WO2009154193A1 - Composition céramique, céramique de phosphore et son procédé de production, et dispositif électroluminescent - Google Patents

Composition céramique, céramique de phosphore et son procédé de production, et dispositif électroluminescent Download PDF

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WO2009154193A1
WO2009154193A1 PCT/JP2009/060928 JP2009060928W WO2009154193A1 WO 2009154193 A1 WO2009154193 A1 WO 2009154193A1 JP 2009060928 W JP2009060928 W JP 2009060928W WO 2009154193 A1 WO2009154193 A1 WO 2009154193A1
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phosphor
powder
ceramic
base material
light
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Japanese (ja)
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均 石沢
嘉信 江面
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株式会社ニコン
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides or oxide-forming salts thereof
    • 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
    • H01L33/502—Wavelength conversion materials

Definitions

  • the present invention relates to a ceramic composition, a phosphor ceramic, a method for producing the same, and a light emitting device.
  • White illumination using light emitting diodes has many advantages such as low power consumption and long life, and does not contain harmful mercury vapor like fluorescent lamps. Expected. In recent years, as white illumination using LEDs, illumination using a blue LED as an excitation light source to excite a yellow phosphor and emit white light is becoming mainstream. In such white illumination, a blue LED having an emission wavelength of 450 to 470 nm is used as an excitation light source, and YAG: Ce (YAG (Y 3 Al 5 O 12 ) doped with Ce 3+ ) is excited as a yellow phosphor. Then, white light is emitted by a combination of yellow light obtained by wavelength conversion of excitation light and blue light as excitation light. Since YAG: Ce phosphor has extremely high luminous efficiency, it can emit white light with high illuminance.
  • a structure of such white illumination for example, a structure in which a resin in which YAG: Ce phosphor particles are dispersed is applied on a blue LED and the blue LED is sealed with this resin is considered.
  • a light emitting element emitting blue light is disposed in a recess provided in a base, and at least a part of the light emitting element is covered with a translucent resin containing a YAG: Ce phosphor. (Patent Document 1).
  • Patent Document 2 discloses a translucent polycrystalline ceramic structure formed from alumina and a YAG: Ce phosphor (Patent Document 2).
  • the present invention has been made in view of such circumstances, and when combined with a light emitter such as an LED, can exhibit excellent heat resistance, can uniformly convert the wavelength of excitation light, Moreover, an object is to provide a phosphor ceramic capable of obtaining a high illuminance. Another object of the present invention is to provide a method for producing such phosphor ceramics, a ceramic composition that is a raw material of the phosphor ceramics, and a light emitting device using the phosphor ceramics.
  • the phosphor ceramic of the present invention contains a base material and phosphor particles dispersed in the base material, and the base material is any one of calcium fluoride, strontium fluoride, and lanthanum fluoride. Or made of calcium fluoride and strontium fluoride, and the phosphor particles are made of YAG: Ce.
  • the ratio of the phosphor particles to the base material is preferably 0.1 to 10% by mass.
  • the phosphor ceramic manufacturing method of the present invention is a phosphor comprising a sintered body in which a ceramic composition containing a raw material powder of a base material and phosphor particles is fired, and the phosphor particles are dispersed in the base material.
  • a raw material powder of the base material is any one of calcium fluoride powder, strontium fluoride powder and lanthanum fluoride powder, or calcium fluoride powder and strontium fluoride. It is a mixed powder made of powder, and the phosphor particles are particles made of YAG: Ce.
  • the method for producing the phosphor ceramic of the present invention it is preferable to further include a step of heating the sintered body while applying pressure.
  • the ceramic composition of the present invention is a ceramic composition containing ceramic powder and phosphor particles, and the ceramic powder is any one of calcium fluoride powder, strontium fluoride powder, and lanthanum fluoride powder. Or a mixed powder composed of calcium fluoride powder and strontium fluoride powder, and the phosphor particles are particles composed of YAG: Ce.
  • the light emitting device of the present invention includes a light emitter and a phosphor layer made of the phosphor ceramic of the present invention disposed on at least one side of the light emitter.
  • the phosphor ceramics of the present invention when combined with a light emitter such as an LED, excellent heat resistance can be exhibited, the wavelength of excitation light can be uniformly converted, and high illuminance can be obtained. Is also possible.
  • a production method suitable for producing the phosphor ceramic of the present invention, a ceramic composition suitably used for the production method, and the phosphor ceramic of the present invention are used. Therefore, it is possible to provide a light-emitting element that can perform uniform wavelength conversion, can obtain high illuminance, and is unlikely to cause reduction in illuminance due to heat.
  • FIG. 2 is a diagram showing a TEM photograph of CaF 2 produced in Example 1.
  • FIG. 2 is a view showing an SEM photograph of the phosphor ceramic soot produced in Example 1.
  • FIG. It is a figure which shows xy chromaticity coordinate obtained with the light emitting element using the fluorescent substance ceramic of each Example.
  • the phosphor ceramic of the present invention contains a base material and phosphor particles dispersed in the base material, and the phosphor particles are made of YAG: Ce.
  • the base material may be any one of calcium fluoride, strontium fluoride, and lanthanum fluoride. Alternatively, the base material may be made of calcium fluoride and strontium fluoride.
  • the ratio of the phosphor particles to the base material is preferably 0.1 to 10% by mass.
  • the phosphor particles contained in the phosphor ceramic may have an average particle diameter of 1 to 20 ⁇ m. More preferably, the average particle size may be 5 to 10 ⁇ m.
  • the phosphor ceramics may have a structure in which YAG: Ce particles are dispersed between and within the crystal grains of the polycrystal formed by the base material.
  • the method for producing phosphor ceramics of the present invention comprises firing a ceramic composition containing a raw material powder of a base material and phosphor particles, and forming a phosphor ceramic comprising a sintered body in which the phosphor particles are dispersed in the base material.
  • the raw material powder of the base material may be one kind of powder selected from calcium fluoride powder, strontium fluoride powder and lanthanum fluoride powder, or a mixed powder consisting of calcium fluoride powder and strontium fluoride powder.
  • the phosphor particles are preferably particles made of YAG: Ce.
  • the ceramic composition may be fired at 700 to 1200 ° C.
  • a step of heating the sintered body while applying pressure may be further included.
  • the step of pressing while sintering may be performed in an inert atmosphere.
  • the light emitting device of the present invention includes a light emitter and a phosphor layer made of the phosphor ceramic of the present invention disposed on at least one side of the light emitter.
  • the light emitter of the light emitting element can be appropriately selected from a semiconductor light emitting diode, an organic EL element and the like.
  • FIG. 1 is a diagram schematically showing a cross-sectional configuration of a light-emitting element according to an embodiment of the present invention.
  • the light emitting element 10 shown in FIG. 1 has a configuration in which a phosphor layer 3 is provided on a light emitting diode (LED 4) that is a light emitter.
  • the phosphor layer 3 is composed of a base material 1 and phosphor particles 2 uniformly dispersed in the base material 1.
  • the type of the LED 4 is not particularly limited. In the following embodiment, an example using a blue LED having an emission wavelength of 450 to 470 nm will be described.
  • the blue light emitted from the LED 4 (arrow B in the figure) excites the phosphor particles 2 contained in the phosphor layer 3 as excitation light, and the wavelength of the excitation light converted thereby.
  • Yellow light emission of about 450 to 700 nm (center wavelength 530 nm) occurs.
  • white light emission (W arrow in the figure) is obtained by blue light emission that is excitation light transmitted through the phosphor layer 3 and yellow light emission generated by wavelength conversion of the excitation light.
  • the phosphor layer 3 is provided on the side where the light emitted from the LED 4 is extracted with respect to the LED 4. Further, the phosphor layer 3 is disposed so as to cover at least the entire surface of the LED 4 on the light emission extraction side in order to cause the entire wavelength conversion of light emission from the LED 4.
  • the phosphor layer 3 is bonded to the LED 4 using, for example, an adhesive (not shown).
  • the base material 1 constituting the phosphor layer 3 is composed of only one of calcium fluoride (CaF 2 ), strontium fluoride (SrF 2 ), and lanthanum fluoride (LaF 3 ) It consists of calcium and strontium fluoride. More specifically, it consists of a sintered body of calcium fluoride, a sintered body of strontium fluoride, a sintered body of lanthanum fluoride, or a mixed sintered body of calcium fluoride and strontium fluoride. In general, a substance having a crystal structure other than cubic does not have crystal orientation matching at the grain boundaries inside the polycrystalline ceramic, so that the sintered body is not transparent. Since alumina is hexagonal, it is not transparent but only translucent.
  • the phosphor particles 2 are particles made of YAG: Ce.
  • YAG: Ce is YAG (Yttrium-Aluminum-Garnet: Yttrium-aluminum oxide having a garnet structure (Y 3 Al 5 O 12 or the like)) doped with Ce 3+ .
  • YAG: Ce may be one in which part of yttrium (Y) is replaced by gadolinium (Gd).
  • the YAG: Ce particles are contained in the form of YAG: Ce particles added at the time of manufacture without causing a reaction with the base material or the like.
  • YAG in YAG: Ce does not change due to reaction with the base material or the like, and Ce 3+ remains unchanged without changing the valence of Ce.
  • the size of the phosphor particles 2 contained in the phosphor layer 3 is preferably 1 to 20 ⁇ m, more preferably 5 to 10 ⁇ m, in terms of average particle diameter. If the phosphor particles 2 are too large, the excitation light from the LED 4 is hindered and the illuminance becomes insufficient, and the phosphor particles 2 are not uniformly dispersed in the base material 1 and may cause uneven emission colors. On the other hand, if the phosphor particles 2 are too small, the excitation light is not sufficiently scattered by the phosphor particles 2, so that the ratio of the excitation light that passes through the phosphor layer 3 increases, resulting in a bluish white light as a whole. is there.
  • the thickness of the phosphor layer 3 is preferably 0.1 to 10 mm, and more preferably 0.5 to 3 mm.
  • the content ratio of the phosphor particles 2 in the phosphor layer 3 is preferably such that the content of the phosphor particles 2 with respect to the base material 1 is 0.1 to 10% by mass, and preferably 0.5 to 5% by mass. And more preferred. If the amount of the phosphor particles 2 is below this lower limit value, the wavelength conversion in the phosphor layer 3 due to the excitation light from the LED 4 does not occur sufficiently, and the desired emission color may not be obtained. On the other hand, if the amount of the phosphor particles 2 exceeds the above upper limit value, the phosphor layer 3 becomes difficult to function as a phosphor, and a desired emission color cannot be obtained. It may become.
  • the thickness of the phosphor layer 3 and the content ratio of the phosphor particles 2 described above are appropriately set according to conditions such as the intensity of light emitted by the LED 4. If the phosphor layer 3 is too thick or the phosphor particles 2 are too thick with respect to the intensity of light emitted by the LED 4, the light transmittance tends to decrease and sufficient illuminance cannot be obtained. On the other hand, if the phosphor layer 3 is too thin or the phosphor particles 2 are too few, sufficient wavelength conversion does not occur and it is difficult to obtain a desired emission color.
  • the amount of the phosphor particles 2 is 0.1 to 10% by mass with respect to the base material 1. Preferably, it is 0.3 to 10% by mass.
  • the amount of the phosphor particles 2 is preferably 0.1 to 1% by mass with respect to the base material 1, and preferably 0.1 to 0.3. More preferably, it is mass%. If these conditions are satisfied, the blue light emission in which the excitation light from the LED 4 is transmitted through the phosphor layer 3 and the yellow light emission generated by wavelength conversion of the excitation light by the phosphor particles 2 are generated in a well-balanced manner. Can be obtained with high illuminance.
  • the phosphor ceramic constituting the phosphor layer 3 can be manufactured as follows. That is, first, calcium fluoride powder, strontium fluoride powder, and lanthanum fluoride powder, which are raw material powders of the base material 1, are prepared, and any one of these powders or calcium fluoride powder and strontium fluoride powder Are mixed with phosphor particles 2 (phosphor particle powder) made of YAG: Ce to prepare a ceramic composition as a raw material of the phosphor layer 3.
  • calcium fluoride powder is prepared by adding water to calcium acetate hydrate to dissolve it, mixing it with hydrofluoric acid aqueous solution obtained by adding water to hydrofluoric acid (hydrofluoric acid), and stirring the mixture. It can be obtained by generating calcium fluoride by the reaction of calcium and hydrofluoric acid, and breaking and pulverizing particles in which the calcium fluoride is aggregated. At this time, it is preferable that the crystal of calcium fluoride generated by the reaction between calcium acetate and hydrofluoric acid is further heated to a temperature of 120 ° C. or higher and 180 ° C. or lower to be sufficiently crystallized.
  • strontium fluoride powder and lanthanum fluoride powder can be similarly obtained by using strontium acetate or lanthanum acetate, respectively, instead of calcium acetate.
  • the raw material powder of the base material 1 and the phosphor particles 2 may be mixed using either dry mixing or wet mixing. From the viewpoint of enabling more uniform mixing, it is preferably performed by wet mixing in a solvent. Specifically, the raw material powder of the base material 1 and the phosphor particles 2 are appropriately weighed, and a solvent such as water or an organic solvent is added thereto to form a slurry, which is mixed by applying the slurry to a powder mixing device. It can be carried out.
  • a powder mixing device a ball mill, a bead mill, a jet mill, a high-speed stirrer, or the like can be applied without particular limitation.
  • the mixing ratio of the raw material powder of the base material 1 and the phosphor particles 2 is preferably the same as the ratio of the base material 1 and the phosphor particles 2 in the phosphor layer 3 described above.
  • the amount ratio of the raw materials does not change due to firing described later. Therefore, the mixing ratio of the raw material powder of the base material 1 and the phosphor particles 2 becomes the ratio of the base material 1 and the phosphor particles 2 almost as it is.
  • the mixing ratio thereof may be the same as the suitable ratio in the base material 1 described above.
  • a ceramic composition obtained by mixing the raw material powder of the base material 1 and the phosphor particles 2 is formed into a formed body.
  • the shape of the obtained molded body is preferably matched with the desired shape of the phosphor layer 3, and can be a plate shape or a hemispherical shape.
  • the molding method of the ceramic composition include a uniaxial pressure molding method or an isotropic pressure molding method as a dry method, and a mud casting method (slip casting), an injection molding method, a plastic molding method and the like as a wet method. It is done. Since the ceramic composition obtained by the above-described method has very high sinterability, it is not always necessary to pressurize the ceramic composition. Therefore, any known forming method can be applied, including a mud casting method that does not have a pressing step.
  • the obtained molded body is fired to obtain a sintered body which is a phosphor ceramic (firing step).
  • the fluorescent material is incorporated into the base material 1 made of a sintered body of calcium fluoride, a sintered body of strontium fluoride, a sintered body of lanthanum fluoride, or a mixed sintered body of calcium fluoride and strontium fluoride.
  • a phosphor ceramic in which the body particles 2 are dispersed is obtained.
  • the suitable conditions for the process from firing the ceramic composition to obtaining the phosphor ceramic vary depending on the type of raw material powder of the base material 1 as follows.
  • the firing is performed in the air, preferably 700 to 1000 ° C., more preferably 750 to 900 ° C., preferably 10 minutes to 3 hours, more preferably It is preferably carried out under conditions of 30 minutes to 1 hour.
  • the above-described baking alone still does not provide sufficient transparency of the calcium fluoride constituting the base material 1, and light emission occurs when the light-emitting element 10 is used. It may not be obtained with sufficient strength. Therefore, in this case, in order to further improve the transparency of the base material 1 made of calcium fluoride, a step of performing heating treatment while applying pressure to the sintered body obtained after the firing step is performed (additional processing). Pressure heating step). By performing such treatment, the base material 1 having higher transparency can be obtained by, for example, extruding closed pores in the calcium fluoride that have been inevitably formed in the state of the sintered body. It becomes like this.
  • This pressure heat treatment is preferably a treatment generally called a hot isostatic pressure heat treatment (HIP).
  • Suitable conditions for such treatment include, for example, conditions in which the sintered body is heated to 700 to 1200 ° C. while applying a pressure of 500 to 2000 kg / cm 2 in an inert atmosphere such as argon.
  • YAG Ce constituting the phosphor particles 2 heated together with the raw material powder of the base material 1 is deactivated. It was extremely difficult to form the phosphor layer 3 having a sufficient amount.
  • the deactivation of YAG: Ce means that YAG: Ce has effective fluorescence characteristics due to a change in the composition of YAG or a change in the valence of Ce doped in YAG. It means not to do.
  • the phosphor layer 3 having sufficient wavelength conversion ability can be formed without deactivating YAG: Ce even when firing is performed at the temperature described above.
  • the firing and the pressure heating treatment can be performed without deactivation of YAG: Ce even at the above-described high temperature, it is possible to form the base material 1 that is dense and highly transparent. .
  • a mixed powder of calcium fluoride powder and strontium fluoride powder is used as the raw material powder of the base material 1, firing is preferably performed in the air at 700 to 1000 ° C., more preferably 750 to 900 ° C., preferably Is preferably carried out under conditions of 10 minutes to 1 hour, more preferably 30 minutes to 1 hour.
  • the present inventors can obtain a sufficiently transparent sintered body even when firing at a lower temperature than in the case of calcium fluoride alone. I found out that Therefore, when a mixed powder of calcium fluoride powder and strontium fluoride powder is used, the sufficiently transparent base material 1 can be formed even by firing in the temperature range as described above. And, since sufficient transparency can be obtained only by firing, the pressure heating step as in the case of using only calcium fluoride powder can be omitted, productivity can be greatly enhanced, and the manufacturing cost can be greatly increased. It is also possible to reduce it.
  • the ratio of the strontium fluoride powder in the mixed powder is preferably 10 mol% or more, and more preferably 30 to 50 mol%.
  • Fluorescent ceramics can be obtained from the ceramic composition as a raw material by such a firing process or pressure heating process.
  • YAG: Ce constituting the phosphor particles 2 is well stabilized by calcium fluoride, strontium fluoride, or lanthanum fluoride contained in the base material 1.
  • the deactivation of YAG: Ce is very difficult to occur, and the emission intensity tends to increase.
  • the rate of change in the intensity of light emitted by YAG: Ce measured in the state of the phosphor ceramic with respect to the intensity of light emitted by YAG: Ce measured in the state of the ceramic composition as the raw material is preferably 70. It is possible to be in the range of -180%, more preferably in the range of 100-200%.
  • the phosphor ceramic is processed into a desired shape as necessary. Then, the phosphor ceramic obtained after processing is arranged on the side from which light emission is extracted with respect to the LED 4, and the phosphor layer 3 is formed on the LED 4. At this time, the phosphor ceramic may be adhered to the LED 4 using an adhesive or the like, may be simply pressed, or may be integrated using a predetermined member. Thus, the light emitting element 10 having the structure shown in FIG. 1 is obtained.
  • the base material 1 of the phosphor layer 3 is made of any one of calcium fluoride, strontium fluoride, and lanthanum fluoride, or made of calcium fluoride and strontium fluoride.
  • the base material 1 of the phosphor layer 3 is made of any one of calcium fluoride, strontium fluoride, and lanthanum fluoride, or made of calcium fluoride and strontium fluoride.
  • the base material is made of resin
  • a metal having good thermal conductivity such as aluminum has been used as a heat sink, but in that case, a sufficient area of the heat sink is required for one LED, so the entire LED It was extremely difficult to reduce the size.
  • the base material is resin
  • sufficient power cannot be input to avoid deterioration of the resin, and as a result, there is a tendency that only dark LED illumination with low illuminance is obtained.
  • the base material 1 is hardly deteriorated, it is not necessary to take a heat dissipation measure as much as that of the resin, so that it is easy to downsize and sufficient power can be supplied. Since it becomes possible, high illuminance can also be obtained. Therefore, when such a light emitting element 10 is used, for example, a large number of LEDs can be integrated in a narrow area, and the illuminance per LED can be improved, so that compact and bright illumination can be realized. .
  • the base material 1 is made of calcium fluoride, strontium fluoride or lanthanum fluoride, the transparency of the base material 1 itself is extremely high. Therefore, the excitation light from the LED 4 and the light emitted by the phosphor particles 2 can be sufficiently transmitted through the phosphor layer 3, thereby obtaining a high illuminance.
  • the base material 1 is composed of the ceramics as described above, in the manufacturing process, the raw material powder of the base material 1 and the phosphor particles 2 can be mixed in powder form and fired as they are,
  • the obtained phosphor layer 3 (phosphor ceramic) is obtained by uniformly dispersing the phosphor particles 2 in the base material 1. Therefore, in the phosphor layer 3, the wavelength conversion of the excitation light from the LED 4 by the phosphor particles 2 can be caused uniformly, and as a result, white light can be emitted uniformly.
  • the base material 1 contains calcium fluoride, strontium fluoride, and lanthanum fluoride, YAG: Ce is stabilized even at high temperature conditions in the firing step and pressure heating step in the manufacturing method as described above. The deactivation is extremely difficult to occur. Therefore, the obtained phosphor layer 3 is in a state in which the base material 1 has excellent transparency by high-temperature treatment and maintains a high activity of YAG: Ce, and can realize high illuminance and good white light emission. .
  • the phosphor ceramic, the light-emitting element, and the manufacturing method thereof according to the present invention are not necessarily limited to the above-described embodiment, and can be appropriately changed without departing from the gist thereof.
  • the light-emitting element 10 described above includes the LED 4 that is a blue LED as a light emitter.
  • the light emitter is not limited to a blue LED, and other than LEDs that can obtain other light emission colors or EL.
  • the light emitters may be applied.
  • the phosphor layer 3 made of the phosphor ceramic of the present invention uniform and good wavelength conversion can be produced, and high heat resistance and high illuminance can be obtained.
  • a light emitting element having the same can be obtained.
  • a blue LED is particularly suitable as the light emitter.
  • the structure of the light emitting element 10 is not limited to the structure of the above-described embodiment, and it is sufficient that a phosphor layer made of phosphor ceramics is disposed at least on the side of taking out light emitted by the light emitter.
  • a phosphor layer made of phosphor ceramics is disposed at least on the side of taking out light emitted by the light emitter.
  • another transparent layer may be provided between the LED 4 and the phosphor layer 3, and a transparent protective layer or the like is provided on the surface of the phosphor layer 3. It may be.
  • Example 1 Distilled water was added to the calcium acetate hydrate and dissolved completely to prepare an aqueous calcium acetate solution. Further, a hydrofluoric acid aqueous solution was prepared by adding distilled water to hydrofluoric acid (hydrofluoric acid) having a concentration of 50%. Next, the aqueous hydrofluoric acid solution was slowly poured into the calcium acetate aqueous solution while stirring the bladed stirring bar at 300 rpm. At this time, an injection port was attached to the side surface of the plastic beaker containing the calcium acetate aqueous solution, and from here, the hydrofluoric acid aqueous solution sucked out by the roller tube pump was injected over 1 hour. The molar ratio of hydrofluoric acid / calcium acetate was set to 4.
  • the obtained slurry of CaF 2 was dried at 100 ° C. to obtain a powder.
  • YAG: Ce particle powder (Sylvania, P-46) was added with various changes between 0.5 and 2.0% by weight, and ethanol was added to form a liquid slurry. This was wet mixed well in an agate mortar. The mixed slurry was dried again to prepare a ceramic composition, and 6 g of the powder was uniaxially press-molded using a mold having a diameter of 30 mm, and various amounts of CaF 2 powder were used. A molded body was obtained.
  • each of the obtained compacts was fired in air at 800 ° C. for 1 hour to obtain a slightly yellowish sintered body.
  • heat is applied to these sintered bodies at 1100 ° C. for 2 hours while applying an isotropic pressure of 1500 kg / cm 2 in an argon atmosphere using a Kobe Steel HIP device (Dr. HIP).
  • An isostatic heat treatment (HIP treatment) was performed to obtain a phosphor ceramic.
  • Example 2 Preparation of ceramic composition, molding, firing (800 ° C., 1 hour) and strontium fluoride (SrF 2 ) powder using strontium acetate instead of calcium acetate in the same manner as in Example 1.
  • HIP treatment (1500 kg / cm 2 , 1100 ° C., 2 hours) was sequentially performed to produce phosphor ceramics.
  • YAG the addition amount of Ce particles was 1 wt% relative to the SrF 2 powder.
  • Example 3 Preparation of ceramic composition, forming, firing (800 ° C., 1 hour), and in the same manner as in Example 1 except that lanthanum fluoride (LaF 3 ) powder was produced using lanthanum acetate instead of calcium acetate, and HIP treatment (1500 kg / cm 2 , 1100 ° C., 2 hours) was sequentially performed to produce phosphor ceramics.
  • YAG the addition amount of Ce particles was 1 wt% with respect to LaF 3 powder.
  • Example 4 The CaF 2 powder obtained in Example 1 and the SrF 2 powder obtained in Example 2 were mixed so that CaF 2 was 70 mol% and SrF 2 was 30 mol% to obtain a mixed powder.
  • the obtained mixed powder was used in place of CaF 2 powder, and the ceramic composition was prepared and formed in the same manner as in Example 1. Thereafter, the obtained molded body was fired in air at 800 ° C. for 1 hour to produce a phosphor ceramic made of a sintered body.
  • the addition amount of YAG: Ce particle powder was 1 weight% with respect to mixed powder.
  • the spectral fluorescence characteristics of the ceramic composition which is a raw material before sintering these phosphor ceramics, were measured in the same manner. Furthermore, as a comparison test, the spectral fluorescence characteristics before and after heating only the YAG: Ce phosphor in air at 1100 ° C. were also measured. In addition, the said measurement was performed using what added 1 weight% of YAG: Ce particle powder as fluorescent substance ceramic of Example 1.
  • the phosphor ceramics of Examples 1 to 4 and the YAG: Ce phosphor of the comparison test were pre-sintered (the state of the ceramic composition in Examples 1 to 4) and sintered. Later, yellow emission intensity (based on an arbitrary scale) of 450 to 700 nm (center wavelength 530 nm) emitted by blue excitation light of 470 nm was obtained. The obtained results are shown in Table 1.
  • the phosphor ceramics of Examples 1 to 4 showed higher emission intensity after sintering than before sintering (ceramic composition).
  • the emission intensity after heating at 1100 ° C. was low. From this, it was found that when YAG: Ce powder was contained in the fluoride as in Examples 1 to 4, the emission intensity did not decrease, but rather increased, even at high temperatures during sintering.
  • each phosphor ceramic obtained in Examples 1 to 4 was processed into a plate having a thickness of 1 mm, and its translucency was confirmed. As a result, each phosphor ceramic obtained in Examples 1 to 4 had translucency. In particular, the phosphor ceramic of Example 4 had high translucency even though the HIP treatment was not performed. When various phosphor ceramics having different concentrations of the YAG: Ce particle powder produced in Example 1 were compared, it was confirmed that the smaller the amount of YAG: Ce particle powder, the higher the translucency.
  • the phosphor ceramics of Examples 1 to 4 were each processed into a diameter of 5 mm and a thickness of 1 mm, and these were transparently bonded onto a blue LED (manufactured by Mitsubishi Electric OSRAM, OS-DP3-B1, main wavelength 470 nm).
  • Various light emitting elements were manufactured by pasting with an agent.
  • FIG. 4 is a diagram showing xy chromaticity coordinates obtained with various light-emitting elements obtained using the phosphor ceramics of Examples 1 to 4.
  • FIG. 4 also shows the results of using various phosphor ceramics having different concentrations of YAG: Ce particle powder in Example 1.
  • the light-emitting element obtained using the phosphor ceramic of Example 1 was confirmed to obtain almost white light emission, but the measured chromaticity was from blue corresponding to the amount of YAG: Ce particle powder. It changed continuously to yellow.
  • the light emitting element using the phosphor ceramic of Example 1 in which the amount of YAG: Ce particle powder is 0.9 to 1.2% by weight can obtain a chromaticity located almost at the center of coordinates, and color rendering. It was confirmed to be a white light source with excellent properties.
  • each light-emitting element obtained using the phosphor ceramic of Example 2, 3 or 4 has a chromaticity located almost at the center of the xy chromaticity coordinates, and is confirmed to be a white light source excellent in color rendering. It was done.
  • FIG. 5 is a diagram showing the total luminous flux spectrum obtained by measuring the total luminous flux of each light emitting element.
  • Example 1 the results obtained with a light emitting device using phosphor ceramics with an amount of YAG: Ce particle powder of 1% by weight are shown. From these results, white light was obtained by synthesizing the blue light of the excitation light and the yellow light of the phosphor particles by any of the light emitting elements obtained using the phosphor ceramics of Examples 1 to 4. It was confirmed that
  • Table 2 shows the results of illuminance and quantum efficiency obtained with each light-emitting element.
  • Table 2 for the light emitting device using the phosphor ceramic of Example 1, each result when the amount of YAG: Ce particle powder is changed between 1.0 and 2.0% by weight is shown.
  • the phosphor ceramic of Example 1 or 4 was processed into a phosphor of 5 mm in diameter and 1 mm in thickness, respectively.
  • 1 wt% of YAG: Ce particle powder was used as the phosphor ceramic of Example 1.
  • 2 wt% of YAG: Ce particle powder is added to a hydrogenated epoxy resin (manufactured by Japan Epoxy Resin, YX8000), dispersed therein, and thermally cured at 100 ° C. And what processed this into the plate shape of thickness 1mm and diameter 5mm was prepared.
  • a phosphor ceramic that exhibits excellent heat resistance and can withstand long-term use can be provided.
  • the light-emitting element using this phosphor ceramic can uniformly convert the wavelength of excitation light, and can obtain high illuminance. Further, since the illuminance is not easily lowered by heat and the light emitter and the phosphor can be separated, the performance of the light emitting element can be maintained at a low cost over a long period of time.

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Abstract

L’invention concerne une céramique de phosphore contenant une matrice et des particules de phosphore dispersées dans la matrice. La céramique de phosphore est caractérisée en ce que la matrice est composée de fluorure de calcium, de fluorure de strontium ou de fluorure de lanthane ou, en variante, de fluorure de calcium et de fluorure de strontium. La céramique de phosphore est également caractérisée en ce que les particules de phosphore sont composées de YAG:Ce.
PCT/JP2009/060928 2008-06-16 2009-06-16 Composition céramique, céramique de phosphore et son procédé de production, et dispositif électroluminescent WO2009154193A1 (fr)

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