where a high transmittance close to 100% is required. Further, in the glasses C10 to C12, light absorption occurs, which causes a problem of heat generation.
  • Table 11 shows glasses D1 to D4 of comparative examples.
  • the glass D1 is a glass corresponding to Example H described in Patent Document 1 described above.
  • the glass D2 is a glass corresponding to Example B1 described in Patent Document 2 described above
  • the glass D3 is a glass corresponding to Example 1 described in Patent Document 3 described above.
  • the data described in Table 11 are numerical values described in each patent document.
  • the glass D4 is an example actually produced experimentally, and is an example in which a glass material that lowers the softening point is not blended.
  • % display of each composition component is converted into mass% and displayed.
  • the value 90% of the internal transmittance of the glass D3 at a wavelength of 588 nm is obtained by converting 95% described in the glass thickness of 1 mm to the value of the glass thickness of 2 mm in the same manner as the others.
  • Glass D1 has a softening point of 600 ° C., and the mold temperature during firing becomes higher than that, which may shorten the mold life.
  • Glass D2 has an internal transmittance of 97% and 99% or less at a wavelength of 400 nm, and is limited to use in fields where a high transmittance close to 100% is required.
  • Glass D3 also has a softening point as low as 350 ° C., but has an internal transmittance of 90% at a wavelength of 588 nm, and cannot be used in fields where high transmittance is required.
  • the glass D4 which is a P2O5-BaO-based glass but does not contain R 2 O (R is at least one selected from Li, Na, K) has a softening point of 572 ° C., and similarly to the glass D1, There is a risk that the life of the mold will be shortened.
  • the phosphor dispersed glass according to the present invention does not include SnO is a component that glass tends to develop color, the Bi 2 O 3, TeO 2 substantially, R to P 2 O 5 -BaO-based glass P 2 O 5 —BaO—R 2 O based glass added with 2 O (R is at least one selected from Li, Na, K), or B 2 O 3 —La 2 O 3 based glass with R 2 B 2 O 3 —La 2 to which O (R is at least one selected from Li, Na, K) and R′O (R ′ is at least one selected from Mg, Ca, Sr, Ba, Zn) is added.
  • R 3 O (R is at least one selected from Li, Na and K) and Al 2 O 3 are added to an O 3 —R 2 O—R′O glass or a SiO 2 —B 2 O 3 glass.
  • SiO 2 -B 2 O 3 -R 2 O-Al 2 O 3 was added Because of the use of glass, as well as a possible firing at a relatively low temperature without deteriorating the mold life, the phosphor dispersed glass using glass to maintain a high transmittance. Therefore, a phosphor-dispersed glass that includes a predetermined phosphor and can uniformly emit a desired color light can be obtained.
  • the internal transmittance of the glass is 99% or more at both the plate thickness of 2 mm and the wavelengths of 400 nm and 588 nm, the primary light and the excited secondary light are well transmitted.
  • a phosphor-dispersed glass that emits light that is a mixture of secondary light and secondary light can be obtained.
  • the LED light-emitting element is a blue light-emitting element and the phosphor is a yellow phosphor
  • a phosphor-dispersed glass that emits white light with a uniform color tone can be obtained as light.

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Abstract

Cette invention concerne un verre à dispersion de phosphore comprenant un verre P2O5-BaO-R2O produit en ajoutant R2O (R représentant au moins un élément choisi parmi Li, Na et K) à un verre P2O5-BaO, un verre B2O3-La2O3-R2O-R'O produit en ajoutant R2O (R représentant au moins un élément choisi parmi Li, Na et K) et R'O (R' représentant au moins un élément choisi parmi Mg, Ca, Sr, Ba et Zn) à un verre B2O3-La2O3, ou un verre SiO2-B2O3-R2O-Al2O3 produit en ajoutant R2O (R représentant au moins un élément choisi parmi Li, Na et K) et Al2O3 à un verre SiO2-B2O3 ; et un procédé de production du verre à dispersion de phosphore.
PCT/JP2010/061763 2009-07-27 2010-07-12 Verre à dispersion de phosphore et son procédé de production WO2011013505A1 (fr)

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WO2013148783A1 (fr) * 2012-03-30 2013-10-03 Corning Incorporated Agent d'encapsulation en verre de borate de bismuth pour luminophores de del
US8822032B2 (en) 2010-10-28 2014-09-02 Corning Incorporated Phosphor containing glass frit materials for LED lighting applications
WO2015012052A1 (fr) * 2013-07-25 2015-01-29 セントラル硝子株式会社 Verre à luminophore dispersé
WO2015093267A1 (fr) * 2013-12-17 2015-06-25 日本電気硝子株式会社 Élément de conversion de longueur d'onde et dispositif électroluminescent
JP2015137283A (ja) * 2014-01-20 2015-07-30 株式会社ネモト・ルミマテリアル 波長変換部材
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US10158057B2 (en) 2010-10-28 2018-12-18 Corning Incorporated LED lighting devices
US8822032B2 (en) 2010-10-28 2014-09-02 Corning Incorporated Phosphor containing glass frit materials for LED lighting applications
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