WO2006051601A1 - 表示装置用蛍光体とその製造方法、およびそれを用いた電界放射型表示装置 - Google Patents
表示装置用蛍光体とその製造方法、およびそれを用いた電界放射型表示装置 Download PDFInfo
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- WO2006051601A1 WO2006051601A1 PCT/JP2004/016860 JP2004016860W WO2006051601A1 WO 2006051601 A1 WO2006051601 A1 WO 2006051601A1 JP 2004016860 W JP2004016860 W JP 2004016860W WO 2006051601 A1 WO2006051601 A1 WO 2006051601A1
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- phosphor
- layer
- zinc sulfide
- display device
- indium
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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
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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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
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
- C09K11/582—Chalcogenides
- C09K11/584—Chalcogenides with zinc or cadmium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
- H01J29/02—Electrodes; Screens; Mounting, supporting, spacing or insulating thereof
- H01J29/10—Screens on or from which an image or pattern is formed, picked up, converted or stored
- H01J29/18—Luminescent screens
- H01J29/20—Luminescent screens characterised by the luminescent material
Definitions
- Phosphor for display device method for manufacturing the same, and field emission display device using the same
- the present invention relates to a phosphor for a display device, a method for manufacturing the same, and a field emission display device using the same.
- field emission display devices field emission display; FED
- electron-emitting devices such as field-emission cold cathode devices display various information in a precise and high-definition manner.
- FED field emission display
- field-emission cold cathode devices display various information in a precise and high-definition manner.
- the basic display principle of FED is the same as that of a cathode ray tube (CRT), and a phosphor is excited by an electron beam to emit light.
- the acceleration voltage (excitation voltage) of the electron beam is 3 to 15 kV, which is lower than that of the CRT, and the current density due to the electron beam is increasing.
- sufficient knowledge has been obtained about the light emission characteristics of the phosphor under such a low voltage / high current density excitation.
- the phosphor constituting the phosphor layer is required to have resistance against an electron beam having a high current density.
- the deterioration of luminance due to electron beam impact can be suppressed by changing the crystal structure of the zinc sulfide phosphor from cubic to hexagonal.
- the hexagonal zinc sulfide phosphor is effective in suppressing luminance deterioration due to a high current density electron beam, the emission color is reduced to the short wavelength side by using a hexagonal crystal structure. It had a problem of shifting. Therefore, there is a strong demand for realizing a high-luminance blue-emitting phosphor and green-emitting phosphor for FED.
- the blue color purity (chromaticity) is increased.
- a zinc sulfide phosphor (ZnS: Ag, A1) using silver (Ag) and aluminum (A1) as an activator has been used as the phosphor with the highest luminance. It has been done.
- phosphors based on zinc sulfide have a problem in that they are easily deteriorated due to high current density electron beams and the emission luminance tends to decrease immediately.
- phosphors for display devices low voltage phosphors
- a metal salt or metal oxide is coated on the surface of the phosphor matrix (ZnS).
- ZnS phosphor matrix
- an activator is doped on the surface of a phosphor matrix by heat treatment after coating (see Patent Document 2).
- activators such as Mn, Cu, Au, and Ag are doped.
- the activator doping technique described in Patent Document 2 only increases the light emission efficiency of a low-voltage electron beam having a shallow penetration depth, and the high-current-density electron of the zinc sulfide phosphor. The luminance deterioration due to the line could not be sufficiently suppressed.
- Patent Document 1 JP-A-2002-226847 (Page 2-3)
- Patent Document 2 Japanese Patent No. 2914631 (Japanese Patent Laid-Open No. 10-338870)
- the problem to be solved by the present invention is that zinc sulfide phosphors used in display devices such as field emission display devices (FEDs) are time-dependent due to excitation of electron beams with high emission density. It is a point that deteriorates.
- FEDs field emission display devices
- the inventors of the present invention have proposed that the surface of zinc sulfide phosphor particles used in display devices such as FEDs is made of indium, yttrium (Y), aluminum (A1), magnesium (Mg), and other metals.
- Y yttrium
- A1 aluminum
- Mg magnesium
- the luminance is obtained only when the indium oxide (InO) layer is formed
- the phosphor for display device of the present invention at least a part of the surface of the zinc sulfide phosphor particle is It is characterized by being covered with a layer of indium oxide (In 2 O 3).
- the phosphor for a display device in which at least a part of the surface of the zinc sulfide phosphor particles is covered with a layer of indium oxide (In 2 O 3).
- the zinc sulfide phosphor on which the indium hydroxide layer is formed includes a step of heat-treating the indium hydroxide to indium oxide.
- the phosphor for a display device of the present invention it is possible to improve luminance deterioration with time due to excitation of electron beam with low voltage and high current density, and also, emission color required for a light emitting component for FED (Light emission chromaticity) can be satisfied. Therefore, by using such a phosphor, FED with improved display characteristics such as color reproducibility and reliability can be achieved while addressing the high current density of the electron beam that excites the phosphor layer. It becomes possible to provide.
- FIG. 1 is a cross-sectional view showing a configuration example of a field emission display device (FED) according to an embodiment of the present invention.
- FED field emission display device
- FIG. 2 is a graph showing the relationship between the total amount of charge injected by electron beam irradiation and the light emission luminance in Example 1 of the present invention.
- a first embodiment of the present invention is a phosphor for a display device that is excited by an electron beam having a low voltage and a high current density, and at least a part of the surface of the zinc sulfide phosphor particle is indium oxide.
- the zinc sulfide phosphor As the zinc sulfide phosphor, a phosphor based on zinc sulfide that emits blue or green light when irradiated with an electron beam having an acceleration voltage of 15 kV or less (eg, 3 to 15 kV) is used.
- a desired luminescent color can be obtained based on the type and amount of the activator contained in zinc sulfide as the phosphor matrix. For example, by containing Ag and A1 or C1 as an activator, a blue emission color can be obtained. By adding Cu, Au and Al, a green emission color can be obtained.
- blue-emitting zinc sulfide phosphors include the general formula: ZnS: Ag, Al
- Ag is the first activator (main activator) that forms the luminescent center, and is 1 X 10_ 5 — 2 X 10_ 3 g for zinc sulfide lg, which is the phosphor matrix. It is preferable to make it contain in the range. It is less than 1 X 10- 5 g relative to the content of the first activator is zinc sulfide lg, also beyond the 2 X 10- 3 g emission luminance and emission chromaticity is reduced. Content of the first activator is zinc sulfide lg against 3 X 10- 5 - 1. 5 X 10- 3 properly preferred is more preferable gesture et to g range of 5 X 10-5 in the range of -1 X 10- 3 g.
- A1 is a second activator (co-activator) that is directly excited by an electron beam, and the first activator is excited by the excitation energy of the second activator.
- the emission luminance of the zinc sulfide phosphor (for example, ZnS: Ag) can be increased by causing the phosphor to emit light.
- the content of the second activator is, 1 X 10- 5 zinc sulfide lg is a phosphor host - 5 X 10- 3 g range and to Rukoto are preferred.
- Derconnection also less than 1 X 10- 5 g with respect to the second activator content is zinc sulfide lg of, also exceed 5 X 10- 3 g reduces the emission brightness, also emission chromaticity to degrade.
- the content of the second activator should be in the range of 5 X 10_ 5 — 2 X 10— 3 g with respect to lg zinc sulfide. More preferably, 1 X 10— 4 — 1 X 10 — The range is 3 g.
- a green-emitting zinc sulfide phosphor As a specific example of a green-emitting zinc sulfide phosphor, a general formula: ZnS: Cu, Au, Al, (wherein c, d and e in the formula cde are zinc sulfide lg which is a phosphor matrix, 1 X 10- 5 ⁇ c ⁇ l X 10_ 3 g, 0 ⁇ d ⁇ 2 X 10- 3 g, 1 X 10- 5 ⁇ c + d ⁇ 2 X 10- 3 g, 1 X 10- 5 ⁇ e ⁇ shows 5 X 10- 3 g of the amount of range, respectively.) phosphor can be cited having a composition substantially represented by.
- Cu and Au are the first activator (main activator) that forms the luminescent center.
- Cu is 1 X 10- 5 1 X 10- for zinc sulfide lg, which is the phosphor matrix. 3 g range, Au is preferably contained in the range of 0- 2 X 10- 3 g. If the content of the first activator is out of the above range, the light emission luminance and the light emission chromaticity are lowered.
- the first activator is either Cu or a combination of Cu and Au. When a combination of Cu and Au is applied, the total amount of these is 1 Adjust so that it is in the range of X 10— 5 — 2 X 10— d g.
- the Cu content as the first activator is, 3 X 10- 5 zinc sulfide lg - 5 X 10 4 and more preferably to g range instrument more preferably 5 X 10_ The range is 5 — 3 X 10_ 4 g.
- the content of Au as the first activator is, 5 X 10_ 5 1.
- 5 X 10_ 3 g is more preferred instrument more preferably in the range of 1 X 10 flush with the zinc sulfide lg
- the range is 1 X 10 3 g.
- the total amount of Cu and Au is more preferably in the range of 5 X 10_ 5 — 1.5 X 10 3 g with respect to zinc sulfide lg, more preferably 1 X 10 1 1 X 10_ 3 g This is the range.
- A1 is a second activator (co-activator) that is directly excited by an electron beam, and the first activator is excited by the excitation energy of the second activator.
- the emission luminance of the zinc sulfide phosphor (for example, ZnS: Cu or ZnS: Cu, Au) can be increased by emitting light.
- the content of the second activator is, 1 X 10- 5 zinc sulfide lg is a phosphor host - preferably in a range of 5 X 1 0_ 3 g. Be less than 1 X 10- 5 g relative to the content of the second activator is zinc sulfide lg, also exceed 5 X 10- 3 g reduces the emission brightness, also emission chromaticity to degrade.
- the second amount of activator is zinc sulfide lg against 5 X 10- 5 - 2 X 10- 3 g is more preferred instrument more preferably in the range of 1 X 10- 4 - 1 X in the range of 10- 3 g.
- activators such as Ag and A1 are uniformly dispersed in the zinc sulfide particles that are the phosphor matrix.
- the state where the activator is uniformly dispersed in the phosphor matrix particles means that the concentration of the activator inside the phosphor matrix particles (concentration distribution in the depth direction from the surface) is measured. Shows an approximately constant concentration distribution.
- Such a phosphor can be obtained by, for example, a method in which a material for forming zinc sulfide as a phosphor matrix and a material for forming an activator are uniformly mixed and fired.
- An In 2 O layer is formed on the surface of such zinc sulfide phosphor particles.
- O layer covers at least a part of the surface of zinc sulfide phosphor particles to prevent luminance degradation
- the thickness of the In 2 O layer is not particularly limited, but the coating amount in terms of In atoms is the phosphor base material.
- the value measured by ICP (inductively coupled plasma) emission spectrometry is in the range of 0.1-1. 0%, measured by XPS analysis (X-ray photoelectron analysis) Therefore, it is desirable to set the range between 6.0 and 60.0%.
- the coverage of In atoms is less than 0.1% by ICP emission spectrometry, there is no effect to improve the luminance degradation of the phosphor.
- the coverage of In atoms exceeds 1.0%, the In O layer has a large effect of blocking the penetration of electron beams.
- the coverage of In atoms is the shape of the InO layer.
- the thickness of the layer can be adjusted by changing the amount of In salt added in the InO layer formation process described later.
- the phosphor for display device according to the first embodiment described above can be manufactured, for example, as described below.
- a predetermined amount of activator raw material is added to the zinc sulfide raw material that is the phosphor base material, and a flux such as potassium chloride or magnesium chloride is added as necessary, and these are wet-treated.
- a phosphor raw material is dispersed in ion-exchanged water to form a slurry, and an activator raw material and a flux are added thereto, and mixed with a stirrer by a conventional method.
- the mixing time is set so that the activator is uniformly dispersed.
- the slurry containing the phosphor raw material and the activator is transferred to a drying container such as a pad, and dried in a drier by a conventional method to obtain a phosphor raw material.
- Such a phosphor material is filled in a heat-resistant container such as a quartz crucible together with appropriate amounts of sulfur and activated carbon.
- a heat-resistant container such as a quartz crucible together with appropriate amounts of sulfur and activated carbon.
- the dried phosphor raw material and sulfur may be mixed for about 30 to 180 minutes using a renderer, etc., and after filling the mixed material in a heat-resistant container, the surface may be covered with sulfur.
- This is fired in a sulfide atmosphere such as a hydrogen sulfide atmosphere or a sulfur vapor atmosphere, or in a reducing atmosphere (for example, an atmosphere of 35% hydrogen and the balance nitrogen).
- the firing conditions are important in controlling the crystal structure of the phosphor matrix (ZnS).
- the firing temperature should be in the range of 800-1200 ° C. preferable. If the firing temperature is less than 800 ° C, the zinc sulfide crystal grains cannot be grown sufficiently. On the other hand, when the firing temperature exceeds 1200 ° C, the desorption of sulfur is conspicuous and the luminance is lowered.
- the firing time is preferably 30 to 180 minutes depending on the set firing temperature.
- the obtained fired product is washed with ion-exchanged water or the like, dried, and further subjected to sieving to remove coarse particles as necessary, whereby the activator is obtained.
- Uniformly dispersed zinc sulfide phosphor eg ZnS: Ag, A1 phosphor or ZnS: Cu, A1 phosphor
- the zinc sulfide phosphor powder is added to an aqueous solution of an indium salt such as indium nitrate or indium chloride and stirred, and further a basic substance (for example, NH 4 OH or NaOH).
- an indium salt such as indium nitrate or indium chloride and stirred
- a basic substance for example, NH 4 OH or NaOH.
- In (OH) indium hydroxide
- this phosphor is filtered and dried, and then the dried product is heat-treated (baked).
- Caro heat is performed in an air atmosphere at a temperature of 400 550 ° C (eg, about 450 ° C) for 1 to 3 hours.
- indium hydroxide is dehydrated to become indium oxide (In 2 O 3).
- the temperature at which the generated hydroxide is dehydrated by heat treatment to become an oxide In indium hydroxide, yttrium hydroxide, aluminum hydroxide, magnesium hydroxide are used. It is getting lower than etc. In other words, only indium hydroxide can be converted from hydroxide to oxide at a sufficiently low temperature (about 450 ° C) at which the zinc sulfide phosphor does not cause luminance degradation.
- the In ⁇ layer is the zinc sulfide phosphor surface.
- a blue light-emitting phosphor layer or a green light-emitting phosphor layer can be formed by a known slurry method or printing method.
- the phosphor for a display device of the first embodiment when used in a field emission display device (FED) that is excited with an electron beam having a low acceleration voltage of 5-15 kV and a high current density, it emits blue light. It is possible to suppress the luminance deterioration of the phosphor or green light emitting phosphor over time and to satisfy the emission color (emission chromaticity) required for the blue light emitting component or green light emitting component for FED. In other words, it is possible to stably obtain high-luminance blue light emission or green light emission with the light emission chromaticity required for the blue light emission component or green light emission component for FED.
- FED field emission display device
- FIG. 1 is a cross-sectional view showing the main configuration of an FED that is a second embodiment of the present invention.
- reference numeral 1 denotes a face plate, which has a phosphor layer 3 formed on a transparent substrate such as a glass substrate 2.
- This phosphor layer 3 has a blue light-emitting phosphor layer, a green light-emitting phosphor layer, and a red light-emitting phosphor layer that are formed corresponding to the pixels, and is separated by a light absorption layer 4 made of a black conductive material. It has a structure.
- the blue light emitting phosphor layer or the green light emitting phosphor layer is composed of the blue light emitting phosphor or the green light emitting phosphor of the first embodiment described above. .
- the phosphor layers other than these can each be composed of various known phosphors.
- the blue light-emitting phosphor layer, the green light-emitting phosphor layer, the red light-emitting phosphor layer, and the light absorption layer 4 that separates them are sequentially and repeatedly formed in the horizontal direction.
- a portion where the phosphor layer 3 and the light absorption layer 4 exist is an image display region.
- Various patterns such as dots or stripes can be applied to the arrangement pattern of the phosphor layer 3 and the light absorption layer 4.
- a metal back layer 5 is formed on the phosphor layer 3.
- the metal back layer 5 is made of a metal film such as an A 1 film, and reflects the light traveling in the rear plate direction, which will be described later, among the light generated in the phosphor layer 3 to improve the luminance.
- the metal back layer 5 has a function of imparting conductivity to the image display region of the face plate 1 to prevent electric charge from being accumulated, and the anode back electrode with respect to the rear plate electron source. Play a role.
- the metal back layer 5 has a function of preventing the phosphor layer 3 from being damaged by ions generated by ionizing the gas remaining in the face plate 1 and the vacuum vessel (envelope) with an electron beam.
- the gas generated from the phosphor layer 3 during use is prevented from being released into the vacuum container (envelope), and the vacuum degree is prevented from being lowered.
- a getter film 6 made of an evaporable getter material made of Ba or the like is formed on the metal back layer 5.
- the getter film 6 efficiently adsorbs gas generated during use.
- the face plate 1 and the rear plate 7 are arranged to face each other, and the space between them is hermetically sealed via the support frame 8.
- the support frame 8 is bonded to the face plate 1 and the rear plate 7 with a frit glass or a bonding material 9 made of In or an alloy thereof, and the face plate 1, the rear plate 7 and the support frame 8
- a vacuum vessel is constructed as an envelope.
- the rear plate 7 includes a substrate 10 made of an insulating substrate such as a glass substrate or a ceramic substrate, or a Si substrate, and a large number of electron-emitting devices 11 formed on the substrate 10.
- These electron-emitting devices 11 include, for example, a field-emission cold cathode, a surface conduction electron-emitting device, and the like, and the surface of the rear plate 7 on which the electron-emitting devices 11 are formed is provided with wiring (not shown). That is, a large number of electron-emitting devices 11 are formed in a matrix according to the phosphors of each pixel, and have interconnected wirings (XY wirings) that drive the matrix-shaped electron emitting devices 11 row by row. ing.
- the support frame 8 is provided with a signal input terminal and a row selection terminal (not shown). These terminals correspond to the cross wiring (XY wiring) of the rear plate 7 described above.
- a reinforcing member (atmospheric pressure support member, spacer) 12 is appropriately disposed between the face plate 1 and the rear plate 7. It ’s good.
- the phosphor for display device of the first embodiment is used as a blue light emitting phosphor layer or a green light emitting phosphor layer that emits light by electron beam excitation, Luminance deterioration is improved, and the service life can be significantly increased.
- ZnS zinc sulfide
- AgNO silver nitrate
- ⁇ 1 ( ⁇ ) ⁇ 9 ⁇ O aluminum nitrate
- the zinc sulfide phosphor powder was added to an aqueous solution containing indium nitrate and stirred, and NaOH, which is a basic substance, was added to adjust the pH of the aqueous solution to 9.0 or higher.
- NaOH which is a basic substance
- the phosphor was filtered and dried, and then the dried product was heat-treated (baked) at a temperature of about 450 ° C for 1.5 hours in an air atmosphere.
- an indium oxide (In 2 O 3) layer was coated on the surface of the zinc sulfide phosphor particles. Note that the coating amount of indium oxide is
- a phosphor layer was formed by a slurry method using the obtained blue light-emitting phosphor.
- a phosphor layer was formed using a cubic zinc sulfide phosphor (ZnS: Ag, A1).
- ZnS: Ag, A1 a cubic zinc sulfide phosphor
- the phosphor layer is formed by dispersing the phosphors obtained in Example 1 and the comparative example in aqueous solutions containing polybulal alcohol and the like to form a slurry, and using these slurry using a spin coater (spin coater).
- the coating was performed on a glass substrate. By adjusting the viscosity of the rotational speed and the slurry spin coating machine to a thickness of each phosphor layer 3 X 10- 3 mg / mm 3 .
- the emission luminance and emission chromaticity of the phosphor layer thus obtained were examined.
- the emission brightness was measured by irradiating each phosphor layer with an electron beam having an acceleration voltage of 10 kV and a current density of 1.2 A / cm 2 .
- the light emission luminance was determined as a relative value when the luminance of the phosphor layer according to the comparative example was 100.
- the emission chromaticity was measured using SR-3 manufactured by Topcon as a chromaticity measuring instrument. Color The measurement of the degree was carried out in a coffin room where the chromaticity at the time of light emission was not affected from the outside. Table 1 shows the measurement results of emission brightness and emission chromaticity.
- the blue light-emitting phosphor obtained in Example 1 has a luminescent color when irradiated with an electron beam having a low acceleration voltage (15 kV or less) and a high current density. It is as good as the one and has the same luminance.
- each phosphor layer was continuously irradiated with an electron beam with an acceleration voltage of 10 kV and a current density of 1.2 A / cm 2 , and the relationship between the total amount of charge injected by the electron beam irradiation and the emission luminance was investigated. It was. Figure 2 shows a graph showing this relationship.
- the green light-emitting phosphor (cubic ZnS: Cu, A1 phosphor), and the red light-emitting phosphor (YOS: Eu phosphor) obtained in Example 1, respectively,
- a phosphor layer was formed thereon to form a face plate.
- the face plate and a rear plate having a large number of electron-emitting devices were assembled through a support frame, and the gap between them was hermetically sealed while vacuuming.
- the FED obtained in this way is excellent in color reproducibility, and is sure to show good display characteristics even after 1000 hours of driving at normal temperature and rated operation.
- the acceleration voltage is as low as 5 to 15 kV, and the current density is high.
- FED field emission display
- the emission color (emission chromaticity) required for the blue emission component or the green emission component can be satisfied. In other words, the ability to stably obtain high-luminance blue light emission or green light emission with the light emission chromaticity required for the blue light emission component or green light emission component for FED is positive.
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PCT/JP2004/016860 WO2006051601A1 (ja) | 2004-11-12 | 2004-11-12 | 表示装置用蛍光体とその製造方法、およびそれを用いた電界放射型表示装置 |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH03234789A (ja) * | 1990-02-10 | 1991-10-18 | Nichia Chem Ind Ltd | 低速電子線励起蛍光体の製造方法 |
JPH09217059A (ja) * | 1996-02-08 | 1997-08-19 | Toshiba Corp | 青色発光蛍光体,その製造方法および蛍光ランプ |
JP2004043568A (ja) * | 2002-07-10 | 2004-02-12 | Hitachi Ltd | 画像表示装置 |
-
2004
- 2004-11-12 WO PCT/JP2004/016860 patent/WO2006051601A1/ja not_active Application Discontinuation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH03234789A (ja) * | 1990-02-10 | 1991-10-18 | Nichia Chem Ind Ltd | 低速電子線励起蛍光体の製造方法 |
JPH09217059A (ja) * | 1996-02-08 | 1997-08-19 | Toshiba Corp | 青色発光蛍光体,その製造方法および蛍光ランプ |
JP2004043568A (ja) * | 2002-07-10 | 2004-02-12 | Hitachi Ltd | 画像表示装置 |
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