Red double-perovskite fluorescent powder for white-light LEDs and preparation method of red double-perovskite fluorescent powder

A technology of red phosphor and double perovskite, which is applied in chemical instruments and methods, luminescent materials, gas discharge lamps, etc., can solve the problem of insufficient intensity of the red light emission area, and achieve good color purity and color rendering , good color rendering and high emission intensity

Active Publication Date: 2012-08-15
武汉视美乐激光显示发展有限公司
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AI-Extracted Technical Summary

Problems solved by technology

[0005] In the double perovskite system reported above (A 2 B I B II o 6 (B II =Mo or W)) in the fluorescent host material, its A-site ions are +2-valent alkaline earth metal ions such as Ca 2+ 、Sr 2+ 、Ba 2+ etc., the symmetry of the double perovskite structure is strong, and the structure can be cubic, tetrag...
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Abstract

The invention relates to a red double-perovskite fluorescent powder for white-light LEDs and a preparation method of the red double-perovskite fluorescent powder. The red double-perovskite fluorescent powder is characterized by comprising double-perovskite components shown in the following formula: (AA'1-xMex)MgMO<6>, wherein the A is one of Na or K, the A' is one of La or Gd or composition of the La and the Gd, the M is one of W or Mo or composition of the W and the Mo, the Me is one of rare-earth element Eu or Pr, and the x is larger than or equal to 0.005 and is smaller than or equal to 0.5. The fluorescent powder is prepared by means of sol-gel, single-phase double-perovskite oxide powder can be obtained at the lower temperature and in shorter time, mixing of ions or atoms can be realized by active ions of rare earth, test period is short and stability is fine.

Application Domain

Gas discharge lamp usageLuminescent compositions

Technology Topic

Rare-earth elementIon +7

Image

  • Red double-perovskite fluorescent powder for white-light LEDs and preparation method of red double-perovskite fluorescent powder
  • Red double-perovskite fluorescent powder for white-light LEDs and preparation method of red double-perovskite fluorescent powder
  • Red double-perovskite fluorescent powder for white-light LEDs and preparation method of red double-perovskite fluorescent powder

Examples

  • Experimental program(4)

Example Embodiment

[0032] Example 1 # ((NaLa 0.99 Eu 0.01 )MgMoO 6 ):
[0033] Composition as shown in Table 1 # As shown, the specific preparation method includes the following steps:
[0034] ①Weigh the solid powder raw materials according to the composition in Table 1. First, dissolve ammonium molybdate and EDTA in ammonia solution, and citric acid in deionized water; dissolve ammonium molybdate and EDTA in ammonia solution and metal ion nitrate solution Mix, stir and heat; then adjust the pH of the completely dissolved citric acid solution to 5 with ammonia, then add it to the mixed solution, finally adjust the pH of the solution with ammonia to 7, and the total concentration of all metal ions in the entire solution system is about 1.0 mol /L, the whole process has been stirring and heating, the heating temperature is 35℃;
[0035] ②Place the prepared solution on a magnetic stirrer, stir for 40 minutes and then unpack, heat at 50℃ and keep stirring for about 2.5 hours to form a sol; then increase the heating temperature to 70℃ and continue to stir until a transparent gel;
[0036] ③Put the gel to continue heating, and a combustion reaction will take place to form a fluffy precursor powder; the precursor powder is slightly ground, placed in an alumina porcelain boat, and then placed in a muffle furnace for pre-fired at 600°C and kept warm 4 Hours, then cool down with the furnace.
[0037] ④ Grind the pre-fired powder, place it in an alumina ceramic crucible, and calcinate at a high temperature of 1000°C, keep it for 6 hours, and then cool down with the furnace.
[0038] ⑤ Grind the obtained product through a 200-mesh sieve, and then dry-press it into a thin circular plate with a powder tablet machine for performance testing.
[0039] The test results are as follows:
[0040] In the process ⑤, the sample processed by the tablet is tested by fluorescence spectroscopy (FL3-221, HOROBA, Jobin Yvon, France). The excitation spectra under 615nm red light and the emission spectra of the powder under excitation at near ultraviolet 395nm are respectively shown figure 1 (a) and figure 2 (a).

Example Embodiment

[0041] Example 2 # ((NaLa 0.5Gd0.48 Eu 0.02 )MgWO 6 ):
[0042] Composition as shown in Table 1 2 # As shown, the specific preparation method includes the following steps:
[0043] ①Weigh the solid powder raw materials according to the composition in Table 1. First, dissolve EDTA in the ammonia solution, ammonium tungstate and citric acid in an appropriate amount of deionized water, respectively heat and stir to dissolve; combine the EDTA ammonia solution and metal ion nitric acid Mix the salt solution, stir and heat; then use ammonia to adjust the pH of the completely dissolved citric acid solution to 6 and add it to the mixed solution; finally, use ammonia to adjust the pH of the mixed solution to 8, and add the ammonium tungstate solution. The total concentration of all metal ions in the solution system is about 1.15mol/L, the whole process has been stirred and heated, and the heating temperature is 30℃;
[0044] ②Place the prepared solution on a magnetic stirrer, stir for 30 minutes and then unpack, heat at 55°C and keep stirring for about 2 hours to form a sol; then increase the heating temperature to 65°C and continue stirring until a transparent gel is formed glue;
[0045] ③Continue heating the gel to form a fluffy precursor powder after the combustion reaction occurs; the precursor powder is slightly ground, placed in an alumina porcelain boat, and then placed in a muffle furnace for pre-burning at 500 ℃ and keeping it warm 6 Hours, then cool down with the furnace.
[0046] ④ Grind the pre-fired powder, place it in an alumina ceramic crucible, and calcinate at a high temperature of 1000°C, keep it for 6 hours, and then cool down with the furnace.
[0047] ⑤ Grind the obtained product through a 200-mesh sieve to obtain Eu-doped double perovskite red phosphor. The prepared phosphor can emit strong red light.

Example Embodiment

[0048] Example 3 # ((KLa 0.99 Pr 0.01 )MgWO 6 ):
[0049] Composition as shown in Table 1 in 3 # As shown, the specific preparation method includes the following steps:
[0050] ①Weigh the solid powder raw materials according to the composition in Table 1. First, dissolve EDTA in the ammonia solution, ammonium tungstate and citric acid in an appropriate amount of deionized water, respectively heat and stir to dissolve; combine the EDTA ammonia solution and metal ion nitric acid Mix the salt solution, stir and heat; then adjust the pH of the completely dissolved citric acid solution to 7 with ammonia water, then add it to the mixed solution; finally adjust the pH of the solution to 7.5 with ammonia water, and add the ammonium tungstate solution to the mixed solution In the whole solution system, the total concentration of all metal ions is about 1.25mol/L, and the whole process has been stirred and heated at a temperature of 30℃;
[0051] ②Place the prepared solution on a magnetic stirrer, stir for 30 minutes and then unpack, heat at 55°C and keep stirring for about 2 hours to form a sol; then increase the heating temperature to 65°C and continue stirring until a transparent gel is formed glue;
[0052] ③ Continue heating the gel to form a fluffy precursor powder after the combustion reaction occurs; the precursor powder is slightly ground, placed in an alumina porcelain boat, and then placed in a muffle furnace to pre-fire at 600°C and keep it warm 4 Hours, then cool down with the furnace.
[0053] ④ Grind the pre-fired powder, put it in an alumina ceramic crucible, calcinate at a high temperature of 950°C, keep it warm for 8 hours, and then cool down with the furnace.
[0054] ⑤ Grind the obtained product through a 200-mesh sieve, and then dry-press it into a thin circular plate with a powder tablet machine for structure and performance testing.
[0055] The test results are as follows:
[0056] In the process ⑤, the sample processed by the tablet is tested for the fluorescence spectrum, and the emission spectrum of the powder under the excitation of 606nm red light and 453nm of blue light is respectively shown figure 1 (b) and figure 2 (b).

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