CN106867508A - A kind of surface treatment method of LED backlight silicate yellow fluorescent powder - Google Patents
A kind of surface treatment method of LED backlight silicate yellow fluorescent powder Download PDFInfo
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- CN106867508A CN106867508A CN201611256491.1A CN201611256491A CN106867508A CN 106867508 A CN106867508 A CN 106867508A CN 201611256491 A CN201611256491 A CN 201611256491A CN 106867508 A CN106867508 A CN 106867508A
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- fluorescent powder
- yellow fluorescent
- surface treatment
- led backlight
- silicate yellow
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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
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
- C09K11/592—Chalcogenides
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Abstract
A kind of surface treatment method of LED backlight silicate yellow fluorescent powder, step is as follows：(1) by alkoxy silane and alcohols in mass ratio 1:The ratio mixing of (1 10), is stirred 12 hours at 10 30 DEG C, and nitric acid is added by 1% 50% titration of its volume ratio, is heated at 60 80 DEG C, is reacted 12 48 hours, is configured to precursor solution；(2) silicate yellow fluorescent powder is carried out into slurry using the isopropanol of 5 50 mass times, is in mass ratio 100 by gained slurry:0.5‑100:5 ratio is added in the precursor solution in step (1), stirring obtain liquid fluorescent material within 16 hours, after at 80 120 DEG C dry 10 24 hours；(3) fluorescent material formed after being dried in step (2) is put into alumina crucible, in a nitrogen atmosphere, in 600 800 DEG C of calcinations 15 hours, 100 mesh sieves are crossed after natural cooling, obtain LED backlight silicate yellow fluorescent powder surface treatment finished product；The characteristics of silicate yellow fluorescent powder for processing out has high-luminous-efficiency, strong moisture resistant ability and strong anti-decay property.
Description
Technical field
The present invention relates to luminescent material preparing technical field, more particularly to a kind of LED backlight silicate yellow fluorescence
The surface treatment method of powder.
Background technology
At present, the silicate yellow fluorescence used in the commercialization such as LCD TV, computer screen and smart mobile phone backlight
Powder lean on substantially import fluorescent material meet, domestic fluorescent material in use generally existing luminous efficiency it is relatively low, in humid air
In easily decompose, the shortcomings of anti-decay property is poor.
The content of the invention
In order to overcome the defect of above-mentioned prior art, it is an object of the invention to provide a kind of LED backlight silicate
The surface treatment method of yellow fluorescent powder, the silicate yellow fluorescent powder for processing out has high-luminous-efficiency, strong moisture resistant ability
The characteristics of with strong anti-decay property.
In order to achieve the above object, the technical proposal of the invention is realized in this way：
A kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its step is as follows：
(1) by alkoxy silane and alcohols in mass ratio 1:The ratio of (1-10) is mixed, and obtains mixed liquor, is pressed
The 1%-50% titration of its volume ratio adds nitric acid, carries out heating response, is configured to precursor solution；
(2) silicate yellow fluorescent powder is carried out into slurry using the isopropanol of its 5-50 times of quality, crosses 500 eye mesh screens,
By gained slurry in mass ratio 100:0.5-100:5 are added in the precursor solution in step (1) and are stirred, and obtain liquid
Fluorescent material, is then dried；
(3) the fluorescent material powder agglomates formed after being dried in step (2) crosses 100 mesh sieves, is put into alumina crucible, in nitrogen
Under atmosphere, calcination is carried out, after 100 mesh sieves after natural cooling, obtain LED backlight and be surface-treated with silicate yellow fluorescent powder
Finished product.
In the step (1), alkoxy silane be tetramethoxy-silicane, tetraethoxysilane, MTMS,
One or two in MTES or dimethyl methoxy silane arbitrarily compare mixture.
In the step (1), alcohols be methyl alcohol, ethanol, ethylene glycol, isopropanol, propane diols or n-butanol in one kind or
Two kinds are arbitrarily compared mixture.
In the step (1), the mass concentration of nitric acid is 1%-40%.
Stirring in the step (1), need to stir 1-2 hours at 10-30 DEG C.
Heating response in the step (1), need to be heated to 60-80 DEG C, react 12-48 hours.
Stirring in the step (2), need to stir 1-6 hours.
Dried in the step (2), need to be dried at 80-120 DEG C 10-24 hours.
In the step (3), nitrogen atmosphere refers to that nitrogen flow is 1-3 cubes m/h.
Calcination in the step (3), need to be calcination 1-5 hours at 600-800 DEG C.
The beneficial effects of the invention are as follows：Processed using distinctive netted silica in surface treatment, calcination portion
Point nitrogen atmosphere is used, so that processing out, luminescent properties are good, the commercial LED silicon that Deliquescence-resistant ability is strong, anti-decay property is superior
Hydrochlorate yellow fluorescent powder.
Specific embodiment
Embodiment one
A kind of surface treatment method of LED backlight silicate yellow fluorescent powder, comprises the steps：
(1) 40g tetraethoxysilanes, 86g ethanol are added in flask, is stirred 1 hour at 30 DEG C, titration adds quality
Concentration is 1% nitric acid 8g, is heated at 80 DEG C, is reacted 12 hours, is configured to precursor solution；
(2) 100g silicate yellow fluorescent powders are crossed into 500 eye mesh screens, by gained using after 1000ml isopropanol slurries
Slurry is added in the precursor solution prepared in step (1), is stirred 1 hour, is then dried 24 hours at 80 DEG C；
(3) the fluorescent material powder agglomates formed after step (2) is dried crosses 100 mesh sieves, is put into alumina crucible, in nitrogen gas
Under atmosphere (nitrogen flow be 1 cube m/h), in 600 DEG C of calcinations 3 hours, 100 mesh sieves are crossed after natural cooling, obtain LED-backlit
Source is surface-treated finished product with silicate yellow fluorescent powder.
Embodiment two
A kind of surface treatment method of LED backlight silicate yellow fluorescent powder, comprises the steps：
(1) 231g tetraethoxysilanes, 1100g ethanol and 55g propane diols are added in flask, 2 is stirred at 30 DEG C small
When, it is 10% nitric acid 69.3g that titration adds mass concentration, is heated at 80 DEG C, is reacted 24 hours, is configured to precursor solution；
(2) 500g silicate yellow fluorescent powders are crossed into 500 eye mesh screens, by gained using after 5000ml isopropanol slurries
Slurry is added in the precursor solution prepared in step (1), stirs 2h, is then dried 24 hours at 100 DEG C；
(3) the fluorescent material powder agglomates formed after step (2) is dried crosses 100 mesh sieves, is put into alumina crucible, in nitrogen gas
Under atmosphere (nitrogen flow be 1 cube m/h), in 700 DEG C of calcinations 3 hours, 100 mesh sieves are crossed after natural cooling, obtain LED-backlit
Source is surface-treated finished product with silicate yellow fluorescent powder.
Embodiment three
A kind of surface treatment method of LED backlight silicate yellow fluorescent powder, comprises the steps：
(1) 36g tetraethoxysilanes, 29g MTMSs and 390g ethanol are added in flask, at 30 DEG C
Stirring 1 hour, titration adds the nitric acid 13g of mass concentration 2%, is heated at 65 DEG C, reacts 12 hours, is configured to presoma molten
Liquid；
(2) 125g silicate yellow fluorescent powders are crossed into 500 eye mesh screens, by gained using after 1680ml isopropanol slurries
Slurry is added in the precursor solution prepared in step (1), stirs 2h, is then dried 24 hours at 100 DEG C；
(3) the fluorescent material powder agglomates formed after step (2) is dried crosses 100 mesh sieves, is put into alumina crucible, in nitrogen gas
Under atmosphere (nitrogen flow be 1 cube m/h), in 700 DEG C of calcinations 5 hours, 100 mesh sieves are crossed after natural cooling, obtain LED-backlit
Source is surface-treated finished product with silicate yellow fluorescent powder.
Claims (10)
1. a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, it is characterised in that step is as follows：(1) will
Alkoxy silane and alcohols in mass ratio 1:The ratio of (1-10) is mixed, and obtains mixed liquor, by its volume ratio
1%-50% titration adds nitric acid, carries out heating response, is configured to precursor solution；(2) silicate yellow fluorescent powder is used
The isopropanol of its 5-50 times of quality carries out slurry, 500 eye mesh screens is crossed, by gained slurry in mass ratio 100:0.5-100:5 add
Enter in the precursor solution in step (1) and be stirred, obtain liquid fluorescent material, be then dried；(3) by step (2)
The fluorescent material powder agglomates formed after middle drying crosses 100 mesh sieves, is put into alumina crucible, in a nitrogen atmosphere, carries out calcination, natural
100 mesh sieves are crossed after cooling, LED backlight silicate yellow fluorescent powder surface treatment finished product is obtained.
2. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In step (1) alkoxy silane is tetramethoxy-silicane, tetraethoxysilane, MTMS, the second of methyl three
One or two in TMOS or dimethyl methoxy silane arbitrarily compare mixture.
3. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In step (1) alcohols is any for one or two in methyl alcohol, ethanol, ethylene glycol, isopropanol, propane diols or n-butanol
Compare mixture.
4. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In the mass concentration of step (1) nitric acid is 1%-40%.
5. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In the stirring in the step (1) need to be stirred 1-2 hours at 10-30 DEG C.
6. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In the heating response in the step (1) need to be heated to 60-80 DEG C, react 12-48 hours.
7. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In the stirring in the step (2) need to be stirred 1-6 hours.
8. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In, dried in the step (2), need to be dried at 80-120 DEG C 10-24 hours.
9. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In nitrogen atmosphere in the step (3) refers to that nitrogen flow is 1-3 cubes m/h.
10. as claimed in claim 1, a kind of surface treatment method of LED backlight silicate yellow fluorescent powder, its feature exists
In calcination in the step (3) need to be calcination 1-5 hours at 600-800 DEG C.
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| CN201611256491.1A CN106867508A (en) | 2016-12-30 | 2016-12-30 | A kind of surface treatment method of LED backlight silicate yellow fluorescent powder |
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| CN201611256491.1A CN106867508A (en) | 2016-12-30 | 2016-12-30 | A kind of surface treatment method of LED backlight silicate yellow fluorescent powder |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101868515A (en) * | 2007-11-22 | 2010-10-20 | 默克专利有限公司 | Surface-modified phosphors |
| CN102899020A (en) * | 2012-10-25 | 2013-01-30 | 江苏博睿光电有限公司 | Silicate fluorescent powder for coating LED and coating method thereof |
| TW201404866A (en) * | 2012-07-20 | 2014-02-01 | Sumitomo Metal Mining Co | Method for fabricating silicate phosphor particles with coated film |
| WO2014104286A1 (en) * | 2012-12-28 | 2014-07-03 | 宇部マテリアルズ株式会社 | Coated phosphor particles and manufacturing process therefor |
-
2016
- 2016-12-30 CN CN201611256491.1A patent/CN106867508A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101868515A (en) * | 2007-11-22 | 2010-10-20 | 默克专利有限公司 | Surface-modified phosphors |
| TW201404866A (en) * | 2012-07-20 | 2014-02-01 | Sumitomo Metal Mining Co | Method for fabricating silicate phosphor particles with coated film |
| CN102899020A (en) * | 2012-10-25 | 2013-01-30 | 江苏博睿光电有限公司 | Silicate fluorescent powder for coating LED and coating method thereof |
| WO2014104286A1 (en) * | 2012-12-28 | 2014-07-03 | 宇部マテリアルズ株式会社 | Coated phosphor particles and manufacturing process therefor |
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