CN1238465C - Diolame fluorescent powder and preparing method thereof - Google Patents
Diolame fluorescent powder and preparing method thereof Download PDFInfo
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- CN1238465C CN1238465C CN 02157221 CN02157221A CN1238465C CN 1238465 C CN1238465 C CN 1238465C CN 02157221 CN02157221 CN 02157221 CN 02157221 A CN02157221 A CN 02157221A CN 1238465 C CN1238465 C CN 1238465C
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- fluorescent material
- film
- coating
- fluorescent powder
- boride
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Abstract
The present invention relates to a coated fluorescent powder whose service life is obviously prolonged, and the improvement of a preparation method of the coated fluorescent powder. The coated fluorescent powder is characterized in that the surface of the fluorescent powder is coated by a compact impermeable borate film or a compound borate film, so the adverse influence of environmental moisture to the fluorescent powder is effectively avoided, and the service life of the fluorescent powder is greatly prolonged. The present invention overcomes the defect that a traditional sol-gel coating method is difficult to form a compact protective film. The coating method has the advantages of convenience, reliability, simplified film-forming process and reduced film-forming cost, and coating effects are similar to that of a chemical vapor deposition method.
Description
Technical field
The present invention relates to a kind of phosphor surface treatment technology, especially can significantly improve the moisture resistance and the anti-ageing change ability of fluorescent material, increase fluorescent material brightness, effect and the coated fluorescent powder in life-span and coating preparation method.
Background technology
The field causes or photoinduced fluroscence powder, can make its generation complicated electricity or photochemical reaction because of airborne moisture, causes the rapid decay of luminous intensity, and the life-span reduces, and makes the luminescent screen blackening, so common the employing at phosphor surface of people wrapped up oxide film (as SiO
2, TiO
2Or Al
2O
3Deng oxide coating), with effectively prevent surrounding environment especially humidity to the infringement of fluorescent material, thereby prolong work-ing life of fluorescent material.
Coating method commonly used has chemical Vapor deposition process and sol-gel method, because the chemical Vapor deposition process film formation time is long, required cost is also than higher, and can lose fluorescent material brightness, thereby the sol-gel method that the more employing of people is easy and simple to handle, the coating cost is low.Be dissolved in organic solvent formation colloidal sol as the United States Patent (USP) 3002861 disclosed metallorganicss such as barium, titanium that contain, and the method for the barium titanate film of on glass and metal, growing; United States Patent (USP) 326133 is openly with titanium compound method at phosphor surface growth titanium deoxid film in ethanolic soln; Chinese patent 96118930 openly is dissolved in organometallics (as titaniferous, aluminum organic compound) in the organic solvent (as ethanol, propyl alcohol), in 450-650 ℃ of air calcination 20-120 minute, make organism decompose the back and obtain anti-aging metal oxide rete at phosphor surface; Chinese patent 98122739 is open with fluorescent material and the organic compound that contains silicon, titanium, zirconium, aluminium and/or baric, the organic compound of lead and the coating liquid uniform mixing that relevant solvent is made into, put into 120 ℃ of vacuum drying oven vacuum-dryings 48 hours, repeat 2-5 time as required, obtain the desired thickness coating, in air, be warming up to 500 ℃ of sintering then 2 hours, organism is fully volatilized, thereby form silicon, titanium, zirconium, aluminum oxide, the method for lead titanate, barium titanate and complex thin film at phosphor surface.
Yet in sol-gel, coating oxide compound and oxysalt colloidal solid are difficult to evenly be adsorbed on phosphor surface, though through aerial sintering, the protective membrane that phosphor surface forms is still fine and close inadequately.Because the quality of fluorescent material coating directly influences the use properties of fluorescent material; therefore; protective membrane with sol-gel method formation; still can not prevent the infringement of surrounding environment fully to fluorescent material; the fluorescent material of being produced still exists the decay of certain luminous intensity very fast; life-span is shorter, and makes the shortcoming of luminescent screen blackening.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and can form fine and close protective membrane, to prevent the infringement of surrounding environment to fluorescent material, the coated fluorescent powder that effectively increases the service life at phosphor surface.
Another object of the present invention is to provide a kind of preparation method of above-mentioned coated fluorescent powder.
The present invention's first purpose realizes main the improvement: select existing wide energy gap and stable for use through the repeated screening test, have low-melting relatively white boron oxide (B again
2O
3) as coating fusing assistant and reagent and other coating oxide compound (for example BaO, TiO
2, ZrO
2, WO
3, ZnO, B
2O
3, Al
2O
3, SiO
2, PbO, Bi
2O
3Wide energy gap and stable oxide) or its oxysalt (for example titanate, zirconate, tungstate, borate, aluminate, silicate, carbonate, phosphoric acid salt, the wide energy gap of vitriol and stable oxysalt) reaction, be formed on fluorescent material the body surface evenly fine and close borate or the compound borate films of parcel, for example
(barium borate),
(aluminum borate),
(boric acid titanium),
(lead borate),
(borosilicic acid barium composite salt),
(titanium barium borate composite salt),
(barium borophosphate composite salt).Specifically, coated fluorescent powder of the present invention is characterized in that said fluorescent material surface coating is the borate or the compound borate film of boron oxide and coating oxide compound or oxysalt reaction generation.
Boron oxide in the coating of the present invention, because fusing point low (450 ℃ are in a liquid state), as the coating fusing assistant, also be tackiness agent and reagent, its effect is to provide a kind of liquid medium for film forming, can form form compact and stable fluid-tight compound coating with other coating oxide compound or oxysalt after making the burning refining, thereby make coating oxide compound or oxysalt can tightly be wrapped in fluorescent material table body, obtain a kind of fine and close coating.Overcome traditional sol-gel method and used coating oxide compound or oxysalt merely, be more difficult to get the deficiency of dense oxide or oxysalt coating.
Coating oxide compound of the present invention can also be by low-boiling compounds (as titanium tetrachloride, trimethyl aluminium, silicon tetrachloride etc.) such as the titanium of gas phase, aluminium, silicon, and they and boride (as boric acid) reaction are at fluorescent material table body deposition coating oxide compound and boron oxide.As:
、
。These oxide compounds also can obtain comparatively fine and close borate films (as boric acid titanium, aluminum borate etc.) by burning refining.
Fluorescent material of the present invention can be various and cause or photoinduced fluroscence powder, as long persistence phosphor of alkali earth aluminate, electrofluor powder, UV-light fluorescent material.As adopting zinc sulphide type electrofluor powder, its protection coating preferably adopts oxide compound (as titanium oxide, zirconium white etc.) or the oxysalt (as barium titanate, boron barium titanate etc.) with high-k, the brightness of favourable enhancing zinc sulfide electrofluor powder and effect.
The present invention forms the coating method that obtains borate or compound borate films at the fluorescent material body surface, it is characterized in that:
(1) with boride, fluorescent material weight 0.25-5%wt coating oxide compound or the oxysalt blend in liquid phase of fluorescent material and fluorescent material weight 0.1-5%wt, filtering drying;
Or with boride blend in liquid phase of fluorescent material and fluorescent material weight 0.1-5%wt, filtering drying obtains being surrounded by the fluorescent material of boride film;
To be surrounded by coating oxide compound or the oxysalt blend in liquid phase of the fluorescent material and the fluorescent material weight 0.25-5%wt of boride film again, filtering drying;
Maybe will be surrounded by the rare gas element constant temperature deposition of the fluorescent material of boride film with low-boiling compounds such as titaniferous, aluminium, silicon;
(2) again through 450-600 ℃ of baking film forming.
Coating boride amount of the present invention is excellent with 0.1-2%wt especially, and coating oxide compound or oxysalt amount are excellent with 0.25-2%wt especially; Said baking film forming is meant that film forming drips not blackening of powder with the 0.1M silver nitrate solution.
Be that coating of the present invention forms, three kinds of methods can be arranged:
The one-pass film-forming method, with the need coated fluorescent powder, contain solvable boride of 0.1-2%wt or boron oxide micro mist, contain mix in the solution of 0.25-2%wt coating oxide compound or oxysalt after, filtering drying is through 450-600 ℃ of baking film forming such as 1-5 hour one-pass film-forming;
Also can adopt two-step approach: earlier fluorescent material is placed the boride solution that contains 0.1-2%wt, filtering drying for example through 450-600 ℃ of baking slightly (as 0.25-0.5 hour), obtains being surrounded by the fluorescent material of boride film; The aforementioned fluorescent material that is surrounded by the boride film that makes is placed the coating oxide compound that contains 0.25-2%wt or the solution of oxysalt, filtering drying was through 450-600 ℃ of baking film forming such as 1-5 hour again.Promptly form the boride film at fluorescent material table body earlier, form borate or two steps of compound borate films again, the coating densification that this method generates than single stage method.
Coating of the present invention can also obtain by solution method and the chemical Vapor deposition process method that combines: soon fluorescent material places and contains 0.1-2%wt boride solution, and filtering drying obtains boride (as boric acid) coating; The fluorescent material that will be surrounded by the boride film again places 80-150 ℃ of constant temperature flask, blast rare gas element 6-12 hour of low-boiling compounds such as titaniferous, aluminium, silicon (as titanium tetrachloride, trimethyl aluminium, silicon tetrachloride etc.), after 450-600 ℃ of baking film forming such as 1-5 hour obtain the borate coating.Examine and filter cost, rare gas element of the present invention is comparatively suitable with nitrogen especially.Show that after testing solution method+chemical Vapor deposition process more can generate fine and close protection coating than sol-gel two-step approach again.
Coated fluorescent powder of the present invention; make coating fusing assistant, tackiness agent and reagent owing to adopt the low melting point boron oxide; after the baking; can make through the coating oxide compound of liquid state-solid state reaction or oxysalt and the boride reaction is stablized, fine and close, waterproof, dystectic vitreous state borate or compound borate are protected coating (containing boron, oxygen and other coating element through trace analysis (ICP, EDX, XPS) coating powder surface); effectively prevented the disadvantageous effect of ambient moisture, greatly prolonged the work-ing life of fluorescent material fluorescent material.Because the intervention of low melting point boron oxide has overcome the difficult shortcoming that obtains fine and close protective membrane that forms of traditional sol-gel method coating; And, do not influence the glow color and the brightness of fluorescent material again substantially because boron oxide is white in color.The inventive method is compared with the pure chemistry vapour deposition process, and is easy to be reliable, and film process is greatly simplified, and the film forming cost greatly reduces, and the coating effect is near the pure chemistry vapour deposition process.
Below in conjunction with several embodiments, understand the present invention with further help.
Embodiment
Comparative example 1: 100g zinc sulphide type electrofluor powder and 1.0g boric acid are dissolved in the water of 75ml, slowly stirred 2 hours at 50 ℃ of constant temperature, behind the filtering drying, again with fluorescent material baking 0.25 hour in 470 ℃ stove, in air, cool off then, obtain being surrounded by the fluorescent material of oxidation boron film.The brightness of this coating powder is constant, and the transformation period has only 1000 hours (seeing attached list).
Comparative example 2: 100g zinc sulphide type electrofluor powder is placed the commercial nano level titanium oxide (TiO of 75ml
2) in the solution, wherein titanium oxide content is 1% of a fluorescent material weight, slowly stirred 3 hours at 50 ℃ of constant temperature, behind the filtering drying, repeat said process twice, again with fluorescent material baking 3 hours in 530 ℃ stove, in air, cool off then, obtain being surrounded by the electrofluor powder of oxidation titanium film.The brightness of this coating powder is constant, and the transformation period has only 1500 hours (seeing attached list).
Embodiment 1: 100g zinc sulphide type electrofluor powder and 1.0g boric acid are dissolved in the water of 75ml, slowly stirred 2 hours at 50 ℃ of constant temperature, behind the filtering drying, again with fluorescent material baking 0.25 hour in 470 ℃ stove, in air, cool off then, obtain being surrounded by the fluorescent material of oxidation boron film.The fluorescent material that again this is surrounded by the oxidation boron film places the commercial nano level titanium oxide solution of 75ml, wherein titanium oxide content is 1% of a fluorescent material weight, slowly stirred 3 hours at 50 ℃ of constant temperature, behind the filtering drying, repeat the process above twice, with fluorescent material baking 3 hours in 530 ℃ stove, in air, cool off then again, obtain being surrounded by the fluorescent material of boric acid titanium film.The brightness of this coating powder is constant, and the transformation period is by being increased to 3500 hours (seeing attached list) in 500 hours.
Embodiment 2: 100g zinc sulphide type electrofluor powder and 1.0g boric acid are placed the commercial nano level titanium oxide solution of 75ml, wherein titanium oxide content is 1% of a fluorescent material weight, slowly stirred 3 hours at 50 ℃ of constant temperature, behind the filtering drying, repeat the process above twice, with fluorescent material baking 3 hours in 530 ℃ stove, in air, cool off then again, obtain being surrounded by the fluorescent material of boric acid titanium film.The brightness of this coating powder is constant, and the transformation period is increased to 3000 hours (seeing attached list).
Embodiment 3: 100g zinc sulphide type electrofluor powder and 1.0g boric acid are placed the commercial nano level aluminum oxide (Al of 70 ℃ of 100ml
2O
3) in the solution, wherein alumina content is 0.9% of a fluorescent material weight, slowly stirs 2.5 hours, behind the filtering drying, repeat the process above four times, again with fluorescent material baking 3 hours in 500 ℃ stove, in air, cool off then, obtain wrapping up the fluorescent material of aluminum borate film.The brightness of this coating powder is constant, and the transformation period is increased to 4000 hours (seeing attached list).
Embodiment 4: 100g zinc sulphide type electrofluor powder is placed the water of 65 ℃ of 100ml, add 2.0g phosphoric acid, add the 2.0g barium acetate, add 1.5g ultra micro boron oxide (B again
2O
3), stir half an hour, regulate pH=8, slowly stirred 1 hour, behind the filtering drying, with fluorescent material baking 2 hours in 550 ℃ stove, in air, cool off then again, obtained the fluorescent material of phosphorus barium borate composite salt film.The brightness of this coating powder is constant, and the transformation period is increased to 3000 hours (seeing attached list).
Embodiment 5: the ethanol that 100g zinc sulphide type electrofluor powder is placed 65 ℃ of 100ml, add the 2.0g barium acetate, add 1.0g titanic ethyl ester and 1.0g boric acid again, slowly stirred 1 hour, behind the filtering drying, with fluorescent material baking 2 hours in 550 ℃ stove, in air, cool off then again, obtained the fluorescent material of boron barium titanate composite salt film.The brightness of this coating powder is constant, and the transformation period is increased to 3500 hours (seeing attached list).
Embodiment 6: 100g fluorescent material is placed the water of 50 ℃ of 100ml, add 1g H
3BO
3, slowly stirred 1 hour, behind the filtering drying, the nitrogen that will contain titanium tetrachloride again blasts 120 ℃ of homothermic and fills in the bag boric acid fluorescent material flask 8 hours, with fluorescent material baking 3 hours in 530 ℃ stove, in air, cool off then again, obtained the fluorescent material of boric acid titanium film at last.Be increased to the invariant half life of the brightness of this coating powder 4500 hours (seeing attached list).
Embodiment 7: 100g long persistence phosphor of alkali earth aluminate and 1.0g boric acid are dissolved in the water of 75ml, slowly stirred 2 hours at 50 ℃ of constant temperature, behind the filtering drying, again with fluorescent material baking 0.25 hour in 470 ℃ stove, in air, cool off then, obtain being surrounded by the fluorescent material of oxidation boron film.The fluorescent material that again this is surrounded by the oxidation boron film places the commercial nano level titanium oxide solution of 75ml, wherein titanium oxide content is 1% of a fluorescent material weight, slowly stirred 3 hours at 50 ℃ of constant temperature, behind the filtering drying, repeat the process above twice, with its baking 3 hours in 530 ℃ stove, in air, cool off then, obtain being surrounded by the long persistence luminescent powder of titanium borate films.The brightness of this coating powder is constant, and the transformation period improves 200%.
The present invention can also use other fluorescent material, replace above-mentioned fluorescent material as long persistence phosphor of alkali earth aluminate, electrofluor powder, UV-light fluorescent material etc., and other boride, coating oxide compound or oxysalt, can obtain comparatively fine and close borate or compound borate coating equally, give an example no longer one by one.
The embodiment coating electrofluor powder transformation period (hour)
| Electrofluor powder | Transformation period (hour) |
| Coating powder not | 500 |
| Comparative example 1 oxidation boron film fluorescent material | 1000 |
| Comparative example 2 oxidation titanium film fluorescent material | 1500 |
| Example 1 boric acid titanium film fluorescent material | 3500 |
| Example 2 boric acid titanium film fluorescent material | 3000 |
| Example 3 aluminum borate film fluorescent material | 4000 |
| Example 4 phosphorus barium borate composite salt film fluorescent material | 3000 |
| Example 5 boron barium titanate composite salt film fluorescent material | 3500 |
| Example 6 boron titanic acid film fluorescent material | 4500 |
Illustrate: the result shows in the table: under the same conditions, boric acid titanium of the present invention (salt) coating effect is better than single boron oxide or titanium oxide protection coating; The luminescent lifetime of boric acid titanium (salt) the film fluorescent material that the two step method coating generates generates the length of coating than single stage method.In addition, the result shows that also the aluminum borate film is than boric acid titanium film protecting fluorescent material; The high-k boron barium titanate composite salt film light-emitting phosphor life-span is longer than phosphorus barium borate composite salt film fluorescent material.
Claims (12)
1, a kind of coated fluorescent powder is characterized in that said fluorescent material surface coating is the borate or the compound borate film of boron oxide and coating oxide compound or oxysalt reaction generation.
2,, it is characterized in that said fluorescent material is zinc sulfide electrofluor powder according to the described coated fluorescent powder of claim 1.
3,, it is characterized in that said coating oxide compound or oxysalt are high dielectric constant oxide or oxysalt according to the described coated fluorescent powder of claim 2.
4,, it is characterized in that said high dielectric constant oxide or oxysalt are titanium oxide, zirconium white or barium titanate, boron barium titanate according to the described coated fluorescent powder of claim 3.
5,, it is characterized in that said coating oxide compound is the titanium of gas phase, aluminium, silicon low-boiling compound according to the described coated fluorescent powder of claim 1.
6, the preparation method of the said coated fluorescent powder of a kind of claim as described above is characterized in that:
(1) with boride, fluorescent material weight 0.25-5%wt coating oxide compound or the oxysalt blend in liquid phase of fluorescent material and fluorescent material weight 0.1-5%wt, filtering drying;
Or with boride blend in liquid phase of fluorescent material and fluorescent material weight 0.1-5%wt, filtering drying obtains being surrounded by the fluorescent material of boride film;
To be surrounded by coating oxide compound or the oxysalt blend in liquid phase of the fluorescent material and the fluorescent material weight 0.25-5%wt of boride film again, filtering drying;
Maybe will be surrounded by the rare gas element constant temperature deposition of the fluorescent material of boride film with titaniferous, aluminium, silicon low-boiling compound;
(2) again through 450-600 ℃ of baking film forming.
7, according to the preparation method of the described coated fluorescent powder of claim 6, it is characterized in that said boride is 0.1-2%wt, coating oxide compound or oxysalt are 0.25-2%wt.
8, according to the preparation method of the described coated fluorescent powder of claim 6, it is characterized in that earlier fluorescent material being placed the blend of boride solution, filtering drying, obtain being surrounded by the fluorescent material of boride film, the blend in liquid phase with coating oxide compound or oxysalt again, filtering drying is again through 450-600 ℃ of baking film forming.
9, according to the preparation method of the described coated fluorescent powder of claim 6, it is characterized in that earlier fluorescent material being placed the blend of boride solution, filtering drying, obtain being surrounded by the fluorescent material of boride film, rare gas element constant temperature with titaniferous, aluminium, silicon low-boiling compound deposits again, again through 450-600 ℃ of baking film forming.
10,, it is characterized in that said constant temperature is 80-150 ℃ according to the preparation method of claim 6 or 9 described coated fluorescent powders.
11,, it is characterized in that said low-boiling compound is titanium tetrachloride, trimethyl aluminium, silicon tetrachloride according to the preparation method of the described coated fluorescent powder of claim 9.
12,, it is characterized in that said rare gas element is a nitrogen according to the preparation method of claim 6 or 9 described coated fluorescent powders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157221 CN1238465C (en) | 2002-12-20 | 2002-12-20 | Diolame fluorescent powder and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157221 CN1238465C (en) | 2002-12-20 | 2002-12-20 | Diolame fluorescent powder and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1510102A CN1510102A (en) | 2004-07-07 |
| CN1238465C true CN1238465C (en) | 2006-01-25 |
Family
ID=34236515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02157221 Expired - Fee Related CN1238465C (en) | 2002-12-20 | 2002-12-20 | Diolame fluorescent powder and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703056B (en) * | 2012-05-09 | 2014-06-25 | 苏州英特华照明有限公司 | Compound enveloped LED (light-emitting diode) phosphor powder grain and enveloping method thereof |
| WO2015146231A1 (en) * | 2014-03-27 | 2015-10-01 | 三井金属鉱業株式会社 | Phosphor and use thereof |
| CN104910902A (en) * | 2015-06-01 | 2015-09-16 | 彩虹集团电子股份有限公司 | Surface treatment method of zinc-manganese silicate green fluorescent powder |
| CN106189490A (en) * | 2016-08-29 | 2016-12-07 | 汕头市派亚油墨有限公司 | Electroluminescent uv ink |
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| Publication number | Publication date |
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| CN1510102A (en) | 2004-07-07 |
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