Granted Patent B2

US 10,954,438 · App. 15/574,539 · Granted Mar 23, 2021

Abstract

Claims (88)

1. A process for synthesizing a color stable Mn 4+ doped phosphor, the process contacting a precursor of formula I, II, III, or IV

A a B b C c D d X x :Mn 4+   (I)

A ai B bi C ci D d X x Y d :Mn 4+   (II)

A 1 3 G 2-m-n Mn m Mg n Li 3 F 12-p O p ,  (III)

AZF 4 :Mn 4+   (IV)

with a fluorine-containing oxidizing agent in gaseous form at an elevated temperature to form the color stable Mn 4+ doped phosphor;

wherein

A is Li, Na, K, Rb, Cs, or a combination thereof;

B is Be, Mg, Ca, Sr, Ba, or a combination thereof;

C is Sc, Y, B, Al, Ga, In, Tl, or a combination thereof;

D is Ti, Zr, Hf, Rf, Si, Ge, Sn, Pb, or a combination thereof;

X is F or a combination of F and at least one of Br, Cl, and I;

Y is O, or a combination of O and at least one of S and Se;

Al is Na or K, or a combination thereof;

G is Al, B, Sc, Fe, Cr, Ti, In, or a combination thereof;

Z is La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, Y, In, or a combination thereof;

0≤a<2;

0≤b<1;

0≤c<1;

0≤d≤1;

0.8≤ai≤1.2;

0.8≤bi≤1.2;

0≤ci≤1.2;

5.0≤x≤7;

0.8≤c+d≤1.2;

a+2b+3c+4d=x;

0.8≤ci+d≤1;

5.0≤x+d≤7.0;

ai+2bi+3ci+4d=x+2d;

0.02≤m≤0.2;

0≤n≤0.4; and

0≤p<1.

2. A process according to claim 1 , wherein the precursor is formula I.

3. A process according to claim 1 , wherein X is F.

4. A process according to claim 1 , wherein Y is O.

5. A process according to claim 1 , wherein B is Ca, Sr, Ba, or a combination thereof.

6. A process according to claim 1 , wherein C is Al, Ga, or a combination thereof.

7. A process according to claim 1 , wherein D is Si, Ge, Ti, or a combination thereof.

8. A process according to claim 1 , wherein the fluorine-containing oxidizing agent is F 2 .

9. A process according to claim 1 , wherein the temperature ranges from about 200° C. to about 700° C.

10. A color stable Mn 4+ doped phosphor prepared by a process according to claim 1 .

11. A lighting apparatus comprising a semiconductor light source; and color stable Mn 4+ doped phosphor prepared by a process according to claim 1 .

12. A backlighting light source apparatus comprising a semiconductor light source; and color stable Mn 4+ doped phosphor prepared by a process according to claim 1 .

13. A liquid crystal display apparatus comprising: a liquid crystal panel; and the backlighting light source apparatus according to claim 12 disposed on a back surface of the liquid crystal panel.

14. A process for synthesizing a color stable Mn 4+ doped phosphor, the process comprising contacting a precursor of formula I with a fluorine-containing oxidizing agent in gaseous form at an elevated temperature to form the color stable Mn 4+ doped phosphor

A a B b C c D d X x :Mn 4+   (I)

wherein

A is Li, Na, K, Rb, Cs, or a combination thereof;

B is Be, Mg, Ca, Sr, Ba, or a combination thereof;

C is Sc, Y, B, Al, Ga, In, Tl, or a combination thereof;

D is Ti, Zr, Hf, Rf, Si, Ge, Sn, Pb, or a combination thereof;

X is F or a combination of F and at least one of Br, Cl, and I;

0≤a<2;

0≤b<1;

0≤c<1;

0≤d≤1;

0.8≤c+d≤1.2;

5.0≤x≤7; and

a+2b+3c+4d=x.

15. A process for synthesizing a color stable Mn 4+ doped phosphor, the process comprising contacting a precursor of formula II with a fluorine-containing oxidizing agent in gaseous form at an elevated temperature to form the color stable Mn 4+ doped phosphor

A ai B bi C ci D d X x Y d :Mn 4+   (II)

wherein

Y is O, or a combination of O and at least one of S and Se;

0.8≤ai≤1.2

0.8≤bi≤1.2

0≤ci≤1.2

0.8≤ci+d≤1

5.0≤x+d≤7.0;

ai+2bi+3ci+4d=x+2d; and

Y is O, or a combination of O and at least one of S and Se, wherein

A is Li, Na, K, Rb, Cs, or a combination thereof;

B is Be, Mg, Ca, Sr, Ba, or a combination thereof;

C is Sc, Y, B, Al, Ga, In, TI, or a combination thereof;

D is Ti, Zr, Hf, Rf, Si, Ge, Sn, Pb, or a combination thereof;

X is F or a combination of F and at least one Br, Cl and I; and

0≤d≤1.

16. A process for synthesizing a color stable Mn 4+ doped phosphor, the process comprising contacting a precursor of formula III with a fluorine-containing oxidizing agent in gaseous form at an elevated temperature to form the color stable Mn 4+ doped phosphor

A 1 3 G 2-m-n Mn m Mg n Li 3 F 12 O p ,  (III)

wherein

A 1 is Na or K, or a combination thereof;

G is Al, B, Sc, Fe, Cr, Ti, In, or a combination thereof;

0.02≤m≤0.2;

0≤n≤0.4; and

0≤p<1.

17. A process for synthesizing a color stable Mn 4+ doped phosphor, the process comprising contacting a precursor of formula IV with a fluorine-containing oxidizing agent in gaseous form at an elevated temperature to form the color stable Mn 4+ doped phosphor

AZF 4 :Mn 4+   (IV)

wherein

Z is La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, Y, In, or a combination thereof, and wherein A is Li, Na, K, Rb, Cs, or a combination thereof.

Assignments (11)