CN111849472B - 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 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. The specific additive is carbon powder (C) and carbon compound (SiC, C) 3 N 4 、B 4 C) Boride (BN), scandium/lutetium/zirconiumOxide or nitride (Sc) of 2 O 3 、Lu 2 O 3 、ZrO 2 、ScN、LuN、Zr 3 N 4 ) One or more of the powders, the low-quality nitride or oxynitride fluorescent material has a chemical formula of A 1‑x Si 2 O 2 N 2 :xEu 2+ 、B 2‑x Si 5 N 8 :xEu 2+ 、B 1‑x AlSiN 3 :xEu 2+ . 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 lighting and backlighting because of their high efficiency, energy saving, and long life, and are known as fourth generation lighting sources after incandescent lamps, fluorescent lamps, and energy saving lamps. Currently, ce is commercially available as "blue LED + YAG 3+ "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, eu 2+ Doped nitrides or oxynitrides are used as a good fluorescent material for white LEDs, and part of the system is commercially applied to the white LEDs. Among them, the document [ G. Li, chem. Mater, 26 (2014) 2991-3001.]And [ V. Bachmann, chem. Mater. 21 (2008) 316-325.]All reported (Ba, ca, sr) Si 2 O 2 N 2 :Eu 2+ The main emission peak of the nitrogen oxide fluorescent material is positioned in the 490-510nm area, 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 fluorescent materials have low internal quantum efficiency and thermal stability, which makes the white LED have poor light conversion efficiency and greatly reduced lifetime, thereby resulting in limited commercial applications. The literature [ Y, li, J, solid State chem., 2008, 181 (3): 515-524.]、[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): 1756-1761.]Separately reported is a blue light excited (Ca, sr) 2 Si 5 N 8 : Eu 2+ And (Ca, sr) AlSiN 3 : Eu 2+ 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 fluorescent powder needs to be prepared under the severe conditions of ultra high temperature and ultra high pressure and is subjected to the strict temperature in the preparation processThe yield of the fluorescent powder is low in the production process, and a large amount of low-quality nitride fluorescent materials with low luminous performance and poor thermal stability exist. Therefore, aiming at the low-quality nitrogen oxide or nitride fluorescent materials, a method for improving the luminous performance and the thermal stability is developed, the product utilization rate can be greatly improved, the production cost is greatly reduced, and the method 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) are known 3 N 4 、B 4 C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc) 2 O 3 、Lu 2 O 3 、ZrO 2 、ScN、LuN、Zr 3 N 4 ) 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 3 N 4 、B 4 C) Boride (BN), oxide or nitride of scandium/lutetium/zirconium (Sc) 2 O 3 、Lu 2 O 3 、ZrO 2 、ScN、LuN、Zr 3 N 4 ) 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 with internal quantum efficiency of more than 65 percent and luminous intensity of 473K kept above 60 percent at room temperature can be obtainedA fluorescent material.
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) 3 N 4 、B 4 C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc) 2 O 3 、Lu 2 O 3 、ZrO 2 、ScN、LuN、Zr 3 N 4 ) And the like.
As an improvement of the technical scheme, the chemical formula of the low-quality nitride or oxynitride fluorescent material in the scheme is A 1-x Si 2 O 2 N 2 :xEu 2+ 、B 2-x Si 5 N 8 :xEu 2+ 、B 1-x AlSiN 3 :xEu 2+ 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: 1300. t is more than or equal to 1500 ℃, and P is more than or equal to 0.1 and less than or equal to 0.5MPa.
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) 3 N 4 、B 4 C) Boride (BN), scandium/lutetium/zirconium oxide or nitride (Sc) 2 O 3 、Lu 2 O 3 、ZrO 2 、ScN、LuN、Zr 3 N 4 ) 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 BaSi 2 O 2 N 2 :Eu 2+ 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 1 2 O 2 N 2 :Eu 2+ 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 obtained by a person skilled in the art without making any creative effort based on the embodiments of the present invention, 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%, the 473K luminous intensity is below 50% at 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 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%, and the 473K luminous intensity is kept at more than 60% at 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) 3 N 4 、B 4 C) Change in rear luminescence property
Examples 12 to 17
The same procedure as in example 1 was followed, except that the quality of the low-quality nitride or oxynitride fluorescent material used was different from the kind and quality of the specific additive.
Table 3 introduction of different kinds of additives (BN, sc) 2 O 3 、Lu 2 O 3 、ZrO 2 ) Change in rear luminescence property
Claims (3)
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 a low-quality nitride or nitrogen oxide 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 a sintered product to obtain a high-quality nitride or nitrogen oxide fluorescent material with improved luminous performance and thermal stability;
wherein, the performance of the low-quality nitride or oxynitride fluorescent material is as follows: the internal quantum efficiency is lower than 50%, and the 473K luminous intensity is kept below 50% at room temperature;
the chemical formula of the low-quality nitride or oxynitride fluorescent material is A 1-x Si 2 O 2 N 2 :xEu 2+ 、B 2-x Si 5 N 8 :xEu 2 + 、B 1-x AlSiN 3 :xEu 2+ 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;
the specific additive is SiC or C 3 N 4 、B 4 C、BN、Sc 2 O 3 、Lu 2 O 3 、ZrO 2 A combination of ScN and LuN, zr 3 N 4 One or more of powders;
the sintering temperature is as follows: 1300. t is more than or equal to 0 ℃ and less than 1500 ℃, and P is more than or equal to 0.1 and less than or equal to 0.5MPa.
2. 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.
3. 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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| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (5)
| Title |
|---|
| A Novel Synthetic Method of Sr2Si5N8:Eu2+ from SrSi2O2N2:Eu2+ by Carbo-Thermal Reduction and Nitridation;Kang Sik Choi et al.;《Journal of Nanoscience and Nanotechnology》;20130301;第13卷(第3期);第1867-1870页 * |
| Achieving an efficient La3Si8N11O4:Eu2+ phosphor via chemical reduction of nano-scale carbon film: Toward white light-emitting diodes;Sheng-Hui Zhang et al.;《Journal of Alloys and Compounds》;20190531;第799卷;第360-367页 * |
| Domination of Second-Sphere Shrinkage Effect To Improve Photoluminescence of Red Nitride Phosphors;Wan-Yu Huang et al.;《Inorg. Chem.》;20141119;第53卷;第12822-12831页 * |
| Improving photoluminescence and thermal stability of CaSi2O2N2:Eu2+ phosphors by codoping lanthanide ions (Ln = Sc, La, Gd, Yb, Lu);Jiarui Hao et al.;《Materials Letters》;20170914;第211卷;第122-125页 * |
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