WO2010053197A1 - Céramique poreuse au phosphore accumulant la lumière - Google Patents

Céramique poreuse au phosphore accumulant la lumière Download PDF

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Publication number
WO2010053197A1
WO2010053197A1 PCT/JP2009/069123 JP2009069123W WO2010053197A1 WO 2010053197 A1 WO2010053197 A1 WO 2010053197A1 JP 2009069123 W JP2009069123 W JP 2009069123W WO 2010053197 A1 WO2010053197 A1 WO 2010053197A1
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phosphorescent phosphor
phosphorescent
porous
volume
ceramic
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PCT/JP2009/069123
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English (en)
Japanese (ja)
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木村裕司
高井康
川添博文
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信越化学工業株式会社
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Priority to JP2010536820A priority Critical patent/JP5551079B2/ja
Publication of WO2010053197A1 publication Critical patent/WO2010053197A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7792—Aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
    • C09K11/582—Chalcogenides
    • C09K11/584—Chalcogenides with zinc or cadmium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
    • C09K11/7407—Chalcogenides
    • C09K11/7421—Chalcogenides with alkaline earth metals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7784—Chalcogenides
    • C09K11/7787—Oxides
    • C09K11/7789—Oxysulfides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/80—Optical properties, e.g. transparency or reflexibility
    • C04B2111/807—Luminescent or fluorescent materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/449—Organic acids, e.g. EDTA, citrate, acetate, oxalate

Definitions

  • the present invention relates to porous phosphorescent phosphor ceramics that can be used for evacuation route display boards, auxiliary lighting, signs, tiles, and the like, and a method for manufacturing the same.
  • Phosphorescent phosphors are usually sold as powders, and it is common to produce molded bodies and display boards by kneading them into transparent resins or dispersing them in paints (for example, Patent Documents 1 and 2). Etc.).
  • Patent Documents 5 and 6 JP-A-8-129351 JP-A-9-146482 JP 2000-319832 A JP-A-10-101371 JP-A-2005-105116, paragraph 0017, etc. JP-A-11-181420, paragraphs 0004, 0010, etc.
  • An object of the present invention is to obtain a ceramic sintered body having a high afterglow luminance that can effectively utilize a phosphor in a deep part in view of the above-described present situation.
  • the present invention is a ceramic containing a phosphorescent phosphor, preferably a ceramic consisting essentially of a phosphorescent phosphor, and the structure thereof is a porous body.
  • the afterglow luminance was several times that of the conventional product, and that fluorescence was emitted to the deep part of the sintered body, resulting in the present invention.
  • the gist of the present invention is a product comprising a ceramic containing a phosphorescent phosphor, preferably a ceramic consisting essentially of phosphorescent phosphor, and having a porous structure, and a method for producing the same.
  • the porous phosphorescent ceramic according to the present invention includes a phosphorescent phosphor, and preferably consists essentially of a phosphorescent phosphor, and has a porosity of 20% by volume or more and less than 80% by volume.
  • the method for producing a porous phosphorescent phosphor ceramic according to the present invention comprises granulating, forming, and reaction sintering a raw material mixture of phosphorescent phosphors.
  • the method for producing porous phosphorescent phosphor ceramics according to the present invention comprises granulating, molding and reaction sintering the phosphorescent phosphor.
  • a ceramic containing a phosphorescent phosphor preferably a ceramic consisting essentially of a phosphorescent phosphor, and having a porous structure, it exhibits an afterglow luminance several times that of a conventional phosphorescent product. Products can be obtained and their utility value is extremely high.
  • the phosphorescent phosphor as referred to in the present invention is a commercially available product that uses zinc sulfide or an alkaline earth metal aluminate as a crystal matrix, but has a long afterglow that can be made into ceramics containing phosphorescent phosphors by sintering. Long-lasting phosphors that can be applied to any ceramic and can be made into a ceramic consisting essentially of phosphorescent phosphors by sintering can be suitably used.
  • Essentially composed of phosphorescent phosphor means that in addition to the phosphorescent phosphor composition component, it may contain a flux component that is a reaction accelerator that may be added in a small amount during phosphor synthesis. It means that. Hereinafter, the same meaning is also expressed when expressing “innocent”.
  • the phosphorescent substance substantially contains 80 to 100 mol%, preferably 90 to 100 mol% of the phosphor component in the composition.
  • M is at least one element of Sr, Ca, Ba, and Mg, and MAl 2 O 4 : Eu, Dy, M 4 Al 14 O 25 : Eu, Dy, Sr 3 MgSi 2.
  • the porosity of the porous phosphorescent phosphor ceramic according to the present invention is preferably 20% or more and less than 80%. If it is less than 20%, the improvement in afterglow strength is insufficient, and if it is 80% or more, the ceramic strength is weak. Hateful. For the same reason, the content is more preferably 30% or more and less than 70%.
  • the porous phosphorescent phosphor ceramic according to the present invention is preferably a solid sintered body.
  • the structure is a connected structure, so that the scattering and concealment of excitation light, which is noticeable in powder-dispersed products, is reduced and penetration into the deep part becomes easy. Based on the same reason, it is considered that the generated afterglow easily reaches the outside from the deep part, which leads to the improvement of the afterglow intensity.
  • the production method of the porous phosphorescent phosphor ceramic according to the present invention is not particularly limited, but as one method, the phosphor powder raw material powder mixture (addition of a small amount of flux components makes the reaction progress uniformly and the afterglow characteristics are improved. Hereinafter, the phosphor powder is simply made into coarse particles by granulation.
  • stirring granulation As a granulation method, stirring granulation; compression granulation in which powder is filled in a cylinder and compression-molded with a piston or the like; slurry containing the raw material powder mixture or the phosphorescent phosphor powder and a solvent such as water is air or the like
  • Conventionally known methods such as spray-drying granulation for spraying, drying and granulating in a countercurrent or co-current airflow can be adopted, and in particular, the viewpoint of uniformity of particle size, good yield, etc.
  • Spray drying granulation can be suitably employed.
  • the binder may be added if necessary, and is not particularly limited.
  • conventionally known ones such as paraffin wax; acrylic resin; PVA; cellulose resin such as ethyl cellulose, methyl cellulose, carboxymethyl cellulose [CMC] can be used.
  • a solution or a powder may be used, but in spray-drying granulation, a solution is desirable.
  • the average particle size of the granulated powder is preferably 50 ⁇ m or more and less than 10 mm. If it is less than 50 ⁇ m, the porosity is low, and if it is 10 mm or more, the strength of the molded body or sintered body is weak, and handling is difficult. More preferably, it is 50 to 500 ⁇ m. A sharper particle size distribution of the granulated powder is preferable because the porosity can be easily increased.
  • the average particle diameter is a value obtained by measurement by a laser diffraction method.
  • the pores can be formed by sintering at about 800 ° C. to 1500 ° C. in a weakly reducing gas atmosphere such as.
  • a more preferable lower limit of the molding pressure is 50 g / cm 2
  • a more preferable upper limit is 500 g / cm 2 .
  • molding and reaction sintering of raw material mixture granulated powder is more preferable and cost-effective than molding and sintering phosphorescent phosphor granulated powder because the strength of ceramics tends to be higher. Is also advantageous.
  • the raw powder mixture or phosphorescent phosphor powder is mixed with carbon decomposable particles such as carbon particles, organic matter, and ice particles that disappear upon firing or drying, and then molded, and then heated and dried to heat.
  • the porous phosphorous storage according to the present invention can also be formed by forming a cavity in the place where the decomposable coarse particles were present and then sintering at a temperature of about 800 to 1500 ° C. in a reducing gas atmosphere to such an extent that the cavity does not collapse Phosphor ceramics can be manufactured.
  • various conventionally known methods for producing porous ceramics can be applied.
  • porous phosphorescent phosphor ceramic of the present invention may be impregnated or coated with a transparent resin material or a glassy glaze for the purpose of surface protection.
  • Example 1 4L of 1% carboxymethylcellulose [CMC] aqueous solution (viscosity 120 mPa ⁇ s (20 ° C)) was added to 615 g of alumina, 890 g of carbonic acid Sr 890 g, oxidized Dy 22 g, oxidized Eu 11 g, and boric acid 30 g.
  • the raw material mixture granulated powder was obtained by spray drying in a countercurrent airflow, and the average particle size of the granulated powder measured by laser diffraction method was 110 ⁇ m.
  • the obtained ceramic was irradiated with 5000 Lx D65 standard light for 10 minutes, and the afterglow luminance after 60 minutes was measured with a luminance meter (LS-100, manufactured by Konica Minolta Co., Ltd.).
  • Example 2 1300 g of a commercially available phosphorescent phosphor powder [median diameter D50: 15.2 ⁇ m (manufactured by Nemotomi Material Co., GLL300F)] 3 L of 1% CMC aqueous solution (supra) is added to the ball mill, and this is mixed with air at 200 ° C. A phosphorescent granulated powder was obtained by spray drying in an air stream. The average particle diameter of the luminous phosphor granulated powder was 130 ⁇ m. 5 g of this was molded into a tablet at a rate of 0.1 kg / cm 2 using a 30 mm ⁇ mold, placed on an alumina plate, and fired at 700 ° C.
  • Example 3 1300 g of a commercially available phosphorescent phosphor powder [median diameter D50: 15.2 ⁇ m (manufactured by Nemotomi Material Co., GLL300F)] 3 L of 1% CMC aqueous solution (supra) is added to the ball mill, and this is mixed with air at 200 ° C. A phosphorescent granulated powder was obtained by spray drying in an air stream. The average particle diameter of the luminous phosphor granulated powder was 130 ⁇ m.
  • Comparative Example 2 5 g of commercially available phosphorescent phosphor powder (GLL300F manufactured by Nemotomi Material) was molded into a tablet shape with a weak pressure of 0.1 kg / cm 2 using a 30 mm ⁇ mold, placed on an alumina plate, and 3 Sintering was performed for a time (under a nitrogen atmosphere) to obtain phosphorescent phosphor ceramics. The porosity of the obtained ceramic was 12%.
  • luminance was measured like Example 1, when the brightness
  • Example 3 A phosphorescent phosphor ceramic was obtained in the same manner as in Example 1 except that the pressure at the time of molding was 10 kg / cm 2 . The porosity of the obtained ceramic was 13%.
  • luminance was measured like Example 1, when the brightness

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Luminescent Compositions (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)

Abstract

Cette invention concerne un corps fritté en céramique ayant une forte luminance persistante, dans lequel un phosphore peut être utilisé avec efficacité dans une portion profonde. L’invention concerne spécifiquement une céramique poreuse au phosphore accumulant la lumière, qui est essentiellement composée d’un phosphore accumulant la lumière et qui présente une porosité comprise entre 20 % et 80 % en volume.
PCT/JP2009/069123 2008-11-10 2009-11-10 Céramique poreuse au phosphore accumulant la lumière WO2010053197A1 (fr)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013535531A (ja) * 2010-07-14 2013-09-12 インテマティックス・コーポレーション 一般用途及びバックライト照明用途の緑色放出ガーネット系蛍光体
US9120975B2 (en) 2006-10-20 2015-09-01 Intematix Corporation Yellow-green to yellow-emitting phosphors based on terbium-containing aluminates
US9359550B2 (en) 2006-10-20 2016-06-07 Intematix Corporation Yellow-green to yellow-emitting phosphors based on halogenated-aluminates
US9428690B2 (en) 2006-10-20 2016-08-30 Intematix Corporation Yellow-green to yellow-emitting phosphors based on terbium-containing aluminates
KR20180044261A (ko) * 2015-06-19 2018-05-02 파브리카 나씨오날 데 모네다 이 띰브레-레알 까사 데 라 모네다 나노구조화 인광 안료 및 그의 용도
JP2020023675A (ja) * 2018-07-27 2020-02-13 堺化学工業株式会社 蓄光材料の製造方法及び蓄光材料
CN111807825A (zh) * 2020-07-20 2020-10-23 江苏师范大学 一种具有多孔隙光通道结构的超高亮度蓄光陶瓷及其应用
JP2020181952A (ja) * 2019-04-26 2020-11-05 株式会社ディスコ チャックテーブル及びチャックテーブルの製造方法
US11387391B2 (en) 2017-02-28 2022-07-12 Osram Gmbh Conversion element, optoelectronic component and method for producing a conversion element
JP2022552054A (ja) * 2019-08-29 2022-12-15 シェンチェン ライティング インスティテュート 蛍光セラミックス及びその製造方法、光源装置

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Cited By (20)

* Cited by examiner, † Cited by third party
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US10190047B2 (en) 2006-10-20 2019-01-29 Intematix Corporation Green-emitting, garnet-based phosphors in general and backlighting applications
US9023242B2 (en) 2006-10-20 2015-05-05 Intematix Corporation Green-emitting, garnet-based phosphors in general and backlighting applications
US9120975B2 (en) 2006-10-20 2015-09-01 Intematix Corporation Yellow-green to yellow-emitting phosphors based on terbium-containing aluminates
US9359550B2 (en) 2006-10-20 2016-06-07 Intematix Corporation Yellow-green to yellow-emitting phosphors based on halogenated-aluminates
US9428690B2 (en) 2006-10-20 2016-08-30 Intematix Corporation Yellow-green to yellow-emitting phosphors based on terbium-containing aluminates
US9458378B2 (en) 2006-10-20 2016-10-04 Intermatix Corporation Green-emitting, garnet-based phosphors in general and backlighting applications
JP2015180741A (ja) * 2010-07-14 2015-10-15 インテマティックス・コーポレーションＩｎｔｅｍａｔｉｘ Ｃｏｒｐｏｒａｔｉｏｎ 一般用途及びバックライト照明用途の緑色放出ガーネット系蛍光体
JP2013535531A (ja) * 2010-07-14 2013-09-12 インテマティックス・コーポレーション 一般用途及びバックライト照明用途の緑色放出ガーネット系蛍光体
KR20180044261A (ko) * 2015-06-19 2018-05-02 파브리카 나씨오날 데 모네다 이 띰브레-레알 까사 데 라 모네다 나노구조화 인광 안료 및 그의 용도
JP2018521171A (ja) * 2015-06-19 2018-08-02 ファブリカ、ナシオナル、デ、モネダ、イ、ティンブレ−レアル、カサ、デ、ラ、モネダＦａｂｒｉｃａ Ｎａｃｉｏｎａｌ Ｄｅ Ｍｏｎｅｄａ Ｙ Ｔｉｍｂｒｅ−Ｒｅａｌ Ｃａｓａ Ｄｅ Ｌａ Ｍｏｎｅｄａ ナノ構造りん光顔料及びその使用
US10899960B2 (en) 2015-06-19 2021-01-26 Consejo Superior De Investigaciones Científicas Nanostructured phosphorescent pigment and uses thereof
KR102557917B1 (ko) * 2015-06-19 2023-07-19 파브리카 나씨오날 데 모네다 이 띰브레-레알 까사 데 라 모네다 나노구조화 인광 안료 및 그의 용도
US11387391B2 (en) 2017-02-28 2022-07-12 Osram Gmbh Conversion element, optoelectronic component and method for producing a conversion element
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JP7342484B2 (ja) 2018-07-27 2023-09-12 堺化学工業株式会社 蓄光材料の製造方法及び蓄光材料
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