Sol-gel doping of optical fiber preform

• US 5,123,940 A
• Filed: 04/12/1991
• Issued: 06/23/1992
• Est. Priority Date: 02/23/1990
• Status: Expired due to Term

• Current Assignee: Fitel USA Corporation
• Original Assignee: AT&T, Inc.
• Inventors: DiGiovanni, David J., MacChesney, John B.
• Primary Examiner(s): Jones, W. Gary
• Assistant Examiner(s): BRUCKNER, JOHN
• Application Number:
  US07/684,624
• Time in Patent Office: 438 Days
• Field of Search: 65/3.11, 65/3.12, 65/18.2, 65/60.52, 65/901, 65/18.1, 501/12
• US Class Current: 65/395
• CPC Class Codes: C03B 2201/06 Doped silica-based glasses
• CPC Class Codes: C03B 2201/34 doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
• CPC Class Codes: C03B 2201/36 doped with rare earth metals and aluminium, e.g. Er-Al co-doped
• CPC Class Codes: C03B 2201/42 doped with titanium
• CPC Class Codes: C03B 37/01838 for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the deposited glass
• CPC Class Codes: C03C 1/008 for the production of films or coatings
• CPC Class Codes: Y02P 40/57 Improving the yield, e-g- reduction of reject rates
• CPC Class Codes: Y10S 65/901 Liquid phase reaction process

Abstract

The method includes collapsing a silica-based glass tube to make a preform and drawing fiber from the preform. Prior to collapsing the tube, one or more glass layers are formed on the inner surface of the tube by dip-coating the surface with a sol comprising a metal alkoxide dissolved in an alcoholic or aqueous solvent, polymerizing the sol to form a gel, and drying and sintering the gel. A substantial portion the dopant, present within the sintered gel, diffuses into at least one adjoining glass region. A wide selection of dopant materials, in the form of salts or alkoxides, are readily incorporated by dissolving them in the solvent.

Claims

1. A method for manufacturing an optical fiber, comprising the steps of:

providing a tube which comprises fused glass and has an inner surface;

processing the tube such that a preform is created, the preform comprising a solid, glass rod and including a finished doped layer which has a final thickness; and

drawing fiber from the preform, wherein the processing step comprises the further steps of;

a) providing a sol or solution which comprises a solvent and at least one polymerizable, glass-forming material, the sol or solution being capable of polymerization with respect to at least one of its components, the sol or solution further comprising, dissolved in the solvent, at least one dopant element in the form of a salt or alkoxide;

b) inducing or permitting the sol or solution to begin polymerizing;

c) applying the sol or solution to the tube inner surface before the polymerization of the sol or solution is complete, such that a thin, adherent film is formed;

d) substantially completing the polymerization of the sol or solution;

e) drying the thin, adherent film, whereby a thin layer of dried gel is formed;

f) sintering the dried gel such that an adherent, thin, glass layer which has an intermediate thickness is formed;

g) optionally forming at least one additional glass layer overlying the layer of step (f); and

h) collapsing the tube such that;

i) during the collapsing step, a substantial portion of the dopant element diffuses out of the layer of step (f) into at least one adjoining glass region, resulting in formation of the finished doped layer;

ii) the final thickness is at least twice the intermediate thickness and iii) a concentration of said dopant is at least half maximum at a midpoint between said intermediate thickness and said final thickness.

2. The method of claim 1, wherein the polymerizable, glass-forming material is a glass-forming metal alkoxide, and the solvent comprises water and/or an alcohol.

3. The method of claim 2, wherein the metal alkoxide further comprises an element selected from the group consisting of silicon, germanium, aluminum, and titanium.

4. The method of claim 2, wherein the metal alkoxide is chosen from the group consisting of tetraethyl orthosilicate, tetramethyl orthosilicate, tetrapropyl orthosilicate, silicon methoxide, aluminum 2-propoxide, aluminum butoxide, titanium ethoxide, germanium ethoxide, germanium propoxide, germanium butoxide, and germanium pentoxide.

5. The method of claim 1, wherein the salt or alkoxide comprises a salt of a rare earth element.

6. The method of claim 5, wherein the salt of a rare earth element is selected from the group consisting of erbium trichloride and neodymium trichloride.

7. The method of claim 1, further comprising, before step (c), the step of vapor-depositing at least one glass vapor-deposited layer on the inner surface of the tube, and wherein during step (h), a substantial portion of the dopant element diffuses into the vapor-deposited layer.

8. The method of claim 7, wherein the vapor-deposited layer is a core layer.

9. The method of claim 7, wherein the vapor-deposited layer is a cladding layer.

10. The method of claim 7, wherein the vapor-depositing step comprises depositing a cladding layer by MCVD.

11. The method of claim 10, wherein the vapor-depositing step further comprises depositing a core layer by MCVD.

12. The method of claim 10, wherein the vapor-depositing step further comprises depositing a porous MCVD soot layer on the inner surface of the MCVD cladding layer, and step (c) comprises soaking the sol or solution into the soot layer.

13. The method of claim 1, wherein step (g) comprises vapor-depositing at least one glass vapor-deposited layer on the layer of step (f) , and wherein during step (h), a substantial portion of the dopant element diffuses into the vapor-deposited layer.

14. The method of claim 13, wherein the vapor-deposited glass layer is a cladding layer.

15. The method of claim 1, further comprising the step of dehydrating the dried gel.

16. The method of claim 1, wherein the dopant element is a refractive index raising element.

17. The method of claim 16, wherein the refractive index raising element is selected from the group consisting of aluminum, germanium, phosphorus, zirconium and titanium.

18. The method of claim 1, wherein the dopant element is a transition metal.

19. The method of claim 1, wherein, during step (c), the viscosity of the sol or solution is less than about 20 centipoise.

20. The method of claim 1, wherein step (f) results in the formation of a glass layer about 0.3 μ

m thick.

21. The method of claim 1, further comprising, after step (e) and before step (f), the step of heating the dried gel to about 500°

C., and applying the sol or solution to the tube inner surface at least one additional time.

22. The method of claim 1, wherein step (c) comprises applying the sol or solution by dip coating.