WO2008018582A1 - Oxyde d'yttrium activé à l'europium et son procédé de fabrication - Google Patents

Oxyde d'yttrium activé à l'europium et son procédé de fabrication Download PDF

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Publication number
WO2008018582A1
WO2008018582A1 PCT/JP2007/065702 JP2007065702W WO2008018582A1 WO 2008018582 A1 WO2008018582 A1 WO 2008018582A1 JP 2007065702 W JP2007065702 W JP 2007065702W WO 2008018582 A1 WO2008018582 A1 WO 2008018582A1
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Prior art keywords
europium
firing
median diameter
yttrium oxide
activated yttrium
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PCT/JP2007/065702
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English (en)
Japanese (ja)
Inventor
Tokuo Suita
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Ishihara Sangyo Kaisha, Ltd.
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Publication date
Application filed by Ishihara Sangyo Kaisha, Ltd. filed Critical Ishihara Sangyo Kaisha, Ltd.
Publication of WO2008018582A1 publication Critical patent/WO2008018582A1/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
    • C09K11/7784—Chalcogenides
    • C09K11/7787—Oxides

Definitions

  • the present invention relates to europium-activated yttrium oxide useful as a red phosphor used for an electron beam-excited light emitting device such as a field emission display (FED) and a method for producing the same.
  • FED field emission display
  • red phosphors used in electron fountain-excited light-emitting elements include europium-activated oxysulfide (Y Eu) OS and europium-activated yttrium oxide (Y Eu) O force S.
  • Europium activated yttrium oxysulfide has been widely used as a red phosphor for image display, but when this is used in field emission displays (FED), (1) Acceleration voltage used in FED ; Excited with an electron beam of about OkV, it is difficult to obtain sufficient emission brightness. (2) Since it contains sulfur, it causes cathode contamination. (3) Luminance deterioration occurs due to electron beam irradiation. There are concerns about the problem. Europium-activated yttrium oxide does not contain sulfur because it does not contain sulfur, but its emission characteristics are not sufficient, and studies have been made to improve emission brightness and lower emission start voltage. Yes.
  • Patent Document 1 a manufacturing method for refiring (annealing) in a reducing atmosphere is known for lowering the emission starting voltage (see Patent Document 1).
  • a method for producing a rare earth oxide by a spray drying method for example, a production method is known in which a rare earth oxalate produced under a specific production condition is spray-dried under a specific condition and then fired (Patent Document). 2).
  • Patent Document 3 a manufacturing method for obtaining a phosphor by thermally decomposing fine droplets made of a solution containing a constituent metal element of the phosphor.
  • Patent Document 1 Japanese Unexamined Patent Publication No. 2000-265168
  • Patent Document 2 JP-A-9 71415
  • Patent Document 3 Japanese Patent Laid-Open No. 2001-220580
  • the red phosphor described in Patent Document 1 can reduce the emission starting voltage, it is required to further improve the emission luminance in order to be used as a red light emitting element of a field emission display (FED). It has been.
  • FED field emission display
  • baking at a high temperature is a preferable production condition.
  • the improvement in crystallinity due to high-temperature firing causes a coarse sintered body due to the accompanying inter-particle sintering, and immediately deteriorates powder characteristics such as dispersibility.
  • the present inventor has made various studies to find a yttrium oxide red phosphor having a good balance between crystallinity and dispersibility.
  • the europium-containing yttrium compound and a flux are mixed in an aqueous system to obtain a slurry.
  • spray drying is performed to obtain spherical secondary particles, and then the obtained secondary particles are fired so that the median diameter after firing is 0.65-0.75 times the median diameter before firing.
  • europium-activated yttrium oxide obtained by setting the median diameter after firing to 2 to 8 m satisfies the above-mentioned contradictory characteristics at the same time, and thus completed the present invention.
  • the present invention has a median diameter measured by the laser diffraction / scattering method in the range of 2 to 8 am, and is calculated from the diffraction peak from the 440 plane measured by the X-ray diffraction method ( ⁇ 2 ⁇ ) cos S (where ⁇ is the diffraction angle and ⁇ 2 ⁇ is the half-value width (deg) of the diffraction peak) is europium-activated yttrium oxide characterized by a maximum of 0.083 deg.
  • the present invention is a method for producing the above yttrium oxide, comprising mixing an europium-containing yttrium compound and a flux in an aqueous system to form a slurry, followed by spray drying to obtain spherical secondary particles. Next, the obtained secondary particles are fired so that the median diameter after firing is 0.65 to 0.75 times the median diameter before firing, so that the median diameter after firing is 2 to 8 m.
  • a method for producing europium-activated yttrium oxide characterized by the following: The invention's effect
  • the europium-activated yttrium oxide of the present invention is excellent in emission luminance due to electron beam irradiation because of improved crystallinity, and is suitable for pasting because it is in a monodispersed state having an appropriate median diameter. It is a phosphor.
  • the present invention is europium-activated yttrium oxide having a median diameter measured by a laser diffraction / scattering method in the range of 2 to 8,1 m and a rotation from a 440 plane measured by an X-ray diffraction method.
  • Calculated from the folding peak (A26) cose (where ⁇ is the diffraction angle and ⁇ 2 ⁇ is the half-value width (deg) of the diffraction peak), it is characterized by 0.083 deg at most.
  • the median diameter and ( ⁇ 2 ⁇ ) cos ⁇ are measured by the following methods, respectively.
  • the median diameter is measured with a laser diffraction / scattering particle size distribution analyzer (model number: LA950) manufactured by Horiba.
  • the dispersion medium is 0.2% sodium hexametaphosphate aqueous solution.
  • the median diameter is calculated on a volume basis with the refractive index of the sample being 1.82 and the refractive index of the dispersion medium being 1.33.
  • step scanning is performed at an angle range of 47.8 ° ⁇ 2 ⁇ 49 ⁇ 2 ° at 0 ⁇ 01 ° / lOsec
  • step scanning is performed at an angle range of 47.8 ° ⁇ 2 ⁇ 49 ⁇ 2 ° at 0 ⁇ 01 ° / lOsec
  • the europium activated yttrium oxide of the present invention has a median diameter calculated by the above method in the range of 2 to 8111. By setting the median diameter in the above range, it becomes suitable for pasting. When the median diameter is smaller than 2 m, monodisperse particles with little sintering are hardly formed. When larger than 8111, voids are likely to be formed in the particles, and it is difficult to form fine particles.
  • the europium activated yttrium oxide of the present invention has ( ⁇ 2 ⁇ ) cos ⁇ calculated by the above method at most 0.083 deg.
  • Lc when expressed in Lc estimated in this way, Lc ⁇ 95.7 nm.
  • the diffraction peak broadening ( ⁇ 2 ⁇ ) includes not only broadening due to the finite crystallite size but also broadening due to crystal distortion, and when the diffraction peak broadening is small, for example, When ( ⁇ 2 ⁇ ) cos ⁇ force S calculated by the above method is 0.083 deg at most, it cannot be ignored. In other words, it is not always appropriate to discuss crystallinity by the value of Lc applying the above-mentioned Shirrer formula! /. Crystal strain is also an important measure of crystallinity. In the present invention, the value of ( ⁇ 2 ⁇ ) cos ⁇ is used as a measure to reflect both the crystallite size and the non-uniform strain of the crystal. When ( ⁇ 2 ⁇ ) cos ⁇ is larger than 0 ⁇ 08 3 deg, the crystallinity is not sufficient, and the emission luminance is inferior.
  • ⁇ ) cos ⁇ simultaneously satisfy the above range.
  • the median diameter in the range of 2 to 8 111 can be achieved by, for example, suppressing sintering between particles by firing at a low temperature and temperature. In this case, only a low crystallinity is obtained.
  • ( ⁇ 2 ⁇ ) cos ⁇ is larger than 0 ⁇ 083 deg.
  • it can be achieved by firing at a high temperature. Greater than 8 in.
  • the two are balanced and calcined. As described later, the calcining is performed, for example, in the temperature range of the melting point of the flux to 1500 ° C, preferably the melting point of the flux to 1400 ° C.
  • the present invention is a method for producing the europium-activated yttrium oxide, wherein the europium-containing yttrium compound and the flux are mixed in an aqueous system to form a slurry, which is then spray-dried to obtain spherical secondary particles.
  • the obtained secondary particles were fired so that the median diameter after firing was 0.65-0.75 times the median diameter before firing, and the median diameter after firing was 2-8111. It is characterized by
  • a europium-containing yttrium compound, a flux are mixed in an aqueous system to form a slurry, which is then spray-dried to obtain spherical secondary particles.
  • the europium-containing yttrium compound referred to in the present invention includes an yttrium compound in which europium is solid-solved inside the yttrium compound, a compound obtained by adsorbing the europium compound on the surface of the yttrium compound, and a mixture of the yttrium compound and the europium compound. It is included.
  • Examples of the europium-containing yttrium compound include europium hydroxide-containing yttrium hydroxide, europium-containing yttrium hydrated oxide, europium oxalate-containing yttrium oxalate, and the like.
  • Europium hydroxide-containing yttrium hydroxide neutralizes the nitrate solution containing yttrium and europium with ammonia water, and europium-containing yttrium hydroxide oxide is filtered and washed with europium hydroxide-containing yttrium hydroxide, followed by partial dehydration by heating.
  • the europium oxalate-containing yttrium oxalate can be produced by adding an oxalic acid solution to a nitrate solution containing yttrium and europium.
  • europium hydroxide-containing yttrium hydroxide obtained by neutralization with aqueous ammonia Reaction conditions such as neutralization temperature and neutralization time can be appropriately set.
  • the europium hydroxide-containing yttrium hydroxide obtained by neutralization is appropriately filtered and washed with water.
  • the europium-containing yttrium compound and the flux are mixed in an aqueous system to form a slurry.
  • fluxes examples include lithium fluoride, sodium fluoride, lithium fluoride, potassium phosphate, sodium phosphate, sodium chloride, and lithium chloride. These can be used alone or in combination. The power to do S.
  • lithium fluoride and / or potassium phosphate is preferably used. Use of lithium fluoride is preferable because the flux hardly remains in the phosphor obtained after firing. Further, potassium phosphate is preferable because crystallization is promoted with a small addition amount.
  • lithium fluoride and potassium phosphate together because the particle shape tends to be spherical.
  • the amount of the flux used is preferably in the range of 0.;! To 15 mol% with respect to the europium-containing yttrium compound. If a flux is used beyond this range, a coarse phosphor is likely to be generated. In addition, the flux component remaining in the phosphor increases, which is undesirable because it adversely affects crystallization. Use of an appropriate amount of flux promotes crystallization during firing, so lower the firing temperature. And sintering between particles can be suppressed.
  • the slurry is spray-dried to obtain spherical secondary particles.
  • spray dryers such as a 4-fluid nozzle system, a 2-fluid nozzle system, and a disk atomizer system.
  • it is easy to produce secondary particles in the above range.
  • Spherical secondary particles having a desired median diameter can be obtained by appropriately setting conditions such as slurry (oxide conversion) concentration, spray air discharge amount, temperature and the like according to the spray dryer to be used.
  • the mouth-pium-activated yttrium oxide of the present invention is obtained as m.
  • the firing atmosphere may be set as appropriate, including an oxidizing atmosphere containing oxygen such as air, or a neutral atmosphere containing a non-oxidizing / non-reducing gas such as nitrogen, but an oxidizing atmosphere such as air is preferred. .
  • the spherical secondary particles are densified by firing.
  • the spherical secondary particles are densified, and europium-activated yttrium oxide in which inter-particle sintering is suppressed is obtained.
  • the firing temperature is a force that can be appropriately set depending on the type and amount of the flux used.
  • the melting point of the flux is preferably 1 to 500 ° C, and preferably the melting point of the flux is 1400 ° C. When the firing temperature is lower than the above range, densification is insufficient and it is difficult to obtain desired crystallinity.
  • the firing temperature is higher than the above range, the crystal distortion increases due to the progress of interparticle sintering, and the dispersibility tends to be poor.
  • the europium-activated yttrium oxide obtained in this way is excellent in crystallinity, and when ( ⁇ 2 ⁇ ) cos ⁇ is used as a measure of crystallinity, the straight line is at most 0.083 deg.
  • the europium-activated yttrium oxide of the present invention is excellent in emission luminance by electron beam excitation. Because it has a median diameter suitable for pasting, it is suitable for a flat panel display utilizing the electron beam excitation luminescence phenomenon, for example, a red phosphor used in a field emission display (FED). is there.
  • FED field emission display
  • Two types of FED are being studied: a low-voltage type using an electron beam accelerated by a voltage of 100 to 3000V as an excitation source and a high-voltage type using an electron beam accelerated by a voltage of 3000V or more as an excitation source. Yes. Since the red phosphor of the present invention can obtain good light emission even with an electron beam accelerated at least at about 100 V, it can be used with any of the above types with a force S.
  • Europium hydroxide-containing yttrium hydroxide and pure water obtained in the previous step were placed in a commercially available juice mixer and stirred to obtain a slurry having a concentration of 8.25 wt% in terms of oxide.
  • P / (Eu + Y) 0. 5 the by dissolving K Roomikuron (molar 0/0) and a quantity of pure water 200 (ml) Slurry
  • 60 g of the obtained spherical secondary particles were calcined in the atmosphere at a temperature of 1380 ° C. for 5 hours using an alumina crucible with a volume of 100 (ml).
  • the fired product was pulverized with a centrifugal pulverizer (manufactured by Nippon Seiki Co., Ltd.) to obtain europium activated yttrium oxide (sample A) of the present invention.
  • Spherical secondary particles having a median diameter of 9.32 m were obtained in the same manner as in Example 1 except that the slurry concentration of europium hydroxide-containing yttrium hydroxide was 7.5 wt%. Subsequent firing and pulverization were carried out in the same manner as in Example 1 to obtain europium-activated yttrium oxide (sample B) of the present invention.
  • Spherical secondary particles having a median diameter of 4.12 m were obtained by the same treatment as in Example 1 except that the slurry concentration of europium hydroxide-containing yttrium hydroxide was 2.5 wt%. Subsequent firing and pulverization were carried out in the same manner as in Example 1 to obtain europium-activated yttrium oxide (sample C) of the present invention.
  • the spray dryer is made by Futakusha: Mobile minor type (atomizer type), spray drying conditions are oxide concentration slurry concentration 5wt%, liquid feed rate 30 (ml / min), dryer inlet temperature Spherical secondary particles having a median diameter of 12.8 m were obtained in the same manner as in Example 1 except that the temperature was 230 ° C and the outlet temperature was 100 ° C. Subsequent firing and pulverization were also carried out in the same manner as in Example 1 to obtain europium-activated yttrium oxide (sample D) as a comparative sample.
  • Spherical secondary particles having a median diameter of 2.53 m were collected by a bag filter in the same manner as in Example 1. Further, subsequent firing and pulverization were performed in the same manner as in Example 1 to obtain a europium-activated yttrium oxide (sample E) as a comparative sample.
  • Example 1 except for baking at 1200 ° C. and baking for 5 hours, the same treatment as in Example 1 was performed to obtain a europium activated yttrium oxide (sample F) as a comparative sample.
  • Example 1 except that the calcination temperature was 1100 ° C. and the calcination was performed for 5 hours, the same treatment as in Example 1 was performed to obtain a europium activated yttrium oxide (sample G) as a comparative sample.
  • the sample was irradiated with an electron beam accelerated at an accelerating voltage of 5 kV under a high vacuum of, and the emission vector from the sample was measured using a multichannel spectrometer.
  • the Y value (emission luminance) in the CIE1931 color system was determined from the obtained emission spectrum. Table 1 shows the relative value with the light emission luminance of Comparative Sample J as 100.
  • the europium-activated yttrium oxide of the present invention (samples A to C) has a dense and monodispersed particle, whereas the comparative sample has a monodispersed state.
  • voids are observed in the particles (sample D), or the inter-particle sintering is advanced (sample E), and the particles are not sufficiently densified (samples F and G), and are coarse. Were produced (sample H, 1).
  • the europium activated yttrium oxide of the present invention (samples A to C) of the present invention having a median diameter in the range of 2 to 8 am and ( ⁇ 2 ⁇ ) cos ⁇ of at most 0 ⁇ 083 deg.
  • the comparative samples D, E, F, G, H, and I which do not satisfy the median diameter and the range of ( ⁇ 2 ⁇ ) cos ⁇ at the same time, it has excellent emission luminance by electron beam excitation. I found out
  • the europium-activated yttrium oxide of the present invention is useful as a red phosphor for an electron fountain-excited light emitting device such as a field emission display (FED).
  • FED field emission display
  • FIG. 1 is a scanning electron micrograph showing the particle shape of sample A.
  • FIG. 2 is a scanning electron micrograph showing the particle shape of Sample B.
  • FIG. 3 is a scanning electron micrograph showing the particle shape of Sample C.
  • FIG. 4 is a scanning electron micrograph showing the particle shape of Sample D.
  • FIG. 5 is a scanning electron micrograph showing the particle shape of sample E.
  • FIG. 6 is a scanning electron micrograph showing the particle shape of Sample F.
  • FIG. 7 is a scanning electron micrograph showing the particle shape of sample G.
  • FIG. 8 is a scanning electron micrograph showing the particle shape of sample H.
  • FIG. 9 is a scanning electron micrograph showing the particle shape of Sample I.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

L'invention concerne un oxyde d'yttrium activé à l'europium qui présente un diamètre moyen compris entre 2 et 8 μm mesuré par un procédé de diffraction / diffusion par laser et un (δ2ϑ)cosϑ de 0,083 degré maximum calculé à partir d'un pic de diffraction à partir d'une face 440 mesurée par un procédé de diffraction par rayons X où ϑ représente un angle de diffraction ; et δ2ϑ représente une largeur de demi valeur (degré) d'un pic de diffraction. Cet oxyde d'yttrium activé à l'europium peut être fabriqué en mélangeant ensemble un composé d'yttrium contenant de l'europium et un flux dans un système d'eau pour préparer une suspension épaisse, en séchant par pulvérisation la suspension épaisse pour préparer des particules secondaires sphériques, et ensuite en cuisant les particules secondaires de sorte que le diamètre moyen après la cuisson soit compris entre de 0,65 et 0,75 fois le diamètre moyen avant la cuisson pour amener le diamètre moyen après cuisson entre 2 et 8 μm. L'oxyde d'yttrium activé à l'europium est une substance fluorescente rouge appropriée aux éléments électroluminescents à excitation par faisceau, par exemple, dans des afficheurs à émission par effet de champ électrique (FED).
PCT/JP2007/065702 2006-08-11 2007-08-10 Oxyde d'yttrium activé à l'europium et son procédé de fabrication WO2008018582A1 (fr)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4948527A (en) * 1989-10-10 1990-08-14 Gte Products Corporation Method of making europium activated yttrium oxide phosphor
JPH08134443A (ja) * 1993-12-17 1996-05-28 Toshiba Corp 蛍光体、陰極線管、蛍光ランプおよび放射線増感紙
JPH0971415A (ja) * 1995-09-01 1997-03-18 Shin Etsu Chem Co Ltd 球状希土類酸化物の製造方法
JP2001220580A (ja) * 1999-12-01 2001-08-14 Mitsubishi Chemicals Corp 蛍光体粒子の製造方法
WO2002044303A1 (fr) * 2000-11-30 2002-06-06 Chubu Chelest Co., Ltd. Procede de production d'un materiau a base d'oxyde metallique fluorescent
JP2004043216A (ja) * 2002-07-09 2004-02-12 Shoei Chem Ind Co 高結晶性複酸化物粉末の製造方法
JP2004067462A (ja) * 2002-08-07 2004-03-04 Shoei Chem Ind Co 高結晶性複酸化物粉末の製造方法
JP2005239960A (ja) * 2004-02-27 2005-09-08 Nisshin Seifun Group Inc 蛍光体微粒子の製造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4948527A (en) * 1989-10-10 1990-08-14 Gte Products Corporation Method of making europium activated yttrium oxide phosphor
JPH08134443A (ja) * 1993-12-17 1996-05-28 Toshiba Corp 蛍光体、陰極線管、蛍光ランプおよび放射線増感紙
JPH0971415A (ja) * 1995-09-01 1997-03-18 Shin Etsu Chem Co Ltd 球状希土類酸化物の製造方法
JP2001220580A (ja) * 1999-12-01 2001-08-14 Mitsubishi Chemicals Corp 蛍光体粒子の製造方法
WO2002044303A1 (fr) * 2000-11-30 2002-06-06 Chubu Chelest Co., Ltd. Procede de production d'un materiau a base d'oxyde metallique fluorescent
JP2004043216A (ja) * 2002-07-09 2004-02-12 Shoei Chem Ind Co 高結晶性複酸化物粉末の製造方法
JP2004067462A (ja) * 2002-08-07 2004-03-04 Shoei Chem Ind Co 高結晶性複酸化物粉末の製造方法
JP2005239960A (ja) * 2004-02-27 2005-09-08 Nisshin Seifun Group Inc 蛍光体微粒子の製造方法

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