Persistent phosphorescent composite material

Patent metadata

Field	Value
Publication number	US-9284485-B2
Application number	US-201314070616-A
Country	US
Kind code	B2
Filing date	Nov 4, 2013
Priority date	Nov 7, 2012
Publication date	Mar 15, 2016
Grant date	Mar 15, 2016

Abstract

The invention relates to a persistent phosphorescent ceramic composite material which is a sintered dense body comprising two or more phases, a first phase consisting of at least one metal oxide and a second phase consisting of a metal oxide containing at least one activating element in a reduced oxidation state. The invention furthermore relates to a method for the preparation of a phosphorescent ceramic composite material as defined in any of the previous claims, the method comprising the following steps: preparing a mixture of a metal oxide and a phosphor; fabricating a green body from the mixture; and heat treating the green body in a reducing atmosphere.

First claim

The invention claimed is:

1. Method for the preparation of a persistent phosphorescent ceramic composite material which is a sintered dense body comprising two or more phases,
a first phase consisting of at least one metal oxide and
a second phase which is a persistent phosphor, wherein the persistent phosphor consists of a metal oxide containing at least one activating element in a reduced oxidation state,
the method comprising the following steps:
preparing a mixture of the first and second phases;
fabricating a green body from the mixture;
treating the fabricated green body with a first sintering step under an oxidizing atmosphere followed by heat treating in a reducing atmosphere as the second sintering step.

2. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 1 , wherein the metal oxide in the first phase is selected from aluminum oxide, zirconium oxide, magnesium oxide, silicon oxide, titanium oxide, barium oxide, beryllium oxide, calcium oxide and chromium oxide.

3. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 1 , wherein the metal oxide in the first phase is zirconia stabilized with a dopant selected from the group consisting of Ce, Mg and Y.

4. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 1 , wherein the metal oxide in the first phase is zirconia stabilized with yttria.

5. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 1 , wherein the metal oxide in the second phase is selected from Ca, Ba, Sr and/or Mg-aluminates, Ca, Ba, Sr and/or Mg silicates, and Ca, and/or Sr aluminosilicates.

6. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 1 , wherein the metal oxide in the second phase is a strontium aluminate.

7. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 6 , wherein the metal oxide in the second phase is a strontium aluminate doped with at least an activating element selected from La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.

8. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 7 , wherein the metal oxide in the second phase is a strontium aluminate doped with Eu and Dy.

9. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 8 , wherein the second phase is a Eu 2+ /Dy 3+ doped Sr 4 Al 14 O 25 phase.

10. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 1 , wherein the amount of the first phase is 5 to 95% by weight and the amount of the second phase is 5 to 95% by weight, relative to the total weight of the two phases.

11. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 10 , wherein the amount of the first phase is 40 to 95% by weight and the amount of the second phase is 5 to 60% by weight, relative to the total weight of the two phases.

12. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 10 , wherein the amount of the first phase is 50 to 95% by weight and the amount of the second phase is 5 to 50% by weight, relative to the total weight of the two phases.

13. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 10 , wherein the amount of the first phase is 50 to 80% by weight and the amount of the second phase is 20 to 50% by weight, relative to the total weight of the two phases.

14. The method for the preparation of a phosphorescent ceramic composite material according to claim 1 , whereby a binder material is added to the mixed material and the fabricated green body is treated in a first step by a heat treatment to remove the binder material.

15. The method for the preparation of a phosphorescent ceramic composite material according to claim 1 , wherein heat treating in a reducing atmosphere is conducted at a temperature in the range of 800 to 1600° C.

16. The method for the preparation of a phosphorescent ceramic composite material according to claim 1 , wherein heat treating in a reducing atmosphere is conducted in an atmosphere of Ar/H 2 or N 2 /H 2 .

17. Method for the preparation of a persistent phosphorescent ceramic composite material which is a sintered dense body comprising two or more phases,
a first phase consisting of at least one metal oxide and
a second phase which is a persistent phosphor, wherein the persistent phosphor consists of, a metal oxide containing at least one activating element in a reduced oxidation state,
the method comprising the following steps:
preparing a mixture of the first and second phases;
fabricating a green body from the mixture;
whereby a binder material is added to the mixed material and the fabricated green body is treated in the first step by a heat treatment to remove the binder material.

18. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 17 , wherein the metal oxide in the first phase is selected from aluminum oxide, zirconium oxide, magnesium oxide, silicon oxide, titanium oxide, barium oxide, beryllium oxide, calcium oxide and chromium oxide.

19. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 17 , wherein the metal oxide in the first phase is zirconia stabilized with a dopant selected from the group consisting of Ce, Mg and Y.

20. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 17 , wherein the metal oxide in the first phase is zirconia stabilized with yttria.

21. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 17 , wherein the metal oxide in the second phase is selected from Ca, Ba, Sr and/or Mg-aluminates, Ca, Ba, Sr and/or Mg silicates, and Ca, and/or Sr aluminosilicates.

22. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 17 , wherein the metal oxide in the second phase is a strontium aluminate.

23. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 22 , wherein the metal oxide in the second phase is a strontium aluminate doped with at least an activating element selected from La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.

24. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 23 , wherein the metal oxide in the second phase is a strontium aluminate doped with Eu and Dy.

25. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 24 , wherein the second phase is a Eu 2+ /Dy 3+ doped Sr 4 Al 14 O 25 phase.

26. The method for the preparation of the persistent phosphorescent ceramic composite material according to claim 17 , wherein the amount of the first phase is 5 to 95% by weight and the amount of the second phase is 5 to 95% by weight, relative to the total weight of the two phases.

Assignees

• Rolex Sa

Inventors

• Berner Detlef
• Girod Romain
• Pujol Ollivier
• Rigot Isabelle

Classifications

• C04B2235/77

  Density · CPC title

• C09K11/025 Primary

  non-luminescent particle coatings or suspension media · CPC title

• C04B2235/661

  Multi-step sintering · CPC title

• C04B2235/5436

  micrometer sized, i.e. from 1 to 100 micron · CPC title

• G04B37/225

  Non-metallic cases · CPC title