IP Library Granted Patent US 12,313,813
Granted Patent B2
US 12,313,813 · App. 18/078,156 · Granted May 27, 2025

Molten core flux formation method and fibers formed therefrom

Inventors: John Ballato (Clemson, SC); Thomasina Zaengle (Clemson, SC); Baris Kukuoz (Anderson, SC); Ursula Gibson (Hanover, NH)
Assignee: Clemson University Research Foundation
G02B1/02C03C27/00G02B6/02
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Quick Facts
Patent No.
US 12,313,813
App. No.
18/078,156
Granted
May 27, 2025
Kind
B2
Abstract

Disclosed are methods for formation of a fiber and fibers that can be formed according to the methods. Formation methods incorporate a “molten core flux method” whereby a solid primary core material is combined with a solid secondary flux material in a multi-phase preform core. In some embodiments, the multi-phase preform core has a liquidus temperature that is reduced relative to the melting temperature of at least the primary core material. A homogeneous liquid melt of the preform core can exhibit a sufficiently low vapor pressure such that a fiber preform incorporating the materials in the core can be thermally drawn. Upon cooling and solidification of the homogeneous core melt, separation of the core components can occur via recrystallization, with one phase being that of the desired primary core material. Methods can be particularly beneficial for forming fibers incorporating high vapor pressure semiconductor materials, e.g., ZnSe or GaAs, in the fiber core.

Claims (23)

1. A method for forming a fiber comprising:

combining a first solid phase that includes a primary core material with a second solid phase acting as a flux material to form a multi-phase preform core;

thermally drawing the preform at drawing conditions to form a fiber, the preform including the multi-phase preform core within a preform glass cladding, wherein the drawing conditions include a drawing temperature that is lower than a melting temperature of the primary core material at the drawing conditions and that is at or higher than the melting temperature of the multi-phase preform core at the drawing conditions, wherein at the drawing temperature the multi-phase preform core becomes a homogeneous melt; and

cooling the thermally drawn fiber, wherein upon the cooling, the homogeneous melt solidifies to form a fiber core.

2. The method of claim 1 , wherein the primary core material comprises a semiconductor material.

3. The method of claim 1 , wherein the flux material comprises one or more metals in either elemental or a compound form.

4. The method of claim 1 , wherein the flux material comprises one or more semiconductors in either elemental or a compound form.

5. The method of claim 1 , wherein the multi-phase preform core comprises a powder or particle mixture.

6. The method of claim 1 , wherein the multiphase preform core comprises a multi-phase solid.

7. The method of claim 1 , wherein the fiber core that includes a third solid phase that includes the primary core material and a fourth solid phase that includes the flux material or a reaction product of the flux material.

8. The method of claim 7 , further comprising thermal treatment of the fiber, such thermal treatment comprising spatially segregating the third solid phase and the fourth solid phase within the fiber core.

9. The method of claim 1 , wherein the draw temperature is from about 10° C. to about 600° C. above a liquidus temperature of the multi-phase preform core at the drawing conditions.

10. The method of claim 1 , wherein the draw temperature is from about 700° C. to about 1200° C.

11. The method of claim 1 , wherein the drawing conditions comprise atmospheric pressure.

12. The method of claim 1 , wherein the drawing conditions comprise a reducing atmosphere or an inert atmosphere.

13. The method of claim 1 , further comprising performing post-formation processing of the fiber.

14. The method of claim 13 , the processing comprising thermal treatment or coating the fiber.

15. A thermally drawn fiber formed in accordance with the method of claim 1 .

16. The thermally drawn fiber of claim 15 , wherein the primary core material comprises a crystalline primary core material which comprises one of a semiconductor material, a high vapor pressure material, or a dopant.

17. The thermally drawn fiber of claim 15 , wherein the primary core material comprises a crystalline primary core material which comprises an arsenide, selenide, sulfide, phosphide, telluride, oxide, or any combination thereof.

18. The thermally drawn fiber of claim 15 , wherein the primary core material comprises a crystalline primary core material which comprises gallium arsenide, indium phosphate, cadmium sulfide, cadmium selenide, cadmium oxide, zinc sulfide, zinc selenide, zinc telluride, zinc oxide, lead sulfide, lead selenide, lead telluride, indium selenide, indium (II) selenide, copper indium selenium, bismuth selenide, indium arsenide, indium gallium arsenide, silicon germanium, mercury sulfide, mercury selenium, mercury telluride, or any combination thereof.

19. The thermally drawn fiber of claim 15 , wherein the flux material comprises one or more metals comprising tin, gold, copper, gallium, antimony, silicon, germanium, bismuth, silver, cadmium, lead, indium, selenium, manganese, or nickel, in elemental or compound form.

20. The thermally drawn fiber of claim 15 , the glass cladding comprises a silica (SiO2), a silicate, a borosilicate, a phosphate, a chalcogenide, or a germanate, wherein the clad optionally includes a dopant.

Assignments (3)
CONFIRMATORY LICENSE Recorded Feb 3, 2025
From: CLEMSON UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 070085/0469 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 27, 2023
From: BALLATO, JOHN; ZAENGLE, THOMASINA; GIBSON, URSULA
To: CLEMSON UNIVERSITY
Reel/Frame 064400/0178 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 27, 2023
From: CLEMSON UNIVERSITY
To: CLEMSON UNIVERSITY RESEARCH FOUNDATION
Reel/Frame 064400/0470 →
Continuity (2)
Provisional Application 63288925 · Dec 13, 2021
Related Publication 20230184997A1 · Jun 15, 2023
References Cited (1)
US 9632245B2 · Wang · 2017 [cited by examiner]