US20090314989A1 - Fluorescent substance composite glass, fluorescent substance composite glass green sheet, and process for producing fluorescent substance composite glass - Google Patents

Fluorescent substance composite glass, fluorescent substance composite glass green sheet, and process for producing fluorescent substance composite glass Download PDF

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Publication number
US20090314989A1
US20090314989A1 US11/919,209 US91920906A US2009314989A1 US 20090314989 A1 US20090314989 A1 US 20090314989A1 US 91920906 A US91920906 A US 91920906A US 2009314989 A1 US2009314989 A1 US 2009314989A1
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glass
fluorescent substance
substance composite
composite glass
powder
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Masaru Iwao
Yoshio Umayahara
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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Assigned to NIPPON ELECTRIC GLASS CO., LTD. reassignment NIPPON ELECTRIC GLASS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: IWAO, MASARU, UMAYAHARA, YOSHIO
Publication of US20090314989A1 publication Critical patent/US20090314989A1/en
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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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • 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
    • 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
    • C03C3/076—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
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • 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
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/04—Particles; Flakes
    • 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
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/30—Methods of making the composites

Definitions

  • the present invention relates to a fluorescent substance composite glass, a fluorescent substance composite glass green sheet and a process for producing a fluorescent substance composite glass.
  • White LEDs are expected to be applied to illumination uses as light sources of the next generation which are to be used in place of incandescent lamps or fluorescent lamps.
  • a fluorescent substance powder is blended in, for example, a mold resin made of an organic type binder resin that seals a luminous plane of an LED chip to mold and a part or all of the emission from the LED chip is absorbed to carry out conversion into a desired wavelength.
  • Patent Reference 1 discloses a method for coating an LED chip by dispersing a fluorescent substance in a non-lead type low-melting point glass such as an SnO 2 —P 2 O 5 type glass or a TeO type glass.
  • Patent Reference 2 discloses use of a fluorescent substance composite glass obtained by molding a glass powder and an inorganic fluorescent substance powder under pressure and baking the molded material to make glass, and dispersing a fluorescent substance powder in the glass.
  • Patent Reference 1 Publication of JP-A 2005-11933
  • Patent Reference 2 Publication of JP-A 2003-258308
  • the non-lead type low-melting point glass such as the SnO 2 —P 2 O 5 type glass or the TeO type glass disclosed in Patent Reference 1 has problems that it has low weatherability and reacts strongly with the fluorescent substance, resulting in deterioration of products.
  • the fluorescent substance composite glass described and disclosed in Patent Reference 2 is one obtained by molding a glass powder and an inorganic fluorescent substance powder under pressure and baking the molded material to make glass, no glass having a low wall thickness can be obtained, giving rise to a problem that no improvement in luminous efficacy can be expected. Also, the molding under pressure has a problem that a glass material having a large size and uniform thickness cannot be produced at low costs.
  • the fluorescent substance composite glass according to the present invention is produced by baking a mixture containing a glass powder and an inorganic fluorescent substance powder, and is characterized in that the energy conversion efficiency to a visible light wavelength region of 380 to 780 nm is 10% or more, when light having an emission peak in a wavelength range of 350 to 500 nm is applied.
  • the fluorescent substance composite glass green sheet according to the present invention is produced by kneading a mixture containing at least a glass powder, an inorganic fluorescent substance powder and an organic type solvent binder resin and molding the mixture into a sheet form.
  • the process for producing a fluorescent substance composite glass according to the present invention includes laminating a restricting member, which does not react with the fluorescent substance composite glass green sheet at the baking temperature of the glass green sheet, on one or both surface(s) of the glass green sheet, then carrying out baking treatment and then removing the restricting member.
  • the fluorescent substance composite glass green sheet of the present invention enables production of a fluorescent substance composite glass having a uniform thickness, a low wall thickness and a large size at low costs.
  • shrinkage and deformation in the direction of the plane can be reduced and therefore, a fluorescent substance composite glass having a low wall thickness and a large size can be obtained.
  • the fluorescent substance composite glass of the present invention which may be produced in this manner is chemically stable, is reduced in wall thickness and has a uniform thickness and therefore has a high energy conversion efficiency.
  • FIG. 1 is an explanatory view for illustrating a process for producing a fluorescent substance composite glass by laminating a restricting member on both surfaces of fluorescent substance composite glass green sheets laminated plurally.
  • FIG. 2 is an explanatory view for illustrating a process for producing a fluorescent substance composite glass by alternately laminating fluorescent substance composite glass green sheets and restricting members.
  • the fluorescent substance composite glass of the present invention is constituted of a sintered body of a glass powder and an inorganic fluorescent substance powder and has a structure in which the inorganic fluorescent substance is dispersed in the glass. For this reason, this fluorescent substance composite glass is chemically stable and can be therefore limited in discoloration even if it is exposed to high power light for a long time. Also, a fluorescent substance composite glass can be obtained which has a low wall thickness, is uniform and has a high energy conversion efficiency.
  • the energy conversion efficiency is preferably 11% or more and more preferably 12% or more.
  • the energy conversion efficiency in the present invention is a value given by the equation: c/(a ⁇ b) ⁇ 100(%) when the energy of the light source is a (W: watt), the energy of light having the same wavelength as that of the light source transmitting the fluorescent substance composite glass is b (W) and the energy of light converted by the wavelength of the light source in the fluorescent substance composite glass is c (W).
  • the porosity of the fluorescent substance composite glass is only required to decrease the porosity of the fluorescent substance composite glass to 10% or less.
  • the porosity is more preferably in a range from 8% or less.
  • the porosity means a value found by the equation: (1 ⁇ actual density/theoretical density) ⁇ 100(%) based on an actual density and a theoretical density measured by the Archimedes' method.
  • the proportion of the glass powder is large. Therefore, if it is baked as it is, the glass is fluidized and easily shrunk in a plane direction by the surface tension of the glass. It is therefore difficult to obtain a fluorescent substance composite glass having a low wall thickness, a uniform thickness and a large size. There is such an idea that the proportion of the inorganic fluorescent substance powder is increased to limit shrinkage in a plane direction.
  • the present invention makes it possible to obtain a fluorescent substance composite glass having a low wall thickness, a uniform thickness and a large size by laminating a restricting member, which does not react with a fluorescent substance composite glass green sheet at the baking temperature of the glass green sheet, on one or both surface(s) of the glass green sheet, then carrying out baking treatment and then removing the restricting member.
  • a restricting member a green sheet containing an inorganic composition or a porous ceramic substrate may be used.
  • any inorganic fluorescent substance powder usually available on the market may be used.
  • the inorganic fluorescent substance include those containing YAG type fluorescent substances, oxides, nitrides, oxide-nitrides, sulfides, rare earth metal acid sulfides, halides, aluminic acid chlorides or halophosphoric acid chlorides.
  • the YAG type fluorescent substances and the oxide fluorescent substances are stable even if they are mixed with the glass and heated to high temperatures.
  • Fluorescent substances such as nitrides, oxide-nitrides, sulfides, rare earth metal acid sulfides, halides, aluminic acid chlorides or halophosphoric acid chlorides are easily reacted with the glass by heating in the sintering process to easily cause abnormal reactions including foaming and discoloring.
  • the degree of these abnormal reactions is significantly increased as the sintering temperature becomes higher.
  • these substances may be used by optimizing the baking temperature and the composition of the glass.
  • the glass powder to be used in the present invention has a function as a medium keeping the inorganic fluorescent substance stably. Also, because the tones of the sintered body are different and there is a difference in reactivity with the inorganic fluorescent substance depending on the composition type of the glass to be used, it is necessary to select the composition of the glass to be used in consideration of various conditions. Moreover, it is important to determine the amount of the inorganic fluorescent substance and thickness of the member suitable to the composition of the glass. Any material may be used as the glass powder without any particular limitation insofar as it is resistant to a reaction with the inorganic fluorescent substance.
  • an SiO 2 —B 2 O 3 —RO (RO represents MgO, CaO, SrO or BaO) type glass, an SiO 2 —B 2 O 3 type glass, SiO 2 —B 2 O 3 —R 2 O (R 2 O represents Li 2 O, Na 2 O or K 2 O) type glass, an SiO 2 —B 2 O 3 —Al 2 O 3 type glass, an SiO 2 —B 2 O 3 —ZnO type glass or a ZnO—B 2 O 3 type glass may be used.
  • the SiO 2 —B 2 O 3 —RO type glass or the ZnO—B 2 O 3 type glass which is resistant to a reaction with the inorganic fluorescent substance in baking is preferably used.
  • the preferable range (mass percentage) of each component in the SiO 2 —B 2 O 3 —RO type glass is as follows: 30 to 70% of SiO 2 , 1 to 15% of B 2 O 3 , 0 to 10% of MgO, 0 to 25% of CaO, 0 to 10% of SrO, 8 to 40% of BaO, 10 to 45% of RO, 0 to 20% of Al 2 O 3 and 0 to 10% of ZnO.
  • the reason why the above ranges are defined is as follows.
  • SiO 2 is a component that forms a network of glass. If the content of SiO 2 is less than 30% by mass, chemical durability tends to be impaired. If the content of SiO 2 exceeds 70% by mass, sintering temperature is made high, so that the fluorescent substance is easily deteriorated. SiO 2 is more preferably in a range from 40 to 60%.
  • B 2 O 3 is a component that drops the melting temperature of the glass to significantly improve the melting ability of the glass. If the content of B 2 O 3 is less than 1% by mass, its effect is scarcely obtained. If the content of B 2 O 3 exceeds 15% by mass, chemical durability of the glass tends to be deteriorated. B 2 O 3 is more preferably in a range from 2 to 10%.
  • MgO is a component that drops the melting temperature of the glass to significantly improve the melting ability of the glass. If the content of MgO exceeds 10% by mass, chemical durability of the glass tends to be deteriorated. MgO is more preferably in a range from 0 to 5%.
  • CaO is a component that drops the melting temperature of the glass to significantly improve the melting ability of the glass. If the content of CaO exceeds 25% by mass, chemical durability of the glass tends to be deteriorated. CaO is more preferably in a range from 3 to 20%.
  • SrO is a component that drops the melting temperature of the glass to significantly improve the melting ability of the glass. If the content of SrO exceeds 10% by mass, chemical durability of the glass tends to be deteriorated. SrO is more preferably in a range from 0 to 5%.
  • BaO is a component that drops the melting temperature of the glass to improve the melting ability of the glass and to suppress the reaction with the fluorescent material. If the content of BaO is less than 8% by mass, its effect on limitation of a reaction with the fluorescent substance tends to be reduced. On the other hand, if the content of BaO exceeds 40% by mass, chemical durability of the glass tends to be deteriorated. BaO is more preferably in a range from 10 to 35%.
  • the amount of RO which is the sum of the amounts of MgO, CaO, SrO and BaO, is preferably 10 to 45%. If the content of RO is less than 10% by mass, the effect of improving the melting ability is scarcely obtained. On the other hand, if the content of RO exceeds 45% by mass, chemical durability is easily deteriorated. RO is more preferably in a range from 11 to 40%.
  • Al 2 O 3 is a component that improves chemical durability. If the content of Al 2 O 3 exceeds 20% by mass, the melting ability of the glass tends to be impaired. Al 2 O 3 is more preferably in a range from 2 to 15%.
  • ZnO is a component that drops the melting temperature of the glass to thereby improve the melting ability of the glass. If the content of ZnO exceeds 10% by mass, chemical durability of the glass tends to be impaired. ZnO is more preferably in a range from 1 to 7%.
  • alkali metal oxides P 2 O 5 , La 2 O 3 or the like may be added.
  • Preferable range (mass percentage) of each component in the Zn—B 2 O 3 type glass is as follows: 5 to 60% of ZnO, 5 to 50% of B 2 O 3 and 0 to 30% of SiO 2 .
  • the reason why the above ranges are defined is as follows.
  • ZnO is a component that forms a network of glass. If the content of ZnO is less than 5% by mass, the sintering temperature becomes higher and therefore, the fluorescent substance is easily deteriorated. On the other hand, if the content of ZnO exceeds 60% by mass, chemical durability tends to be deteriorated. ZnO is more preferably in a range from 20 to 50%.
  • B 2 O 3 is a component that forms a network of glass. If the content of B 2 O 3 is less than 5% by mass, the sintering temperature becomes high and the fluorescent substance is therefore easily deteriorated. If the content of B 2 O 3 exceeds 50% by mass, on the other hand, chemical durability tends to be impaired. B 2 O 3 is more preferably in a range from 10 to 50%.
  • SiO 2 is a component that improves the durability of the glass. If the content of SiO 2 exceeds 30% by mass, the sintering temperature becomes so high that the fluorescent substance is easily deteriorated. SiO 2 is more preferably in a range from 0.1 to 25%.
  • alkali metal oxides alkali earth metal oxides, Al 2 O 3 or the like may be added.
  • the energy conversion efficiency of the fluorescent substance composite glass is changed according to the type and content of the fluorescent substance particles dispersed in the glass and the wall thickness of the fluorescent substance composite glass. It is only necessary for the content of the fluorescent substance and the wall thickness of the fluorescent substance composite glass to be adjusted so that the energy conversion efficiency is optimum. However, if the fluorescent substance is excessive, it is difficult to sinter and the porosity is increased, giving rise to the problem that excited light is hardly efficiently applied to the fluorescent substance and the mechanical strength of the fluorescent substance composite glass is easily reduced. On the other hand, if the content of the fluorescent substance is too low, it is difficult to make the fluorescent substance emit light sufficiently.
  • the proportion of the contents of the glass and the fluorescent substance by mass is preferably adjusted to a range from 99.99:0.01 to 70:30, more preferably a range from 99.95:0.05 to 80:20 and particularly preferably 99.92:0.08 to 85:15.
  • a binder, a plasticizer, a solvent and the like are used together with the glass powder and the inorganic fluorescent substance powder.
  • the SiO 2 —B 2 O 3 —RO(RO represents MgO, CaO, SrO or BaO) type glass, the SiO 2 —B 2 O 3 type glass, the SiO 2 —B 2 O 3 —R 2 O (R 2 O represents Li 2 O, Na 2 O or K 2 O) type glass, the SiO 2 —B 2 O 3 —Al 2 O 3 type glass, the SiO 2 —B 2 O 3 —ZnO type glass or the ZnO—B 2 O 3 type glass may be used as mentioned above.
  • the SiO 2 —B 2 O 3 —RO type glass or the ZnO—B 2 O 3 type glass which is resistant to a reaction with the inorganic fluorescent substance in baking, is preferably used.
  • SiO 2 —B 2 O 3 —RO type glass it is preferable to use a glass powder containing the following components: 30 to 70% of SiO 2 , 1 to 15% of B 2 O 3 , 0 to 10% of MgO, 0 to 25% of CaO, 0 to 10% of SrO, 8 to 40% of BaO, 10 to 45% of RO, 0 to 20% of Al 2 O 3 and 0 to 10% of ZnO (mass percentage).
  • the ZnO—B 2 O 3 type glass it is preferable to use a glass powder containing the following components: 5 to 60% of ZnO, 5 to 50% of B 2 O 3 and 0 to 30% of SiO 2 (mass percentage).
  • the inorganic fluorescent substance powder YAG type fluorescent substances, oxides, nitrides, oxide-nitrides, sulfides, rare earth metal acid sulfides, halides, aluminic acid chlorides or halophosphoric acid chlorides as described above are preferably used.
  • the proportion of the contents of the glass and the fluorescent substance is preferably adjusted to a range from 99.99:0.01 to 70:30 by mass at any rate, though it may be properly adjusted according to the type and content of the fluorescent substance powder and the wall thickness of the fluorescent substance composite glass.
  • the proportion of the glass powder and the inorganic fluorescent substance powder in the green sheet is usually about 50 to 80% by mass.
  • the binder is a component that strengthens the dried film and imparts flexibility to the film.
  • the content of the binder is usually about 0.1 to 30% by mass.
  • a polyvinylbutyral resin, a methacrylic resin or the like may be used as the binder. These resins may be used either singly or by mixing them.
  • the plasticizer is a component that controls the drying speed and imparts flexibility to the dried film.
  • the content of the plasticizer is usually about 0 to 10% by mass.
  • the plasticizer for example, dibutyl phthalate, butylbenzyl phthalate and the like may be used. These materials may be used either singly or by mixing them.
  • the solvent is a material that makes a slurry of the materials.
  • the content of the solvent is usually about 1 to 30% by mass.
  • the solvent for example, toluene, methyl ethyl ketone and the like may be used either singly or by mixing them.
  • the process for manufacturing the fluorescent substance composite glass green sheet there is a method in which the above glass powder and the inorganic fluorescent substance powder are mixed and the binder, the plasticizer, the solvent and the like are added in fixed amounts to the obtained mixture to make a slurry.
  • the slurry is molded into a sheet form on a film such as polyethylene terephthalate (PET) by a doctor blade method.
  • PET polyethylene terephthalate
  • the molded sheet is dried to remove the organic type solvent binder, thereby making a fluorescent substance composite glass green sheet.
  • the fluorescent substance composite glass green sheet produced by the above method and a restricting member which does not react with the fluorescent substance composite glass green sheet at the baking temperature of the fluorescent substance composite glass green sheet are prepared and cut into desired sizes.
  • the restricting member is laminated on one or both surface(s) of the fluorescent substance composite glass green sheet and the both are integrated with each other by thermocompression bonding to form a laminate, which is then baked to obtain a sintered body.
  • the restricting member is removed to obtain a fluorescent substance composite glass.
  • a fluorescent substance composite glass can be manufactured, which is chemically stable, has a large size, reduced in wall thickness, has a uniform thickness and gives a high energy conversion efficiency.
  • a green sheet containing an inorganic composition or a porous ceramic substrate may be used as the restricting member.
  • any material may be used as the inorganic composition without any particular limitation insofar as it is not sintered at the baking temperature of the fluorescent substance composite glass green sheet.
  • Al 2 O 3 , MgO, ZrO 2 , TiO 2 , BeO and BN may be used either singly or as a mixture.
  • the green sheet containing an inorganic composition may be obtained by using the same mixing ratio and production method as the above fluorescent substance composite glass green sheet.
  • any porous ceramic may be used without any particular limitation insofar as it is resistant to adhesion to the fluorescent substance composite glass.
  • SiAl 2 O 5 , Al 2 O 3 , MgO and ZrO 2 may be used as the restricting member.
  • the fluorescent substance complex green sheet and the restricting member may be cut after the laminate is formed. This makes it possible to obtain a fluorescent substance composite glass reduced in a variation of dimensions before and after the composite glass is baked.
  • plural fluorescent substance complex green sheets and restricting members may be alternately laminated, thermocompression bonded and baked to obtain a large amount of the fluorescent substance composite glass. Also, if it is intended to obtain a thicker fluorescent substance composite glass, a method may be adopted in which plural fluorescent substance complex green sheets are laminated and a restricting member is laminated on one or both surface(s) of the laminated fluorescent substance composite glass green sheet, followed by thermocompression bonding and baking treatment to thereby obtain the intended composite glass.
  • the laminate is preferably baked at 750 to 1000° C.
  • the reason is that a dense sintered body is scarcely obtained at a temperature lower than 750° C.
  • the inorganic fluorescent substance is deteriorated and the glass is easily reacted with the inorganic fluorescent substance at a temperature higher than 1000° C.
  • an unsintered inorganic composition is left unremoved on the surface of the fluorescent substance composite glass after the baking treatment.
  • the inorganic composition left unremoved can be removed by carrying out ultrasonic cleaning.
  • a fluorescent substance composite glass green sheet was manufactured in the following manner.
  • Glass raw materials made of various oxides were compounded in such a manner as to obtain a composition containing 50% of SiO 2 , 5% of B 2 O 3 , 10% of CaO, 25% of BaO, 5% of Al 2 O 3 and 5% of ZnO based on mass percentage. After these components were uniformly mixed, the mixture was put in a platinum crucible and melted at 1400° C. for 2 hours to obtain uniform glass. This glass was crushed using alumina balls and classified to obtain a glass powder having an average particle diameter of 2.5 ⁇ m.
  • an inorganic fluorescent substance powder (YAG fluorescent substance powder, manufactured by KASEI OPTONIX, LTD., average particle diameter: 8 ⁇ m) was added to the produced glass powder in a mass ratio of 95:5 and these components were mixed to produce a mixture powder. Then, 30% by mass of a methacrylic acid resin as a binder, 3% by mass of dibutyl phthalate as a plasticizer and 20% by mass of toluene as a solvent were added to 100 of the produced mixture powder and these components were mixed to make a slurry. In succession, the above slurry was molded into a sheet on a PET film by a doctor blade method and dried to obtain a fluorescent substance composite glass green sheet 50 ⁇ m in thickness.
  • YAG fluorescent substance powder manufactured by KASEI OPTONIX, LTD., average particle diameter: 8 ⁇ m
  • an alumina powder (ALM-21, manufactured by Sumitomo Aluminum Co., average particle diameter: 2 ⁇ m) was used to obtain an alumina green sheet 200 ⁇ m in thickness in the same mixing ratio and method as in the method of producing the fluorescent substance composite glass green sheet as described above.
  • each green sheet was cut into a size of 100 ⁇ 100 mm and three fluorescent substance composite glass green sheets were laminated on the above alumina green sheet as shown in FIG. 1 .
  • the alumina green sheet was laminated on the above glass green sheets and these sheets were integrated by thermocompression bonding to produce a laminate, which was then baked at 900° C. Thereafter, the baked laminate was subjected to ultrasonic cleaning to remove an unsintered alumina layer left unremoved on the obtained sintered body to thereby manufacture a fluorescent substance composite glass having a size of 100 ⁇ 100 mm and a wall thickness of 120 ⁇ m.
  • the fluorescent substance composite glass obtained in this manner was irradiated with blue light from behind the fluorescent substance glass, to obtain white transmitted light. Also, the fluorescent substance composite glass was subjected to tests to measure energy conversion efficiency and porosity, to find that the energy conversion efficiency was 16% and the porosity was 2%.
  • the fluorescent substance complete glass green sheet produced in Example 1 and a mullite substrate which was a porous ceramic as the restricting member were prepared.
  • the mullite substrate and the fluorescent substance composite glass green sheet were cut into a size of 100 ⁇ 100 mm. Then, as shown in FIG. 2 , four mullite substrates and three fluorescent substance glass green sheets were alternately laminated, integrated by thermocompression bonding to produce a laminate and baked at 900° C. After that, the mullite substrates were removed to produce three fluorescent substance composite glasses each having a size of 100 ⁇ 100 mm and a wall thickness of 40 ⁇ m.
  • the fluorescent substance composite glass obtained in this manner was irradiated with blue light from behind the fluorescent substance glass, to obtain white transmitted light. Also, the fluorescent substance composite glass was subjected to tests to measure energy conversion efficiency and porosity, to find that the energy conversion efficiency was 13% and the porosity was 2%.
  • Glass raw materials made of various oxides were compounded in such a manner as to obtain a composition containing 35% of ZnO, 40% of B 2 O 3 , 10% of SiO 2 , 10% of Na 2 O and 5% of Al 2 O 3 based on mass percentage. After these components were uniformly mixed, the mixture was put in a platinum crucible and melted at 1100° C. for 2 hours to obtain uniform glass. This glass was crushed using alumina balls and classified to obtain a glass powder having an average particle diameter of 2.5 ⁇ m.
  • an inorganic fluorescent substance powder (YAG fluorescent substance powder, manufactured by KASEI OPTONIX, LTD., average particle diameter: 8 ⁇ m) was added to the produced glass powder in a mass ratio of 95:5 and these components were mixed to produce a mixture powder. Then, 30% by mass of a methacrylic acid resin as a binder, 3% by mass of dibutyl phthalate as a plasticizer and 20% by mass of toluene as a solvent were added to 100 of the produced mixture powder and these components were mixed to make a slurry. In succession, the above slurry was molded into a sheet on a PET film by a doctor blade method and dried to obtain a fluorescent substance composite glass green sheet 50 ⁇ m in thickness.
  • YAG fluorescent substance powder manufactured by KASEI OPTONIX, LTD., average particle diameter: 8 ⁇ m
  • the manufactured fluorescent substance composite glass green sheet was used to manufacture a fluorescent substance composite glass having a size of 100 ⁇ 100 mm and a wall thickness of 40 ⁇ m, in the same manner as in Example 1.
  • the baking temperature the baking was carried out at 600° C.
  • the fluorescent substance composite glass obtained was irradiated with blue light from behind the fluorescent substance glass, to obtain white transmitted light.
  • the fluorescent substance composite glass was subjected to tests to measure energy conversion efficiency and porosity, to find that the energy conversion efficiency was 17% and the porosity was 1%.
  • the energy conversion efficiency was found by using a spectrophotometer to measure the energy (a) of a light source, the energy (b) of light having the same wavelength as the light source transmitted through the fluorescent substance composite glass and the energy (c) of light converted by the wavelength of the light source in the fluorescent substance composite glass and by calculating from the equation: c/(a ⁇ b) ⁇ 100(%).
  • the porosity was found by using the Archimedes' method to measure an actual density and a theoretical density and by calculating from the equation: (1 ⁇ actual density/theoretical density) ⁇ 100(%).

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US20080180018A1 (en) * 2006-11-01 2008-07-31 Nec Lighting, Ltd. Fluorescent substance containing glass sheet, method for manufacturing the glass sheet and light-emitting device
US20100102344A1 (en) * 2007-03-01 2010-04-29 Yoshinori Ueji Led device and illuminating apparatus
US9950949B2 (en) * 2008-04-29 2018-04-24 Schott Ag Conversion material, particularly for a white or colored light souce comprising a semiconductor light source, a method for the production thereof, as well as a light source comprising said conversion material
US20120057337A1 (en) * 2008-04-29 2012-03-08 Rainer Liebald Conversion material, particularly for a white or colored light souce comprising a semiconductor light source, a method for the production thereof, as well as a light source comprising said conversion material
US10988408B2 (en) 2008-04-29 2021-04-27 Schott Ag Conversion material for white or colored light source, method of production, and light source having the conversion material
US8541805B2 (en) 2010-05-13 2013-09-24 Panasonic Corporation Mounting substrate and manufacturing method thereof, light-emitting module and illumination device
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US11901494B2 (en) 2010-06-21 2024-02-13 Micron Technology, Inc. Packaged LEDs with phosphor films, and associated systems and methods
US11081625B2 (en) 2010-06-21 2021-08-03 Micron Technology, Inc. Packaged LEDs with phosphor films, and associated systems and methods
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
US20120107622A1 (en) * 2010-10-28 2012-05-03 Nicholas Francis Borrelli Phosphor containing glass frit materials for led lighting applications
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US9428686B2 (en) * 2011-12-01 2016-08-30 Arthur Shiao Photo-luminescence coating and application thereof
US20130337242A1 (en) * 2011-12-01 2013-12-19 Arthur Shiao Photo-luminescence coating and application thereof
US20190010079A1 (en) * 2017-07-04 2019-01-10 Platinum Optics Technology (suzhou) Inc. Fluorescent Glass For Light Emitting Diode And Manufacturing Method Thereof
US11999648B2 (en) 2018-04-25 2024-06-04 Nippon Electric Glass Co., Ltd. Wavelength conversion member and light emitting device using same
US11530798B2 (en) 2019-04-18 2022-12-20 Nippon Electric Glass Co., Ltd. Wavelength conversion member, method for manufacturing same, and light emission device

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WO2006120827A1 (ja) 2006-11-16
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