CN115216296A - Synthesis method of efficient blue fluorescent powder for excitation of purple light LED - Google Patents
Synthesis method of efficient blue fluorescent powder for excitation of purple light LED Download PDFInfo
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- CN115216296A CN115216296A CN202210948854.7A CN202210948854A CN115216296A CN 115216296 A CN115216296 A CN 115216296A CN 202210948854 A CN202210948854 A CN 202210948854A CN 115216296 A CN115216296 A CN 115216296A
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- 239000000843 powder Substances 0.000 title claims abstract description 31
- 230000005284 excitation Effects 0.000 title claims abstract description 21
- 238000001308 synthesis method Methods 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000011282 treatment Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 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
- 239000011265 semifinished product Substances 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 4
- 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
- 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
- 239000000463 material Substances 0.000 claims description 9
- 238000000498 ball milling Methods 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
- 238000001035 drying Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 238000010189 synthetic method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 239000000203 mixture Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract 1
- 239000012798 spherical particle Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000009877 rendering Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010304 firing Methods 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
- 238000012858 packaging process 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
- 238000000967 suction filtration Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
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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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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to a synthesis method of efficient blue fluorescent powder for excitation of a purple light LED, belonging to the technical field of inorganic chemical industry 5‑y (PO 4 )3Cl x ：yEu 2+ Wherein 1 < x < 3,0 < y < 0.5; the raw materials required for 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 treatment; (4) secondary sintering; (5) processing a semi-finished product; and (6) sieving the finished product. The blue fluorescent powder prepared by the invention has a spherical particle size morphology, high concentration, can emit blue fluorescent light when being applied to the excitation of a purple light (400 nm) LED, has the advantages of high luminous conversion efficiency and the like, and is easier for batch production in the industrial production process.
Description
Technical Field
The invention relates to a synthetic method of high-efficiency blue fluorescent powder for excitation of a purple light LED, belonging to the technical field of inorganic chemical industry.
Background
The main reason is that the existing product has small granularity and low concentration, the light conversion intensity is difficult to match with the used large-grain yellow-green powder and nitride red powder with the granularity of about 20 mu m, especially in the fields of LED illumination, backlight and color rendering devices, the requirement on the color rendering index is more than 95, the packaged parameters not only ensure that the color rendering index meets the requirement, but also have the requirement on the improvement of the luminous efficiency, therefore, in the excitation process of a purple LED chip, the luminous efficiency of the blue component and the yield in the packaging process are improved, and the aim of obtaining the blue fluorescent powder with high brightness and high performance is to achieve the invention.
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: the synthesis method of the high-efficiency blue fluorescent powder for excitation of the purple light LED is characterized in that the chemical composition of the blue fluorescent powder is Sr 5-y (PO 4 ) 3 Cl x ：yEu 2+ And 1 < x < 3, and 0 < y < 0.5; the raw materials required for 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 treatment; (4) secondary sintering; (5) processing a semi-finished product; and (6) sieving the finished product.
On the basis of the technical scheme, the invention can also make the following improvements:
further, 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 5-10, and the material ball ratio is 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 moisture introduced in the air can be effectively removed, so that the raw materials are more intact in the crystal production process, and the product is more uniform in particle size and easy to disperse.
Further, the pre-sintering temperature is 600-650 ℃, and the pre-sintering time is 4 hours.
Further, in the step (3), a screen mesh is adopted for dry screening to perform loosening treatment, and the mesh number of the screen mesh is 200 meshes.
Further, the specific steps of the step (4) are as follows: the materials after loosening treatment are put into an alumina crucible, sintered for 3 to 5 hours at 1050 to 1200 ℃ under the protection of reducing atmosphere, and naturally cooled 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, then washing for multiple times by using deionized water, and performing suction filtration and drying by using ethanol.
Further, the powder obtained by drying and cooling the powder at room temperature in the step (6) is sieved to obtain the powder.
The invention has the advantages that: the blue fluorescent powder prepared by the invention has a particle size shape close to a spherical shape and high concentration, can emit blue fluorescent light when being applied to the excitation of a purple light (400 nm) LED, and has the advantages of high luminous conversion efficiency and the like, so the blue fluorescent powder can also be applied to the field of white light LED illumination. The body components of strontium chloride, europium chloride and ammonium chloride are added excessively, the excessive components are used as reaction assistants in the synthesis process to play a role in fluxing, and other various low-melting-point assistants are not required to be introduced, so that the material is easier to treat in the industrial production process, is convenient for mass production and is easier to realize industrial production.
Drawings
FIG. 1 is an SEM photograph of a product of example 4 of the present invention;
FIG. 2 is a graph of the emission spectrum of the product of example 4 under the excitation of a 400nm ultraviolet chip.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
A synthetic method of high-efficiency blue fluorescent powder for excitation of a purple light LED comprises the following steps:
(1) Material mixing: the raw materials are accurately weighed according to the component molar ratio, and the traditional ball milling mode is adopted in the mixing mode, so that the industrial production is easier. Wherein, the ball milling medium adopts phi 5-10 high-purity zirconia balls. And (3) the material ball ratio is 1.
Table 1: the ingredients of examples 1-5 were weighed in units/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: in the above examples 1 to 5, the pre-firing oxidation temperature is preferably 650 ℃ and the sintering time is preferably 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 of the raw materials is more complete in the secondary sintering process, and the final product has the advantage of higher product brightness.
(3) Loosening treatment: examples 1-5 all loosening treatments were dry sieved 200 mesh. After loosening treatment, the reduction can be more sufficient in the secondary sintering process.
(4) And (3) secondary sintering: selecting CO and H in reducing atmosphere 2 And N 2 In the present embodiment, H is used as the reducing atmosphere 2 And N 2 Mixed gas of which H 2 The content is controlled at 20 percent.
(5) Semi-finished product treatment: and (3) crushing, sieving and dispersing the materials after secondary sintering, washing the materials for a plurality of times by using deionized water, and then filtering, filtering and drying the materials by using ethanol.
(6) Sieving a finished product: the powder after drying and cooling at room temperature is sieved by a 200-mesh sieve to obtain 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 ratio components: according to the addition ratios of the embodiments 1 to 5, strontium chloride, europium chloride and ammonium chloride in the components are added according to a non-stoichiometric ratio, and the strontium chloride, the europium chloride and the ammonium chloride are used as raw materials of chlorides, so that the requirements of component structural elements can be met, the effect of a fluxing agent in a 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 invention has high brightness and large particle size, the average particle size is more than 20 μm, the brightness of example 4 reaches 142 lumens, the center particle size reaches 22.6 μm, the result of SEM image in FIG. 1 shows that the particle size is relatively uniform, no ultrafine particles below 5 μm are present, no adhesion is present, the dispersibility is good, and the peak value appears at 450nm in the emission spectrogram under the excitation of the ultraviolet chip in FIG. 2, which shows that the synthesized product can emit blue light under the excitation of a purple light (400 nm) LED.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A synthetic method of high-efficiency blue fluorescent powder for purple light LED excitation is characterized in that,
the chemical composition of the blue fluorescent powder is Sr 5-y (PO 4 ) 3 Cl x ：yEu 2+ ，1﹤x≤3，0﹤y≤0.5；
The raw materials required for 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) Burdening and mixing;
(2) Primary presintering;
(3) Loosening treatment;
(4) Secondary sintering;
(5) Processing a semi-finished product;
(6) And (4) sieving a finished product.
2. The method for synthesizing the efficient blue fluorescent powder for excitation of the violet LED according to claim 1, wherein in the step (1), the raw materials are weighed according to components and are uniformly mixed in a ball milling mode.
3. The method for synthesizing high-efficiency blue fluorescent powder for violet LED excitation according to claim 2, wherein the ball milling medium in the step (1) adopts high-purity zirconia balls with the diameter of 5-10, and the ball-milling ratio is 1-2.
4. The method for synthesizing high-efficiency blue fluorescent powder for violet LED excitation according to claim 1, wherein the pre-sintering temperature in the step (2) is 600-700 ℃ and the pre-sintering time is 3-5 hours.
5. The method for synthesizing high-efficiency blue fluorescent powder for excitation of a purple light LED according to claim 4, wherein the pre-sintering temperature is 600-650 ℃, and the pre-sintering time is 4 hours.
6. The method for synthesizing high efficiency blue phosphor for violet LED excitation according to claim 1, wherein step (3) is performed with a dry sieving with a 200 mesh screen.
7. The method for synthesizing high-efficiency blue fluorescent powder for violet LED excitation according to claim 1, wherein the specific steps of the step (4) are as follows: the materials after loosening treatment are put into an alumina crucible, sintered for 3 to 5 hours at 1050 to 1200 ℃ under the protection of reducing atmosphere, and naturally cooled to room temperature.
8. The method of claim 7, wherein the method comprises the step of combining a high efficiency blue phosphor for violet LED excitationIn the reducing atmosphere, CO and H 2 And N 2 One or more than one mixed gas.
9. The method for synthesizing high-efficiency blue fluorescent powder for purple light LED excitation according to claim 1, wherein the semi-finished product treatment of the step (5) comprises crushing treatment, sieving treatment, disintegration treatment, then washing with deionized water for multiple times, and suction-filtering and drying with ethanol.
10. The method for synthesizing the efficient blue fluorescent powder for the excitation of the purple light LED according to claim 1, wherein the efficient blue fluorescent powder obtained in the step (6) by drying, cooling and sieving the powder at room temperature is obtained.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080067918A1 (en) * | 2006-09-19 | 2008-03-20 | Koito Manufacturing Co., Ltd. | Light emitting module |
| 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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- 2022-08-09 CN CN202210948854.7A patent/CN115216296B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080067918A1 (en) * | 2006-09-19 | 2008-03-20 | Koito Manufacturing Co., Ltd. | Light emitting module |
| 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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