CN115216296B - Synthetic method of efficient blue fluorescent powder for excitation of ultraviolet LED - Google Patents
Synthetic method of efficient blue fluorescent powder for excitation of ultraviolet LED Download PDFInfo
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- CN115216296B CN115216296B CN202210948854.7A CN202210948854A CN115216296B CN 115216296 B CN115216296 B CN 115216296B CN 202210948854 A CN202210948854 A CN 202210948854A CN 115216296 B CN115216296 B CN 115216296B
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- 239000000843 powder Substances 0.000 title claims abstract description 26
- 230000005284 excitation Effects 0.000 title claims abstract description 18
- 238000010189 synthetic method Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 239000011265 semifinished product Substances 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 6
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229910001631 strontium chloride Inorganic materials 0.000 claims abstract description 6
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims abstract description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims abstract description 3
- 229910001940 europium oxide Inorganic materials 0.000 claims abstract description 3
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims abstract description 3
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 3
- HKSVWJWYDJQNEV-UHFFFAOYSA-L strontium;hydron;phosphate Chemical compound [Sr+2].OP([O-])([O-])=O HKSVWJWYDJQNEV-UHFFFAOYSA-L 0.000 claims abstract description 3
- 230000002194 synthesizing effect Effects 0.000 claims abstract 6
- 239000000463 material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001308 synthesis method Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 3
- 238000011068 loading method Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 239000012798 spherical particle Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 3
- 238000009877 rendering Methods 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7737—Phosphates
- C09K11/7738—Phosphates with alkaline earth metals
- C09K11/7739—Phosphates with alkaline earth metals with halogens
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to a high-efficiency blue color for excitation of a purple light LEDA method for synthesizing fluorescent powder belongs to the technical field of inorganic chemical industry, and the chemical composition of the blue fluorescent powder is Sr 5‑y (PO 4 )3Cl x ：yEu 2+ X is less than or equal to 3 and y is less than or equal to 0 and less than or equal to 0.5; the raw materials required by synthesis comprise 2 to 10 percent of diammonium hydrogen phosphate, 50 to 60 percent of strontium hydrogen phosphate, 10 to 25 percent of strontium carbonate, 10 to 25 percent of strontium chloride, 1.5 to 5 percent of europium oxide, 0.2 to 2.5 percent of europium chloride and 1 to 5 percent of ammonium chloride; the method specifically comprises the following steps: (1) batching and mixing; (2) primary presintering; (3) loosening; (4) secondary sintering; (5) semi-finished product treatment; and (6) sieving the finished product. The blue fluorescent powder prepared by the method has the advantages of nearly spherical particle morphology, high concentration, capability of emitting blue fluorescence when being applied to excitation of ultraviolet (400 nm) LEDs, high luminescence conversion efficiency and the like, and is easier for mass production in the industrial production process.
Description
Technical Field
The invention relates to a synthesis method of high-efficiency blue fluorescent powder for excitation of a purple light LED, and belongs to the technical field of inorganic chemical industry.
Background
The invention aims to provide fluorescent powder for a purple light LED, which has the problems of low luminous efficiency, poor conversion efficiency and the like of blue light components, mainly because the existing products have smaller granularity and lower concentration, the light conversion intensity of the fluorescent powder is difficult to match with large-particle yellow-green powder and nitride red powder with the granularity of about 20 mu m, the color rendering index is required to be more than 95 in the fields of LED illumination, backlight and color rendering devices, and the parameters after encapsulation are required to ensure that the color rendering index meets the requirements and the luminous efficiency is improved, so that the luminous efficiency of the blue light components is improved and the yield is improved in the encapsulation process in the excitation process of the purple light LED chip, and the blue fluorescent powder with high brightness and high performance is obtained.
Disclosure of Invention
Aiming at the defects of small granularity and low brightness of the existing blue fluorescent powder, the invention provides a synthesis method of high-efficiency blue fluorescent powder for exciting a purple light LED, and the blue fluorescent powder with large granularity, high brightness and high performance is prepared.
The technical scheme for solving the technical problems is as follows: a synthesis method of high-efficiency blue fluorescent powder for excitation of ultraviolet LEDs is characterized in that the chemical composition of the blue fluorescent powder is Sr 5-y (PO 4 ) 3 Cl x ：yEu 2+ X is less than or equal to 3 and y is less than or equal to 0 and less than or equal to 0.5; the raw materials required by synthesis comprise 2 to 10 percent of diammonium hydrogen phosphate, 50 to 60 percent of strontium hydrogen phosphate, 10 to 25 percent of strontium carbonate, 10 to 25 percent of strontium chloride, 1.5 to 5 percent of europium oxide, 0.2 to 2.5 percent of europium chloride and 1 to 5 percent of ammonium chloride;
the method specifically comprises the following steps: (1) batching and mixing; (2) primary presintering; (3) loosening; (4) secondary sintering; (5) semi-finished product treatment; and (6) sieving the finished product.
Based on the technical scheme, the invention can also make the following improvements:
in the step (1), the raw materials are weighed according to the components and are uniformly mixed in a ball milling mode.
Furthermore, the ball milling medium in the step (1) adopts high-purity zirconia balls with phi of 5-10, and the ball ratio is 1:1-2.
Further, the pre-sintering temperature in the step (2) is 600-700 ℃, and the pre-sintering time is 3-5 hours. After pre-sintering, partial volatile impurities in the raw materials and water introduced in the air can be effectively removed, so that the raw materials are more perfect in the crystal production process, and the product granularity is more uniform and is easy to disperse.
Further, the pre-sintering temperature is 600-650 ℃, and the pre-sintering time is 4 hours.
Further, the step (3) adopts a screen mesh dry type sieving to carry out loosening treatment, and the mesh number of the screen mesh is 200 mesh.
Further, the specific steps of the step (4) are as follows: and (3) filling the loose materials into an alumina crucible, sintering for 3-5 hours at 1050-1200 ℃ under the protection of a reducing atmosphere, and naturally cooling to room temperature.
Further, the reducing atmosphere is CO and H 2 And N 2 One or more than one mixed gas.
Further, the semi-finished product treatment in the step (5) comprises crushing treatment, sieving treatment and disintegration treatment, and then the semi-finished product treatment is washed for multiple times by deionized water, filtered by ethanol and dried.
And (3) further, the powder obtained in the step (6) is obtained after the powder is dried and cooled to room temperature and then is sieved.
The invention has the advantages that: the blue fluorescent powder produced by the invention has the advantages of nearly spherical morphology, high concentration, blue fluorescence emission when being applied to excitation of ultraviolet (400 nm) LEDs, high luminescence conversion efficiency and the like, and can be applied to the field of white light LED illumination. The main components of strontium chloride, europium chloride and ammonium chloride are excessively added, and the excessive components play a role of fluxing as reaction auxiliary agents in the synthesis process, so that other various low-melting-point auxiliary agents are not required to be introduced, the main components are easier to treat in the industrial production process, the mass production is convenient, and the industrial production is easier.
Drawings
FIG. 1 is an SEM image of the product of example 4 of the invention;
FIG. 2 is a graph showing the emission spectrum of the product of example 4 of the present invention under excitation of a 400nm ultraviolet chip.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
A synthesis method of high-efficiency blue fluorescent powder for excitation of a purple light LED comprises the following steps:
(1) And (3) material mixing: each raw material is accurately weighed according to the molar ratio of the components, and the traditional ball milling mode is adopted as the mixing mode, so that the industrial production is easier. Wherein, the ball milling medium adopts high-purity zirconia balls with phi of 5-10. The ball ratio is 1:1-2.
Table 1: the ingredients of examples 1-5 were weighed in units of g.
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| SrHPO 4 | 50.509 | 49.761 | 45.500 | 49.72 | 57.685 |
| (NH 4 ) 2 HPO 4 | 2.595 | 2.386 | 6.545 | 5.96 | 4.841 |
| SrCO 3 | 21.757 | 20.006 | 21.951 | 13.33 | 23.192 |
| SrCl 2 | 21.682 | 23.924 | 21.875 | 23.90 | 9.245 |
| Eu 2 O 3 | 3.458 | 1.590 | 3.489 | 4.76 | 3.686 |
| EuCl 2 | 0.255 | 2.334 | 0.640 | 2.33 | 1.353 |
| NH 4 Cl | 2.000 | 1.000 | 2.000 | 3.000 | 5.000 |
(2) Primary presintering: the preferred pre-sintering oxidation temperatures for examples 1-5 above are at 650 c for 4 hours. In the presintering process, partial volatile impurities in the raw materials and trace moisture absorbed in the air can be removed within the temperature range of 600-650 ℃, so that the crystal growth is more complete in the secondary sintering process, and the final product has the advantage of higher brightness.
(3) Loosening: examples 1-5 all used dry screening with a 200 mesh screen. The reduction in the secondary sintering process can be more sufficient through the loosening treatment.
(4) Secondary sintering: the reducing atmosphere selects CO and H 2 And N 2 Any one or more than one mixed gas is adopted as the reducing atmosphere in the embodiment, H is adopted 2 And N 2 Mixed gas, wherein H 2 The content is controlled at 20%.
(5) Semi-finished product treatment: crushing, sieving and disintegrating the material after secondary sintering, cleaning the material with deionized water for several times, and then filtering and drying the material with ethanol.
(6) And (5) sieving a finished product: the powder after being dried and cooled to room temperature is sieved by a 200-mesh sieve, thus obtaining the product of the invention.
Table 2: reaction conditions and product Performance data sheets for examples 1-5
The components of the invention adopt non-stoichiometric components: according to the adding proportion of the embodiments 1-5, strontium chloride, europium chloride and ammonium chloride in the components are added according to non-stoichiometric proportion, and the strontium chloride, the europium chloride and the ammonium chloride are taken as raw materials of the chloride, so that the requirements of component structural elements can be met, the fluxing agent effect in the synthesis process is realized, the reaction temperature in the synthesis process is reduced, and the synthesis of crystals is facilitated.
As can be seen from the data in Table 2 and FIGS. 1-2, the synthesized product of the present invention has high brightness, large particle size, average particle size of more than 20 μm, brightness of example 4 up to 142 lumen, center particle size up to 22.6 μm, relatively uniform particle size, no ultrafine particles below 5 μm, no adhesion, good dispersibility, and peak at 450nm as seen from the emission spectrum of the ultraviolet chip excitation in FIG. 2, indicating that the present invention can emit blue light under excitation of ultraviolet (. About.400 nm) LED.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (6)
1. A synthesis method of blue fluorescent powder for excitation of a purple light LED is characterized in that,
the chemical composition of the blue fluorescent powder is Sr 5-y (PO 4 ) 3 Cl：yEu 2+ ，0﹤y≤0.5；
The raw materials required by synthesis comprise 2 to 10 percent of diammonium hydrogen phosphate, 50 to 60 percent of strontium hydrogen phosphate, 10 to 25 percent of strontium carbonate, 10 to 25 percent of strontium chloride, 1.5 to 5 percent of europium oxide, 0.2 to 2.5 percent of europium chloride and 1 to 5 percent of ammonium chloride;
the method specifically comprises the following steps:
(1) Mixing materials;
(2) Pre-sintering for 4 hours at the temperature of 600-650 ℃;
(3) Loosening, wherein in the step (3), a screen mesh is adopted for dry sieving to carry out loosening, and the mesh number of the screen mesh is 200 mesh;
(4) The secondary sintering comprises the following specific steps: loading the loose materials into an alumina crucible, sintering for 3-5 hours at 1050-1200 ℃ under the protection of reducing atmosphere, and naturally cooling to room temperature;
(5) Semi-finished product treatment;
(6) And (5) sieving the finished product.
2. The method for synthesizing blue fluorescent powder for excitation of ultraviolet LED according to claim 1, wherein in the step (1), the raw materials are weighed according to the components and are uniformly mixed by adopting a ball milling mode.
3. The method for synthesizing blue fluorescent powder for excitation of ultraviolet LEDs according to claim 2, wherein the ball milling medium in the step (1) adopts high-purity zirconia balls with phi of 5-10, and the ball ratio is 1:1-2.
4. The method for synthesizing blue phosphor for excitation of ultraviolet LED according to claim 1, wherein the reducing atmosphere is CO, H 2 And N 2 One or more than one mixed gas.
5. The method for synthesizing blue phosphor for excitation of violet LED according to claim 1, wherein the semi-finished product treatment of step (5) comprises crushing treatment, sieving treatment, disintegration treatment, washing with deionized water for multiple times, and suction-filtering with ethanol and drying.
6. The method of synthesizing blue phosphor for violet LED excitation according to claim 1, wherein the operation of step (6) is: sieving the powder after being dried and cooled to room temperature.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102414296A (en) * | 2009-05-01 | 2012-04-11 | 奥斯兰姆施尔凡尼亚公司 | Phosphor blend and fluorescent lamp containing same |
| JP2012104531A (en) * | 2010-11-08 | 2012-05-31 | Koito Mfg Co Ltd | Light emitting module |
| JP2012114333A (en) * | 2010-11-26 | 2012-06-14 | Koito Mfg Co Ltd | Light-emitting module |
| CN103073073A (en) * | 2013-01-30 | 2013-05-01 | 吉林大学 | Synthetic method of transition metal sulfide |
| CN104312583A (en) * | 2014-09-28 | 2015-01-28 | 彩虹集团电子股份有限公司 | Preparation method of near ultraviolet excited red fluorescent powder for LEDs (light emitting diodes) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5323308B2 (en) * | 2006-09-19 | 2013-10-23 | 株式会社小糸製作所 | Light emitting module |
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- 2022-08-09 CN CN202210948854.7A patent/CN115216296B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102414296A (en) * | 2009-05-01 | 2012-04-11 | 奥斯兰姆施尔凡尼亚公司 | Phosphor blend and fluorescent lamp containing same |
| JP2012104531A (en) * | 2010-11-08 | 2012-05-31 | Koito Mfg Co Ltd | Light emitting module |
| JP2012114333A (en) * | 2010-11-26 | 2012-06-14 | Koito Mfg Co Ltd | Light-emitting module |
| CN103073073A (en) * | 2013-01-30 | 2013-05-01 | 吉林大学 | Synthetic method of transition metal sulfide |
| CN104312583A (en) * | 2014-09-28 | 2015-01-28 | 彩虹集团电子股份有限公司 | Preparation method of near ultraviolet excited red fluorescent powder for LEDs (light emitting diodes) |
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