Controlled atmosphere when sintering a frit to a glass plate

• US 20090297861A1
• Filed: 05/30/2008
• Published: 12/03/2009
• Est. Priority Date: 05/30/2008
• Status: Active Grant

• Current Assignee: Corning Incorporated
• Original Assignee: Corning Incorporated
• Inventors: Banks, Andrew Douglas, Boek, Heather Debra, Howles, Jason Arthur
• Granted Patent: US 8,147,632 B2
• Time in Patent Office: Days
• US Class Current: 428/428
• CPC Class Codes: C03B 19/06 by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
• CPC Class Codes: C03C 27/06 Joining glass to glass by processes other than fusing fusing C03B23/20; units for use as elements for closing wall or like openings and comprising two or more parallel glass panes in spaced relationship, the panes being permanently secured together E06B3/66
• CPC Class Codes: C03C 3/21 containing titanium, zirconium, vanadium, tungsten or molybdenum
• CPC Class Codes: C03C 8/08 containing phosphorus
• CPC Class Codes: C03C 8/24 Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
• CPC Class Codes: H10K 50/8426 Peripheral sealing arrangements, e.g. adhesives, sealants
• CPC Class Codes: Y10T 428/131 Glass, ceramic, or sintered, fused, fired, or calcined metal oxide or metal carbide containing [e.g., porcelain, brick, cement, etc.]

Abstract

A method is described herein for controlling the oxygen level within an oven while sintering a frit to a glass plate where the sintered frit and glass plate are subsequently sealed to another glass plate to form a sealed glass package. Examples of the sealed glass package include a light-emitting device (e.g., organic light emitting diode (OLED) device), a photovoltaic device, a food container, and a medicine container.

Claims

1. A method for sintering a frit to a glass plate, said method comprising the steps of:

providing the glass plate;

depositing a frit onto the glass plate;

placing the glass plate with the deposited frit into an oven;

sintering the frit to the glass plate within the oven by;

ramping-up a temperature within the oven to a predetermined temperature, where the predetermined temperature is higher than a glass transition temperature (T_g) of a glass within the frit but less than a crystallization temperature of the glass in the frit;

holding the predetermined temperature within the oven for a predetermined time; and

maintaining an oxygen level within the oven at a predetermined level within a range of about 1,200 ppm-22,220 ppm while holding the predetermined temperature within the oven for the predetermined time; and

ramping-down a temperature within the oven; and

removing the glass plate with the sintered frit from the oven.

2. The method of claim 1, wherein said maintaining step further includes a step of selecting the predetermined oxygen level in the oven that is within the range of about 1,200 ppm-22,220 ppm based on a desired sealing power to be used in a subsequent step to seal the glass plate with the sintered frit to another glass plate to form a sealed glass package.

3. The method of claim 2, wherein said selecting step further includes a step of using a linear relationship represented by sealing power=0.4 (% O₂)+y-intercept where the y-intercept corresponds to the lowest sealing power for the lowest oxygen level when determining the predetermined oxygen level based on the desired sealing power.

4. The method of claim 1, wherein said sintering step prior to the ramping-up step further includes steps of ramping-up a temperature within the oven to a second predetermined temperature and holding the second predetermined temperature within the oven for a predetermined time, where the second predetermined temperature is high enough to volatize organic ingredients within a dispersant vehicle in the frit but not higher than a glass transition temperature (T_g) of the glass in the frit.

5. The method of claim 1, wherein the frit includes glass that is doped with at least one transition metal including iron, copper and vanadium.

6. The method of claim 1, wherein the frit includes glass that is doped with a lanthanide.

7. The method of claim 1, wherein the frit includes powdered antimony-vanadate-phosphate glass, β

-eucryptite filler, and 2,2,4-trimethyl-1,3-pentadiol monoisobutyrate dispersant vehicle.

8. A method for sealing a glass package, said method comprising the steps of:

providing a first glass plate and a second glass plate;

depositing a frit onto the first glass plate, where the frit includes a glass, a filler and a dispersant vehicle;

placing the first glass plate with the deposited frit into an oven;

sintering the frit to the first glass plate within the oven by;

ramping-up a temperature within the oven from a first temperature to a second temperature by a first ramp rate with a predetermined temperature/predetermined time;

holding the second temperature within the oven for a predetermined time, where the second temperature is high enough to volatize organic ingredients within the dispersant vehicle in the frit but not higher than a glass transition temperature (T_g) of the glass in the frit;

ramping-up a temperature within the oven from the second temperature to a third temperature by a second ramp rate with a predetermined temperature/predetermined time;

holding the third temperature within the oven for a predetermined time, where the third temperature is higher than the glass transition temperature (T_g) of the glass in the frit but less than a crystallization temperature of the glass in the frit;

maintaining an oxygen level within the oven at a predetermined level within a range of about 1,200 ppm-22,220 ppm while holding the third temperature within the oven for the predetermined time;

ramping-down a temperature within the oven from the third temperature to a fourth temperature by a third ramp rate with a predetermined temperature/predetermined time;

ramping-down a temperature within the oven from the fourth temperature to a fifth temperature by a fourth ramp rate with a predetermined temperature/predetermined time; and

removing the first glass plate with the frit from the oven;

placing the second glass plate on the frit attached to the first glass plate; and

using a sealing device at a predetermined sealing power to heat the frit such that the frit melts and forms a seal which connects the first glass plate to the second glass plate.

9. The method of claim 8, wherein said maintaining step further includes a step of selecting the predetermined oxygen level in the oven that is within the range of about 1,200 ppm-22,220 ppm based on the predetermined sealing power to be used by the sealing device to heat the frit such that the frit melts and forms the seal which connects the first glass plate to the second glass plate.

10. The method of claim 9, wherein said step of selecting further includes a step of using a linear relationship represented by sealing power=0.4 (% O₂)+y-intercept where the y-intercept corresponds to the lowest sealing power for the lowest oxygen level when determining the predetermined oxygen level based on the desired sealing power.

11. The method of claim 8, wherein said sintering step is performed in less than 8 hours.

12. The method of claim 8, wherein said sintering step is performed in less than 6 hours.

13. The method of claim 8, wherein said sintering step is performed in less than 3.5 hours.

14. The method of claim 8, wherein the oven is located in a clean room.

15. The method of claim 8, wherein the frit includes glass that is doped with at least one transition metal, where the at least one transition metal is absorbent at a specific wavelength of light which is emitted from the sealing device.

16. The method of claim 8, wherein the frit includes glass that is doped with a lanthanide, where the lanthanide is absorbent at a specific wavelength of light which is emitted from the sealing device.

17. The method of claim 8, wherein said first holding step further includes the steps of limiting an air supply and turning on a reducing-inert gas supply in which the reducing-inert gas displaces a desired amount of the air within the oven.

18. The method of claim 8, wherein said first ramping-down step further includes the step of maintaining a flow of reducing-inert gas within the oven.

19. The method of claim 8, wherein said second ramping-down step further includes the steps of turning off a reducing-inert gas supply and turning on an air supply in which air substantially displaces the reducing-inert gas within the oven.

20. The method of claim 8, wherein:

said first ramping-up step further includes turning on an air supply when the first temperature of about 25°

C. and the second temperature of about 325°

C.;

said first holding step further includes limiting the air supply after about 1 hour and turning on a reducing-inert gas supply for about 8 minutes before performing said second ramping-up step;

said second ramping-up step has the second temperature of about 325°

C. and the third temperature of about 385°

C.-415°

C.;

said second holding step further includes maintaining the flow of the reducing-inert gas to maintain the predetermined oxygen level and maintaining the third temperature of about 385°

C.-415°

C. for about 0.5-2.0 hours;

said first ramping-down step has the third temperature of about 385°

C.-415°

C. and the fourth temperature of about 300°

C.; and

said second ramping-down step further includes turning off the reducing-inert gas supply and turning on the air supply with the fourth temperature of about 300°

C. and the fifth temperature of about 60°

C.

21. The method of claim 8, wherein said sealing device is used to heat the frit in a manner where a substantially constant temperature is maintained in the frit along a sealing line while the frit melts and forms the seal which connects the first glass plate to the second glass plate.

22. The method of claim 8, further comprising the step of depositing at least one component onto the second glass plate prior to placing the second glass plate on the frit attached to the first glass plate and prior to using the sealing device to heat the frit to form the seal which connects the first glass plate to the second glass plate.

23. The method of claim 8, wherein said glass package is:

an organic light emitting diode (OLED) device a photovoltaic device;

a food container;

or

a medicine container

25. The sealed glass package of claim 23, wherein said transition metal-lanthanide doped glass frit which forms the seal has a brown color.

24. A sealed glass package comprising:

a first glass plate; and

a second glass plate, wherein the first glass plate and the second glass plate are connected to one another by a transition metal-lanthanide doped glass frit which formed a seal between the first glass plate and the second glass plate, wherein the transition metal-lanthanide doped glass frit has a predetermined color and desired oxidation state due to a using an 1,200 ppm-22,220 ppm oxygen controlled sintering process which was performed to attach the transition metal-lanthanide doped glass frit to the first glass plate before the second glass plate was placed on top of the sintered transition metal-lanthanide doped glass frit and the sintered transition metal-lanthanide doped glass frit was melted to form the seal between the first glass plate and the second glass plate.