CN111849472A - Method for improving luminous performance and thermal stability of low-quality nitride or oxynitride fluorescent material - Google Patents
Method for improving luminous performance and thermal stability of low-quality nitride or oxynitride fluorescent material Download PDFInfo
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Abstract
The invention relates to a method for improving the luminous performance and the thermal stability of a low-quality nitride or oxynitride fluorescent material with low luminous efficiency and poor thermal stability. The method comprises the following steps: fully mixing a low-quality nitride or nitrogen oxide fluorescent material and a specific additive according to a certain proportion, uniformly grinding, sieving, then placing in a sintering furnace, controlling a certain temperature and pressure for sintering, cooling to room temperature along with the furnace, grinding, washing and drying a sintered product to obtain the nitride or nitrogen oxide fluorescent material with improved luminous performance and thermal stabilityHigh quality nitride or oxynitride phosphors. The specific additive is carbon powder (C) and carbon compound (SiC, C)3N4、B4C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc)2O3、Lu2O3、ZrO2、ScN、LuN、Zr3N4) One or more of the powders, the low-quality nitride or oxynitride fluorescent material has a chemical formula of A1‑xSi2O2N2:xEu2+、B2‑xSi5N8:xEu2+、B1‑xAlSiN3:xEu2+. The method disclosed by the invention is green and environment-friendly, low in cost and mild in condition, can greatly improve the luminous performance of the nitride or oxynitride fluorescent material, greatly improves the thermal stability of the nitride or oxynitride fluorescent material, and increases the application value of the nitride or oxynitride fluorescent material in the field of illumination.
Description
Technical Field
The invention relates to a method for improving the luminous performance and the thermal stability of a low-quality nitride or oxynitride fluorescent material, in particular to a method for improving the luminous performance and the thermal stability of a low-quality nitride or oxynitride with low internal quantum efficiency and poor thermal stability.
Background
Since the advent of white Light Emitting Diodes (LEDs), white Light Emitting Diodes (LEDs) have been widely used in high-end applications such as illumination and backlight due to their characteristics of high efficiency, energy saving, and long lifetimeThe application field is known as a fourth generation lighting source after incandescent lamps, fluorescent lamps and energy-saving lamps. Currently, Ce is commercially available as "blue LED + YAG3+"the white light generated by the combination has color reducibility and color rendering index, etc., and further development of the white light is limited due to the lack of cyan and red fluorescent components. With the urgent need of people for high-quality illumination and other effects, a fluorescent material with excellent luminous performance is urgently required to be searched for to make up the deficiency of cyan and red spectrums in the white light LED and improve the comprehensive performance of the white light LED.
In recent years, Eu2+Doped nitrides or oxynitrides are used as a good fluorescent material for white light LEDs, and part of the system is commercially applied to the white light LEDs. Among them, the document [ G. Li, chem. mater., 26 (2014) 2991-3001.]And [ V.Bachmann, chem. Mater. 21 (2008) 316-.]All reported (Ba, Ca, Sr) Si2O2N2:Eu2+The main emission peak of the nitrogen oxide fluorescent material is positioned in the area of 490-510nm, can be effectively excited by near ultraviolet and blue light, and can be used as a cyan fluorescent material for full-spectrum illumination; however, the common existence of such fluorescent materials is that the internal quantum efficiency and thermal stability are low, so that the light conversion efficiency of the white light LED is poor, and the lifetime is greatly reduced, thereby causing the commercial application thereof to be limited. Document [ Y.Li, J. Solid State chem., 2008, 181(3): 515-.]、[T. Suehiro, Ind. Eng.Chem. Res., 2013, 52(22): 7453-7456.]、[H. Watanabe, J. Am. Ceram. Soc., 2009,92(3): 641-648.]And [ G, Li, center, int, 2016, 42(1): 1756-.]Separately reported is a blue light excited (Ca, Sr)2Si5N8: Eu2+And (Ca, Sr) AlSiN3: Eu2+The main emission peak of the nitride red fluorescent material is adjustable at 600-660nm, and the nitride red fluorescent material can be used as effective supplement of red light components in a white light LED, so that the color rendering index is improved; however, the phosphor needs to be prepared under the severe conditions of ultra-high temperature and ultra-high pressure, and is affected by factors such as strict temperature, pressure, atmosphere and raw materials in the preparation process, and the phosphor has low yield in the production process, and a large amount of low-quality nitride fluorescent materials with low luminescence performance and poor thermal stability exist. Therefore, the method aims at the low-quality nitrogen oxides or nitride fluorescence of the above types The optical material develops a method for improving the luminous performance and the thermal stability, can greatly improve the product utilization rate, greatly reduces the production cost, and has important guiding significance for the production of related system products.
At present, the methods of matrix regulation (cation doping/anion displacement and the like) and preparation process improvement (step synthesis, coprecipitation and the like) are used for improving the comprehensive performance of the fluorescent material, and the like, and the reports are more, but the problem that the luminous performance of the existing fluorescent material is difficult to improve is not solved. Carbon powder (C) and carbon compounds (SiC, C)3N4、B4C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc)2O3、Lu2O3、ZrO2、ScN、LuN、Zr3N4) The fluorescent material has stronger structural rigidity, and at present, methods for improving the luminescence property and the thermal stability property by adding the specific additive into the fluorescent material to increase the rigidity of the fluorescent material are not reported similarly.
Disclosure of Invention
The invention aims to provide a method for improving the luminous performance and the thermal stability of a low-quality nitride or oxynitride fluorescent material. Specific additives (carbon powder (C) and carbon compounds (SiC and C) with strong rigid structure are adopted 3N4、B4C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc)2O3、Lu2O3、ZrO2、ScN、LuN、Zr3N4) Etc.) into low-quality nitride or oxynitride fluorescent materials to achieve improved luminescence performance and improved thermal stability; after the low-quality nitride or oxynitride fluorescent material is processed, the nitride or oxynitride fluorescent material with internal quantum efficiency of more than 65% and luminous intensity of 473K kept at room temperature of more than 60% can be obtained.
In order to achieve the purpose, the technical scheme of the invention is as follows:
fully mixing the low-quality nitride or oxynitride fluorescent material with a specific additive according to a certain proportion, uniformly grinding, sieving, then placing in a sintering furnace, sintering under a certain temperature and pressure, cooling to room temperature along with the furnace, and grinding, washing and drying the sintered product to obtain the high-quality nitride or oxynitride fluorescent material with improved luminous performance and thermal stability.
As an improvement of the technical scheme, the performance of the low-quality nitride or oxynitride fluorescent material involved in the scheme is as follows: the internal quantum efficiency is lower than 50%, and the 473K luminous intensity is kept below 50% at room temperature.
As an improvement of the technical proposal, the specific additives used in the proposal are carbon powder (C) and carbon compounds (SiC, C) 3N4、B4C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc)2O3、Lu2O3、ZrO2、ScN、LuN、Zr3N4) And the like.
As an improvement of the technical proposal, the chemical formula of the low-quality nitride or oxynitride fluorescent material in the proposal is A1-xSi2O2N2:xEu2+、B2-xSi5N8:xEu2+、B1-xAlSiN3:xEu2+A represents one or a combination of more than two of Ca, Sr, Mg and Ba; b represents one or the combination of two of Ca and Sr; x is the molar concentration of divalent Eu doping substitution A or B, and x is more than 0 and less than or equal to 0.2.
As an improvement of the technical scheme, the adding proportion of the specific additive used in the scheme is that the specific additive accounts for the mass percent of the fluorescent material, and the weight is more than 0 and less than or equal to 3.5 percent.
As an improvement of the above technical solution, the sintering temperature in the solution is: t is more than or equal to 1300 ℃ and less than or equal to 1500 ℃, and P is more than or equal to 0.1 and less than or equal to 0.5 MPa.
As an improvement of the technical scheme, after a specific additive is introduced into the low-quality nitride and oxynitride fluorescent material, the performance of the obtained nitride or oxynitride fluorescent material is greatly improved, wherein the internal quantum efficiency is greater than 65%, and the 473K luminous intensity is kept above 60% at room temperature.
Compared with the prior art, the invention has the advantages and positive effects that:
1. The invention introduces specific additives (carbon powder (C) and carbon compounds (SiC and C)3N4、B4C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc)2O3、Lu2O3、ZrO2、ScN、LuN、Zr3N4) One or more of the powder) can effectively improve the luminous performance and the thermal stability of low-quality nitride and oxynitride, and the method is green and environment-friendly, low in cost and mild in condition.
2. The performance of the nitride and oxynitride fluorescent material improved by the method is greatly improved, the internal quantum efficiency is more than 65 percent, and the 473K luminous intensity is kept above 60 percent at room temperature.
3. The special additive used in the invention has the advantages of easily available raw materials and low cost, and can improve the practical use of the low-quality fluorescent material.
Drawings
FIG. 1 shows low quality BaSi2O2N2:Eu2+A trend graph of relative luminous intensity change of the nitrogen oxide fluorescent material after a specific additive (taking SiC as an example) is introduced;
FIG. 2 shows low-quality BaSi in example 12O2N2:Eu2+The nitrogen oxide fluorescent material is treated by introducing a specific additive (taking SiC as an example) to obtain a change trend graph of the thermal stability of a sample.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.
Examples 1-17 are treatments for improving the luminescent properties and thermal stability of low-quality nitride or oxynitride fluorescent materials by introducing specific additives.
Example 1
3.3656g of low-quality nitride or oxynitride fluorescent material (the internal quantum efficiency is less than 50 percent, the 473K luminous intensity is less than 50 percent of the room temperature) and 0.0409g of SiC are put into agate grinding to be fully mixed, ground uniformly, sieved, then placed into a sintering furnace to be sintered at 1300-1500 ℃ and 0.1-0.5MPa, cooled to the room temperature along with the furnace, and the sintered product is ground, washed and dried to obtain the high-quality nitride or oxynitride fluorescent material (the internal quantum efficiency is more than or equal to 65 percent, and the 473K luminous intensity is kept more than 60 percent of the room temperature) with improved luminous performance and improved thermal stability.
Examples 2 to 5
The procedure is the same as in example 1, except that the quality of the low-quality nitride or oxynitride fluorescent material used is different from the quality of the specific additive SiC.
TABLE 1 changes in luminescence properties after introduction of specific additives (SiC)
Examples 6 to 11
The procedure is the same as in example 1 except that the quality of the low-quality nitride or oxynitride fluorescent material used is different from the kind and quality of the specific additive.
Table 2 introduction of different kinds of additives (SiC, C)3N4、B4C) Change in rear luminescence property
Examples 12 to 17
The procedure is the same as in example 1 except that the quality of the low-quality nitride or oxynitride fluorescent material used is different from the kind and quality of the specific additive.
Table 3 introduction of different kinds of additives (BN, Sc)2O3、Lu2O3、ZrO2) Change in rear luminescence property
Claims (7)
1. A method for improving the luminous performance and the thermal stability of a low-quality nitride or oxynitride fluorescent material is characterized by comprising the following steps of: fully mixing the low-quality nitride or oxynitride fluorescent material with a specific additive according to a certain proportion, uniformly grinding, sieving, then placing in a sintering furnace, sintering under a certain temperature and pressure, cooling to room temperature along with the furnace, and grinding, washing and drying the sintered product to obtain the high-quality nitride or oxynitride fluorescent material with improved luminous performance and thermal stability.
2. The method as claimed in claim 1, wherein the performance of the low-quality nitride or oxynitride fluorescent material is selected from the group consisting of: the internal quantum efficiency is lower than 50%, and the 473K luminous intensity is kept below 50% at room temperature.
3. The method for improving the luminescent property and thermal stability of the low-quality nitride or oxynitride fluorescent material according to claim 1, wherein the specific additive is carbon powder (C), carbon compound (SiC, C)3N4、B4C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc)2O3、Lu2O3、ZrO2、ScN、LuN、Zr3N4) And the like.
4. The method of claim 1A method for improving the luminous performance and thermal stability of low-quality nitride or oxynitride fluorescent material is characterized in that the chemical formula of the low-quality nitride or oxynitride fluorescent material is A1-xSi2O2N2:xEu2+、B2-xSi5N8:xEu2+、B1-xAlSiN3:xEu2+A represents one or a combination of more than two of Ca, Sr, Mg and Ba; b represents one or the combination of two of Ca and Sr; x is the molar concentration of divalent Eu doping substitution A or B, and x is more than 0 and less than or equal to 0.2.
5. The method as claimed in claim 1, wherein the specific additive is added in a proportion of 0 wt% or more and 3.5 wt% or less relative to the fluorescent material.
6. The method of claim 1, wherein the sintering temperature is selected from the group consisting of: t is more than or equal to 1300 ℃ and less than or equal to 1500 ℃, and P is more than or equal to 0.1 and less than or equal to 0.5 MPa.
7. The method for improving the luminescent performance and the thermal stability of the low-quality nitride or oxynitride fluorescent material according to claim 1, wherein the obtained high-quality nitride or oxynitride fluorescent material has the following properties: the internal quantum efficiency is more than 65%, and the 473K luminous intensity is kept above 60% at room temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023123349A1 (en) * | 2021-12-31 | 2023-07-06 | 苏州君诺新材科技有限公司 | Nitrogen oxide green fluorescent material, preparation method, and device |
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| CN103155707A (en) * | 2010-09-10 | 2013-06-12 | 渲染材料公司 | Silicon carbidonitride based phosphors and lighting devices using the same |
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Patent Citations (2)
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| CN103155707A (en) * | 2010-09-10 | 2013-06-12 | 渲染材料公司 | Silicon carbidonitride based phosphors and lighting devices using the same |
| CN103881706A (en) * | 2012-12-21 | 2014-06-25 | 有研稀土新材料股份有限公司 | Nitrogen oxide fluorescent powder, preparation method thereof and luminescent device containing the fluorescent powder |
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| JIARUI HAO ET AL.: "Improving photoluminescence and thermal stability of CaSi2O2N2:Eu2+ phosphors by codoping lanthanide ions (Ln = Sc, La, Gd, Yb, Lu)", 《MATERIALS LETTERS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023123349A1 (en) * | 2021-12-31 | 2023-07-06 | 苏州君诺新材科技有限公司 | Nitrogen oxide green fluorescent material, preparation method, and device |
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