WO2005031785A1 - プラズマディスプレイ装置およびそれに用いる蛍光体の製造方法 - Google Patents
プラズマディスプレイ装置およびそれに用いる蛍光体の製造方法 Download PDFInfo
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- WO2005031785A1 WO2005031785A1 PCT/JP2004/014431 JP2004014431W WO2005031785A1 WO 2005031785 A1 WO2005031785 A1 WO 2005031785A1 JP 2004014431 W JP2004014431 W JP 2004014431W WO 2005031785 A1 WO2005031785 A1 WO 2005031785A1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
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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
- C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
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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
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
- C09K11/592—Chalcogenides
- C09K11/595—Chalcogenides with zinc or cadmium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7784—Chalcogenides
- C09K11/7787—Oxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7797—Borates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
- H01J11/20—Constructional details
- H01J11/34—Vessels, containers or parts thereof, e.g. substrates
- H01J11/42—Fluorescent layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
- H01J2211/20—Constructional details
- H01J2211/34—Vessels, containers or parts thereof, e.g. substrates
- H01J2211/42—Fluorescent layers
Definitions
- the present invention relates to a plasma display device and a method for manufacturing a phosphor used therein.
- the present invention provides a projector having a phosphor layer that emits light when excited by ultraviolet light.
- the present invention relates to a spray device and a method for manufacturing a phosphor used in the spray device.
- the plasma display device performs full-color display by additively mixing the so-called three primary colors (red, green, and blue).
- the plasma display device is provided with a phosphor layer that emits each of the three primary colors red (R), green (G), and blue (B).
- the phosphor particles are excited by ultraviolet rays generated in the discharge cells of the PDP, and generate visible light of each color.
- the reason for crushing and sieving (classifying) the phosphor particles lightly is as follows. In other words, when a phosphor layer is formed on a PDP, a method of screen printing using phosphor particles of each color as a paste, or an ink jet method of discharging and applying the paste from a nozzle is used. If the classification is not performed, large agglomerates are contained in the phosphor, so that when the paste is applied using these phosphors, application unevenness or nozzle clogging occurs. Therefore, the phosphor that has been lightly pulverized and classified has a smaller particle size and a uniform particle size distribution, so that a cleaner coating surface can be obtained.
- Z n 2 S i 0 4 The method for producing a green phosphor made of Mn, the ratio of S i 0 2 against the Z Itashita is greater than the stoichiometric ratio (2 Z n O / S I_ ⁇ 2) , 1.5 Zn ⁇ / S i 0 2, and the phosphor is produced by firing in air (atmospheric pressure) at 1200 ° C to 130 ° C. It is disclosed in the handbook (pp. 219-220 Ohmsha, 1991). Therefore Z n 2 S i ⁇ 4: the surface of the Mn crystal is covered with an excess of S i 0 2, the phosphor surface is negatively charged.
- the discharge characteristics may be deteriorated, for example, as described in Japanese Patent Application Laid-Open No. H11-868735 / Japanese Patent Application Laid-Open No. 2001-236693. It is disclosed in the gazette.
- ink jet coating method in which a negatively charged green phosphor ink is continuously applied from a thin nozzle, nozzle clogging and coating unevenness occur.
- the cause of the clogging and uneven coating may be that ethyl cellulose in the ink is less likely to be adsorbed on the surface of the negatively charged green phosphor.
- Z n 2 S i 0 4 To positively charged negatively charged surface of Mn, an oxide of positively charged or a method of laminating co one preparative, apparently a mixture of green phosphor positively charged UeTadashi A method of charging has been devised. When the oxide was laminated, the brightness was reduced, and when two types of phosphors having different charging states were applied, clogging and uneven application were likely to occur.
- Z n 2 S I_ ⁇ 4 When you create a Mn, were mixed in advance the ratio of Z nO and S I_ ⁇ 2 2: 1 or more (2Z 1 or more under Motohi of Z nZS i), fluorescence and the vapor pressure of Z Itashita is utilizing higher Ri by the vapor pressure of S i 0 2 the body in the air or in nitrogen at one atmosphere when firing at 1 2 0 0 ° C ⁇ 1 3 0 0 ° C There is also a method in which ZnO is first scattered (sublimated) during firing. However, even in such a case, there is a problem that Si 0 2 becomes rich near the surface of the crystal and is negatively charged.
- the present invention has been made in view of such problems, and has as its object to prevent deterioration of a phosphor layer and to improve luminance, life, and reliability of a PDP. Disclosure of the invention
- a plasma display device includes a plurality of discharge cells arranged, a phosphor layer of a color corresponding to each discharge cell, and a phosphor layer excited by ultraviolet light.
- the phosphor layer is Z n 2 S i O 4: has a green phosphor layer having a Mn, Z n 2 S i ⁇ 4: consisting of Mn
- the green phosphor is characterized in that at least the element ratio between zinc (Zn) and silicon (Si) near the surface is 2 Z1 or more and the activator is Mn.
- the application state of the phosphor layer can be uniformly formed by setting the charged state of the green phosphor crystal to positively charged or 0-charged phosphor particles, and the phosphor brightness can be improved. Prevents deterioration and also shines PPD The degree of life, life, and reliability can be improved.
- FIG. 1 is a plan view showing a state in which a front glass substrate of a PDP used in a plasma display device according to an embodiment of the present invention is removed.
- FIG. 2 is a perspective view showing the structure of the image display area of the PDP.
- FIG. 3 is a block diagram of the plasma display device according to the embodiment of the present invention.
- FIG. 4 is a cross-sectional view showing the structure of a PDP image display area used in the plasma display device according to the embodiment of the present invention.
- FIG. 5 is a schematic configuration diagram of an ink coating apparatus used for forming a phosphor layer of the PDP.
- FIG. 6 is a schematic sectional view of a firing furnace used for main firing of the green phosphor.
- a green phosphor of Zn 2 Si 0 4 : Mn having a zinc silicate crystal structure ZnO, Si 0 2 and an activator Mn 0 2 are mixed and mixed.
- a calcined powder is prepared by calcining in the air at 0 to 900 ° C, and then the calcined powder is completely shielded by Zn ⁇ powder, and then the powder is added to the powder.
- Z n 2 S i used in the PDP 0 4 green phosphor Mn has been created mainly in solid reciprocal Obo, stoichiometry than Z nO and S I_ ⁇ 2 for brightness enhancement It is made with a composition that is higher than the theoretical ratio. Therefore the Z n 2 S i ⁇ 4: the surface of the Mn crystal is in the state of being covered with S i 0 2.
- the vapor pressure of the firing Z n 0 is higher than the vapor pressure of S i 0 2 at 1 0 0 0 ° C or higher Therefore, Zn near the surface scatters quickly (sublimation)
- Si 0 2 increases on the phosphor surface.
- Z n O is not scattered (sublimed), 1000 ° and baked at C below, the ratio of Z n / S i is Z n 2 S i ⁇ 4 2Z1:
- Mn is synthesized, lower crystallinity Therefore, a high-luminance phosphor cannot be obtained.
- the present invention the element ratio of Z n 0 and S i ⁇ 2 formulated 2.
- Z n the crucible 2 S i 0 4 put Mn mixed composition, (shields) completely surrounds the circumference thereof in Z n O
- Z n 2 S i 0 4 in the crucible and covered Z n O side inlet is in the furnace : set to a temperature slightly higher than the M n, n 2 (nitrogen), n 2 - H 2 (nitrogen - hydrogen), n 2 - 0 2 (nitrogen - oxygen) by firing in, the Z N_ ⁇
- Z n 2 S i 0 4 enclose around Mn calcined powder in Z nO, set to a temperature of Z n O side in the furnace slightly higher, the Z n O side at the firing temperature saturated steam by keeping the enhanced pressure, Z n 2 S i ⁇ 4: thereby preventing scattering of Z n O in Mn calcined powder of (Hua Nobori).
- Examples of the method for manufacturing the phosphor body include a solid-phase sintering method using an oxide or a carbonate material and a flux, a method of hydrolyzing these in an aqueous solution using an organic metal salt or a nitrate, or adding an alkali metal or the like.
- the precursor of the phosphor is prepared using a co-precipitation method, which is then precipitated, and then heat-treated to produce a calcined powder, or in a furnace where an aqueous solution containing the phosphor material is heated.
- There is a liquid spraying method or the like which is produced by spraying a liquid.
- the phosphor precursor or calcined powder produced by any of the methods when firing Zn 2 Si 4 : Mn at 100 ° C. or more, Z n 2 S i 0 4: Mn, screened by Z n O (Z n 2 S , i 0 4: the Mn powder is sealed with Z n O), 1 0 0 0 ° C ⁇ 1 3 5 0 ° C It was found that the main baking prevented the scattering of Zn 0 from the surface during the baking, and was effective in improving the characteristics of the Zn 2 Si 0 4 : Mn phosphor.
- a solid phase reaction method of the green phosphor of the present invention is used as an example of a method for producing a green phosphor.
- the manufacturing method will be described.
- Z nO, S I_ ⁇ 2, Mn C0 3 or the like carbonates and oxides of the composition of the phosphor matrix (Z n, - x Mn x ) 2 S i 0 4 S i than the molar ratio of A slightly larger amount of Z ⁇ relative to ⁇ 2 is blended (element mixing ratio of Z ⁇ and S i ⁇ 2 is 2.1 Z 1 to 2.0 Z 1).
- a liquid phase method for producing a phosphor from an aqueous solution the following is performed. That is, an organic metal salt (for example, alkoxide, acetylacetone) or a nitrate containing an element (Zn, Si, Mn) constituting the phosphor is converted to an elemental ratio of Zn / Si of 2 Dissolve in water with a composition that gives 1 to 2.0 Z1 and hydrolyze to produce a coprecipitate (hydrate). After that, it is calcined in the air at 600 ° C. (: up to 900 ° C.) Then, as in the above-described solid-phase reaction method, Z ⁇ powder or Z is placed around the crucible containing the calcined powder.
- an organic metal salt for example, alkoxide, acetylacetone
- a nitrate containing an element (Zn, Si, Mn) constituting the phosphor is converted to an elemental ratio of Zn / Si of 2 Dissolve in water with
- N 2 — H 2 the green phosphor was fired at 1 0 0 0 ° C ⁇ 1 3 5 0 ° C during at least one of an atmosphere of N 2 -0 2.
- the reason for limiting the ratio of Zn to Si to 2.1 Z 1 to 2.0 / 1 is that the Zn element is made slightly excessive, so that Zn 2 Si ⁇ 4 becomes positively charged. This is to make it easier.
- the ratio of Zn is 2.1 or more, the Zn between crystal lattices increases and the brightness decreases.
- the ratio of Zn is 2.0 or less, the charge tends to be negative (single). Is preferably 2.1 Z 1 to 2.0 / 1.
- the reason why the firing temperature was limited to 100 ° C. to 135 ° C. is that below 100 ° C., the vapor pressure of Zn 0 and Si 0 2 is low, so Z N_ ⁇ scattering of (sublimation) is hardly possible S i 0 2 rich phase to less near the surface but, Z n 2 S i ⁇ 4: is the crystallinity is poor phosphor having high brightness of Mn is not obtained .
- 1 3 becomes a 5 CTC above, with respect to vapor pressure S i 0 2 vapor pressure of Z N_ ⁇ , relatively large, Z in Z ⁇ ⁇ n 2 S i ⁇ 4: covering the Mn effects together but fades slightly, it proceeds excessively sintering of Z n 2 S i 0 4, the particle size is too large, in order to decrease the brightness.
- each color phosphor used in the plasma display device of the present invention will be described.
- the specific phosphor particles used for the green phosphor layer were manufactured by the above-mentioned manufacturing method! (Zn Mrix) 2 S i 0 4 ], and the value of x is preferably 0.01 ⁇ ⁇ 0.2 because of excellent luminance and luminance deterioration.
- the compound represented by x can be used.
- the luminance is preferably high.
- FIG. 1 is a plan view showing a state where a front glass substrate of a PDP used in a plasma display device according to an embodiment of the present invention is removed
- FIG. 2 is a perspective view showing a structure of an image display area of the PDP.
- the number of display electrode groups, display scan electrode groups, address electrode groups, and the like are partially omitted for clarity.
- the PDP 100 has a front glass substrate 101 (not shown), a rear glass substrate 102, N display electrodes 103, and N display scans.
- Electrode 104 (the number is indicated when the N-th line is indicated), M address electrodes 107 group (the number is indicated when the M-th line is indicated), and the hermetic seal layer 1 indicated by oblique lines 2 1 It has an electrode matrix with a three-electrode structure consisting of the display electrode 103, the display scan electrode 104, and the address electrode 107, and the display electrode 103, the display scan electrode 104, and the address electrode 107.
- a display cell is formed at the intersection, and an image display area 123 is formed.
- the PDP 100 has a display electrode 103, a display scan electrode 104, a dielectric glass layer 105, and a MgO layer on one main surface of the front glass substrate 101.
- a front panel on which a protective layer 106 is disposed, and an address electrode 107, a dielectric glass layer 108, a partition wall 109, and a phosphor layer 1 on one main surface of a rear glass substrate 102 It consists of a back panel on which 10R, 110G, and 110B are arranged.
- a discharge gas is sealed in a discharge space 122 formed between the front panel and the back panel.
- the plasma display device is connected to the PDP driving device 150 shown in FIG. Make up.
- the plasma display device has a display driver circuit 153, a display scan driver circuit 154, and an address driver circuit 155 in the PDP 100. Attempt to light up under the control of controller 15 2. A discharge voltage is applied to the display scan electrode 104 and the address electrode 107 corresponding to the cell to be addressed, and an address discharge is performed between them.After that, a pulse voltage is applied between the display electrode 103 and the display scan electrode 104. A sustain discharge is performed by applying the voltage. Due to the sustain discharge, ultraviolet light is generated in the cell, and the phosphor layer excited by the ultraviolet light emits light to turn on the cell, and an image is displayed by a combination of lighting and non-lighting of each color cell.
- FIG. 4 is a cross-sectional view showing a structure of an image display area of a PDP used in the plasma display device according to the embodiment of the present invention.
- the front panel alternately has N display electrodes 103 and display scan electrodes 104 (only two electrodes are shown in FIG. 2) on a front glass substrate 101.
- N display electrodes 103 and display scan electrodes 104 only two electrodes are shown in FIG. 2
- the front panel After being formed in a stripe pattern in parallel, it is fabricated by covering the surface with a dielectric glass layer 105, and further forming a Mg ⁇ protective layer 106 on the surface of the dielectric glass layer 105. You.
- the display electrode 103 and the display scan electrode 104 are electrodes composed of a transparent electrode made of ITO and a bus electrode made of silver, and a silver paste for the bus electrode is applied by screen printing. Then, it is formed by firing.
- the dielectric glass layer 105 is formed by applying a paste containing a lead-based glass material by screen printing, and then baking it at a predetermined temperature and a predetermined time (for example, 20 minutes at 560 ° C.). To a thickness of about 20 m.
- the paste containing a glass material of the lead-based e.g., P B_ ⁇ (7 0 wt%), B 2 ⁇ 3 (1 5 wt%), S i 0 2 (1 0 wt%) and A 1 2 0
- an organic binder ⁇ -one-pineol with 10% ethylcellulose dissolved
- the organic binder is obtained by dissolving a resin in an organic solvent.
- acryl resin can be used as a resin
- butyl carbitol can be used as an organic solvent.
- Darisel Trioleate may be mixed with such an organic binder.
- the MgO protective layer 106 is made of magnesium oxide (MgO), and is formed to a predetermined thickness (about 0.5 m) by, for example, a sputtering method or a CVD method (chemical vapor deposition method). Is done.
- MgO magnesium oxide
- the rear panel is formed by screen printing silver electrodes for electrodes on the rear glass substrate 102, and then firing it to form M address electrodes 107 in a row.
- a paste containing a lead-based glass material is applied thereon by a screen printing method to form a dielectric glass layer 108, and the paste also containing a lead-based glass material is repeated at a predetermined pitch by a screen printing method.
- baking is performed to form partition walls 109.
- the partition walls 109 the discharge space 122 is divided into one cell (unit light emitting region) in the line direction.
- the gap dimension W of the partition wall 109 is specified to be about 130 ⁇ m to 240 in accordance with the HD-TV of 32 inches to 50 inches.
- Green phosphor layer 1 1 0 G is the element ratio of Z NZS i 2. a 1 / 1 ⁇ 2. 0/1, Z n 2 S i ⁇ 4: the around the calcined powder of Mn Z n 0 Shield with 100.
- C ⁇ 1 3 5 0 ° C in N 2, N 2 - 0 2 , N 2 _H 2 of is formed from a green phosphor firing in at least one atmosphere.
- a paste-like phosphor ink composed of phosphor particles and an organic binder is applied and fired at a temperature of 400 to 590 ° C to burn out the organic binder.
- the phosphor layers 110 R, 110 G, and 110 B formed by binding the respective phosphor particles are formed.
- the thickness L of the phosphor layers 110 R, 110 G, and 110 B in the stacking direction on the address electrodes 107 is about 8 to 25 times the average particle size of the phosphor particles of each color. It is desirable to form. That is, fireflies In order to ensure the brightness (luminous efficiency) when a certain amount of ultraviolet light is applied to the photoconductor layer, the phosphor layer absorbs the ultraviolet light generated in the discharge space without transmitting it.
- the particle size is sufficiently small and spherical, such as phosphor particles obtained by a hydrothermal synthesis method, even if the number of stacked layers is the same as compared to the case where non-spherical particles are used, fluorescent light will not be emitted. Since the total surface area of the phosphor particles increases as the packing density of the body layer increases, the surface area of the phosphor particles contributing to actual light emission in the phosphor layer increases, and the luminous efficiency further increases.
- the front panel and the rear panel manufactured in this manner are overlapped so that each electrode of the front panel and an address electrode of the rear panel are orthogonal to each other, and a sealing glass is inserted around the panel periphery.
- This is baked at, for example, about 450 ° C. for 10 to 20 minutes to form an airtight seal layer 121, thereby sealing.
- the discharge space 1 2 in 2 high vacuum e.g., 1. 1 X 1 0- 4 P a
- N e- X e system of inert gas A PDP 100 is produced by filling a discharge gas such as this at a predetermined pressure.
- the ink applicator 200 is provided with a server 210, a pressure pump 220, a header 230, and the like, and is supplied from a server 210 that stores phosphor ink.
- the phosphor ink is supplied to the header 230 by being pressurized by the pressurizing pump 220.
- the header 230 is provided with an ink chamber 230a and a nozzle 240, and the phosphor ink that is pressurized and supplied to the ink chamber 230a is continuously supplied from the nozzle 240. It is designed to be ejected.
- the diameter D of this nozzle 240 prevents nozzle clogging. It is desirable that the distance between the partition walls 109 should be 30 zm or more and that the distance between the partition walls 109 (approximately 130 im to 200 wm) should be less than 30 zm to prevent protrusion from the partition walls 109 during coating. Preferably, it is usually set to 30 X m to 130 m.
- the header 230 is configured to be linearly driven by a header scanning mechanism (not shown).
- the header 230 scans the header 230 and continuously discharges the phosphor ink 250 from the nozzle 240. Thereby, the phosphor ink is uniformly applied to the grooves between the partition walls 109 on the rear glass substrate 102.
- the viscosity of the phosphor used is kept in the range of 150 to 5000 centipoise (CP) at 25 ° C.
- the server 210 is provided with a stirrer (not shown), and the stirring prevents precipitation of particles in the phosphor ink.
- the header 230 is integrally formed including the ink chamber 230a and the nozzle 240, and is produced by subjecting a metal material to machine processing and electric discharge machining.
- the method for forming the phosphor layer is not limited to the above method, and various methods such as a photolithography method, a screen printing method, and a method of disposing a film in which phosphor particles are mixed and the like can be used.
- a method is available.
- the phosphor ink is prepared by mixing phosphor particles of each color, a binder, and a solvent so as to have a concentration of 150 to 500,000 centipoise (CP). If necessary, a surfactant and silica may be used. , A dispersant (0.1 to 5 wt%) and the like may be added.
- the compound represented by ⁇ is used. 'These are compounds in which some of the ⁇ elements that make up the parent material have been replaced by Eu.
- the substitution amount X of the Eu element with respect to the 0 element is in the range of 0.05 ⁇ ⁇ ⁇ 0.20. If the replacement amount is larger than this, the luminance will increase but the luminance will deteriorate significantly.
- the amount is less than this substitution amount, the composition ratio of Eu, which is the emission center, decreases, and the luminance decreases, so that the phosphor cannot be used as a phosphor.
- the green phosphor is calcined at an elemental ratio of ZnSSi of 2.1 / 1 to 2.01, and is sealed in Zn ⁇ in N 2 , N 2 —H 2 , N 2 2 - 0 2 baked form was in [(Z r ⁇ - x Mn x ) 2 S it ⁇ 4 the compound represented by is used.
- [(Z n, _ x Mn x ) 2 S I_ ⁇ 4] part of Z n elements constituting the host material is a compound substituted with M n.
- the substitution amount X of the Mn element with respect to the Zn element is preferably in the range of 0.01 ⁇ x ⁇ 0.20.
- a compound represented by Ba x X M g A 1 10 ⁇ 17 : E u x or B a ⁇ x — y S r y M g A 1 10 O 17 : E 1 ⁇ is used.
- B a, X M g A 1 10 O 17:.. E u x, B a,, ⁇ r y Mg A 1 10 ⁇ 17: E u x, a part of B a elements constituting the host material Is a compound substituted with Eu or Sr.
- the substitution amounts X and y of the Eu element with respect to the Ba element are preferably in the ranges of 0.03 ⁇ x ⁇ 0.20 and 0.1 ⁇ y ⁇ 0.5.
- ethyl cellulose or acryl resin is used as a binder to be mixed with the phosphor ink (0.1wt% to 10wt% of the ink is mixed).
- polymers such as PMA and PVA can be used as the binder, and organic solvents such as ethylene glycol and methyl ether can be used as the solvent.
- organic solvents such as ethylene glycol and methyl ether can be used as the solvent.
- the phosphor particles those produced by a solid phase reaction method, an aqueous solution method, a spray firing method, or a hydrothermal synthesis method are used. An example of a specific method for producing these phosphor particles will be described below.
- B a be produced with aqueous solution method, _ x Mg A 1) 0 O 17: describes work made how the blue phosphor E u x.
- a raw material comprising barium nitrate B a (N_ ⁇ 3) 2, magnesium nitrate Mg (N0 3) have aluminum nitrate A 1 (N_ ⁇ 3) nitrate EUR
- the molar ratio of Pium E u (N0 3 ) 2 is 1 x: l: 10: x (0.03 ⁇ x ⁇ 0.
- the aqueous medium is preferably ion-exchanged water or pure water because it does not contain impurities. However, even if these contain a non-aqueous solvent (methanol, ethanol, etc.), they can be used.
- the hydrated mixture is placed in a container made of a material having corrosion resistance and heat resistance, such as gold or platinum. Temperature (100 to 30)
- the phosphor particles obtained by hydrothermal synthesis have a spherical shape, a smaller particle size than those produced by a conventional solid-phase reaction, and an average particle size of 0.05 im to 2. It is formed to about 0 m.
- spherical means that the axis diameter ratio (short axis diameter / long axis diameter) of most fluorescent particles is, for example, 0.9 or more 1.
- a blue phosphor can be produced by a spraying method in which the hydrate mixture is sprayed from a nozzle into a high-temperature furnace to synthesize the phosphor without putting the hydrate mixture in a gold or platinum container.
- B a to produce a solid phase reaction method x y S r y Mg A 1 10 O 17:.. Describes a method for manufacturing a blue fluorescent body E u x.
- this is reduced in a reducing atmosphere, for example, in an atmosphere of 5% of hydrogen and 95% of nitrogen at a predetermined temperature (100 ° C. to 160 ° C.) for a predetermined time (2 hours).
- a reducing atmosphere for example, in an atmosphere of 5% of hydrogen and 95% of nitrogen at a predetermined temperature (100 ° C. to 160 ° C.) for a predetermined time (2 hours).
- phosphor powder is created by air classification.
- Oxides, nitrates, and hydroxides were mainly used as raw materials for the phosphor, but organometallic compounds containing elements such as Ba, Sr, Mg, Al, and Eu, such as metal alkoxides, Phosphors can also be prepared using acetylaceton or the like.
- FIG. 6 is a schematic cross-sectional view of a firing furnace used when main firing the green phosphor.
- sintering furnace main body 3 0 0 consisting electric furnace, Z n O or A 1 2 0 3 made of a first crucible 3 1 0, Z N_ ⁇ powder 3 3 0 surrounding the crucible 3 1 0, further they were housed and Z n O or a 1 2 0 3 made of the second crucible 3 5 0, is composed of the heating heat Isseki 340 provided on the outer periphery thereof, calcination fluorescence first crucible 3 1 within 0 Body powder 320 is stored.
- Raw material is zinc oxide (Z n 0), silicon oxide (S I_ ⁇ 2), manganese oxide Mn O in a molar ratio of Z n and Mn 1- X: (0. 0 1 ⁇ X ⁇ 0. 2 0) It was mixed so that the element ratio of then Z n and S i is 2. 1Z1 ⁇ 2. 0Z1 in so as to mix the raw material as required with fluxes (Z n F 2, Mn F 2) . This mixture is calcined at 65 ° C. to 900 ° C. for 2 hours.
- the heater 340 of the furnace is provided around the ZnO second crucible 350 and the ZnO powder 330, the first crucible 310 and the second crucible 350 Z n O powder 3 3 towards 0 Z n 2 S i 0 4: it is a high child slightly temperature than calcined phosphor powder 3 2 0 of Mn. Power control and N.
- 0Z 1 in the formulation of the next Z n (N0 3) 2 and [S i (O ⁇ C 2 H 5) 4 ] Are mixed and poured into ion-exchanged water to prepare a mixed solution.
- a hydrate is formed by dropping a basic aqueous solution, for example, an aqueous ammonia solution, into the mixed solution.
- the hydrate 6 0 0 ° (: was calcined at ⁇ 9 0 0 ° C, then with the pre-sintered product in the same manner as the solid phase method, A 1 2 ⁇ 3 or Z n O made of the first Put in crucible 310, and surround this first crucible 310 with Zn0 powder 330 and second crucible 350, and N 2 , N 2 — 0 2 , N 2 — H 2 atmosphere
- the green phosphor is produced by firing at 1000 ° C. to 135 ° C. in the inside.
- (Y, G d) 0 3 describes red phosphor E u x.
- nitrate Ittoriumu Y 2 ( ⁇ 0 3) as a raw material 3 and water nitrate Gadori Miumu Gd 2 (N0 3) 3 and boric acid H 3 B 0 3 and europium nitrate E u 2 (N0 3) 3 and a molar ratio of 1 one x: 2: x (0. 0 5 ⁇ x ⁇ 0: 2 0)
- Mix so that the ratio of Y to Gd is 65:35, heat-treat in air at 1200 ° C to 135 ° C for 2 hours, classify and red phosphor Get.
- Y 2x 0 3 In the case of the red phosphor of E u x, in mixture preparation step, nitric I Tsu thorium Y 2 (Nyu_ ⁇ 3) 2 and europium nitrate E u (NO 3) as a raw material 2 Is dissolved in ion-exchanged water so that the molar ratio becomes 2—x: x (0.05 ⁇ x ⁇ 0.30) to prepare a mixed solution.
- a basic aqueous solution for example, an aqueous ammonia solution
- a basic aqueous solution for example, an aqueous ammonia solution
- the hydrate and ion-exchanged water are placed in a container made of a corrosion-resistant and heat-resistant material such as platinum or gold.
- Hydrothermal synthesis is carried out for 3 to 12 hours under the conditions of 00 ° C to 300 ° C and a pressure of 0.2 M to 10 MPa. Thereafter, drying of the obtained compound, the desired Y 2x ⁇ 3:.
- the phosphor layers are classified into red phosphors, and the phosphor layers 110 R and 110 B of the PDP 100 described above are phosphors that have been conventionally used.
- 0 for G was used green phosphor particles whose surface is positively charged in constituting the phosphor [(Z n Mn) 2 S i 0 4 ].
- Each manufactured plasma display device has a size of 42 inches (HD-TV specification with a rib pitch of 150 m).
- the thickness of the dielectric glass layer is 20 m, and the thickness of the MgO protective layer is 0.5 ⁇ . m, distance between display electrode and display scan electrode Was manufactured to be 0.08 mm.
- the discharge gas sealed in the discharge space is a gas containing a mixture of 5% xenon and mainly neon at a predetermined discharge gas pressure.
- the Zn 2 S i ⁇ 4 Mn green phosphor particles used in the plasma display device of samples 1 to 10 have an element ratio of Zn and Si of 2.1 Z 1 to 2.0 / 1, put calcined powder of the phosphor in the first crucible 3 1 0 a 1 2 0 3 or Z N_ ⁇ made.
- Table 1 shows the synthesis conditions of each phosphor used for these samples.
- Samples 1-4 were prepared by solid phase synthesis as a green phosphor (. Z ⁇ ,, ⁇ , ) the 2 S i 0 4, the red phosphor (Y, Gd), X B 0 3: the E u x, the blue phosphor (B a, X M g a 1 10 O 17:. E u x) Ru der those combinations with each.
- the method of phosphor synthesis the substitution ratio of Mn and Eu as emission centers, that is, the substitution ratio of Mn to Zn element, and the substitution ratio of Eu to Y and Ba elements, and the case of green color
- the element ratio of Zn and Si and the firing conditions were changed as shown in Table 1.
- Samples 5-9 were prepared by a liquid phase method as a green phosphor (aqueous solution method) to (Z n ,. x Mn x) 2 S I_ ⁇ 4, red phosphor Y 2x ⁇ 3: ⁇ ⁇ ⁇ , the blue phosphor ⁇ a _ x _ y S r y M g a 1 10 ⁇ ⁇ :! those combination with E u x.
- the conditions of the phosphor synthesis method, the element ratio of Zn and Si in the case of green, and the firing conditions were changed as shown in Table 1.
- the phosphor ink used to form the phosphor layer was prepared by using each of the phosphor particles shown in Table 1 and mixing a phosphor, a resin, a solvent, and a dispersant.
- the viscosity (25 ° C.) of the phosphor ink As a result of measuring the viscosity (25 ° C.) of the phosphor ink at that time, the viscosity was kept in the range of 150 to 50,000 CP in all cases. Observation of the formed phosphor layers revealed that all of the phosphor layers were uniformly coated with the phosphor ink.
- the diameter of the nozzle used for coating at this time was 100 m, and the average particle size of the phosphor particles used in the phosphor layer was 0.1 m to 3.0 m, and the maximum particle size was 8 m. The following particles are used.
- Sample 10 was a sample in which the element ratio of Zn / Si at the time of mixing the raw material of the green phosphor was 1.9 / 1
- Sample 11 was also a sample in which the element ratio of Zn / Si was 2
- Sample 1 2 is a green phosphor in the conventional example, the element ratio Z NZS i during feed formulation 2. 0/1, fired only at ordinary crucible (A 1 2 0 3 crucible) This is a sample.
- Sample 1 3 the ratio of Zn / Si at the time of mixing the raw material of the green phosphor is 2.0Z1, and the calcining temperature of the calcined powder is the same as that of the present invention. In this sample, the temperature was lowered to 900 ° C.
- the element ratios of Zn and Si near the surface (approximately 10 nm) of the prepared samples 1 to 9 and comparative sample 10 were measured using XPS (X-ray photoelectron spectroscopy).
- the luminance of the PDP when it was completely white and the luminance of the green and blue phosphor layers were measured using a luminance meter.
- a sustaining pulse with a voltage of 185 V and a frequency of 100 kHz is applied to the plasma display device for 1000 hours continuously. Then, the PDP brightness before and after that was measured, and the rate of change in brightness deterioration (brightness after application—brightness before application—brightness before application of Z> * 100) was determined from the PDP brightness.
- the body has deteriorated crystallinity, resulting in a panel with low green brightness.
- the comparative sample 12 is a green phosphor prepared by a conventional manufacturing method, Z ⁇ is selectively sublimated from the surface, and the ratio of Z n / S i is 1.9 2/1 and S i becomes rich and becomes negatively charged, the rate of green luminance degradation during accelerated life is large, and address errors and nozzle clogging occur.
- Comparative Sample 1 3 is about the first crucible is covered with Z N_ ⁇ powder, since the sintering temperature is 9 0 0 ° C and lower, Z n 2 S I_ ⁇ 4: Crystallization of Mn is insufficient However, the panel is low in luminance and greatly deteriorates in green luminance.
- the ratio of ZnSSi was blended at an elemental ratio of 2.01 to 2.1 / 1, and the calcined powder was put into a crucible, and the surroundings were surrounded with Zn ⁇ powder, Since the green phosphors of Samples 1 to 9 of the present invention, which were prepared at 100 ° C. to 135 ° C., had a positive charge or a zero charge, the decrease in the luminance of green and blue was low, and There is no address error or nozzle clogging during phosphor application.
- a green phosphor that is a static-negatively charged positive or 0, neon ions phosphor is present in the panel discharge space (N e +) or CH X based ions (CH X +) and other positive ions are less susceptible to impact, so it is considered that luminance degradation has been reduced, and blue is slightly less susceptible to ion impact.
- the green phosphors of the phosphor layer (Z ⁇ ,,, ⁇ ,) the charged state of the 2 S i 0 4 on the positive (+) or 0, the phosphor layer
- the coating condition of the PDP can be made uniform and prevention of deterioration can be achieved, and at the same time, the brightness, life and reliability of the PDP can be improved, which is useful for improving the performance of plasma display devices.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Luminescent Compositions (AREA)
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Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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US10/536,362 US7261917B2 (en) | 2003-09-26 | 2004-09-24 | Plasma display and method of producing phosphor used therein |
EP04773519A EP1580785A4 (en) | 2003-09-26 | 2004-09-24 | PLASMA DISPLAY AND METHOD FOR PRODUCING A FLUORINE USING THEREOF |
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JP2003335270A JP2005100890A (ja) | 2003-09-26 | 2003-09-26 | プラズマディスプレイ装置 |
JP2003-335270 | 2003-09-26 |
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WO2005031785A1 true WO2005031785A1 (ja) | 2005-04-07 |
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PCT/JP2004/014431 WO2005031785A1 (ja) | 2003-09-26 | 2004-09-24 | プラズマディスプレイ装置およびそれに用いる蛍光体の製造方法 |
Country Status (6)
Country | Link |
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US (1) | US7261917B2 (ja) |
EP (1) | EP1580785A4 (ja) |
JP (1) | JP2005100890A (ja) |
KR (1) | KR100714222B1 (ja) |
CN (1) | CN100394531C (ja) |
WO (1) | WO2005031785A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1600490A1 (en) * | 2004-05-26 | 2005-11-30 | Matsushita Electric Industrial Co., Ltd. | Phosphor having resistance to deterioration caused by ultraviolet rays and gas discharge display device of which image quality is not readily deteriorated over time |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
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KR20070116590A (ko) * | 2005-02-28 | 2007-12-10 | 코니카 미놀타 메디칼 앤드 그래픽 가부시끼가이샤 | 형광체 및 플라즈마 디스플레이 패널 |
KR100696697B1 (ko) * | 2005-11-09 | 2007-03-20 | 삼성에스디아이 주식회사 | 플라즈마 디스플레이 패널 |
JP2007191588A (ja) * | 2006-01-19 | 2007-08-02 | Bando Chem Ind Ltd | 青色発光蛍光材料およびその利用 |
CN102071025A (zh) * | 2010-12-31 | 2011-05-25 | 四川虹欧显示器件有限公司 | Pdp荧光粉材料 |
WO2012114692A1 (ja) * | 2011-02-24 | 2012-08-30 | パナソニック株式会社 | プラズマディスプレイパネル |
JPWO2012114691A1 (ja) * | 2011-02-24 | 2014-07-07 | パナソニック株式会社 | プラズマディスプレイパネル |
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JPS54145386A (en) * | 1978-05-02 | 1979-11-13 | Matsushita Electric Ind Co Ltd | Production of zinc silicate phosphor |
JPH02283791A (ja) * | 1988-12-22 | 1990-11-21 | Gte Prod Corp | マンガンで活性化した珪酸亜鉛蛍光体の製造のための焼成及びミリング処理方法 |
JPH06145659A (ja) * | 1992-11-07 | 1994-05-27 | Nichia Chem Ind Ltd | 真空紫外線励起発光素子 |
JPH1186735A (ja) * | 1997-09-12 | 1999-03-30 | Fujitsu Ltd | プラズマディスプレイパネル |
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JP2003183649A (ja) * | 2001-12-21 | 2003-07-03 | Matsushita Electric Ind Co Ltd | プラズマディスプレイ装置 |
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JPH01186735A (ja) * | 1988-01-19 | 1989-07-26 | Toshiba Corp | ジャイロトロン発振管 |
US6197218B1 (en) * | 1997-02-24 | 2001-03-06 | Superior Micropowders Llc | Photoluminescent phosphor powders, methods for making phosphor powders and devices incorporating same |
EP1267383B1 (en) * | 1997-11-06 | 2007-01-03 | Matsushita Electric Industrial Co., Ltd. | Plasma display panel and method of producing the same |
KR100319488B1 (ko) * | 1999-05-29 | 2002-01-05 | 김충섭 | 규화아연계 녹색 형광체 |
CN1324630C (zh) * | 2001-12-25 | 2007-07-04 | 松下电器产业株式会社 | 等离子体显示屏及其制法 |
KR100456982B1 (ko) * | 2002-02-28 | 2004-11-10 | 한국과학기술연구원 | Pdp용 녹색 형광체의 제조 방법 |
-
2003
- 2003-09-26 JP JP2003335270A patent/JP2005100890A/ja active Pending
-
2004
- 2004-09-24 CN CNB2004800033527A patent/CN100394531C/zh not_active Expired - Fee Related
- 2004-09-24 EP EP04773519A patent/EP1580785A4/en not_active Withdrawn
- 2004-09-24 KR KR1020057013794A patent/KR100714222B1/ko not_active IP Right Cessation
- 2004-09-24 US US10/536,362 patent/US7261917B2/en not_active Expired - Fee Related
- 2004-09-24 WO PCT/JP2004/014431 patent/WO2005031785A1/ja active IP Right Grant
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JPS54145386A (en) * | 1978-05-02 | 1979-11-13 | Matsushita Electric Ind Co Ltd | Production of zinc silicate phosphor |
JPH02283791A (ja) * | 1988-12-22 | 1990-11-21 | Gte Prod Corp | マンガンで活性化した珪酸亜鉛蛍光体の製造のための焼成及びミリング処理方法 |
JPH06145659A (ja) * | 1992-11-07 | 1994-05-27 | Nichia Chem Ind Ltd | 真空紫外線励起発光素子 |
JPH1186735A (ja) * | 1997-09-12 | 1999-03-30 | Fujitsu Ltd | プラズマディスプレイパネル |
JP2001236893A (ja) * | 1999-12-14 | 2001-08-31 | Matsushita Electric Ind Co Ltd | プラズマディスプレイ装置 |
JP2001234165A (ja) * | 2000-02-24 | 2001-08-28 | Nemoto & Co Ltd | 真空紫外線励起型蛍光体 |
JP2003183649A (ja) * | 2001-12-21 | 2003-07-03 | Matsushita Electric Ind Co Ltd | プラズマディスプレイ装置 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1600490A1 (en) * | 2004-05-26 | 2005-11-30 | Matsushita Electric Industrial Co., Ltd. | Phosphor having resistance to deterioration caused by ultraviolet rays and gas discharge display device of which image quality is not readily deteriorated over time |
US7270774B2 (en) | 2004-05-26 | 2007-09-18 | Matsushita Electric Industrial Co., Ltd. | Phosphor having resistance to deterioration caused by ultraviolet rays, and gas discharge display device of which image quality is not readily deteriorated over time |
Also Published As
Publication number | Publication date |
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EP1580785A4 (en) | 2009-09-16 |
KR20050109471A (ko) | 2005-11-21 |
EP1580785A1 (en) | 2005-09-28 |
JP2005100890A (ja) | 2005-04-14 |
CN100394531C (zh) | 2008-06-11 |
US7261917B2 (en) | 2007-08-28 |
KR100714222B1 (ko) | 2007-05-02 |
CN1745451A (zh) | 2006-03-08 |
US20060071588A1 (en) | 2006-04-06 |
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