Low temperature joining of phosphate glass

• US 6,652,972 B1
• Filed: 11/01/1999
• Issued: 11/25/2003
• Est. Priority Date: 11/01/1999
• Status: Expired due to Fees

• Current Assignee: Schott Glass Technologies, Inc.
• Original Assignee: Schott Glass Technologies, Inc.
• Inventors: Conzone, Samuel, Marker, Alexander J., Hayden, Joseph S.
• Primary Examiner(s): Jones, Deborah
• Assistant Examiner(s): Piziali, Andrew T
• Application Number:
  US09/430,885
• Time in Patent Office: 1,485 Days
• Field of Search: 428/426, 428/428, 428/432, 428/446, 428/448, 428/688, 428/689, 428/697, 428/702, 428/704, 156/99, 156/104, 156/106, 427/164, 427/165
• US Class Current: 428/426
• 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 3/17 containing aluminium or beryllium
• CPC Class Codes: C03C 4/0071 for laserable glass
• CPC Class Codes: G02B 6/12 of the integrated circuit kind electric integrated circuits H01L27/00
• CPC Class Codes: G02B 6/12002 Three-dimensional structures
• CPC Class Codes: G02B 6/13 Integrated optical circuits characterised by the manufacturing method
• CPC Class Codes: G02B 6/30 for use between fibre and thin-film device

Abstract

A method for the low temperature joining of similar and/or different phosphate glass by mating at low temperature glass components by an aqueous solution containing phosphorus. In preferred embodiments, the phosphate glasses are polished, cleaned, and brought together with the phosphate-containing solution between the polished surfaces. Vacuum may be applied to assist in making the joint. The composite is optionally heat treated to increase strength, chemical durability, and optical performance. The bond thereby formed has low birefringence, is strong, and is virtually photonically invisible. The joints now make possible, for example, substrates for virtually no loss signal splitters and other high-end optical components at low cost. Large hybrid performs substrates composed of multiple glass components may be prepared and segmented, providing an inexpensive novel substrate for the photonics industry. Active lasing phosphate glasses may be joined by the present invention method to passive non-lasing glasses for use in laser and related applications.

Claims

1. A glass composite comprising:

a first phosphate glass surface;

a second phosphate glass surface; and

between and in contact with both of said surfaces, a phosphorus-containing solution which is liquid at room temperature.

2. A glass composite as claimed in claim 1, wherein the phosphorus-containing solution is an aqueous solution.

8. A glass composite as claimed in claim 1, wherein the solution is acidic.

9. A glass composite as claimed in claim 1, wherein the solution is basic.

10. A glass composite as claimed in claim 9, wherein the solution contains alkali or alkaline earth elements.

11. A glass composite as claimed in claim 8, wherein the solution contains phosphoric acid.

12. A glass composite as claimed in claim 1, wherein the solution comprises:

water in an amount of from about 15-99.9 weight %,

phosphorus in an amount equivalent to about 0.1-85 weight % P₂O₅.

13. A glass composite as claimed in claim 11, wherein the solution comprises

water in an amount of from about 50-90 weight %,

phosphorus in an amount equivalent to about 5-35 weight % P₂O₅

Na₂O in a amount of from about 1-20 weight %,

K₂O in an amount of from about 1-20 weight %,

Al₂O₃ in an amount of from about 0-5 weight %, and

SiO₂ in an amount of from about 0-15 weight %.

14. A glass composite as claimed in claim 11, wherein the solution comprises

water in an amount of from about 70-90 weight %,

phosphorus in an amount equivalent to about 10-30 weight % P₂O₅

Na₂O in a amount of from about 1-20 weight %, and

SiO₂ in an amount of from about 0-8 weight %.

35. A composite of claim 1, wherein said phosphorus-containing solution consists essentially of an aqueous solution.

36. A composite of claim 1, wherein said phosphorus-containing solution consists of an aqueous solution.

3. A glass composite comprising:

a first phosphate glass surface;

a second phosphate glass surface; and

between and in contact with said surfaces, a phosphorus-containing solution which is an aqueous solution of phosphoric acid.

4. A glass composite as claimed in claim 3, wherein the aqueous solution of phosphoric acid contains phosphorus equivalent to an amount of from 0.1 to 85 weight % of P₂O₅.

5. A glass composite as claimed in claim 4, wherein the aqueous solution of phosphoric acid contains phosphorus equivalent to an amount of from 0.1 to 30 weight % of P₂O₅.

6. A glass composite as claimed in claim 5, wherein the aqueous solution of phosphoric acid contains phosphorus equivalent to an amount of from 0.1 to 20 weight % of P₂O₅.

7. A glass composite as claimed in claim 6, wherein the aqueous solution of phosphoric acid contains phosphorus equivalent to an amount of from 10-20 weight % of P₂O₅.

15. A glass composite comprising:

a first phosphate glass interface;

a second phosphate glass interface; and

between and in contact with both of said interfaces, a layer comprising a cured phosphorus containing solution which was liquid at room temperature.

16. A glass composite comprising:

a first phosphate glass interface;

a second phosphate glass interface; and

between and in contact with both of said interfaces, a condensed phosphate layer that links the two interfaces and was formed from a phosphorous containing solution which was liquid at room temperature.

17. A glass composite as claimed in claim 16, wherein the condensed phosphate layer is a —

P—

O—

P—

O—

P—

layer.

18. A glass composite prepared by joining two phosphate glass substrates together by curing therebetween, and in contact with both of said substrates, a phosphorus-containing aqueous solution.

37. A glass composite of claim 18 wherein said solution is liquid at room temperature.

19. A method of bonding two phosphate glass surfaces comprising curing therebetween, and in contact with both of said surfaces, a phosphorus-containing aqueous solution.

20. A method as claimed in claim 19, further comprising a subsequent heat treatment.

21. A method as claimed in claim 20, wherein the heat treatment occurs at a temperature below the glass transition temperature of each phosphate glass surface.

22. A method as claimed in claim 20, wherein the heat treatment occurs at a temperature of from about 60°

C. to about 550°

C.

23. A method as claimed in claim 22, wherein the heat treatment occurs at a temperature of from about 100°

C. to about 500°

C.

24. A method as claimed in claim 23, wherein the heat treatment occurs at a temperature of from about 200°

C. to about 400°

C.

25. A method as claimed in claim 24, wherein the heat treatment occurs at a temperature of from about 350°

C. to about 400°

C.

26. A method as claimed in claim 19, wherein the curing is conducted for at least three days followed by a heat treatment.

27. A method as claimed in claim 19, wherein the curing is conducted for about a week.

28. A method as claimed in claim 27, wherein the curing is followed by a heat treatment.

29. A method as claimed in claim 19, wherein the two phosphate glass surfaces each have surface features equal to or less than 200 nm in height.

30. A method as claimed in claim 29, wherein the two phosphate glass surfaces are each polished.

38. A method of claim 19 wherein said solution is liquid at room temperature.

31. In a photonic device comprising a phosphate glass component, the improvement wherein said phosphate glass component is a glass composite comprising:

a first phosphate glass surface;

a second phosphate glass surface; and

between and in contact with said surfaces, a phosphorus-containing solution, which is an aqueous solution,

and wherein said aqueous solution has been cured.

32. A photonic device as claimed in claim 31, wherein the photonic device is a multiple-wavelength laser array.

33. A photonic device as claimed in claim 32, wherein the photonic device is a low-loss splitting device.

34. A photonic device as claimed in claim 33, wherein the photonic device is a self-cooling laser.