WO2010090312A1 - Procédé de fabrication de particules de corps émettant de la lumière, phosphorescentes, recouvertes de verre - Google Patents

Procédé de fabrication de particules de corps émettant de la lumière, phosphorescentes, recouvertes de verre Download PDF

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Publication number
WO2010090312A1
WO2010090312A1 PCT/JP2010/051788 JP2010051788W WO2010090312A1 WO 2010090312 A1 WO2010090312 A1 WO 2010090312A1 JP 2010051788 W JP2010051788 W JP 2010051788W WO 2010090312 A1 WO2010090312 A1 WO 2010090312A1
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WIPO (PCT)
Prior art keywords
glass
phosphor
particles
layer
mixture
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PCT/JP2010/051788
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English (en)
Japanese (ja)
Inventor
博 水上
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アライズ・コーポレート株式会社
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Publication of WO2010090312A1 publication Critical patent/WO2010090312A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • 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
    • 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
    • C03C2214/12—Polymers

Definitions

  • the present invention relates to a method for producing luminous phosphor particles used for, for example, signs for evacuation guidance, guidance lines, white lines on roads, decorative patterns, and the like, and in particular, phosphorescent phosphors having excellent water resistance and low luminance unevenness.
  • the present invention relates to a method for producing particles.
  • phosphorescent phosphors that are excited by ultraviolet rays or the like and have a long afterglow observed, such as MAl 2 O 4 (M is calcium, strontium, or barium) are used as mother crystals and activated by lanthanoids such as europium.
  • MAl 2 O 4 M is calcium, strontium, or barium
  • lanthanoids such as europium.
  • a luminous phosphor has been developed (see, for example, Patent Document 1).
  • the phosphorescent phosphor is made of a glass material or the like because the phosphorescent phosphor and the ceramic base material or the glass material are mixed and fired and then pulverized to form phosphorescent phosphor particles.
  • the problem of water resistance was not sufficiently solved.
  • the phosphor particles are not mixed in a uniform amount in the phosphor particles here, and there is a problem that unevenness occurs in emission luminance for each particle.
  • the particles are formed by pulverization, there is a problem that the sizes of the particles are uneven, that is, the particle size distribution is large and the luminance unevenness is similarly generated. Therefore, the yield was low and the production cost was problematic.
  • the present invention has been made in view of the above problems, and the object of the present invention is to store phosphorescent phosphor particles in which substantially all phosphorescent phosphor particles are coated with glass and have improved water resistance. Another object of the present invention is to provide glass-coated phosphorescent phosphor particles having a uniform size of phosphor particles and containing the same amount of phosphor in each particle and a method for producing the same.
  • the present invention forms a plurality of glass fine particle and resin adhesive mixture layers on a temporary holding member using screen printing using a mask having a large number of holes having the same diameter.
  • a phosphor particle layer containing phosphor particles and glass particles is formed, and further, a mixture layer of glass fine particles and a resin adhesive is formed thereon using the mask. Accordingly, the formation of the phosphor particles layer and the mixture layer is repeated and further laminated, and then the particulate laminate is fired, whereby the particle diameter is uniform, and the phosphor is blended in a uniform amount in each particle, and
  • the above-mentioned problem has been solved by producing luminous phosphor particles substantially coated with luminous phosphor particles with glass.
  • the gist of the present invention is as follows: (1) A mixture layer (A) by screen-printing a mixture of glass fine particles and a resin adhesive on a temporary holding member on which a mask having a large number of holes having the same diameter is placed. (2) Before the mixture layer (A) is solidified, a mixture of phosphor particles and glass particles is placed on the mixture layer (A) to solidify the mixture layer (A). The phosphor layer (B) is formed, and the mask plate and the temporary holding member used in the steps (3) and (1) are aligned and placed on the phosphor layer (B). A mixture layer (A) is formed by screen printing an adhesive mixture, and (4) the steps (2) and (3) are repeated as necessary to form a mixture layer of 3 layers or 5 layers or more.
  • the glass fine particles used for the mixture layer (A) may be any glass particles that can be mixed with a resin adhesive and screen-printed, but have a low softening temperature so that the phosphor can be easily coated with glass.
  • a glass frit having a particle size of 5 to 30 ⁇ m is particularly preferable.
  • the resin adhesive used for the mixture layer (A) may be any as long as it can be screen-printed.
  • the glass particles and the phosphor particles used in the phosphor layer (B) preferably have the same size as each other.
  • the size of the glass particles is 0.5 that of the phosphor particles.
  • Glass particles and phosphor particles are selected so as to be in the range of ⁇ 2 times. Since the phosphor layer (B) is formed by adhering to the adhesive in the mixture layer (A) before the mixture layer (A) is solidified, it is formed into a layer.
  • the particle diameter of the phosphor particles is the thickness of the phosphor layer (B). For this reason, the magnitude
  • the weight ratio of the glass particles to the phosphor particles in the phosphor layer (B) is preferably in the range of 7: 3 to 9: 1. If the amount of glass particles is small, the phosphor particles after firing are not preferable because the phosphor particles are not completely covered with glass. On the other hand, if the relative amount of the phosphor particles is too small, the luminance of the phosphor particles is decreased, which is not preferable.
  • the stack of the mixture layer (A) and the phosphor layer (B) is 3 layers or 5 layers or more is determined according to the hole diameter of the mask.
  • the resin adhesive in the mixture layer is removed by firing and shrinks in the thickness direction of the particulate laminate, so the total of the particulate laminate before firing
  • the thickness is 1.5 to 3 times, preferably around 2 times the diameter of the mask hole.
  • the thickness of the mixture layer (A) is approximately the same as the thickness of the mask used for screen printing, and the thickness of the phosphor layer (B) is approximately the same as the particle size of the phosphor particles or glass particles. If the hole diameter and thickness of the mask to be masked and the particle diameter of the luminous phosphor particles are determined, the required number of laminations is determined.
  • Firing the temporary holding member on which the granular laminate is placed is heated in a firing furnace at 300 to 500 ° C. for 1 hour or longer, and the resin adhesive in the granular laminate is baked and removed so as not to be carbonized. By firing at 600 to 800 ° C., the glass particles are fused to form luminous phosphor particles substantially entirely covered with glass.
  • the distance between the formed holes is equal to or larger than the diameter of the holes. However, if the distance is too large, the number of points of the mixture layer (A) formed by one screen printing is obtained. This reduces production efficiency. Further, it is preferable in terms of production efficiency that the holes are arranged periodically.
  • the granular laminate becomes a resin thin layer. Can be easily produced.
  • the luminous phosphor particles are formed such that the initial luminance after being immersed in water at room temperature for 48 hours is 85% or more of the initial luminance before being immersed in water.
  • glass-coated phosphorescent phosphor particles having a uniform particle size and a uniform distribution of phosphorescent particles on each particle and excellent in water resistance can be easily produced.
  • the luminous phosphor particles having a desired particle diameter can be obtained by changing the hole diameter of the mask.
  • the luminous phosphor particles of the present invention have a uniform particle size, sieving is not required and the yield is improved.
  • FIG. 1 is an explanatory diagram of an embodiment of the production method of the present invention.
  • a water-soluble surface 2 for example, dextrin
  • a resin thin layer 3 for example, an acrylic resin adhesive is applied thereon.
  • a hardened layer is prepared (I in FIG. 1), and a mask 4 in which holes of a desired size (for example, a diameter of 1000 ⁇ m) are periodically vacated is formed on the resin thin layer 3.
  • a mixture layer (A) is formed by screen-printing a mixture of glass fine particles and a resin adhesive (II in FIG. 1).
  • the distance between the mask hole and the hole is preferably larger than the diameter of the mask hole.
  • the distance between the holes is preferably 500 ⁇ m or more, more preferably 1 to 1.5 mm.
  • the thickness of the mask is not particularly limited, but is preferably about half the diameter of the mask hole.
  • the thickness of the mask is preferably about 200 to 300 ⁇ m.
  • the layer thickness of the mixture layer (A) is approximately the same as the plate thickness of the mask.
  • the shape of the mask hole is not limited to a circle, but may be an ellipse, a polygon such as a rectangle or a hexagon, but if the hole shape is extremely distorted, the resulting phosphorescent phosphor glass particles become distorted. This is not preferable.
  • the “hole diameter” in this specification is the diameter of a circle inscribed in the hole.
  • the material of the glass fine particles may be any material as long as it is transparent to the excitation light and light emission of the phosphor. However, in order to completely cover the phosphor with glass after firing, a material having a low softening temperature is preferable.
  • the particle size of the glass fine particles may be any particle size as long as it can be mixed with a resin adhesive and screen printed. Examples of preferable glass fine particles include glass frit having a particle size of 5 to 30 ⁇ m.
  • the resin adhesive is not particularly limited as long as it can be adjusted to a viscosity capable of screen printing, and examples thereof include an adhesive made of an acrylic resin and a solvent.
  • the mixing ratio of the glass fine particles and the resin adhesive is not particularly limited, but a weight ratio of 3: 1 to 1: 3 is preferable.
  • the phosphor particles (B) are formed by arranging the phosphor particles and glass particles on the mixture layer (A) (III in FIG. 1).
  • the phosphor layer (B) is formed in the manner of drawing a sand picture. That is, the phosphorescent material or glass particles placed on the mixture layer (A) are bonded onto the mixture layer (A) by the resin adhesive in the mixture layer (A) to form the phosphorescent material layer (B). Since the phosphor particles or glass particles that have fallen into the gaps between the mixture layers (A) are not adhered, they can be removed by a method such as shaking the temporary holding member.
  • Phosphors are known phosphors such as oxide phosphors such as strontium aluminate activated with lanthanoids such as europium, and sulfide phosphors such as phosphors doped with barium calcium sulfide. Either is acceptable.
  • the particle diameter of the phosphor particles may be smaller than the diameter of the mask hole, and the average particle diameter is preferably about half the diameter of the mask hole.
  • the mask hole has a diameter of 500 ⁇ m
  • phosphor particles having a maximum particle size of 500 ⁇ m or less and an average particle size of around 250 ⁇ m are preferable.
  • the particle size of the glass particles that form the phosphor layer together with the phosphor particles is preferably about the same as the particle size of the phosphor particles.
  • the material of the glass particles may be any material as long as it is transparent to the excitation light and light emission of the phosphor, and examples thereof include borosilicate glass.
  • the mixing ratio of phosphor particles and glass particles is preferably in the range of 9: 1 to 7: 3 in terms of the weight ratio of glass: phosphor. If the amount of glass particles is small, the phosphor-coated phosphor particles after firing are not preferable because the phosphor particles are not completely covered with glass. If the amount of the phosphor particles is too small, the luminance of the glass-coated phosphor particles is reduced, which is not preferable.
  • the mixture layer (A) is further formed on the phosphor layer (B) by screen printing. At this time, the mixture layer (A) can be formed on the phosphor layer (B) by placing the mask plate used in the previous step and the temporary holding member in alignment (IV in FIG. 1). .
  • FIG. 1 shows an example in which the granular laminate has three layers. However, if necessary, the phosphor layer and the mixture layer may be alternately laminated to form five or more layers.
  • the number of layers of the granular laminate is preferably set so that the total thickness of the granular laminate before firing is 1 to 3 times the diameter of the mask hole. Since the thickness of the mixture layer (A) is substantially the same as the mask plate thickness, and the thickness of the phosphor layer (B) is approximately the same as the average particle size of the phosphor particles, the approximate total of the granular laminates The thickness can be easily estimated and the preferred number of layers can be estimated.
  • the total thickness of the three layers is about 650 ⁇ m
  • the five layers are about 1100 ⁇ m
  • the seven layers are about 1550 ⁇ m.
  • the total thickness of the laminate before firing is preferably about 500 to 1500 ⁇ m. Therefore, the mixture layer (A) and the phosphor layer (B) have a three-layer or five-layer structure. Is the best. In order to manufacture large phosphorescent phosphor glass particles, if the mask hole is enlarged, the mask thickness should be increased or the particle size of the phosphor particles should be increased so that the number of laminations does not become excessive. It is preferable to enlarge it.
  • the resin adhesive of the granular laminate After the resin adhesive of the granular laminate is solidified, it is immersed in water for several seconds to dissolve the water-soluble surface 2, and the resin thin layer 3 on which the granular laminate is placed is peeled from the substrate 1 of the temporary holding member, and the resin The granular laminate is fired while being placed on the thin layer 3.
  • the baking is carried out at 300 to 500 ° C. for 1 hour or longer to incinerate and remove the resin adhesive in the resin thin layer and the mixture layer (A) so that the resin is not carbonized.
  • the temperature may be maintained at any temperature of 300 to 500 ° C., or may be slowly raised to be in the range of 300 to 500 ° C. for 1 hour or more.
  • the glass particles are then fused together by maintaining at 600-800 ° C. for 5-30 minutes.
  • the glass-coated phosphor particles produced by the production method described above have a uniform particle size, and the phosphor content in each particle is uniform, so that brightness unevenness is reduced.
  • the phosphor since the phosphor is almost completely covered with glass, it has excellent water resistance, and even when the phosphorescent phosphor particles are immersed in water, there is little decrease in luminance. % Or more of the initial luminance can be maintained.
  • Example 1 A dextrin layer (water-soluble layer) is formed on the surface of cardboard (temporary holding member base material), and a resin adhesive (screen printing oil manufactured by Ferro Japan) is screen-printed with a solid plate to form a temporary holding member. .
  • a metal mask having a plate thickness of about 200 ⁇ m in which holes having a diameter of 1000 ⁇ m are periodically vacated at intervals of about 1000 ⁇ m is placed, and 10 parts by weight of a glass frit having a particle size of 5 to 10 ⁇ m (manufactured by Nippon Frit Co., Ltd.)
  • a mixture layer (A) having a thickness of about 200 ⁇ m was formed by screen-printing a mixture in which 8 parts by weight of the resin adhesive was mixed.
  • the mask plate and the temporary holding member used in the previous step are aligned and placed, and the mixture layer (A) is formed on the phosphorescent material layer (B) by screen printing.
  • a granular laminate having a layer structure was formed.
  • the temporary holding member was immersed in water for several seconds to dissolve the dextrin layer, and a granular laminate was periodically arranged on the resin film.
  • the obtained granular laminate was baked in a baking furnace together with the resin film. Firing was performed by slowly raising the temperature, taking 1 hour or more at 300 to 500 ° C., then maintaining at about 700 ° C. for about 15 minutes, and then slowly cooling to room temperature to obtain glass-coated phosphorescent phosphor particles.
  • the obtained glass-coated luminous phosphor particles were approximately spherical.
  • 97% or more by weight ratio was in the range of 1000 ⁇ m to 1400 ⁇ m, and the particle size was uniform.
  • the obtained glass-coated luminous phosphor particles were immersed in water at room temperature for 48 hours, and the initial luminance before and after immersion in water was measured.
  • the initial luminance before immersion in water was 66 mcd / m 2 , 48 hours.
  • the initial luminance after being immersed in water was 60 mcd / m 2 , and the initial luminance of about 91% before being immersed in water was maintained.
  • the initial luminance is the luminance of the luminous phosphor particles when the phosphor particles are irradiated with a 200 Lux D65 fluorescent lamp for 20 minutes and then moved to a dark place.
  • the mixing ratio between the glass and the phosphor in the phosphor layer is preferably 9: 1 to 7: 3 by weight.
  • the initial luminance before immersion in water was 61 mcd / m 2
  • the initial luminance after immersion was At 50 mcd / m 2
  • phosphorescent phosphor particles having excellent water resistance and a uniform particle size and phosphorescent substance distribution can be obtained, and phosphorescent light can be stored not only indoors but also on outdoor signs, guide lines, road white lines, etc.
  • the body can be used.
  • base material of temporary holding member 2 water-soluble surface 3: water-insoluble resin thin layer 4: mask A: mixture layer B: phosphorescent material layer

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)
  • Illuminated Signs And Luminous Advertising (AREA)
  • Road Repair (AREA)
  • Road Signs Or Road Markings (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention porte sur un procédé de fabrication de particules de corps émettant de la lumière, phosphorescentes, avec une excellente résistance à l'eau et avec une dimension de particule uniforme et une distribution uniforme de matière phosphorescente. Sur un élément de retenue temporaire, (1) un masque ayant des trous ménagés de façon périodique est monté, et de multiples couches de mélange (A) sont formées par sérigraphie d'un mélange de fines particules de verre et d'un agent adhésif formé de résine ; (2) avant que l'agent adhésif formé de résine ne durcisse, des particules de matière phosphorescente et des particules de verre sont étalées sur les couches de mélange (A), formant une couche de matière phosphorescente (B) sur les couches de mélange (A) ; (3) le masque utilisé à l'étape (1) est aligné et monté sur la couche de matière phosphorescente (B) et une couche de mélange (A) est formée par sérigraphie d'un mélange de fines particules de verre et d'un agent adhésif formé de résine ; (4) par répétition de l'étape (2) et de l'étape (3) selon les besoins, un stratifié granulaire est formé avec trois couches, cinq couches ou plus, la couche de mélange (A) et la couche de matière phosphorescente (B) étant empilées de façon alternée, et (5) des particules de corps émettant de la lumière, phosphorescentes, revêtues de verre, sont fabriquées par cuisson du stratifié granulaire.
PCT/JP2010/051788 2009-02-09 2010-02-08 Procédé de fabrication de particules de corps émettant de la lumière, phosphorescentes, recouvertes de verre WO2010090312A1 (fr)

Applications Claiming Priority (2)

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JP2009027694A JP2010180380A (ja) 2009-02-09 2009-02-09 ガラス被覆蓄光性発光体粒子及びその製造方法
JP2009-027694 2009-11-27

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130263872A1 (en) * 2010-10-22 2013-10-10 Yasunori Iwamoto Process for producing phosphorescent body and phosphorescent body produced by the process, and nail stone including phosphorescent body
WO2015198939A1 (fr) * 2014-06-23 2015-12-30 コドモエナジー株式会社 Procédé de fabrication d'un corps phosphorescent particulaire, corps phosphorescent particulaire, marque de sécurité de prévention de collision avec le verre et marque de guidage d'évacuation

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5946087B2 (ja) * 2012-03-23 2016-07-05 国立研究開発法人産業技術総合研究所 蓄光部材

Citations (4)

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Publication number Priority date Publication date Assignee Title
JPS60176933A (ja) * 1984-02-20 1985-09-11 Shigaken 蓄光螢光性のガラス繊維及びガラス小球の製造方法
JPS62148330A (ja) * 1985-12-23 1987-07-02 Matsushita Electric Works Ltd 彩虹ビ−ズの製法
JPH08151219A (ja) * 1994-11-28 1996-06-11 Nakashima:Kk 金属光沢を有するガラス微粒子およびその製法
JPH1143349A (ja) * 1997-04-28 1999-02-16 Kurasutaa Technol Kk 蓄光素材並びにその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5044181B2 (ja) * 2006-09-27 2012-10-10 アライズ・コーポレート株式会社 蓄光性発光体の製造方法
JP4338749B2 (ja) * 2006-10-25 2009-10-07 株式会社サカイ・シルクスクリーン 蓄光板の製造方法及び蓄光板

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60176933A (ja) * 1984-02-20 1985-09-11 Shigaken 蓄光螢光性のガラス繊維及びガラス小球の製造方法
JPS62148330A (ja) * 1985-12-23 1987-07-02 Matsushita Electric Works Ltd 彩虹ビ−ズの製法
JPH08151219A (ja) * 1994-11-28 1996-06-11 Nakashima:Kk 金属光沢を有するガラス微粒子およびその製法
JPH1143349A (ja) * 1997-04-28 1999-02-16 Kurasutaa Technol Kk 蓄光素材並びにその製造方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130263872A1 (en) * 2010-10-22 2013-10-10 Yasunori Iwamoto Process for producing phosphorescent body and phosphorescent body produced by the process, and nail stone including phosphorescent body
US9005760B2 (en) * 2010-10-22 2015-04-14 Yasunori Iwamoto Process for producing phosphorescent body and phosphorescent body produced by the process, and nail stone including phosphorescent body
WO2015198939A1 (fr) * 2014-06-23 2015-12-30 コドモエナジー株式会社 Procédé de fabrication d'un corps phosphorescent particulaire, corps phosphorescent particulaire, marque de sécurité de prévention de collision avec le verre et marque de guidage d'évacuation
JP2017057138A (ja) * 2014-06-23 2017-03-23 コドモエナジー株式会社 粒状蓄光体並びにこれを用いたガラス衝突防止安全マーク及び避難誘導用マーク
JPWO2015198939A1 (ja) * 2014-06-23 2017-04-20 コドモエナジー株式会社 粒状蓄光体の製造方法

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