CN112300785B - Preparation method of fluorescent slurry - Google Patents
Preparation method of fluorescent slurry Download PDFInfo
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- CN112300785B CN112300785B CN202011175542.4A CN202011175542A CN112300785B CN 112300785 B CN112300785 B CN 112300785B CN 202011175542 A CN202011175542 A CN 202011175542A CN 112300785 B CN112300785 B CN 112300785B
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- slurry
- fluorescent
- mass ratio
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- bombardment
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- 239000002002 slurry Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 49
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 20
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 10
- 239000000084 colloidal system Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical group CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- 239000011159 matrix material Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
Classifications
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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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention prepares aluminum chloride solution into slurry carrier through gel-sol technology, disperses silver oxide colloid into silicon dioxide matrix in isopropanol solution to prepare anti-bombardment sol, mixes the slurry carrier, the anti-bombardment sol and fluorescent material in proportion to obtain fluorescent slurry, and the slurry has the remarkable characteristics of high thermal stability, strong anti-bombardment capability, good thermal conductivity and the like in the application of laser display devices.
Description
Technical field:
the invention belongs to the technical field of laser display manufacturing, and particularly relates to a preparation method of fluorescent slurry.
The background technology is as follows:
with the progress of society and the development of economy, the living standard of people is higher and higher, and higher requirements are also put forward on household appliances in daily life, and display devices are no exception. From the conventional cathode ray display to the liquid crystal display, the image quality and color of the display device are greatly improved, and at present, demands are mainly focused on healthier and more quality viewing modes, so that laser display is generated. Compared with liquid crystal display, laser display has the remarkable characteristics of wide color gamut, large size, eye protection and the like, is outstanding in next-generation display devices, and has wide future.
Currently, commercial laser display generally adopts a laser fluorescence technology, namely a single-color laser pumping colorful rotary all-inorganic phosphor technology, which is a brand new low-cost colorful display technology. The use of blue lasers in this technology to convert fluorescent materials to light of other wavelengths places higher demands on the fluorescent materials. The fluorescent material used in the laser display must have high thermal stability, strong bombardment resistance and good thermal conductivity, and the existing fluorescent material has poor bombardment resistance and is easy to attenuate, so that the display picture is poor, and therefore, the development of the laser display technology needs a fluorescent material with stronger bombardment resistance.
The invention comprises the following steps:
in order to overcome the defects of the prior art, the invention aims to provide a preparation method of fluorescent slurry, which has the remarkable advantages of high thermal stability, strong bombardment resistance, good thermal conductivity and the like, and can be widely applied to laser display devices.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing fluorescent paste, comprising the following steps:
step one, preparing a slurry carrier:
uniformly mixing aluminum chloride, isopropyl alcohol and water according to the mass ratio of (4-10) to (4-6), slowly adding a proper amount of catalyst at 60-80 ℃, stirring for 8-24h, and preserving the heat for 48-96h at 30-40 ℃ to obtain the aluminum oxide gel A. Uniformly mixing isopropanol and polymerization inhibitor according to the mass ratio of 50-100:1 to obtain dispersion solution B. And (3) adding the A into the B at normal temperature, stirring for 2-6h, and obtaining the slurry carrier at the rotating speed of 8000-12000 rmp.
Step two, preparing bombardment-resistant sol:
uniformly mixing a silane coupling agent, isopropyl alcohol and water according to the mass ratio of 1 (3-6) (0.4-0.8), adding a certain amount of nano silver oxide colloid at normal temperature, stirring for 2-4h, and rotating at the speed of 5000-8000rmp to obtain the anti-bombardment sol.
Preparing fluorescent slurry;
uniformly mixing self-made fluorescent powder and isopropanol according to the mass ratio of 1 (10-20) to obtain powder slurry fluorescent powder, and uniformly mixing the powder slurry fluorescent powder, a slurry carrier and bombardment-resistant sol according to the mass ratio of 20-30 to 50-60 to 10-30 to obtain the fluorescent slurry.
The catalyst is ethylene oxide.
The mass ratio of the catalyst to the aluminum chloride is (0.3-1.3): 1.
The polymerization inhibitor is one or two of nonylphenol polyoxyethylene ether.
The mass ratio of the polymerization inhibitor to the aluminum chloride is (0.01-0.6): 1.
The silane coupling agent is gamma-methacryloxypropyl trimethoxy silane (kh-570).
The granularity of the nano silver oxide colloid is 50-100 nanometers.
The mass ratio of the nano silver oxide to the silane coupling agent is (0.125-0.167) 1.
The molecular formula of the fluorescent powder is Y 3 Al 5 O 12 :Ce、Lu 3 Al 5 O 12 One of Ce
The invention has the main advantages that:
1. the fluorescent slurry prepared by the invention has the remarkable advantages of high thermal stability, strong bombardment resistance, good thermal conductivity and the like;
2. the fluorescent slurry prepared by the invention has simple process and convenient application, and is easy to be applied to actual production.
The specific embodiment is as follows:
the present invention will be described in further detail with reference to examples.
Example 1
A method for preparing fluorescent paste, comprising the following steps:
step one, preparing a slurry carrier:
143.10g of isopropanol, 114.40g of water and 28.60g of aluminum chloride are sequentially added into a conical flask, uniformly stirred, 11.44g of ethylene oxide is slowly added at 60 ℃, stirred for 10 hours, and then the mixture is kept at 35 ℃ for 48 hours to obtain alumina gel A. Into a beaker were added 0.66g of NP-10 and 39.48g of isopropyl alcohol, and stirred well to obtain a dispersion solution B. And (3) adding the A into the B at normal temperature, stirring for 2.5h, and obtaining the slurry carrier at the rotating speed of 8000 rmp.
Step two, preparing bombardment-resistant sol:
adding 35.81g kh-570, 179.05g isopropanol and 17.91g water into a conical flask, uniformly mixing, adding 5.37g of 30-80nm silver oxide colloid at normal temperature, stirring for 2 hours, and rotating at 5000rmp to obtain the anti-bombardment sol.
Preparing fluorescent slurry;
sequentially adding into beaker139.65g of isopropanol and 13.72g of homemade Y 3 Al 5 O 12 The Ce fluorescent powder is uniformly mixed to obtain the powder slurry fluorescent powder. 148.70g of powder slurry fluorescent powder, 335.81g of slurry carrier and 205.91g of anti-bombardment sol are added into a beaker and uniformly mixed to obtain the fluorescent slurry.
Example two
A method for preparing fluorescent paste, comprising the following steps:
step one, preparing a slurry carrier:
46.48g of isopropanol, 43.24g of water and 10.81g of aluminum chloride are sequentially added into a conical flask, uniformly stirred, 8.65g of ethylene oxide is slowly added at 60 ℃, stirred for 12 hours, and then the mixture is kept at 35 ℃ for 52 hours to obtain alumina gel A. Into a beaker were added 0.41g of NP-8 and 34.92g of isopropyl alcohol, and stirred well to obtain a dispersion solution B. And (3) adding the A into the B at normal temperature, stirring for 2 hours, and obtaining the slurry carrier at the rotating speed of 10000 rmp.
Step two, preparing bombardment-resistant sol:
adding 7.46g kh-570, 26.11g isopropanol and 3.73g water into a conical flask, uniformly mixing, adding 0.97g of 70-120nm silver oxide colloid at normal temperature, stirring for 2.5h, and rotating at 6000rmp to obtain the anti-bombardment sol.
Preparing fluorescent slurry;
62.25g of isopropanol and 4.15g of homemade Y were added sequentially to a beaker 3 Al 5 O 12 The Ce fluorescent powder is uniformly mixed to obtain the powder slurry fluorescent powder. 57.89g of powder slurry fluorescent powder, 138.92g of slurry carrier and 34.73g of anti-bombardment sol are added into a beaker and uniformly mixed to obtain the fluorescent slurry.
Example III
A method for preparing fluorescent paste, comprising the following steps:
step one, preparing a slurry carrier:
2545.10g of isopropanol, 1871.40g of water and 374.28g of aluminum chloride are sequentially added into a reaction kettle, uniformly stirred, 299.45g of ethylene oxide is slowly added at 65 ℃, stirred for 24 hours, and then the mixture is kept at 35 ℃ for 96 hours to obtain alumina gel A. 157.20g NP-12 and 10217.84g isopropyl alcohol were added to the reaction vessel and stirred uniformly to obtain a dispersion solution B. And (3) adding the A into the B at normal temperature, stirring for 6 hours, and obtaining the slurry carrier at the rotating speed of 11000 rmp.
Step two, preparing bombardment-resistant sol:
687.26kh-570 g, 3436.30g of isopropanol and 549.81g of water are added into a reaction kettle and mixed uniformly, 106.52g of 70-120nm silver oxide colloid is added at normal temperature, and the mixture is stirred for 4 hours at a rotating speed of 8000rmp, so that the anti-bombardment sol is obtained.
Preparing fluorescent slurry;
5635.64g of isopropanol and 352.19g of homemade Lu were added sequentially to a reaction vessel 3 Al 5 O 12 The Ce fluorescent powder is uniformly mixed to obtain the powder slurry fluorescent powder. 5617.90g of powder slurrying fluorescent powder, 15321.56g of slurry carrier and 4596.47g of anti-bombardment sol are added into a reaction kettle and uniformly mixed to obtain the fluorescent slurry.
Claims (5)
1. A method for preparing fluorescent paste, comprising the steps of:
step one, preparing a slurry carrier:
uniformly mixing aluminum chloride, isopropyl alcohol and water according to the mass ratio of 1:4-10:4-6, slowly adding a proper amount of catalyst at 60-80 ℃, stirring for 8-24 hours, and preserving heat at 30-40 ℃ for 48-96 hours to obtain alumina gel A; uniformly mixing isopropanol and a polymerization inhibitor according to a mass ratio of 50-100:1 to obtain a dispersion solution B; adding the A into the B at normal temperature, stirring for 2-6h at 8000-12000rmp to obtain a slurry carrier;
step two, preparing bombardment-resistant sol:
uniformly mixing a silane coupling agent, isopropyl alcohol and water according to the mass ratio of 1:3-6:0.4-0.8, adding a certain amount of nano silver oxide colloid at normal temperature, stirring for 2-4h, and rotating at the speed of 5000-8000rmp to obtain bombardment-resistant sol;
preparing fluorescent slurry;
uniformly mixing self-made fluorescent powder and isopropanol according to the mass ratio of 1:10-20 to obtain powder slurry fluorescent powder, and uniformly mixing the powder slurry fluorescent powder, a slurry carrier and anti-bombardment sol according to the mass ratio of 20-30:50-60:10-30 to obtain the fluorescent slurry;
the catalyst is ethylene oxide;
the mass ratio of the catalyst to the aluminum chloride is 0.3-1.3:1;
the mass ratio of the nano silver oxide to the silane coupling agent is 0.125-0.167:1;
the molecular formula of the self-made fluorescent powder is Y 3 Al 5 O 12 :Ce、Lu 3 Al 5 O 12 One of Ce.
2. The method of producing a phosphor paste according to claim 1, wherein the polymerization inhibitor is one of NP-8, NP-10, and NP-12.
3. The method for producing a phosphor paste according to claim 1, wherein a mass ratio of the polymerization inhibitor to the aluminum chloride is 0.01 to 0.6:1.
4. The method of preparing a phosphor paste according to claim 1, wherein the silane coupling agent is gamma-methacryloxypropyl trimethoxysilane kh-570.
5. The method for preparing a fluorescent paste according to claim 1, wherein the particle size of the nano silver oxide colloid is 30-80nm or 70-120nm.
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| CN202011175542.4A CN112300785B (en) | 2020-10-28 | 2020-10-28 | Preparation method of fluorescent slurry |
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| CN202011175542.4A CN112300785B (en) | 2020-10-28 | 2020-10-28 | Preparation method of fluorescent slurry |
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2020
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