(Oxy)nitride phosphor powder and method of producing same
View Patent ↗An (oxy)nitride phosphor powder has a fluorescence peak wavelength of 610 to 625 nm and also has higher external quantum efficiency than the conventional one. The (oxy)nitride phosphor powder includes an α-type SiAlON and aluminum nitride, represented by the compositional formula: Ca x1 Eu x2 Si 12−(y+z) Al (y+z) O z N 16−z wherein x1, x2, y, z fulfill the following formulae: 1.60≦x1+x2≦2.90, 0.18≦x2/x1≦0.70, 4.0≦y≦6.5, 0.0≦z≦1.0. The powder can additionally contain Li in an amount of 50 to 10000 ppm. The content of the aluminum nitride may be more than 0 mass % to less than 33 mass %.
1. An (oxy)nitride phosphor powder containing an α-SiAlON crystal phase and aluminum nitride crystal phase, represented by the composition formula:
Ca x1 Eu x2 Si 12−(y+z) Al (y+z) O z N 16−z
wherein x1, x2, y and z are 1.60≦x1+x2≦2.90, 0.18≦x2/x1≦0.70, 4.0≦y≦6.5 and 0.0≦z≦1.0.
2. The (oxy)nitride phosphor powder according to claim 1 , wherein the content of aluminum nitride crystal phase is from more than 0 mass % to less than 33 mass %.
3. The (oxy)nitride phosphor powder according to claim 1 , further containing from 50 to 10,000 ppm of Li.
4. The (oxy)nitride phosphor powder according to claim 1 , wherein a fluorescence having a peak wavelength in a wavelength region of 610 to 625 nm is emitted by excitation with light having a wavelength of 450 nm and an external quantum efficiency in the light emission is 50% or more.
5. The (oxy)nitride phosphor powder according to claim 1 , wherein a 50% diameter (D 50 ) in a particle size distribution curve measured by a laser diffraction/scattering particle size distribution measuring apparatus is 10.0 to 20.0 μm and specific surface area is 0.2 to 0.6 m 2 /g.
6. A method of producing the (oxy)nitride phosphor powder according to claim 1 , comprising:
a first step of mixing a silicon source substance, an aluminum source substance, a calcium source substance, and a europium source substance to provide a composition represented by the composition formula:
Ca x1 Eu x2 Si 12−(y+z) Al (y+z) O z N 16−z
wherein x1, x2, y and z are
1.60≦x1+x2≦2.90,
0.18≦x2/x1≦0.70,
4.0≦y≦6.5,
0.0≦z≦1.0, followed by firing at a temperature of 1,500 to 2,000° C. in an inert gas atmosphere to obtain a fired (oxy)nitride represented by the formula above, and
a second step of heat-treating the fired (oxy)nitride, wherein the heat treatment in the second step is performed at a temperature of 1,100 to 1,600° C. in an inert gas atmosphere or a reducing atmosphere.
7. A method of producing the (oxy)nitride phosphor powder according to claim 1 , comprising:
a first step of mixing a silicon source substance, an aluminum source substance, a calcium source substance, and a europium source substance to provide a composition represented by the composition formula:
Ca x1 Eu x2 Si 12−(y+z) Al (y+z) O z N 16−z
wherein x1, x2, y and z are
1.60≦x1+x2≦2.90,
0.18≦x2/x1≦0.70,
4.0≦y≦6.5,
0.0≦z≦1.0, followed by firing at a temperature of 1,500 to 2,000° C. in an inert gas atmosphere to obtain a fired (oxy)nitride represented by the formula above, and
a second step of heat-treating the fired (oxy)nitride, wherein the heat treatment in the second step is performed in the presence of Li at a temperature of 1,450° C. to less than the firing temperature in an inert gas atmosphere or a reducing atmosphere.
8. The method according to claim 6 , wherein the silicon source substance is a silicon nitride powder and the silicon nitride powder has an oxygen content of 0.2 to 0.9 mass %, an average particle size of 1.0 to 12.0 μm and a specific surface area of 0.2 to 3.0 m 2 /g.
9. The method according to claim 7 , wherein the silicon source substance is a silicon nitride powder and the silicon nitride powder has an oxygen content of 0.2 to 0.9 mass %, an average particle size of 1.0 to 12.0 μm and a specific surface area of 0.2 to 3.0 m 2 /g.