CN106634950A - Scratch-resistant polymethyl-methacrylate-coated rare-earth-doped fluorescent powder and preparation method thereof - Google Patents
Scratch-resistant polymethyl-methacrylate-coated rare-earth-doped fluorescent powder and preparation method thereof Download PDFInfo
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- CN106634950A CN106634950A CN201611043957.XA CN201611043957A CN106634950A CN 106634950 A CN106634950 A CN 106634950A CN 201611043957 A CN201611043957 A CN 201611043957A CN 106634950 A CN106634950 A CN 106634950A
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- fluorescent powder
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- polymethyl methacrylate
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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
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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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
- C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
Abstract
The invention discloses a scratch-resistant polymethyl-methacrylate-coated rare-earth-doped fluorescent powder and a preparation method thereof. The invention is characterized in that the fluorescent powder is prepared from the following raw materials in parts by weight: 2-4 parts of nano silicon oxide, 2-5 parts of Eu2O3, 1-3 parts of polypropylene, 10-20 parts of La(NO3)3.6H2O, 2-5 parts of cetyl trimethylammonium bromide, 30-40 parts of Na2WO4.2H2O, 2-4 parts of calcium silicate, 4-9 parts of silicon dioxide, 30-50 parts of dilute nitric acid, a right amount of distilled water, a right amount of ethanol, 15-25 parts of polymethyl methacrylate, 30-40 parts of ethyl acetate, 5-8 parts of polyethyleneglycol and 3-5 parts of aluminum oxide. In the fluorescent powder synthesis process, the silicon dioxide is added as the nucleus, thereby providing the crystal nucleus for the crystallization of the fluorescent powder so as to promote the crystallization, and enlarging the grains of the fluorescent powder; and the luminescence specific area is large, thereby increasing the light effect and lowering the cost. The added nano silicon oxide and the like improve the scratch resistance of the material.
Description
Technical field
The present invention relates to a kind of fluorescent material and preparation method thereof, and in particular to a kind of scratch-resistant, polymethyl methacrylate
Rare earth doping fluorescent powder of parcel and preparation method thereof.
Background technology
Rare-earth tungstate luminescent material is a good fluorescence host material, and its stable chemical nature, quenching concentration is high,
Therefore the rare earth ion that can be adulterated is dense, this can improve to a certain extent the luminosity of prepared luminescent powder.
NaLa(WO4)2Itself it is self-activate luminescence material, when there is outside energy, NaLa (WO4)2In electronic energy from O2—'s
The 2p tracks of excitation state move to W6+Center room track, exactly this reason, so NaLa (WO4)2Luminescent powder has one
Wide, strong charge-transfer band.Total consideration, the little halfwidth for having higher quantum yield and transmitting band under near ultraviolet excitated
Output to high brightness it is critical that.Eu3+NaLa (the WO of doping4)2Fluorescent material can be with effectively by near ultraviolet band
(380nm-410nm) light is excited, and it can very smoothly from NaLa (WO from the energy that the external world is absorbed4)2Matrix is passed
Pass active ions Eu3+, and finally launch fluorescence.
Zhang Xing is in its master thesis《The preparation of rare-earth-dopping yttrium aluminum garnet and Tungstate fluorescent powder and luminescent properties
Research》In, using Eu2O3、La(NO3)3、Na2WO4It is prepared for a kind of NaLa (WO4)2 :Eu3+Fluorescent material, but its resistance to bombardment
It is not good enough, it is relatively costly.
The content of the invention
Think deeply based on more than, the present invention is intended to provide a kind of resistance to bombardment property preferable, brightness is strong, cost is relatively low, encapsulation light efficiency
Good rear-earth-doped Tungstate fluorescent powder, and preparation method thereof.
The technical problem to be solved is realized using following technical scheme：
The rare earth doping fluorescent powder of a kind of scratch-resistant, polymethyl methacrylate parcel, it is characterised in that be by following weight portion
Raw material make：
Nano silicon oxide 2-4, Eu2O3 2-5, polypropylene 1-3, La (NO3)3·6H2O 10-20, cetyl trimethylammonium bromide
2-5, Na2WO4·2H2O 30-40, calcium silicates 2-4, silica 4-9, dust technology 30-50, distillation appropriate amount of water, appropriate amount of ethanol,
Polymethyl methacrylate 15-25, ethyl acetate 30-40, polyethylene glycol 5-8, alundum (Al2O3) 3-5；
The mass fraction of the dust technology is 10-30%；
Described a kind of scratch-resistant, rare earth doping fluorescent powder of polymethyl methacrylate parcel and preparation method thereof, its feature
It is to be made up of following steps：
A. Eu is added in dilute nitric acid solution2O3So as to it is completely dissolved；By La (NO3)3·6H2After O is soluble in water, add together
Enter in above-mentioned solution, stir 8-25min, add cetyl trimethylammonium bromide, Na2WO4·2H2O, and continue to stir 10-
30 minutes；
B. rapid a resulting solutions PH of pacing add silica, calcium silicates to neutrality, and autoclave is proceeded to after stirring
In, 15-20h is incubated under the conditions of 150-200 DEG C；Cooling afterwards, precipitation is filtered, and with distilled water, alcohol flushing 2-3 time, then
50-80 DEG C of insulation 5-10h in baking oven is proceeded to, obtains wrapping up silica, the NaLa (WO of calcium silicates4)2 :Eu3+Fluorescent material；
C. polymethyl methacrylate is dissolved in ethyl acetate, adds polypropylene, polyethylene glycol, nano silicon oxide, three oxygen
Change two aluminium, after stirring, be coated onto step b gained phosphor surface and form film, that is, obtain with silica as core,
And have film wrap up fluorescent material.
Described a kind of scratch-resistant, rare earth doping fluorescent powder of polymethyl methacrylate parcel and preparation method thereof, its
It is characterised by, step c painting method adopts spin-coating method.
The invention has the beneficial effects as follows：In fluorescent material building-up process, add silica as core, be on the one hand fluorescence
The crystallization of powder provides nucleus, promotes it to crystallize, and the fluorescent powder grain on the other hand obtaining is big, and the specific surface area that lights is big,
So as to increase its light efficiency, reduces cost；The polymethyl methacrylate coating of doping alchlor is formed with phosphor surface
Film, greatly improves the resistance to bombardment performance of fluorescent material, so as to extend its service life；Meanwhile, film water white transparency, no
While affecting its light efficiency, its resistance to ag(e)ing is improve；The alundum (Al2O3) of doping further increases the intensity of film layer, shows
Work improves its property；Coordinate nano silicon oxide of addition etc., improve the effect of material scratch-resistant.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.
Embodiment
The rare earth doping fluorescent powder of a kind of scratch-resistant, polymethyl methacrylate parcel, it is characterised in that be by following heavy
The raw material of amount part is made：
Nano silicon oxide 4, Eu2O3 5, polypropylene 3, La (NO3)3·6H2O 20, cetyl trimethylammonium bromide 5,
Na2WO4·2H2O 40, calcium silicates 4, silica 9, dust technology 50 distills appropriate amount of water, appropriate amount of ethanol, poly-methyl methacrylate
Ester 25, ethyl acetate 40, polyethylene glycol 8, alundum (Al2O3) 5；
The mass fraction of the dust technology is 10-30%；
Described a kind of scratch-resistant, rare earth doping fluorescent powder of polymethyl methacrylate parcel and preparation method thereof, its feature
It is to be made up of following steps：
A. Eu is added in dilute nitric acid solution2O3So as to it is completely dissolved；By La (NO3)3·6H2After O is soluble in water, add together
Enter in above-mentioned solution, stir 8-25min, add cetyl trimethylammonium bromide, Na2WO4·2H2O, and continue to stir 10-
30 minutes；
B. rapid a resulting solutions PH of pacing add silica, calcium silicates to neutrality, and autoclave is proceeded to after stirring
In, 15-20h is incubated under the conditions of 150-200 DEG C；Cooling afterwards, precipitation is filtered, and with distilled water, alcohol flushing 2-3 time, then
50-80 DEG C of insulation 5-10h in baking oven is proceeded to, obtains wrapping up silica, the NaLa (WO of calcium silicates4)2 :Eu3+Fluorescent material；
C. polymethyl methacrylate is dissolved in ethyl acetate, adds polypropylene, polyethylene glycol, nano silicon oxide, three oxygen
Change two aluminium, after stirring, be coated onto step b gained phosphor surface and form film, that is, obtain with silica as core,
And have film wrap up fluorescent material.
Described a kind of scratch-resistant, rare earth doping fluorescent powder of polymethyl methacrylate parcel and preparation method thereof, its
It is characterised by, step c painting method adopts spin-coating method.
The present invention technical parameter be：When excitation wavelength is 393nm, the most strong emission peak of fluorescent material is located at 590-620nm.
Claims (3)
1. the rare earth doping fluorescent powder that a kind of scratch-resistant, polymethyl methacrylate are wrapped up, it is characterised in that be by following weight
The raw material of part is made：
Nano silicon oxide 2-4, Eu2O3 2-5, polypropylene 1-3, La (NO3)3·6H2O 10-20, cetyl trimethylammonium bromide
2-5, Na2WO4·2H2O 30-40, calcium silicates 2-4, silica 4-9, dust technology 30-50, distillation appropriate amount of water, appropriate amount of ethanol,
Polymethyl methacrylate 15-25, ethyl acetate 30-40, polyethylene glycol 5-8, alundum (Al2O3) 3-5；
The mass fraction of the dust technology is 10-30%.
2. a kind of scratch-resistant according to claim 1, polymethyl methacrylate parcel rare earth doping fluorescent powder and its
Preparation method, it is characterised in that be made up of following steps：
A. Eu is added in dilute nitric acid solution2O3So as to it is completely dissolved；By La (NO3)3·6H2After O is soluble in water, add together
To in above-mentioned solution, 8-25min is stirred, add cetyl trimethylammonium bromide, Na2WO4·2H2O, and continue to stir 10-30
Minute；
B. rapid a resulting solutions PH of pacing add silica, calcium silicates to neutrality, and autoclave is proceeded to after stirring
In, 15-20h is incubated under the conditions of 150-200 DEG C；Cooling afterwards, precipitation is filtered, and with distilled water, alcohol flushing 2-3 time, then
50-80 DEG C of insulation 5-10h in baking oven is proceeded to, obtains wrapping up silica, the NaLa (WO of calcium silicates4)2 :Eu3+Fluorescent material；
C. polymethyl methacrylate is dissolved in ethyl acetate, adds polypropylene, polyethylene glycol, nano silicon oxide, three oxygen
Change two aluminium, after stirring, be coated onto step b gained phosphor surface and form film, that is, obtain with silica as core,
And have film wrap up fluorescent material.
3. a kind of scratch-resistant according to claim 2, polymethyl methacrylate parcel rare earth doping fluorescent powder and its
Preparation method, it is characterised in that step c painting method adopts spin-coating method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611043957.XA CN106634950A (en) | 2016-11-24 | 2016-11-24 | Scratch-resistant polymethyl-methacrylate-coated rare-earth-doped fluorescent powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611043957.XA CN106634950A (en) | 2016-11-24 | 2016-11-24 | Scratch-resistant polymethyl-methacrylate-coated rare-earth-doped fluorescent powder and preparation method thereof |
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| CN106634950A true CN106634950A (en) | 2017-05-10 |
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| CN201611043957.XA Pending CN106634950A (en) | 2016-11-24 | 2016-11-24 | Scratch-resistant polymethyl-methacrylate-coated rare-earth-doped fluorescent powder and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111923A (en) * | 2018-10-09 | 2019-01-01 | 贵州师范大学 | One kind can be by ultraviolet light, black light or blue light activated red fluorescence powder and preparation method thereof |
| CN110564036A (en) * | 2019-08-27 | 2019-12-13 | 湖南登科材料科技有限公司 | rare earth doped modified plastic composite master batch and preparation method thereof |
-
2016
- 2016-11-24 CN CN201611043957.XA patent/CN106634950A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111923A (en) * | 2018-10-09 | 2019-01-01 | 贵州师范大学 | One kind can be by ultraviolet light, black light or blue light activated red fluorescence powder and preparation method thereof |
| CN110564036A (en) * | 2019-08-27 | 2019-12-13 | 湖南登科材料科技有限公司 | rare earth doped modified plastic composite master batch and preparation method thereof |
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Application publication date: 20170510 |