A kind of highly efficient and stable LED nitride red phosphor and preparation method thereof
A red phosphor and nitride technology, applied in the field of red phosphor and its preparation, can solve the problems of poor thermal stability, harsh preparation process conditions, low luminous intensity, etc. efficient effect
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Embodiment 1
[0036] According to stoichiometric Ca 0.19 Sr 0.8 AlSi 0.95 Ta 0.025 Bi 0.025 N 2.923 o 0.115 : 0.01Eu, in a nitrogen or argon-protected glove box, wait for H in the glove box 2 O content ≤ 0.1ppm, O content ≤ 0.1ppm, weigh Ca 3 N 2 3.13g, Sr 3 N 2 25.86g, Si 3 N 4 14.81g, Ta 2 o 5 1.84g, Bi 2 o 3 1.94g, AlN 13.66g, Eu 2 o 3 0.59g, put the raw materials weighed above into a mortar, grind them, mix them evenly, place them in a Mo crucible, put the crucible into a pressure furnace, and vacuumize it three times through a vacuum pump, and then fill it with nitrogen to normal pressure , heating to raise the temperature in the crucible to 1450°C and keep it warm for 4 hours, then fill it with nitrogen, raise the pressure of the pressure furnace to 0.5MPa and stop the pressure, raise the temperature to raise the temperature in the crucible to 1700°C and keep it warm for 4 hours, during the heating process The heating rate is 8°C / min, then the temperature is lower...
Embodiment 2-23
[0038] prepared Ca 0.19 Sr 0.8 AlSi 0.95 Ta 0.025 Bi 0.025 N 2.923 o 0.115 : 0.01Eu fluorescent powder, different from Example 1 is that the type of flux and the amount of flux (accounting for the mass percent of the mixture) have been changed, and other process conditions are all the same as in Example 1. The relative brightness, peak wavelength, half-width and K value (D90-D10) / D50 of the phosphor powder prepared in Examples 2-23 were tested, and the test results are shown in Table 1.
[0039] Table 1
[0040]
[0041] It can be seen from Table 1 that the brightness of the prepared phosphor is relatively improved, the peak wavelength is shortened, the half-peak width is reduced, and the particle uniformity is good, compared with the use of P to replace Si sites by replacing Si with equal amounts of Ta and Bi. The sample performance of adding flux is better than the sample performance without adding flux, and when the addition ratio of flux is 6wt%, the effect is be...
Embodiment 24-28
[0043] prepared Ca 0.19 Sr 0.8 AlSi 0.95 Ta 0.025 Bi 0.025 N 2.882 o 0.177 : 0.01Eu fluorescent powder, different from embodiment 2 is to adopt AlF 3 and MgCl 2 The combination flux, other processing conditions are all identical with embodiment 2. The relative brightness, peak wavelength, half-width and K value (D90-D10) / D50 of the phosphor powder prepared in Examples 24-28 were tested, and the test results are shown in Table 2.
[0044] Table 2
[0045]
[0046] It can be seen from Table 2 that by using combined fluxes, its spectral performance is further improved, and the particles are uniform, among which AlF 3 :MgCl 2 =1:2 (mass ratio) the best effect.
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