IP Library Granted Patent US 8,470,201
Granted Patent B2
US 8,470,201 · App. 13/523,019 · Granted Jun 25, 2013

Al

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Quick Facts
Patent No.
US 8,470,201
App. No.
13/523,019
Granted
Jun 25, 2013
Kind
B2
Abstract

An oxide phosphor that is highly durable and produces visible light when excited by exposure to near-ultraviolet excitation light, comprising an oxide having the composition represented by the formula (Al 2 O 3 ) x .(SiO 2 ) 1-x , where 0<x<1, and an activating element M.

Claims (32)

1. A method comprising:

mixing a source of an activating element M with an oxide of formula (Al 2 O 3 ) x .(SiO 2 ) 1-x to form a mixture; and

sintering the mixture;

wherein:

M is Ce, Sm, Eu, Yb, or Dy;

an amount of M is 0.06 mol % relative to the total moles of Al and Si; and

x is 0.5≦x≦0.7.

2. The method of claim 1 , wherein sintering is conducted at a temperature of 1000° C. to 1800° C.

3. The method of claim 1 , wherein sintering is conducted at a temperature of 1100° C. to 1700° C.

4. The method of claim 1 , wherein sintering is conducted at a temperature of 1200° C. to 1600° C.

5. The method of claim 1 , wherein sintering is conducted from 1 to 10 hours.

6. The method of claim 1 , wherein the sintering is conducted under vacuum, in a nitrogen atmosphere, in an air atmosphere, or in a hydrogen atmosphere.

7. The method of claim 1 , wherein the oxide is prepared from a sol-gel.

8. The method of claim 1 , wherein the oxide is a mullite of formula 3Al 2 O 3 .2SiO 2 , 3Al 2 O 3 .1.75SiO 2 , or 3Al 2 O 3 .1.55SiO 2 .

9. The method of claim 1 , wherein the source of the activating element M is an oxide, hydroxide, chloride, fluoride, carbonate, sulfate, nitrate, or acetate of M.

10. The method of claim 1 , wherein the activating element is Ce or Eu.

11. The method of claim 1 further comprising preparing the oxide by mixing tetraethyl orthosilicate with aluminum nitrate and ammonium hydroxide in ethanol to form a first mixture; heating the first mixture;

removing the solvent to form an amorphous gel; and sintering the amorphous gel to provide a precursor to the oxide of formula (Al 2 O 3 ) x .(SiO 2 ) 1-x .

12. The method of claim 11 , wherein the precursor to the oxide is a mullite precursor.

13. The method of claim 1 , wherein the mixing is conducted in the presence of ethanol.

14. The method of claim 1 , wherein the source of the activating element M is Eu 2 O 3 ; Dy 2 O 3 , Yb 2 O 3 , CeO 2 , or Sm 2 O 3 .

15. A method comprising:

preparing an oxide of formula (Al 2 O 3 ) x ).(SiO 2 ) 1-x from a sol-gel and concurrently mixing the starting materials of the oxide with the source of an activating element M; and

sintering the mixture;

wherein:

M is Ce, Sm, Eu, Yb, or Dy;

an amount of M is 0.06 mol % relative to the total moles of Al and Si; and

x is 0.5≦x≦0.7.

16. The method of claim 15 , wherein the oxide is a mullite of formula 3Al 2 O 3 .2SiO 2 , 3Al 2 O 3 .1.75SiO 2 , or 3Al 2 O 3 .1.5SiO 2 .

17. The method of claim 15 , wherein the source of the activating element M is an oxide, hydroxide, chloride, fluoride, carbonate, sulfate, nitrate, or acetate of M.

18. The method of claim 15 , wherein the source of the activating element M is Eu 2 O 3 ; Dy 2 O 3 , Yb 2 O 3 , CeO 2 , or Sm 2 O 3 .

19. The method of claim 15 , wherein the oxide is prepared by mixing tetraethyl orthosilicate with aluminum nitrate and ammonium hydroxide in ethanol to form a first mixture; heating the first mixture; removing the solvent to form an amorphous gel; and sintering the amorphous gel to provide a precursor to the oxide of formula (Al 2 O 3 ) x .(SiO 2 ) 1-x .

Assignments (3)
RELEASE OF SECURITY INTEREST Recorded Jul 31, 2019
From: CRESTLINE DIRECT FINANCE, L.P.
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 049924/0794 →
SECURITY INTEREST Recorded Jan 29, 2019
From: EMPIRE TECHNOLOGY DEVELOPMENT LLC
To: CRESTLINE DIRECT FINANCE, L.P.
Reel/Frame 048373/0217 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 5, 2012
From: OTA, MASATO
To: SHIBAURA INSTITUTE OF TECHNOLOGY
Reel/Frame 029241/0810 →