CN111778020A - Processing method for improving luminous efficiency and moisture resistance of stannate red light material - Google Patents
Processing method for improving luminous efficiency and moisture resistance of stannate red light material Download PDFInfo
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Abstract
The invention discloses a processing method for improving the luminous efficiency and moisture resistance of a stannate red light material. The method adopts a same-element low-valence ion reduction method to form a core-shell structure, so that the luminous efficiency and the moisture resistance of the acid salt red light material are effectively improved, namely Sn metal or salt solution of Sn2+ is used for soaking stannate red light material A2SnF6: Mn4+ and BSnF6: Mn4+, wherein A is one or more than 2 of Li, Na, K, Rb and Cs, and B is one or more than 2 of Mg, Ca, Sr, Ba and Zn. The method has the advantages that: no new impurity is introduced, the raw materials are cheap and easy to obtain, the process is simple and easy to implement, the conditions are mild, the cost is low, the performance of the red light material is effectively improved, and the method is favorable for large-scale industrial production.
Description
Technical Field
The invention relates to an optimization method of inorganic solid luminescent material property, in particular to a processing method for improving the luminous efficiency and moisture resistance of stannate red light material.
Background
White light leds (leds) have attracted much attention in comparison with conventional illumination sources (fluorescent or incandescent lamps) due to their low power consumption and long life. Most commercial White Light LEDs (WLEDs) are formed by phosphor conversion, where a yellow phosphor is essential, such as YAG: Ce, converting blue Light from GaN chips to White Light [ Shang M, Li C, Lin J.how to product White Light in a Single-Phase Host chem. Soc. Rev. 2014, 45(18):1372-86 ]. Therefore, there has been great interest in the synthesis of phosphors with PL spectra well matched to InGaN chips, especially with broad excitation bands in the blue region. However, such a WELD has a low color rendering index of about 70 at color temperatures above 5000K, which cannot meet the requirements of indoor room lighting, and much effort has been focused on developing a novel red phosphor capable of strong absorption in the blue region to match the electroluminescence of the LED chip. In particular, Eu2+ doped red nitride is widely used in the WLEDs market [ Pust P, Weiler V, Hecht C, et al, Narrow-band red-emitting Sr [ LiAl3N4]: Eu2+ as a next-generation LED-phosphor material. nat. mater. 2014, 13(9):891 ] due to its excellent luminous efficiency and thermal stability. However, red nitride phosphors suffer from two major drawbacks, the harsh synthesis requirements and the lack of air-sensitive metal nitrides requiring very high cost; too wide an emission band, resulting in low color purity of the light, is limited in indoor lighting. Therefore, it is highly desirable to explore new efficient red phosphors based on a simple method of low cost raw materials.
The Mn4+ series doped red fluorescent powder developed in recent years is concerned due to the abundant raw materials and mild synthesis conditions (in air). More importantly, Mn4+ has excellent spectral characteristics as an emission center, having a broad absorption band of blue and a set of sharp emission peaks of red, which is highly desirable for applications in WLEDs with high color rendering indices. The ancient teacher reports that a red fluorescent powder K2TiF6: Mn4+ is obtained by a simple ion exchange method, and the luminous quantum yield of the fluorescent powder is as high as 98%. The ideal warm white light for high performance white LEDs (CRI = 81 and CCT = 3556K) was achieved by synthesizing K2TiF6 Mn4+ [ Zhu H, Lin C, Luo W, et al, high proximate LED non-raw-earth-extruded phosphor for warm white light-emitting diodes, nat. commu., 2014, 5:4312 ]. HF, which is corrosive and volatile, is a necessity for the synthesis of Mn4+ doped fluorides because of its two functions, forming an acidic environment or decomposing KMnO4 to produce Mn (vi) and providing F-to obtain [ MnF6] 2-complex instead of MnO2 hydrate. The group of Adachi reported the raman scattering spectra and luminescence properties of Na2SnF6, Cs2SnF6, znsnnf 6.6 h2o, k2snf6.6 h2o and BaSnF6 for hexafluorostannate. In the structures of these hexafluorostannates, Mn4+ can replace the hexagonal Sn4+ site, since Mn4+ and Sn4+ of the same charge valence have similar ion sizes. Mn4+ in hexafluorosilicate emits red light in the region between 600nm and 700nm, similar to Mn4+ doped hexafluorosilicate and hexafluorotitanate.
However, the luminous efficiency and thermal stability of the Mn4+ doped stannate red phosphor need to be improved to meet the application in white LEDs.
Disclosure of Invention
In summary, in order to overcome the drawbacks and disadvantages of the prior art, the present invention provides a processing method for improving the luminous efficiency and moisture resistance of a stannate red light material.
In order to achieve the above object, the technical scheme of the invention provides a method for improving the luminous efficiency and moisture resistance of a stannate red light material, which comprises the following steps: firstly, adding Sn metal or salt of Sn2+ into water to form solution; secondly, putting the red light material A2SnF6: Mn4+ and BSnF6: Mn4+ into the solution to be fully soaked, and stirring; and thirdly, carrying out suction filtration and air drying to obtain an optimized product.
Further setting: a in the A2SnF6 Mn4+ and BSnF6 Mn4+ is one or more than 2 of Li, Na, K, Rb and Cs, B is one or more than 2 of Mg, Ca, Sr, Ba and Zn, and the central ions are Sn4 +.
By adopting the technical scheme, the method adopts the same-element low-valence ion reduction method to form a core-shell structure, so that the luminous efficiency and the moisture resistance of the acid-salt red-light material are effectively improved, namely Sn metal or salt solution of Sn2+ is used for soaking the stannate red-light material A2SnF6: Mn4+ and BSnF6: Mn4+, wherein A is one or more than 2 of Li, Na, K, Rb and Cs, and B is one or more than 2 of Mg, Ca, Sr, Ba and Zn. The surface of red light materials A2SnF6: Mn4+ and BSnF6: Mn4+ is reduced into Mn2+ by utilizing the weak reducibility of a salt solution of Sn metal or Sn2+, and the red light materials are discharged into the solution to form a shell layer with low Mn4+ concentration, so that the non-radiative cross relaxation among luminescent particles is effectively reduced, the luminescent efficiency is greatly increased, and the moisture resistance of the luminescent particles is improved. The method has the advantages that: no new impurity is introduced, the raw materials are cheap and easy to obtain, the process is simple and easy to implement, the conditions are mild, the cost is low, the performance of the red light material is effectively improved, and the method is favorable for large-scale industrial production.
In order to further achieve the purpose of the invention, the mass ratio of the red light material A2SnF6: Mn4+ or BSnF6: Mn4+ to the solution is preferably 30-70%.
In order to further achieve the purpose of the invention, preferably, the salt of Sn2+ is stannous chloride SnCl2, and the mass ratio of the salt solution of Sn2+ is 1-10%.
In order to further achieve the purpose of the invention, preferably, the salt of Sn2+ is stannous oxide SnO, and the mass ratio of the salt solution of Sn2+ is 1-10%.
In order to further achieve the purpose of the invention, preferably, the red light material is soaked in the weak reducing solution for 10 to 30 minutes.
For further achieving the purpose of the invention, preferably, the stirring speed of the red light material in the weak reducing solution is 1000-2000 rpm.
By adopting the technical scheme, the A2SnF6 Mn4+ or BSnF6 Mn4+ red light material has strong absorption peaks in the near ultraviolet region (about 380 nm) and the blue light region (about 460 nm) of the excitation spectrum, the emission spectrum is positioned in the red light region, and the red light material has strong luminous efficiency and thermal stability and can be applied to a white light LED.
Compared with the prior art, the invention has the following advantages and beneficial effects: the surface of red light materials A2SnF6: Mn4+ and BSnF6: Mn4+ is reduced into Mn2+ by utilizing the weak reducibility of a salt solution of Sn metal or Sn2+, and the red light materials are discharged into the solution to form a shell layer with low Mn4+ concentration, so that the non-radiative cross relaxation among luminescent particles is effectively reduced, the luminescent efficiency is greatly increased, and the moisture resistance of the luminescent particles is improved. Simple process and easy industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a comparison of emission spectra of a material NaRbSnF6: Mn4+ soaked in accordance with the inventive example 1 technique with that of un-soaked NaRbSnF6: Mn4 +;
FIG. 2 is a comparison of XRD patterns of the NaRbSnF6: Mn4+ soaked material and the un-soaked NaRbSnF6: Mn4+ soaked material according to the technique of example 1 of the present invention;
FIG. 3 is a comparison of the luminescence intensity and moisture resistance of the soaked materials of the technology of example 1 of the present invention, NaRbSnF6: Mn4+, and un-soaked NaRbSnF6: Mn4 +.
Detailed Description
The invention will be further described with reference to examples and figures, but the scope of the invention as claimed is not limited to the examples shown.
Example 1
Adding stannous oxide SnO into 100 mL of water to form a salt solution with the mass of 5%, putting red light materials NaRbSnF6: Mn4+ into the solution with the mass proportion of 50%, stirring at the stirring speed of 1500 rpm for sufficient soaking, soaking for 20 minutes, and then carrying out suction filtration and air drying to obtain the optimized product. The product treated in this example fluoresces deep red under near ultraviolet irradiation. The emission peak table of the embodiment is unchanged as shown in FIG. 1, but the intensity is greatly enhanced; XRD as shown in figure 2 shows that the product treated by the technology of the invention is pure-phase NaRbSnF 6; as shown in the attached figure 3, the NaRbSnF6: Mn4+ product obtained by the embodiment has increased luminous intensity and greatly enhanced moisture resistance. The XRD and fluorescence spectra of the other examples are substantially similar to those of the present example and are not described.
Example 2
Adding stannous oxide SnO into 100 mL of water to form a 1% saline solution, putting a red light material NaRbSnF6: Mn4+ into the solution in a mass ratio of 30% to fully soak, stirring at a stirring speed of 2000 rpm, soaking for 10 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 3
Adding stannous oxide SnO into 100 mL of water to form a 10% saline solution, putting a red light material NaRbSnF6: Mn4+ into the solution in a mass ratio of 70%, stirring at a stirring speed of 2000 rpm for sufficient soaking, soaking for 30 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 4
Adding stannous oxide SnO into 100 mL of water to form a salt solution with the mass of 9%, putting a red light material NaRbSnF6: Mn4+ into the solution with the mass ratio of 30%, stirring at the stirring speed of 1000 rpm for sufficient soaking, soaking for 20 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 5
Adding stannous chloride SnCl2 into 100 mL of water to form 10% salt solution, putting red light material BaSnF6: Mn4+ into the solution in a mass ratio of 20%, stirring at a stirring speed of 1500 rpm for sufficient soaking, soaking for 30 minutes, and then carrying out suction filtration and air drying to obtain the optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 6
Adding stannous chloride SnCl2 into 100 mL of water to form a salt solution with the mass of 5%, putting a red light material BaSnF6: Mn4+ into the solution with the mass proportion of 30%, stirring at the stirring speed of 1000 rpm for sufficient soaking, soaking for 20 minutes, and then carrying out suction filtration and air drying to obtain the optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 7
Adding stannous chloride SnCl2 into 100 mL of water to form a saline solution with the mass of 8%, putting a red light material BaSnF6: Mn4+ into the solution with the mass proportion of 70%, stirring at the stirring speed of 2000 rpm for sufficient soaking, soaking for 15 minutes, then carrying out suction filtration and air drying to obtain the optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 8
Adding metal Sn particles into 100 mL of water to form a salt solution with the mass of 8%, putting a red light material Na2SnF6: Mn4+ into the solution with the mass proportion of 70% to fully soak, stirring at the stirring speed of 2000 rpm, soaking for 15 minutes, then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 9
Adding stannous oxide SnO into 100 mL of water to form a salt solution with the mass of 9%, putting a red light material Na2SnF6: Mn4+ into the solution with the mass proportion of 30% to fully soak, stirring at the stirring speed of 1000 rpm, soaking for 20 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 10
Adding stannous chloride SnCl2 into 100 mL of water to form 10% salt solution, putting a red light material Na2SnF6: Mn4+ into the solution in a mass ratio of 20%, stirring at a stirring speed of 1500 rpm for sufficient soaking, soaking for 30 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 11
Adding stannous chloride SnCl2 into 100 mL of water to form a salt solution with the mass of 5%, putting a red light material Na2SnF6: Mn4+ into the solution with the mass proportion of 30%, stirring at the stirring speed of 1000 rpm for sufficient soaking, soaking for 20 minutes, and then carrying out suction filtration and air drying to obtain the optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 12
Adding metal Sn particles into 100 mL of water to form a salt solution with the mass of 8%, putting a red light material Cs2SnF6: Mn4+ into the solution with the mass proportion of 70% to fully soak, stirring at the stirring speed of 2000 rpm, soaking for 15 minutes, then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 13
Adding stannous oxide SnO into 100 mL of water to form a salt solution with the mass of 9%, putting a red light material Cs2SnF6: Mn4+ into the solution with the mass proportion of 30% to fully soak, stirring at the stirring speed of 1000 rpm, soaking for 20 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
Example 14
Adding stannous chloride SnCl2 into 100 mL of water to form 10% by mass of salt solution, putting a red light material Cs2SnF6: Mn4+ into the solution in a mass ratio of 20% to fully soak, stirring at a stirring speed of 1500 rpm, soaking for 30 minutes, and then carrying out suction filtration and air drying to obtain an optimized product. The product treated by the embodiment fluoresces deep red under near ultraviolet irradiation, and compared with the sample which is not treated, the product of the embodiment has greatly enhanced luminous intensity and moisture resistance.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (7)
1. A processing method for improving the luminous efficiency and moisture resistance of a stannate red light material is characterized by comprising the following steps: first, adding Sn metal or Sn into water2+A salt forming solution; second, the red light material A is added2SnF6:Mn4+And BSnF6:Mn4+Adding the mixture into the solution for soaking fully, and stirring; and thirdly, carrying out suction filtration and air drying to obtain an optimized product.
2. The process of claim 1, wherein the process comprises the steps of: a. the2SnF6:Mn4+And BSnF6:Mn4+In AOne or more than 2 of Li, Na, K, Rb and Cs, B one or more than 2 of Mg, Ca, Sr, Ba and Zn, and Sn as central ions4+。
3. The process of claim 1, wherein the process comprises the steps of: red light material A2SnF6:Mn4+Or BSnF6:Mn4+The mass ratio of the solution to the solution is 30-70%.
4. The process of claim 1, wherein the process comprises the steps of: sn (tin)2+The salt being stannous chloride SnCl2，Sn2+The mass ratio of the salt solution is 1-10%.
5. The process of claim 1, wherein the process comprises the steps of: sn (tin)2+The salt is stannous oxide SnO, Sn2+The mass ratio of the salt solution is 1-10%.
6. The process of claim 1, wherein the process comprises the steps of: soaking for 10-30 minutes.
7. The process of claim 1, wherein the process comprises the steps of: the stirring speed is 1000-2000 rpm.
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Application publication date: 20201016 |