WO2006109938A1 - Lamp having good maintenance behavior of brightness and color coordinations - Google Patents
Lamp having good maintenance behavior of brightness and color coordinations Download PDFInfo
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- WO2006109938A1 WO2006109938A1 PCT/KR2006/001150 KR2006001150W WO2006109938A1 WO 2006109938 A1 WO2006109938 A1 WO 2006109938A1 KR 2006001150 W KR2006001150 W KR 2006001150W WO 2006109938 A1 WO2006109938 A1 WO 2006109938A1
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- Prior art keywords
- phosphor
- lamp
- phase
- bam
- lamp according
- Prior art date
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- 238000012423 maintenance Methods 0.000 title description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 163
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims description 32
- 239000013078 crystal Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229910052788 barium Inorganic materials 0.000 claims description 8
- 229910052693 Europium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims description 7
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 229910052712 strontium Inorganic materials 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 238000009125 cardiac resynchronization therapy Methods 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 4
- 150000002602 lanthanoids Chemical class 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 description 40
- 230000006866 deterioration Effects 0.000 description 27
- 230000008569 process Effects 0.000 description 23
- 238000010438 heat treatment Methods 0.000 description 20
- 238000004519 manufacturing process Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 230000008859 change Effects 0.000 description 12
- 239000012298 atmosphere Substances 0.000 description 11
- 229910001512 metal fluoride Inorganic materials 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 230000001681 protective effect Effects 0.000 description 10
- 230000003247 decreasing effect Effects 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 150000001768 cations Chemical class 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- -1 Al O Chemical compound 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910020068 MgAl Inorganic materials 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910001960 metal nitrate Inorganic materials 0.000 description 2
- 229920001220 nitrocellulos Polymers 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 241001167556 Catena Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 241000206607 Porphyra umbilicalis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000004703 alkoxides Chemical group 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- DXNVUKXMTZHOTP-UHFFFAOYSA-N dialuminum;dimagnesium;barium(2+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mg+2].[Mg+2].[Al+3].[Al+3].[Ba+2].[Ba+2] DXNVUKXMTZHOTP-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
-
- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
-
- 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7777—Phosphates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J61/00—Gas-discharge or vapour-discharge lamps
- H01J61/02—Details
- H01J61/30—Vessels; Containers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J61/00—Gas-discharge or vapour-discharge lamps
- H01J61/02—Details
- H01J61/38—Devices for influencing the colour or wavelength of the light
- H01J61/42—Devices for influencing the colour or wavelength of the light by transforming the wavelength of the light by luminescence
- H01J61/44—Devices characterised by the luminescent material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
Definitions
- the present invention relates to a lamp including a specific phosphor and having good ability to maintain brightness and color coordinates, and more particularly, to a lamp using a phosphor in which a magnetoplumbite phase is epitaxially formed on a phosphor having a ⁇ alumina phase.
- barium magnesium aluminate (BAM; [(Ba, Eu + )MgAl O ]) phosphors are used in CCFLs (Cold Cathode Fluorescent Lamps) or EEFLs (External Electrode Fluorescent Lamps) for BLUs (Back Light Units) of LCDs or three-wavelength fluorescent lamps.
- BAM barium magnesium aluminate
- the deterioration of the BAM phosphor is known as the main reason to cause the deterioration of luminous properties of the phosphors generated under gas discharge during the use of the application product.
- the deterioration (change in color coordinates) of luminous properties of the BAM phosphor greatly affects the change in color coordinates of the three-wavelength lamp.
- Japanese Patent Laid-open Publication No. 2003-82345 discloses a method of oxidizing part of Eu + to Eu + without the use of additional compounds, and a method of forming an oxide film or a fluoride film with the addition of Al, Si or La.
- Japanese Patent Laid-open Publication No. 2003-82344 discloses a method of increasing positive charges through substitution of Al or Mg with a tetravalent element (Ti, Zr, Hf, Si, Sn, Ge, or Ce), in order to prevent deterioration of the phosphor.
- Japanese Patent Laid-open Publication No. 2003-382343 discloses a method of coating BAM with oxide, such as SiO , Al O , ZnO, MgAl O , Ln O , LaPO or Zn SiO , or
- Japanese Patent Laid-open Publication No. 2002-348570 discloses a technique for heat treating a BAM phosphor containing silicon at 500 ⁇ 800°C in air so as to prevent deterioration of the phosphor under vacuum UV light.
- Korean Patent Laid-open Publication No. 2003-14919 discloses a technique for surface treating only a selective portion of the surface of a phosphor, thereby minimizing a decrease in performance due to coating.
- Korean Patent Laid-open Publication No. 2002-0025483 discloses a technique for continuously coating the surface of a BAM phosphor with SiO to a thickness of 5-40 nm to cover the surface of the phosphor such that the phosphor does not deteriorate.
- Patent Laid-open Publication No. 2000-303065 discloses a technique for coating a BAM phosphor, which is a phosphor for use in vacuum UV light, with borates, phosphates, silicates, halogens, nitrates, sulfates and carbonates containing Ba or Sr as a cation in order to prevent the thermal degradation of the phosphor.
- Japanese Patent Laid-open Publication No. 2002-080843 discloses a technique for coating a first BAM phosphor with second phosphor powder that emits UV light, to prevent the decrease in performance of the first phosphor.
- the luminous efficiency varies with the thickness of the film.
- the surface treatment amount is large, the decrease in efficiency is also large but the ability to maintain brightness is good.
- the surface treatment material may entail a negative result of coagulating phosphor particles due to its action as a binder, as well as the positive function as a protective film.
- the phosphor thus coagulated exhibits poor dispersiblity upon actual use and therefore cannot be formed into a uniform coating film, undesirably leading to non-uniform color coordinates or brightness. Disclosure of Invention Technical Problem
- an object of the present invention is to provide a lamp using a phosphor having high initial brightness and good ability to maintain brightness and color coordinates.
- the present invention provides to a lamp using a phosphor in which a magne- toplumbite phase is epitaxially formed on the surface of a phosphor having a ⁇ alumina phase.
- a BAM phosphor particularly [(M ,
- the magnetoplumbite phase may be formed without the use of additional compounds, or may be formed through chemical bonding with material having a magnetoplumbite (MP) structure.
- MP magnetoplumbite
- the lamp may be used as BLU lamps, for example, CCFLs or EEFLs, for use in display devices such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or as lamps for illumination systems.
- BLU lamps for example, CCFLs or EEFLs
- display devices such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or as lamps for illumination systems.
- the magnetoplumbite is a material having a structure very similar to ⁇ alumina phase, and, as an example, the magnetoplumbite may be a material represented by Formula 1 below:
- M (II) is Ca, Sr, Pb or Eu
- M' (III) is Al, Ga or mixtures thereof.
- the magnetoplumbite may be represented by Formula 2 below: [21] Formula 2
- M (III) is lanthanide including La, Ce, Pr, Nd, Sm, Eu or Gd
- M" ( ⁇ ) is Ni, Co, Fe, Mn or Mg
- M' (III) is Al, Ga or mixtures thereof.
- the magnetoplumbite may be represented by Formula 3 below:
- M I ⁇ is La, Ce or mixtures thereof, and M' m is Al, Ga or mixtures thereof.
- the magnetoplumbite phase selectively chemically surface-modifies only the specific crystal plane of the phosphore having a ⁇ alumina phase, particularly the BAM phosphor, that is, the crystal plane lying parallel to the c axis of the crystal thereof.
- a BAM phosphor having a changed composition is heat treated to improve only ability to maintain brightness, or a BAM phosphor, which has an original composition and preferred emission color, is simply coated with a protective film, thus forming a phosphor.
- the present invention is characterized by using a phosphor in which the specific crystal plane of a phosphor having a ⁇ alumina phase, that is, the plane lying parallel to the c axis of crystal thereof, is selectively surface-modified with a magnetoplumbite crystal structure that is chemically bonded with the phosphor having a ⁇ alumina phase, particularly the BAM phosphor and is physicochemically similar to a ⁇ alumina phase as the crystal structure of the phosphor.
- the specific crystal plane of a phosphor having a ⁇ alumina phase that is, the plane lying parallel to the c axis of crystal thereof
- a magnetoplumbite crystal structure that is chemically bonded with the phosphor having a ⁇ alumina phase
- BAM phosphor is physicochemically similar to a ⁇ alumina phase as the crystal structure of the phosphor.
- the phosphor used in the present invention has properties that deteriorate little upon high-temperature heat treatment required in the process of manufacturing a lamp when the phosphor is applied to an actual application product such as CCFL.
- CCFL when manufacturing a CCFL, there is less decrease in luminous efficiency or in emission color purity resulting from deterioration of the properties of the phosphor by permeation of water into the crystal structure of the phosphor at high temperature (700 ⁇ 750°C).
- the change in emission color from deep blue to greenish blue increase of y value in C.I.E. color coordinates) does not occur. Thereby, it is possible to fabricate CCFLs/EEFLs having high brightness and little change in color coordinates.
- the phosphor used in the present invention since the phosphor used in the present invention has strong chemical bonding between the magnetoplumbite phase, serving as a protective film, and the ⁇ alumina phase of the phosphor, it is highly resistant to mechanical damage, unlike a conventional BAM phosphor having a simple protective film. Hence, there is no trouble related to mechanical damage accompanied by the use of the phosphor, thereby enabling the fabrication of application products having high quality.
- the phosphor used in the present invention is prepared according to the following processes. For convenience, although methods of preparing the BAM phosphor, wherein M' (m) is Al, are described below, the methods may be applied to other phosphors.
- the present process provides a method of preparing a phosphor by heat treating a
- BAM phosphor having a ⁇ alumina phase in an oxidation atmosphere without the use of additional material to form a magnetoplumbite phase on the BAM phosphor.
- M is Ca, Sr, Ba, or mixtures thereof.
- the ratio of O /N is
- the heating temperature (T) is 800 ⁇ 1200°C, and preferably 950 ⁇ 1050°C.
- the heating time (t) ranges from 1 minute to 10 hours, and preferably from 0.5 hours to 3 hours.
- the heating temperature (T) and heating time (t) may be optimized depending on the amount of BAM of ⁇ alumina phase to be treated, the ratio of O /N , and the heating temperature.
- the magnetoplumbite phase thus formed is 0.5-5 nm thick, and preferably 0.5-2 nm thick.
- the present process provides a method of preparing a phosphor by mixing a BAM phosphor with metal fluoride and then heat treating the mixture at 650 ⁇ 850°C for 0.5-2 hours in an oxidation atmosphere having a ratio of O /N of 0.01-100% to form r & 2 2 a magnetoplumbite phase on the surface of the BAM phosphor.
- metal fluoride examples include divalent metal fluorides, such as MgF , ZnF or SnF , or trivalent metal fluorides, such as AlF or GaF .
- divalent metal fluorides such as MgF , ZnF or SnF
- trivalent metal fluorides such as AlF or GaF .
- the metal fluoride is used
- the present process provides a method of preparing a phosphor by exchanging Ba or Eu ion, present in the conductive layer of a BAM phosphor having a ⁇ alumina phase that has a layered structure wherein spinel layer(MgAl O ) and a conductive layer ⁇ (M , Eu + )O] are continuously laminated, with a cation (M) capable of forming a magnetoplumbite phase and then heat treating such a phosphor in an oxidation atmosphere to form the magnetoplumbite phase on the surface of the BAM phosphor.
- M cation
- the ratio of O /N in the oxidation atmosphere is preferably 0.01-100%, and the heat treatment is preferably conducted at 650 ⁇ 850°C for 0.5-2 hours.
- fluoride of cation able to form the magnetoplumbite phase may be used when exchanging the ion.
- the heat treatment temperature may be decreased to 650 ⁇ 750°C.
- Examples of the cation (M) include Ca + , Sr + , Eu + , La + or Gd + , and the fluoride of cation is used in an amount of 0.001-0.02 g, based on 1 g of the BAM phosphor.
- the BAM phosphor is mixed with the ion exchange material, after which the mixture is heat treated at 650 ⁇ 750°C for 1-2 hours at a heating rate of 10°C/min under controlled oxygen partial pressure and is then cooled at a rate of 10°C/min, thereby preparing a phosphor having water resistance.
- the present process provides preparation of a phosphor by mixing a BAM phosphor of ⁇ alumina phase with metal fluoride and metal nitrate and then heat treating the mixture at 650 ⁇ 750°C for 0.5-2 hours in an inert atmosphere to form a magne- toplumbite phase on the surface of the BAM phosphor.
- the process provides preparation of a phosphor having excellent water resistance, that is, low deterioration of the luminous properties, by simultaneously adopting the process using the metal fluoride (Preparation Process II- 1) and also the process of exchanging the Ba or Eu ion present in the conductive layer of the BAM phosphor with the cation capable of forming the magnetoplumbite phase (Preparation Process II-2).
- the metal fluoride is exemplified by divalent metal fluorides, such as MgF , ZnF or SnF , or trivalent metal fluorides, such as AlF or GaF .
- divalent metal fluorides such as MgF , ZnF or SnF
- trivalent metal fluorides such as AlF or GaF .
- the metal (L) of metal nitrate includes Ca + , Sr + , Eu + , La + or Gd + , and is used in an amount of 0.001-0.02 g, based on 1 g of the BAM phosphor.
- the inert atmosphere may be maintained using nitrogen, argon, or gas mixture thereof.
- M is Mg + or Al +
- L is Ca + , Sr + , or trivalent lanthanide such as Eu +
- the BAM phosphor is mixed with MF (1-20 mmol/g BAM, preferably 18 mmol/g BAM) and L(NO ) yH O (1-10 mmol/g BAM, preferably 6-9 mmol/g BAM)
- the present process provides a method of preparing a phosphor by mixing a BAM phosphor with material having a magnetoplumbite phase and then heat treating the mixture in an inert atmosphere.
- the material having a magnetoplumbite phase is prepared by mixing M X , M (NO
- M is lanthanide such as Eu + , Ce + or La +
- X is Cl “ or NO "
- M is Mg +
- OR is alkoxide.
- the M is preferably used in an amount of 0.002-0.05 mmol, based on 1 g of the BAM phosphor.
- the inert atmosphere includes nitrogen, argon or a gas mixture thereof, and the heat treatment temperature is 800- 1000 0 C.
- the present process includes adding the material having the magnetoplumbite phase to the phosphor, and heat treating the mixture to form a protective film of the magnetoplumbite phase on the surface of the BAM phosphor of ⁇ alumina phase, as simply represented by Reaction 4 below:
- the phosphor in which the magnetoplumbite phase is epitaxially formed on the phosphor having a ⁇ alumina phase, particularly the BAM phosphor [(M , Eu + )MgAl O ], may be used as a blue phosphor or as a green phosphor.
- the lamp using the phosphor according to the present invention may be a monochromatic lamp using only the above phosphor or a monochromatic or polychromatic lamp additionally using one or more other phosphors.
- the above phosphor may be applied to lamps using a typical process known in the art.
- the lamp of the present invention may be a BLU lamp used for display devices, such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or a lamp for use in illumination systems.
- the BLU lamp may be a CCFL or EEFL.
- the present invention provides display devices, such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or illumination systems, each of which includes the lamp mentioned above.
- display devices such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or illumination systems, each of which includes the lamp mentioned above.
- the lamp of the present invention has initial brightness and mechanical properties superior to those of conventional lamps. Further, a phosphor, in which a magne- toplumbite phase as a protective film is epitaxially formed on the surface of a phosphor having a ⁇ alumina phase, particularly a BAM phosphor, is highly resistant to thermal deterioration caused by a lamp manufacturing process and to deterioration by vacuum UV light due to mercury discharge, and thus can prevent a decrease in brightness and a change in color coordinates of the lamp during the lamp manufacturing process and lighting process. Therefore, the lamp manufactured using the above phosphor can have good ability to maintain brightness and color coordinates. Mode for the Invention
- the phosphor was ball milled, washed with water, and then dried, thus obtaining a phosphor having a composition of Ba Eu MgAl O (BAM: Eu 2+ ).
- IPA Isopropyl Alcohol
- BA Butyl Acetate
- the blue phosphor for manufacturing the lamp the phosphors of Preparative Examples 1 and 2 were used.
- As the red and green phosphors conventional phosphors (red-Y O :Eu, and green-(La, Ce)PO :Tb) were used.
- the mixing ratio of trichromatic phosphors was red: 43.60 wt%, green: 33.20 wt%, and blue: 23.20 wt%.
- the slurry was prepared by mixing 500 g of the phosphors with 250 ml of a solution comprising IPA+BA, 40 ml of binding agent slurry, and 2 ml of neutralization solution and adjusting the viscosity of the mixture to 10 sec using an NC (nitrocellulose) solution.
- the mixture solution was rolled for 72 hours and then applied on the lamp.
- the same red/green phosphors were used.
- the change in color coordinates was represented by the difference between the initial color coordinates of the lamp and the color coordinates thereof after 2000 hours. As such, as the difference was decreased, the ability to maintain color coordinates was determined to be good.
- the blue phosphor for manufacturing the lamp the phosphors of Preparative Examples 1 and 2 were used.
- the red and green phosphors conventional phosphors (red-Y O :Eu, and green-(La, Ce)PO :Tb) were used.
- the mixing ratio of trichromatic phosphors was red: 25.8 wt%, green: 27.7 wt%, and blue: 45.5 wt%.
- the slurry was prepared by mixing 500 g of the phosphors with 250 ml of a solution comprising IPA+BA admixed at 50:50, 40 ml of binding agent slurry, and 2 ml of a neutralization solution, and adjusting the viscosity of the mixture to 9.6 sec using an NC solution.
- the mixture solution was rolled for 72 hours and then applied on the lamp.
- the lamp of the present invention has initial brightness and mechanical properties superior to those of conventional lamps.
- a phosphor in which a magne- toplumbite phase as a protective film is epitaxially formed on the surface of a phosphor having a ⁇ alumina phase, particularly a BAM phosphor, is highly resistant to thermal deterioration caused by a lamp manufacturing process and to deterioration by vacuum UV light due to mercury discharge, and thus can prevent a decrease in brightness and a change in color coordinates of the lamp during the lamp manufacturing process and lighting process. Therefore, the lamp manufactured using the above phosphor can have good ability to maintain brightness and color coordinates.
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Abstract
Disclosed herein is a lamp including a specific phosphor and having good ability to maintain brightness and color coordinates. Particularly, this invention provides a lamp using a phosphor in which a magnetoplumbite phase is epitaxially formed on the surface of a phosphor having a β alumina phase.
Description
Description
LAMP HAVING GOOD MAINTENANCE BEHAVIOR OF BRIGHTNESS AND COLOR COORDINATIONS
Technical Field
[1] The present invention relates to a lamp including a specific phosphor and having good ability to maintain brightness and color coordinates, and more particularly, to a lamp using a phosphor in which a magnetoplumbite phase is epitaxially formed on a phosphor having a β alumina phase. This application claims the benefit of the filing date of Korean Patent Application No. 10-2005-0026517, filed on March 30, 2005, in the Korean Intellectual Property Office, the disclosure of which is incorporated herein in its entirety by reference. Background Art
[2] Generally, barium magnesium aluminate (BAM; [(Ba, Eu +)MgAl O ]) phosphors are used in CCFLs (Cold Cathode Fluorescent Lamps) or EEFLs (External Electrode Fluorescent Lamps) for BLUs (Back Light Units) of LCDs or three-wavelength fluorescent lamps.
[3] Unlike other phosphors (red-Y O :Eu or green- (La5Ce)PO :Tb) used for three- wavelength lamps (CCFLs or EEFLs), the BAM phosphor suffers because deterioration, such as low luminous properties, severely occurs in the process of burning an organic material serving as a binder (Binder Burn-Out Step = BBO Step) at 700~750°C upon heat treatment for the fabrication of actual application products, for example, fluorescent lamps, CCFLs, or EEFLs. The deterioration of the BAM phosphor is known as the main reason to cause the deterioration of luminous properties of the phosphors generated under gas discharge during the use of the application product. In particular, it is known that the deterioration (change in color coordinates) of luminous properties of the BAM phosphor greatly affects the change in color coordinates of the three-wavelength lamp.
[4] Thus, depending on the deterioration of the phosphor, the brightness and color coordinates of the lamp are gradually decreased compared to initial lighting. Moreover, the change in color coordinates undesirably results in varied color temperature of the lamp, therefore decreasing performance of display products.
[5] Hence, in order to minimize the deterioration of the BAM phosphor itself, thorough research has been conducted as follows.
[6] Japanese Patent Laid-open Publication No. 2003-82345 discloses a method of oxidizing part of Eu + to Eu + without the use of additional compounds, and a method of forming an oxide film or a fluoride film with the addition of Al, Si or La. Japanese
Patent Laid-open Publication No. 2003-82344 discloses a method of increasing positive charges through substitution of Al or Mg with a tetravalent element (Ti, Zr, Hf, Si, Sn, Ge, or Ce), in order to prevent deterioration of the phosphor. Further, Japanese Patent Laid-open Publication No. 2003-382343 discloses a method of coating BAM with oxide, such as SiO , Al O , ZnO, MgAl O , Ln O , LaPO or Zn SiO , or
2 2 3 2 4 2 3 4 2 4 fluoride such as Si(OF) , La(OF) , or Al(OF) and then heat treating such BAM at
4 3 3
300~600°C in air so as to prevent adsorption of water or carbon dioxide due to the lack of oxygen present in the conductive layer of BAM.
[7] Further, Japanese Patent Laid-open Publication No. 2002-348570 discloses a technique for heat treating a BAM phosphor containing silicon at 500~800°C in air so as to prevent deterioration of the phosphor under vacuum UV light. Korean Patent Laid-open Publication No. 2003-14919 discloses a technique for surface treating only a selective portion of the surface of a phosphor, thereby minimizing a decrease in performance due to coating. Korean Patent Laid-open Publication No. 2002-0025483 discloses a technique for continuously coating the surface of a BAM phosphor with SiO to a thickness of 5-40 nm to cover the surface of the phosphor such that the phosphor does not deteriorate. US Patent No. 5,998,047 discloses a technique for coating the surface of a BAM phosphor with catena polyphosphates such that the phosphor does not deteriorate due to UV light. Japanese Patent Laid-open Publication No. 2000-303065 discloses a technique for coating a BAM phosphor, which is a phosphor for use in vacuum UV light, with borates, phosphates, silicates, halogens, nitrates, sulfates and carbonates containing Ba or Sr as a cation in order to prevent the thermal degradation of the phosphor. Also, Japanese Patent Laid-open Publication No. 2002-080843 discloses a technique for coating a first BAM phosphor with second phosphor powder that emits UV light, to prevent the decrease in performance of the first phosphor.
[8] In addition, research into improvement of the properties of phosphor for increasing the ability to maintain brightness of a lamp as a specific application product example is as follows.
[9] According to Japanese Patent Laid-open Publication Nos. Hei. 11-172244 and
9-231944, Japanese Patent Laid-open Publication Nos. 2002-348570, 2003-147350, 2003-226872, and 2004-244604, when the surface of a phosphor is treated with nitric acid and metal oxide, such as La O , Y O , SiO , or Gd O , to form a 5-100 nm thick of
2 3 2 3 2 2 3 rare earth metal oxide film on the surfaces of the phosphor particles (Japanese Patent Laid-open Publication No. Hei. 11-172244), or when the surface of a phosphor is coated with carbonates of rare earth metal (Japanese Patent Laid-open Publication Nos. 2003-147350, 2003-226872, 2004-244604), deterioration of brightness due to vacuum UV light was reported to decrease. However, the above patents reported only
decreased degree of brightness and not a decrease in initial brightness itself of the phosphor due to coating, and also do not mention ability to maintain color coordinates.
[10] In the case where the protective film is formed on the surface of the phosphor, the luminous efficiency varies with the thickness of the film. When the surface treatment amount is large, the decrease in efficiency is also large but the ability to maintain brightness is good. Further, the surface treatment material may entail a negative result of coagulating phosphor particles due to its action as a binder, as well as the positive function as a protective film. The phosphor thus coagulated exhibits poor dispersiblity upon actual use and therefore cannot be formed into a uniform coating film, undesirably leading to non-uniform color coordinates or brightness. Disclosure of Invention Technical Problem
[11] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a lamp using a phosphor having high initial brightness and good ability to maintain brightness and color coordinates. Technical Solution
[12] The present invention provides to a lamp using a phosphor in which a magne- toplumbite phase is epitaxially formed on the surface of a phosphor having a β alumina phase.
[13] As for the phosphor having a β alumina phase, a BAM phosphor, particularly [(M ,
Eu2+)MgAl O ] or [(M11, Eu2+)(Mg, Mn)Al O ], wherein the Mπ is Ba, Ca, Sr or mixtures thereof, and part of or all of the AIs are substituted with Ga, may be used
[14] The magnetoplumbite phase may be formed without the use of additional compounds, or may be formed through chemical bonding with material having a magnetoplumbite (MP) structure.
[15] The lamp may be used as BLU lamps, for example, CCFLs or EEFLs, for use in display devices such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or as lamps for illumination systems.
[16] The magnetoplumbite is a material having a structure very similar to β alumina phase, and, as an example, the magnetoplumbite may be a material represented by Formula 1 below:
[17] Formula 1
[18] M (II)M'(III) O
1 12 19
[19] in Formula 1, M (II) is Ca, Sr, Pb or Eu, and M'(III)is Al, Ga or mixtures thereof.
[20] In addition, as an example, the magnetoplumbite may be represented by Formula 2 below:
[21] Formula 2
[22] M 2 (m>M"(II)M'(III)
11O19
[23] in Formula 2, M (III) is lanthanide including La, Ce, Pr, Nd, Sm, Eu or Gd, M"(π)is Ni, Co, Fe, Mn or Mg, and M'(III)is Al, Ga or mixtures thereof.
[24] In addition, as an example, the magnetoplumbite may be represented by Formula 3 below:
[25] Formula 3
[26] M3 010M^ nO18
[27] in Formula 3, M Iπ is La, Ce or mixtures thereof, and M' m is Al, Ga or mixtures thereof.
[28] The magnetoplumbite phase selectively chemically surface-modifies only the specific crystal plane of the phosphore having a β alumina phase, particularly the BAM phosphor, that is, the crystal plane lying parallel to the c axis of the crystal thereof.
[29] According to conventional techniques, a BAM phosphor having a changed composition is heat treated to improve only ability to maintain brightness, or a BAM phosphor, which has an original composition and preferred emission color, is simply coated with a protective film, thus forming a phosphor. However, the present invention is characterized by using a phosphor in which the specific crystal plane of a phosphor having a β alumina phase, that is, the plane lying parallel to the c axis of crystal thereof, is selectively surface-modified with a magnetoplumbite crystal structure that is chemically bonded with the phosphor having a β alumina phase, particularly the BAM phosphor and is physicochemically similar to a β alumina phase as the crystal structure of the phosphor. The advantages and effects of the phosphor used in the present invention are described below.
[30] First, the phosphor used in the present invention has properties that deteriorate little upon high-temperature heat treatment required in the process of manufacturing a lamp when the phosphor is applied to an actual application product such as CCFL. For example, when manufacturing a CCFL, there is less decrease in luminous efficiency or in emission color purity resulting from deterioration of the properties of the phosphor by permeation of water into the crystal structure of the phosphor at high temperature (700~750°C). For example, according to the present invention, the change in emission color from deep blue to greenish blue (increase of y value in C.I.E. color coordinates) does not occur. Thereby, it is possible to fabricate CCFLs/EEFLs having high brightness and little change in color coordinates.
[31] Second, in application products manufactured using the above phosphor, performance thereof, for example, over time, brightness is decreased less and color coordinates is changed less compared to application products manufactured using a conventional BAM phosphor, and therefore the lifetime of the product manufactured using
the above phosphor can be increased.
[32] Third, since the phosphor used in the present invention has strong chemical bonding between the magnetoplumbite phase, serving as a protective film, and the β alumina phase of the phosphor, it is highly resistant to mechanical damage, unlike a conventional BAM phosphor having a simple protective film. Hence, there is no trouble related to mechanical damage accompanied by the use of the phosphor, thereby enabling the fabrication of application products having high quality.
[33] The phosphor used in the present invention is prepared according to the following processes. For convenience, although methods of preparing the BAM phosphor, wherein M'(m) is Al, are described below, the methods may be applied to other phosphors.
[34] (Preparation Process I)
[35] The present process provides a method of preparing a phosphor by heat treating a
BAM phosphor having a β alumina phase in an oxidation atmosphere without the use of additional material to form a magnetoplumbite phase on the BAM phosphor.
[36] This process is represented by Reaction 1 below:
[37] Reaction 1
[38]
O2ZN2 ^1Eu2+)MgAI1A7 >- Eu3+MgAl11O19 + (M^Eu2+)MgAI10O17 heating l ' * lυ "
(Temp -T. Tinned)
_ „ , , _ a . ,„, protective layer „
BAM of βphasfid) of MP phase BAM of P phase(2)
[39]
[40] In Reaction 1, M is Ca, Sr, Ba, or mixtures thereof. The ratio of O /N is
0.01-100%, preferably 0.01-10%, and more preferably 0.1-5%. The heating temperature (T) is 800~1200°C, and preferably 950~1050°C. The heating time (t) ranges from 1 minute to 10 hours, and preferably from 0.5 hours to 3 hours. The heating temperature (T) and heating time (t) may be optimized depending on the amount of BAM of β alumina phase to be treated, the ratio of O /N , and the heating temperature. The magnetoplumbite phase thus formed is 0.5-5 nm thick, and preferably 0.5-2 nm thick.
[41] (Preparation Process II) Formation of Magnetoplumbite Phase at Low Temperatures
[42] (Preparation Process II- 1)
[43] The present process provides a method of preparing a phosphor by mixing a BAM phosphor with metal fluoride and then heat treating the mixture at 650~850°C for 0.5-2 hours in an oxidation atmosphere having a ratio of O /N of 0.01-100% to form r & 2 2
a magnetoplumbite phase on the surface of the BAM phosphor.
[44] Examples of the metal fluoride include divalent metal fluorides, such as MgF , ZnF or SnF , or trivalent metal fluorides, such as AlF or GaF . The metal fluoride is used
2 3 3 in an amount of 0.001-0.02 g, and preferably 0.001-0.01 g, based on 1 g of the BAM phosphor.
[45] (Preparation Process II-2)
[46] The present process provides a method of preparing a phosphor by exchanging Ba or Eu ion, present in the conductive layer of a BAM phosphor having a β alumina phase that has a layered structure wherein spinel layer(MgAl O ) and a conductive layer{(M , Eu +)O] are continuously laminated, with a cation (M) capable of forming a magnetoplumbite phase and then heat treating such a phosphor in an oxidation atmosphere to form the magnetoplumbite phase on the surface of the BAM phosphor. The ratio of O /N in the oxidation atmosphere is preferably 0.01-100%, and the heat treatment is preferably conducted at 650~850°C for 0.5-2 hours. In this case, in order to decrease the heat treatment temperature, fluoride of cation able to form the magnetoplumbite phase may be used when exchanging the ion. In the case where the fluoride of cation is used, the heat treatment temperature may be decreased to 650~750°C.
[47] Examples of the cation (M) include Ca +, Sr +, Eu +, La + or Gd +, and the fluoride of cation is used in an amount of 0.001-0.02 g, based on 1 g of the BAM phosphor.
[48] According to this process, the BAM phosphor is mixed with the ion exchange material, after which the mixture is heat treated at 650~750°C for 1-2 hours at a heating rate of 10°C/min under controlled oxygen partial pressure and is then cooled at a rate of 10°C/min, thereby preparing a phosphor having water resistance.
[49] This process is represented by Reaction 2 below:
[50] Reaction 2
[51] <Preparation Process II-2 using Ion Exchange Step>
[52]
controlled oxygen
controlled oxygen partial pressure
[53]
[54] 1) The BAM phosphor is mixed with MF at a predetermined ratio, after which the mixture is heat treated at 650~750°C while maintaining predetermined oxygen partial pressure.
[55] 2) The MF of 1) may be prepared according to the following procedure:
[56] M(NO ) yH O + xNH F → MF + xNH NO + yH O
3 x 2 4 x 4 3 -7 2
[57] (Preparation Process II-3)
[58] The present process provides preparation of a phosphor by mixing a BAM phosphor of β alumina phase with metal fluoride and metal nitrate and then heat treating the mixture at 650~750°C for 0.5-2 hours in an inert atmosphere to form a magne- toplumbite phase on the surface of the BAM phosphor.
[59] That is, the process provides preparation of a phosphor having excellent water resistance, that is, low deterioration of the luminous properties, by simultaneously adopting the process using the metal fluoride (Preparation Process II- 1) and also the
process of exchanging the Ba or Eu ion present in the conductive layer of the BAM phosphor with the cation capable of forming the magnetoplumbite phase (Preparation Process II-2).
[60] The metal fluoride is exemplified by divalent metal fluorides, such as MgF , ZnF or SnF , or trivalent metal fluorides, such as AlF or GaF . Such metal fluoride is
2 3 3 preferably used in an amount of 0.001-0.02 g, based on 1 g of the BAM phosphor. In the present process, the amount of MF , such as MgF or AlF , may be controlled, x 2 3 thereby changing the heat treatment temperature. [61] The metal (L) of metal nitrate includes Ca +, Sr +, Eu +, La + or Gd +, and is used in an amount of 0.001-0.02 g, based on 1 g of the BAM phosphor. [62] The inert atmosphere may be maintained using nitrogen, argon, or gas mixture thereof. [63] According to the present process, the BAM phosphor is uniformly mixed with the additives and then dried to obtain a mixed phosphor which is then heat treated at
650~850°C for 0.5-2 hours at a heating rate of 10°C/min in a controlled inert atmosphere and is thereafter cooled at a rate of 10°C/min, thereby preparing the phosphor used in the present invention. [64] This process, which is used to promote the formation of the magnetoplumbite phase, simultaneously adopts the processes of II- 1 and II-2, represented by Reaction 3 below:
[65] Reaction 3
[66]
[69] 1) The BAM phosphor is mixed with MF (1-20 mmol/g BAM, preferably 18 mmol/g BAM) and L(NO ) yH O (1-10 mmol/g BAM, preferably 6-9 mmol/g BAM)
3 x 2 at a predetermined ratio, and the mixture is heat treated at 650~850°C in an inert atmosphere such as nitrogen atmosphere.
[70] 2) MF and L(NO ) yH O of 1) may be prepared using the following stock x 3 x 2 solutions:
[71] Stock solutions of M(NO ) yH O, x(NH )F, L(NO ) zH O
3 x 2 4 3 w 2 [72] (Preparation Process III) [73] The present process provides a method of preparing a phosphor by mixing a BAM phosphor with material having a magnetoplumbite phase and then heat treating the mixture in an inert atmosphere.
[74] The material having a magnetoplumbite phase is prepared by mixing M X , M (NO
) and Al(OR) , in which M is lanthanide such as Eu +, Ce + or La +, X is Cl" or NO ", M is Mg +, and OR is alkoxide. The M is preferably used in an amount of 0.002-0.05 mmol, based on 1 g of the BAM phosphor.
[75] The inert atmosphere includes nitrogen, argon or a gas mixture thereof, and the heat treatment temperature is 800- 10000C.
[76] The present process includes adding the material having the magnetoplumbite phase to the phosphor, and heat treating the mixture to form a protective film of the magnetoplumbite phase on the surface of the BAM phosphor of β alumina phase, as simply represented by Reaction 4 below:
[77] Reaction 4
[78]
(BafEu2')MgA[10O17 (83,Eu2+)MgAI10O17
BAM of p phase CD BAM of β phase (2) n itrogen
+ *- * h eatin g
Λ* «ι lift i» >. 2+ Λ« ■■ . I \ protective laver of M P phase
[79]
[80] The phosphor, in which the magnetoplumbite phase is epitaxially formed on the phosphor having a β alumina phase, particularly the BAM phosphor [(M , Eu +)MgAl O ], may be used as a blue phosphor or as a green phosphor. The lamp using the phosphor according to the present invention may be a monochromatic lamp using only the above phosphor or a monochromatic or polychromatic lamp additionally using one or more other phosphors. The above phosphor may be applied to lamps using a typical process known in the art.
[81] The lamp of the present invention may be a BLU lamp used for display devices, such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or a lamp for use in illumination systems. The BLU lamp may be a CCFL or EEFL.
[82] Further, the present invention provides display devices, such as fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs, or illumination systems, each of which includes the lamp mentioned above.
Advantageous Effects
[83] The lamp of the present invention has initial brightness and mechanical properties superior to those of conventional lamps. Further, a phosphor, in which a magne-
toplumbite phase as a protective film is epitaxially formed on the surface of a phosphor having a β alumina phase, particularly a BAM phosphor, is highly resistant to thermal deterioration caused by a lamp manufacturing process and to deterioration by vacuum UV light due to mercury discharge, and thus can prevent a decrease in brightness and a change in color coordinates of the lamp during the lamp manufacturing process and lighting process. Therefore, the lamp manufactured using the above phosphor can have good ability to maintain brightness and color coordinates. Mode for the Invention
[84] A better understanding of the present invention may be obtained through the following examples which are set forth to illustrate, but are not to be construed as the limit of the present invention.
[85] <Preparative Example 1>
[86] Ba, Eu, Mg and Al were mixed together at a molar ratio of 0.9:0.1 : 1.0: 10, and AlF was added thereto as flux in a predetermined amount. The mixture was burned at 14000C for 2 hours in a gas mixture atmosphere comprising nitrogen/hydrogen mixed at a volume ratio of 95:5.
[87] After the completion of the burning process, the phosphor was ball milled, washed with water, and then dried, thus obtaining a phosphor having a composition of Ba Eu MgAl O (BAM: Eu2+).
0 1 10 17
[88] <Preparative Example 2>
[89] 200 g of the BAM:Eu + phosphor prepared in Preparative Example 1 was placed in a furnace, maintained at 95O0C for 2 hours at a heating rate of 5°C/min while supplying the gas mixture of N +O (a volume ratio of 99.9:0.1), and then cooled at a rate of 5°C/min, thus obtaining a desired phosphor.
[90] <Preparative Example 3>
[91] 500 g of the BAM:Eu + phosphor prepared in Preparative Example 1 was mixed with 1.25 g of AlF , after which the mixture was placed in a furnace, maintained at 75O0C for 1 hour at a heating rate of 5°C/min while supplying the gas mixture of N +air(2.5 wt% air/N +air gas mixture), and then cooled at a rate of 5°C/min, thus obtaining a desired phosphor.
[92] <Preparative Example 4>
[93] 1 g of the BAM:Eu + phosphor prepared in Preparative Example 1, 0.2975 mmol
(0.0608 g) of aluminum isopropoxide (Al(O1Pr) ), 0.0035 mmol (0.00152 g) of cerium nitrate (Ce(NO ) -(6H O)), and 0.0215 mmol (0.0093 g) of lanthanum nitrate (La(NO ) •(6H O)) were stirred along with 10 ml of distilled water and then heated to remove the solvent. The dried phosphor powder was heat treated at 9000C for 2 hours in a nitrogen atmosphere (heating rate: 10°C/min), thus obtaining a desired phosphor.
[94] Experimental Example 1> [95] Deterioration Test of Monochromatic CCFL by Vacuum UV light [96] The color coordinates of the phosphor of the present invention in a powder state and the color coordinates thereof after manufacturing the CCFL through a BBO step were compared with the change in color coordinates of a conventional BAM phosphor without a protective film, and the extent of decrease in luminous properties was measured (thermal deterioration). As the extent of change (Δx, Δy) was decreased, the ability to maintain color coordinates of the phosphor was judged to be excellent.
[97] Upon manufacturing the lamp, the phosphors prepared in Preparative Examples 1 and 2 were used. 500 g of the blue phosphor was mixed with 250 ml of a solution comprising IPA (Isopropyl Alcohol) and BA (Butyl Acetate) admixed at 50:50, 40 ml of bonding agent slurry, and 2 ml of neutralization solution, and the viscosity was adjusted to 10 sec using a solution of NC (Nitrocellulose). The mixture solution was rolled for 72 hours and then applied on the lamp. The size of the lamp for the experiment was set to Φ=2.4 mm and L=400 mm.
[98] Using the phosphors prepared in Preparative Examples 1 and 2, a blue monochromatic CCFL was manufactured and then measured for luminous properties thereof. The results are given in Table 1 below. From these results, it can be seen that the lamp using the phosphor prepared in Preparative Example 2 has luminous properties superior to the lamp manufactured using the conventional BAM phosphor (Preparative Example 1).
[99] Such results were obtained by comparing the measurement value immediately after manufacturing the lamp (0 hours) with the measurement value of the phosphor in a powder state, excluding the deterioration due to vacuum UV light under mercury vapor. The phosphor of Preparative Example 2 was more resistant to thermal deterioration caused by the lamp manufacturing process (BBO step) than was the conventional phosphor (Preparative Example 1).
[100] Table 1
[101] [Note] 1. Relative Brightness after heat treatment at 6000C was taken as 100% [102] 2. Φ=2.4 mm, L=400mm, [103] 3. Difference between color coordinates of phosphor in powder state after heat
treatment at 6000C and color coordinates thereof after manufacturing the lamp
[104] [105] Experimental Example 2> [106] Lifetime Test of Monochromatic CCFL [107] The lifetime test (700 hours) of the CCFL manufactured in Experimental Example 1 was conducted. The results are given in Table 2 below. The change in color coordinates (Δx, Δy) was represented by the difference between the initial color coordinates of the lamp and the color coordinates thereof after 700 hours. Hence, unlike in Experimental Example 1, the difference of color coordinates observed in Experimental Example 2 shows the deterioration of the phosphor due to vacuum UV light under mercury vapor. As the above difference was decreased, the ability to maintain color coordinates was judged to be good.
[108] In the properties (ability to maintain brightness/color coordinate) of the phosphor prepared in Preparative Example 2, the brightness maintenance was increased by 13% and the changes in color coordinates (Δx, Δy) were 45% and 50%, respectively, compared to the conventional BAM phosphor (Preparative Example 1). From these results, the phosphor of Preparative Example 2 was confirmed to be resistant to deterioration of phosphor in vacuum UV light.
[109] Table 2
[HO] [Note] 1. The brightness of lamp at 0 hours was taken as 100% (Φ=2.4 mm, L=400mm,) [111] 2. Difference between color coordinates (x,y) of lamp at 0 hours and color coordinates thereof after 700 hours
[112] [113] Experimental Example 3> [114] Lifetime Test of Trichromatic CCFL [115] In order to evaluate the effects of the phosphor according to the present invention and the conventional BAM phosphor on the deterioration of a trichromatic lamp (CCFL), a trichromatic lamp was manufactured using the same red-Y O :Eu and green- (La5Ce)PO :Tb phosphors and the lifetime test (2000 hours) was conducted.
4
[116] As the blue phosphor for manufacturing the lamp, the phosphors of Preparative Examples 1 and 2 were used. As the red and green phosphors, conventional phosphors
(red-Y O :Eu, and green-(La, Ce)PO :Tb) were used. The mixing ratio of trichromatic phosphors was red: 43.60 wt%, green: 33.20 wt%, and blue: 23.20 wt%. The slurry was prepared by mixing 500 g of the phosphors with 250 ml of a solution comprising IPA+BA, 40 ml of binding agent slurry, and 2 ml of neutralization solution and adjusting the viscosity of the mixture to 10 sec using an NC (nitrocellulose) solution. The mixture solution was rolled for 72 hours and then applied on the lamp. The size of the lamp for experiment was set to Φ=2.4 mm and L=400 mm, and the mean color coordinates of the lamp were x = 0.3 and y = 0.3.
[117] The initial color coordinates of the lamp were set as (x,y=0.3) in all experiments. The same red/green phosphors were used. Thus, the deterioration of the properties of the lamp was judged based on the deterioration of the properties of the blue phosphor used. The change in color coordinates was represented by the difference between the initial color coordinates of the lamp and the color coordinates thereof after 2000 hours. As such, as the difference was decreased, the ability to maintain color coordinates was determined to be good.
[118] The results of the lifetime test (2000 hours) of the trichromatic CCFL manufactured using each of the phosphor of Preparative Example 2 and the conventional BAM phosphor (Preparative Example 1) are given in Table 3 below. In the properties (ability to maintain brightness/color coordinate) of the phosphor prepared in Preparative Example 2, the brightness maintenance was increased by 4% and the changes in color coordinates (Δx, Δy) were 31% and 36%, respectively, compared to the conventional BAM phosphor (Preparative Example 1). From these results, the properties (ability to maintain brightness/color coordinate) of the trichromatic CCFL manufactured using the phosphor of Preparative Example 2 were confirmed to be superior to those of the lamp manufactured using the conventional BAM phosphor.
[119] Table 3
[120] [Note] 1. The brightness of lamp at 0 hours was taken as 100% (Φ=2.4 mm, L=400mm,) [121] 2. Difference between color coordinates (x,y) of lamp at 0 hours and color coordinates thereof after 2000 hours
[122] [123] Experimental Example 4>
[124] Lifetime Test of Trichromatic EEFL [125] In order to evaluate the effects of the phosphor of the present invention and the conventional BAM phosphor on deterioration of trichromatic lamp (EEFL), a comparison experiment similar to Experimental Example 3 was conducted.
[126] As the blue phosphor for manufacturing the lamp, the phosphors of Preparative Examples 1 and 2 were used. As the red and green phosphors, conventional phosphors (red-Y O :Eu, and green-(La, Ce)PO :Tb) were used. The mixing ratio of trichromatic phosphors was red: 25.8 wt%, green: 27.7 wt%, and blue: 45.5 wt%. The slurry was prepared by mixing 500 g of the phosphors with 250 ml of a solution comprising IPA+BA admixed at 50:50, 40 ml of binding agent slurry, and 2 ml of a neutralization solution, and adjusting the viscosity of the mixture to 9.6 sec using an NC solution. The mixture solution was rolled for 72 hours and then applied on the lamp. The size of the lamp for experiment was set to Φ=4.0 mm and L=600 mm, and the mean color coordinates of the lamp were x = 0.248 and y = 0.224.
[127] Since the same red/green phosphors were used, the deterioration of the properties of the lamp could be judged based on the deterioration of the properties of the blue phosphor used. The change in color coordinates was represented by the difference between the initial color coordinates of the lamp and the color coordinates thereof after 1000 hours. As such, as the difference was decreased, the ability to maintain color coordinates was determined to be good.
[128] The results of the lifetime test (1000 hours) of the trichromatic EEFL manufactured using each of the phosphor of Preparative Example 2 and the conventional BAM phosphor (Preparative Example 1) are given in Table 4 below. In the properties (ability to maintain brightness/color coordinate) of the phosphor prepared in Preparative Example 2, the brightness maintenance was increased by 1.6 % and the changes in color coordinates (Δx, Δy) were 41.7% and 36.4%, respectively, compared to the conventional BAM phosphor (Preparative Example 1). From these results, the properties (ability to maintain brightness/color coordinate) of the trichromatic EEFL manufactured using the phosphor of Preparative Example 2 were confirmed to be superior to those of the lamp manufactured using the conventional BAM phosphor.
[129] Table 4
[130] [Note] 1. The brightness of lamp at 0 hours was taken as 100% (Φ=4.0 mm,
L=600mm,)
[131] 2. Difference between color coordinates (x,y) of lamp at 0 hours and color coordinates thereof after 1000 hours
[132]
Industrial Applicability
[133] The lamp of the present invention has initial brightness and mechanical properties superior to those of conventional lamps. Further, a phosphor, in which a magne- toplumbite phase as a protective film is epitaxially formed on the surface of a phosphor having a β alumina phase, particularly a BAM phosphor, is highly resistant to thermal deterioration caused by a lamp manufacturing process and to deterioration by vacuum UV light due to mercury discharge, and thus can prevent a decrease in brightness and a change in color coordinates of the lamp during the lamp manufacturing process and lighting process. Therefore, the lamp manufactured using the above phosphor can have good ability to maintain brightness and color coordinates. Such results greatly affect the ability to maintain brightness and color coordinates of trichromatic CCFL/EEFLs manufactured using the same red/green phosphors. Consequently, the CCFL/EEFLs using the phosphor can have high ability to maintain brightness and color coordinates.
[134] Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
[135]
Claims
[I] A lamp, using a phosphor in which a magnetoplumbite phase is epitaxially formed on a surface of a phosphor having a βalumina phase.
[2] The lamp according to claim 1, wherein the phosphor having a β alumina phase includes a BAM phosphor [(M11, Eu2+)MgAl1 O17] or [(M11, Eu2+)(Mg, Mn)Al1 O17 ] (where M is Ba, Ca, Sr, or mixtures thereof, and part of or all of AIs can be substituted with Ga).
[3] The lamp according to claim 1, wherein the phosphor having a β alumina phase is a blue phosphor or a green phosphor.
[4] The lamp according to claim 1, which is a monochromatic lamp or a polychromatic lamp.
[5] The lamp according to claim 1, which is used for a back light unit of a display device.
[6] The lamp according to claim 5, wherein the display device is selected from the group consisting of fluorescent display plates, X-ray photographic tubes, LCDs, PDPs, and CRTs.
[7] The lamp according to claim 5, which is a cold cathode fluorescent lamp or an external electrode fluorescent lamp.
[8] The lamp according to claim 1, which is used for an illumination system.
[9] The lamp according to claim 1, wherein the magnetoplumbite phase comprises material represented by Formula 1, 2, or 3 below: Formula 1 M 1 (π)M'(πi) 12 O 19
Formula 2
M 2 (III)M"(II)M'(m) 11 O 19
Formula 3
M (m)M'(III) O
3 11 18 wherein M (II) is Ca, Sr, Pb or Eu, M'(πi) is Al, Ga or mixtures thereof,
M (III) is lanthanide including La, Ce, Pr, Nd, Sm, Eu or Gd, M"(II)is Ni, Co, Fe, Mn or Mg, and M (III) is La, Ce or mixtures thereof.
[10] The lamp according to claim 1, wherein the magnetoplumbite phase is 0.5-5 nm thick.
[I I] The lamp according to claim 1, wherein the magnetoplumbite phase selectively chemically surface-modifies a crystal plane lying parallel to a c axis of crystal of the phosphor having a βalumina phase.
[12] A display device, comprising the lamp of any one of claims 1 to 11.
[13] The display device according to claim 12, which is selected from the group consisting of fluorescent display plates, X-ray photographic tubes, LCDs, PDPs and CRTs. [14] An illumination system, comprising the lamp of any one of claims 1 to 4 and claims 9-11.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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EP06732731A EP1888709A4 (en) | 2005-03-30 | 2006-03-29 | Lamp having good maintenance behavior of brightness and color coordinations |
CNA200680001090XA CN101124297A (en) | 2005-03-30 | 2006-03-29 | Lamp having good maintenance behavior of brightness and color coordinations |
JP2007536624A JP2008517092A (en) | 2005-03-30 | 2006-03-29 | Long life and high color coordinate retention lamp |
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KR20050026517 | 2005-03-30 | ||
KR10-2005-0026517 | 2005-03-30 |
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WO2006109938A1 true WO2006109938A1 (en) | 2006-10-19 |
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PCT/KR2006/001150 WO2006109938A1 (en) | 2005-03-30 | 2006-03-29 | Lamp having good maintenance behavior of brightness and color coordinations |
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US (1) | US7652416B2 (en) |
EP (1) | EP1888709A4 (en) |
JP (1) | JP2008517092A (en) |
KR (1) | KR100758101B1 (en) |
CN (1) | CN101124297A (en) |
TW (1) | TWI319777B (en) |
WO (1) | WO2006109938A1 (en) |
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US7736536B2 (en) * | 2006-07-11 | 2010-06-15 | Intematix Corporation | Compositions comprising a mixture of a BAM phosphor and at least one other hexaaluminate |
KR20100022405A (en) * | 2008-08-19 | 2010-03-02 | 삼성에스디아이 주식회사 | Blue bam phosphor for plasma display panel and plasma display panel having phosphor layer formed of the same |
US20100133987A1 (en) * | 2008-12-02 | 2010-06-03 | Industrial Technology Research Institute | Phosphor and white light illumiantion device utilizing the same |
US8358059B2 (en) * | 2008-12-02 | 2013-01-22 | Industrial Technology Research Institute | Phosphor, white light illumination device and solar cell utilizing the same |
TWI406928B (en) * | 2010-03-18 | 2013-09-01 | Ind Tech Res Inst | Blue phosphors, white light illumination devices and solar cells utilizing the same |
WO2018207703A1 (en) * | 2017-05-11 | 2018-11-15 | 三菱ケミカル株式会社 | Light emitting device and phosphor |
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- 2006-03-29 EP EP06732731A patent/EP1888709A4/en not_active Withdrawn
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Also Published As
Publication number | Publication date |
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KR100758101B1 (en) | 2007-09-11 |
TWI319777B (en) | 2010-01-21 |
KR20060106744A (en) | 2006-10-12 |
US20060238101A1 (en) | 2006-10-26 |
CN101124297A (en) | 2008-02-13 |
TW200644035A (en) | 2006-12-16 |
JP2008517092A (en) | 2008-05-22 |
US7652416B2 (en) | 2010-01-26 |
EP1888709A1 (en) | 2008-02-20 |
EP1888709A4 (en) | 2010-12-08 |
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