WO2014166085A1 - Verre microcristallin au ce:yag pour led en lumière blanche, et son procédé de préparation - Google Patents

Verre microcristallin au ce:yag pour led en lumière blanche, et son procédé de préparation Download PDF

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WO2014166085A1
WO2014166085A1 PCT/CN2013/074038 CN2013074038W WO2014166085A1 WO 2014166085 A1 WO2014166085 A1 WO 2014166085A1 CN 2013074038 W CN2013074038 W CN 2013074038W WO 2014166085 A1 WO2014166085 A1 WO 2014166085A1
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glass
mol
melt
yag
resistance furnace
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PCT/CN2013/074038
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Chinese (zh)
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王元生
陈大钦
张瑞
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中国科学院福建物质结构研究所
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Priority to PCT/CN2013/074038 priority Critical patent/WO2014166085A1/fr
Publication of WO2014166085A1 publication Critical patent/WO2014166085A1/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
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/14—Silica-free oxide glass compositions 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
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
    • 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
    • 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
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • 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
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/122—Silica-free oxide glass compositions containing oxides of As, Sb, Bi, Mo, W, V, Te as glass formers
    • 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
    • C03C3/142—Silica-free oxide glass compositions containing boron containing lead
    • 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
    • C03C3/145—Silica-free oxide glass compositions containing boron 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
    • C03C3/14—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
    • C03C3/16—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
    • 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
    • C03C3/253—Silica-free oxide glass compositions containing germanium

Definitions

  • the present invention relates to the field of solid luminescent materials, and more particularly to a Ce:YAG microcrystalline glass which can be used for white LEDs and a method for preparing the same.
  • LED lighting lamps with unique advantages such as energy saving and durability have attracted great attention.
  • LED white light-emitting diode
  • Common commercial white LEDs are packaged by a blue InGaN chip and a Ce 3+ yttrium aluminum garnet (YAG) phosphor.
  • the phosphor is mixed in an epoxy resin and applied to the chip.
  • the blue portion of the InGaN LED chip is absorbed by the phosphor to cause yellow light, and the unabsorbed blue light is mixed with the yellow light emitted by the phosphor to obtain white light.
  • Glass-ceramic also known as glass-ceramic
  • glass-ceramic is a composite material in which micro/nanocrystals are uniformly embedded in an inorganic glass matrix. It combines the advantages of crystal and glass materials and can have optical properties similar to or better than crystals. There is an advantage similar to the preparation method of glass material, high thermal stability and high chemical stability. Its thermal conductivity is much greater than that of epoxy resins.
  • glass-ceramics are easily processed into flat sheets or hollow bulbs that are directly overlaid on the chip. Therefore, it can be used to replace conventional phosphors to construct new white LEDs (avoiding epoxy or silica gel). Compared to conventional LED devices, this new device offers significant advantages in light color stability and long life.
  • the first method is used to prepare a patent for a glass-ceramic for a white LED, such as: Chinese invention patent CN102092951A, "Transparent glass ceramic material for ultraviolet light excitation white LED and its preparation technology" applied by Chen Daqin and others of the Fujian Institute of Physical Structures, Chinese Academy of Sciences, in which the crystal phase contained in the glass ceramic is Dy:CeF3. This material cannot be excited by commercial blue chip to produce white light emission.
  • the second method is used to prepare a patent for a glass-ceramic for a white LED, such as:
  • Chinese invention patent CN101643315B "White light LED low melting point fluorescent glass and preparation method thereof" applied by Wuhan University of Technology, the patent also discloses a crystal glass containing Ce:YAG crystal phase, the glass matrix component is Si0 2 -Al 2 0 3 -B 2 0 3 -CaO-ZnO-Na 2 0-MgO.
  • the material is also poor in transparency and poor in luminescent properties (see also, Chen Zhenxia, Research on Low-melting Luminescent Glass for LED, Master's thesis of Wuhan University of Technology, May 2010).
  • the invention provides a crystallized glass based on a new component formula and a preparation method thereof, wherein the material has high transparency and the quantum efficiency of yellow light emission is up to 94% under blue light excitation, which is an excellent and can be applied to white LEDs.
  • New glass-ceramic materials
  • the invention provides a Ce:YAG glass-ceramic and a preparation method thereof.
  • the material of the invention is unique in composition, high in transparency and excellent in luminescent properties, and can be used for constructing white LEDs.
  • the controllable preparation of the glass-ceramic material is realized by mixing and co-melting the commercial micro-scale Ce: YAG phosphor with the low-melting glass. The results of the spectral test indicate that the Ce:YAG glass-ceramic of the present invention emits bright yellow light under the excitation of 465 nm blue light, and its maximum quantum efficiency is up to 94%, which is combined with a commercial blue chip to produce white light emission.
  • a glass substrate characterized in that the glass component content (mol%) of the glass substrate is as follows: 0-10mol% SiO 2; 0-40mol% GeO 2; 20-60 mol% Te0 2; 0-25mol% B 2 O 3; 0-15mol% P 2 O 5; 0-10mol% Al 2 O 3; 0 -20 mol% Ae 2 O; 0-20 mol% ZnO; 0-15 mol% BaO; 0-20 mol% Sb 2 0 3 ; 0-20 mol% La 2 0 3 ; 0-10 mol% Bi 2 0 3 ;
  • Ae is selected from the group consisting of Li, Na or K; and the total molar amount of the above components is 100 mol%.
  • a Ce:YAG glass-ceramic characterized in that the glass substrate of the glass-ceramic is as described above. Specifically, the composition and percentage (mol%) of the glass substrate are as follows:
  • Ae is selected from Li, Na or K
  • the total molar amount of the above components is 100 mol%.
  • the preferred amounts of the components are as follows:
  • SK) 2 is preferably 2-8 mol%, more preferably 3-6 mol%, still more preferably 4-5 mol%;
  • Ge0 2 is preferably 5-30 mol%, 10-25 mol%, 15-20 mol%,;
  • Te0 2 is preferably 20-55 mol%, more preferably 24-50 mol%, still more preferably 30-46 mol%, or more preferably 36-45 mol%, still more preferably 38-40 mol%;
  • B 2 0 3 is preferably 5-20 mol%, more preferably 7-19 mol%, still more preferably 8-16 mol%, or more preferably 10-15 mol%, ll-12 mol%;
  • P 2 0 5 is preferably 5-10 mol%, more preferably 6-8 mol%;
  • A1 2 0 3 is preferably 2-8 mol%, more preferably 4-6 mol%;
  • Ae 2 0 is preferably 8-18 mol%, more preferably 10-16 mol%, still more preferably 12-15 mol%;
  • BaO is preferably 5-14 mol%, preferably 8-10 mol%
  • La 2 0 3 is preferably 5-15 mol%
  • ZnO is preferably 6-18 mol%, more preferably 10-16 mol%, still more preferably ll-15 mol%;
  • Sb 2 0 3 is preferably 5-15 mol%, more preferably 9-10 mol%;
  • Bi 2 0 3 is preferably 5-6 mol%.
  • the present invention also provides a Ce:YAG glass-ceramic capable of realizing yellow light emission under blue light excitation, the glass substrate of the glass-ceramic being as described above.
  • the glass matrix component and the percentage (mol%) of the glass ceramics are as follows:
  • Ae is selected from Li, Na or K
  • the total molar amount of the above components is 100 mol%.
  • the preferred amounts of the components are as follows:
  • SK) 2 is preferably 2-8 mol%, more preferably 3-6 mol%, still more preferably 4-5 mol%;
  • Ge0 2 is preferably 5-30 mol%, 10-25 mol%, 15-20 mol%,;
  • Te0 2 is preferably 20-55 mol%, more preferably 24-50 mol%, still more preferably 30-46 mol%, or more preferably 36-45 mol%, still more preferably 38-40 mol%;
  • B 2 0 3 is preferably 5-20 mol%, more preferably 7-19 mol%, still more preferably 8-16 mol%, or more preferably 10-15 mol%, ll-12 mol%;
  • P 2 0 5 is preferably 5-10 mol%, more preferably 6-8 mol%;
  • A1 2 0 3 is preferably 2-8 mol%, more preferably 4-6 mol%;
  • Ae 2 0 is preferably 8-18 mol%, more preferably 10-16 mol%, still more preferably 12-15 mol%;
  • BaO is preferably 5-14 mol%, preferably 8-10 mol%
  • La 2 0 3 is preferably 5-15 mol%
  • ZnO is preferably 6-18 mol%, more preferably 10-16 mol%, still more preferably ll-15 mol%;
  • Sb 2 0 3 is preferably 5-15 mol%, more preferably 9-10 mol%;
  • Bi 2 0 3 is preferably 5-6 mol%.
  • the Ce:YAG glass-ceramic according to the present invention is characterized in that the microstructure is characterized in that Ce:YAG fluorescent crystallites are uniformly embedded in the oxide glass matrix.
  • the Ce:YAG glass-ceramic according to the present invention has a Ce:YAG phosphor powder in an amount of from 1 to 15% by weight, preferably from 2 to 10% by weight, more preferably from 5 to 8% by weight, based on the glass substrate.
  • the ratio of Ce:YAG is determined in the present invention. Two factors are considered: on the one hand, the formability and transparency of the sample are ensured, and on the other hand, high luminous efficiency is ensured.
  • the present invention also provides a method of preparing Ce:YAG glass-ceramics, characterized in that the method comprises a two-step melt quenching method.
  • the method further comprises annealing the obtained bulk glass ceramic to eliminate internal stress.
  • the method includes the following steps:
  • the powder raw materials are mixed and ground uniformly, and then placed in a crucible.
  • the step (1) it is heated to 700 to 1100 ° C in an electric resistance furnace.
  • the powder raw material is melted by holding for 1-5 hours, preferably 2-4 hours.
  • step (1) the glass melt is taken out and quickly poured into a mold to form a bulk precursor glass.
  • the phosphor is added and further ground for 1-5 hours, preferably 2-4 hours for melting.
  • the glass melt is taken out and quickly poured into a mold to form a bulk glass ceramic.
  • step (2) it is heated to 550 - 850 ° C in an electric resistance furnace.
  • the powder is 1-5 hours, preferably 2-4 hours to melt the powder material.
  • the two-step melt quenching method specifically includes the following steps:
  • the ruthenium used in the preparation may be graphite ruthenium, platinum ruthenium or corundum ruthenium.
  • a transparent glass ceramic in which Ce: YAG crystal grains are uniformly embedded in an oxide glass substrate can be obtained.
  • Transparent glass-ceramics emit bright yellow light at 465 nm blue light, and their maximum luminescence quantum efficiency is 94%.
  • the invention further relates to the use of a glass-ceramic, characterized in that the glass-ceramic is used as a fluorescent material.
  • the glass ceramics are used to construct a white light LED excited by a blue chip.
  • the microcrystalline glass of the invention has simple preparation process, low cost, no toxicity and no pollution, good thermal and chemical stability and excellent optical characteristics, and can be developed for constructing a white LED excited by a blue chip.
  • Figure 1 is a physical photograph of the glass ceramic of Example 1;
  • Figure 2 is an X-ray diffraction pattern of the glass ceramic of Example 1;
  • Figure 3 is an excitation spectrum diagram of Example 1 glass-ceramic corresponding to 566 nm emission
  • Example 4 is a fluorescent optical pattern of the glass ceramic of Example 1 excited at a wavelength of 465 nm;
  • Figure 5 is a graph showing quantum efficiency measurement data of the glass ceramic of Example 1;
  • Figure 6 is a combined luminescence photograph of the glass ceramic of Example 1 under blue light excitation
  • Figure 7 is a photograph of a photo of the glass ceramic of Example 2.
  • Figure 8 is a luminescence photograph of a physical sample after coupling of the glass ceramic of Example 2 and a blue chip. detailed description
  • the steel was melted for 2 hours to melt, and then the glass melt was taken out and quickly poured into a mold to form a bulk precursor glass; the obtained precursor glass was crushed, ground in an agate mortar, and then added. 5 wt% of the Ce:YAG phosphor was further ground for 2 hours, placed in a crucible, then placed in a resistance furnace and heated to 700 ° C and then held for 1 hour to melt, and then the glass melt was taken out and quickly poured into the mold. Forming in the middle, obtaining bulk glass-ceramics (as shown in Fig. 1); finally, the obtained crystallized glass is placed in an electric resistance furnace and annealed at 300 ° C to eliminate internal stress.
  • X-ray diffraction data indicated that a YAG microcrystalline phase was precipitated in the glass matrix (as shown in Figure 2).
  • the samples were surface polished and their room temperature excitation and emission spectra were measured using a FLS920 fluorescence spectrometer.
  • the ratio is accurately weighed, placed in an agate mortar, mixed in an agate mortar and ground uniformly, placed in a platinum crucible, placed After heating to 1100 ° C in an electric resistance furnace, it was kept for 2 hours to be melted, and then the glass melt was taken out and quickly poured into a mold to form a bulk precursor glass; the obtained precursor glass was broken, in an agate mortar.
  • the pure Te0 2 , B 2 0 3 , P 2 0 5 , A1 2 0 3 , Na 2 C0 3 , ZnO and Sb 2 0 3 powders will be analyzed as 55Te0 2 : 7B 2 0 3 : 8P 2 O s :
  • the ratio of 4A1 2 0 3 : 8Na 2 C0 3 : 9ZnO: 9Sb 2 0 3 (molar ratio) is accurately weighed, placed in an agate mortar, mixed in an agate mortar and ground uniformly, and placed in a platinum crucible. Put it into an electric resistance furnace and heat it to 750 ° C, then keep it for 2 hours to melt it.
  • Example 7 take out the glass melt and quickly pour it into the mold to form a block-shaped precursor glass. Break the obtained precursor glass and grind it in agate. After grinding in a crucible, add 5 wt% of Ce:YAG phosphor and further grind for 2 hours, then place it in a crucible, then heat it to 600 ° C in an electric resistance furnace and then heat it for 1 hour to melt it. Then, melt the glass. The body was taken out and quickly poured into a mold to form a bulk glass ceramic. Finally, the obtained crystallized glass was placed in an electric resistance furnace and annealed at 300 ° C to eliminate internal stress. The crystallized glass is coupled to a commercial 465 nm blue chip to emit bright white light under blue light excitation.
  • Example 7 Example 7
  • the pure Ge0 2 , Te0 2 , P 2 0 5 , Li 2 0, Sb 2 0 3 and La 2 0 3 powders will be analyzed as 25Ge0 2 : 30TeO 2 : 5P 2 0 5 : 15Li 2 0: 20Sb 2 O 3 : 5La 2 0 3 (molar ratio)
  • the ratio is accurately weighed, placed in an agate mortar, mixed in an agate mortar and ground uniformly, placed in a platinum crucible, and placed in an electric resistance furnace to 700 ° C.
  • Example 8 After the second heat preservation for 2 hours to melt, and then the glass melt was taken out and quickly poured into a mold to form a block precursor glass; the obtained precursor glass was crushed, ground uniformly in an agate mortar, and 5 wt% was added. The Ce:YAG phosphor was further ground for 2 hours and then placed in a crucible, then heated in an electric resistance furnace to 550 ° C and then held for 1 hour to melt, and then the glass melt was taken out and quickly poured into a mold to form. A bulk glass ceramic was obtained; finally, the obtained crystallized glass was placed in an electric resistance furnace and annealed at 300 ° C to eliminate internal stress. The crystallized glass is coupled to a commercial 465 nm blue chip to emit bright white light under blue light excitation.
  • Example 8 Example 8
  • the pure Te0 2 , P 2 0 5 , Na z O and ZnO powders will be analyzed as 60TeO 2 : 10P 2 O 5 : 20Na 2 O:
  • the ratio of ⁇ (molar ratio) was accurately weighed and placed in an agate mortar. It was mixed and ground in an agate mortar and placed in a platinum crucible. It was heated to 850 ° C in an electric resistance furnace and then kept for 2 hours to melt. Then, the glass melt is taken out and quickly poured into a mold to form a bulk precursor glass; the obtained precursor glass is crushed, ground uniformly in an agate mortar, and 15 wt% of Ce: YAG phosphor is further added.
  • the % Ce:YAG phosphor was further ground for 2 hours and then placed in a crucible, then placed in an electric resistance furnace and heated to 750 ° C for 1 hour to melt, and then the glass melt was taken out and quickly poured into a mold. Forming to obtain a bulk glass ceramic; finally, the obtained crystallized glass was placed in an electric resistance furnace and annealed at 300 ° C to eliminate internal stress.
  • the crystallized glass is coupled to a commercial 465 nm blue chip to emit bright white light under blue light excitation.

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention concerne un verre microcristallin au Ce:YAG, pouvant réaliser une émission de lumière jaune dans les conditions d'une excitation en lumière bleue, et son procédé de préparation. L'invention concerne un verre microcristallin au Ce:YAG, pouvant réaliser une émission de lumière jaune dans les conditions d'une excitation en lumière bleue, et son procédé de préparation. Le verre microcristallin comprend les composants de substrat de verre suivants (% en moles) : 0-10 % en moles de SiO2, 0-40 % en moles de GeO2, 20-60 % en moles de TeO2, 0-25 % en moles de B2O3, 0-15 % en moles de P2O5, 0-10 % en moles de Al2O3, 0-20 % en moles de Ae2O, 0-20 % en moles de ZnO, 0-15 % en moles de BaO, 0-20 % en moles de Sb2O3, 0-20 % en moles de La2O3, 0-10 % en moles de Bi2O3, Ae étant choisi parmi Li, Na ou K, et la teneur en microcristaux de Ce:YAG étant de 1-15 % en poids par rapport au substrat de verre à base d'oxyde. Le verre microcristallin peut émettre une lumière jaune après excitation par une lumière bleue, et la lumière jaune et la lumière bleue sont combinées pour générer une lumière blanche intense, de sorte que le verre microcristallin peut être utilisé pour la construction d'une LED en lumière blanche excitée par une puce en lumière bleue.
PCT/CN2013/074038 2013-04-10 2013-04-10 Verre microcristallin au ce:yag pour led en lumière blanche, et son procédé de préparation WO2014166085A1 (fr)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106892562A (zh) * 2016-12-26 2017-06-27 温州大学 一种用流延法制备三明治状的Ce：YAG微晶玻璃片的方法
CN107572777A (zh) * 2017-09-21 2018-01-12 上海应用技术大学 一种led照明用碲酸盐透明荧光玻璃的制备方法
CN109111120A (zh) * 2018-10-26 2019-01-01 浙江工业大学 一种暖白光led用可自发析晶荧光微晶玻璃及其制备方法
CN112456796A (zh) * 2020-12-21 2021-03-09 中国计量大学 一种金属粒子增强稀土掺杂宽色域荧光玻璃及其制备方法

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CN106892562A (zh) * 2016-12-26 2017-06-27 温州大学 一种用流延法制备三明治状的Ce：YAG微晶玻璃片的方法
CN107572777A (zh) * 2017-09-21 2018-01-12 上海应用技术大学 一种led照明用碲酸盐透明荧光玻璃的制备方法
CN109111120A (zh) * 2018-10-26 2019-01-01 浙江工业大学 一种暖白光led用可自发析晶荧光微晶玻璃及其制备方法
CN112456796A (zh) * 2020-12-21 2021-03-09 中国计量大学 一种金属粒子增强稀土掺杂宽色域荧光玻璃及其制备方法

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