Fabrication of nanoporous glass fiber for flexible bioscaffolds and other products

Patent metadata

Field	Value
Publication number	US-9701566-B2
Application number	US-201113273577-A
Country	US
Kind code	B2
Filing date	Oct 14, 2011
Priority date	Oct 14, 2010
Publication date	Jul 11, 2017
Grant date	Jul 11, 2017

Abstract

Provided herein are novel nanoporous glass fibers, and methods of preparing and using such fibers. In some embodiments, articles are made from particular glass starting materials, such as soda-lime phosphosilicate glass fabricated by melt-quench methods. The articles include nanoporous fibers that can be used alone, or sewn, woven, bundled, and otherwise incorporated to form nanoporous articles, including bioactive articles.

First claim

The invention claimed is:

1. A method of making a nanoporous ceramic material comprising steps of:
drawing a melt composition to form at least one fiber of a phospho-silicate glass having essentially no spinodal phase separation;
heating the fiber to a temperature sufficient to convert at least a portion of the phospho-silicate glass to an amorphous ceramic with spinodal phase separation of at least two phases; and
removing at least a portion of one of the at least two phases from the fiber, thereby producing a biocompatible fiber with interconnected nanoporosity.

2. The method of claim 1 wherein said phospho-silicate glass has the formula 20.9Na 2 O-7.1K 2 O-18CaO-2P 2 O 5 -52SiO 2 (mol %).

3. The method of claim 1 wherein said removing comprises selectively leaching said one of said at least two phases.

4. The method of claim 1 , wherein said biocompatible fiber is characterized by the absence of pores greater than about 60 nm.

5. The method of claim 4 , wherein said biocompatible fiber is characterized by an average pore diameter of less than about 20 nanometers.

6. The method of claim 1 , wherein the fiber has an average diameter of about 100 to about 150 μm.

7. The method of claim 1 , wherein the biocompatible fiber has a pore volume of about 40% to about 68% of the fiber volume.

8. A method of making a nanoporous fiber comprising glass material, the method comprising the steps of:
heating a starting material comprising a phospho-silicate glass to form a melt;
drawing the melt to form at least one fiber;
heat treating the at least one fiber to form an amorphous heat-treated fiber with spinodal phase separation of at least two phases; and
removing at least a portion of one of the at least two phases from the at least one heat-treated fiber, thereby producing a biocompatible fiber with interconnected nanoporosity having pores no greater than about 60 nm.

9. The method according to claim 8 , wherein the starting material comprises a glass of the formula 20.9Na 2 O-7.1K 2 O-18CaO-2P 2 O 5 -52SiO 2 (mol %).

10. The method according to claim 9 , wherein the step of heat treating comprises heating at a temperature of between about 600 to about 1100 degrees C. for a time of between about 45 minutes to about 1.5 hours.

11. The method of claim 9 , wherein said removing comprises selectively leaching said one of said at least two phases.

12. The method according to claim 11 , wherein the leaching solution has a pH of less than about 7, and wherein the leaching solution comprises an inorganic mineral acid.

13. The method according to claim 12 , wherein the leaching solution is a 1N HCl solution.

14. The method according to claim 11 , wherein the leaching step is carried out for about 1 h in 1N HCl at between about 55 to about 75 degree C.

15. The method of claim 11 , wherein the step of leaching is performed for a time sufficient to produce nanopores t comprising between about 40% to about 68% of the fiber by volume.

16. The method according to claim 8 , wherein the nanoporous fiber comprises nanopores having an average pore diameter of less than about 30 nanometers.

17. A method of making a nanoporous ceramic material comprising steps of:
providing a melt composition for forming a phospho-silicate glass;
drawing a phospho-silicate glass melt composition to form at least one fiber;
heating the fiber to a form a ceramic with interconnected spinodal phase separation having at least two phases; and
leaching the fiber to remove one of said at least two phases, thereby producing a nanoporous fiber having no pores larger than about 60 nm, wherein said nanoporous fiber is biocompatible.

18. The method of claim 17 wherein said phospho-silicate glass has the formula 20.9Na 2 O-7.11K 2 O-18CaO-2P 2 O 5 -52SiO 2 (mol %).

19. A method of making a nanoporous ceramic material comprising steps of:
drawing a melt composition in air to solidify said melt composition at a first temperature to form at least one fiber of a phospho-silicate glass;
heating the fiber to a second temperature greater than said first temperature to convert at least a portion of the phospho-silicate glass to an amorphous ceramic with spinodal phase separation of at least two phases; and
removing at least a portion of one of the at least two phases from the fiber, thereby producing a biocompatible fiber with interconnected nanoporosity.

20. The method of claim 19 , wherein said second temperature is at least 600 C.

21. The method of claim 19 , wherein said first temperature is room temperature.

22. The method of claim 19 , wherein said phospho-silicate glass has the formula 20.9Na 2 O-7.1K 2 O-18CaO-2P 2 O 5 -52SiO 2 (mol %).

Assignees

• Moawad Hassan M M
• Jain Himanshu
• Univ Lehigh

Inventors

• Moawad Hassan M M
• Jain Himanshu

Classifications

• C03C13/006

  Glass-ceramics fibres · CPC title

• Y10T428/2975

  Tubular or cellular · CPC title

• C03C25/66

  Chemical treatment, e.g. leaching, acid or alkali treatment (dehydroxylation C03C25/64) · CPC title

• C03B37/022 Primary

  from molten glass in which the resultant product consists of different sorts of glass or is characterised by shape, e.g. hollow fibres {, undulated fibres, fibres presenting a rough surface (C03B37/025 takes precedence)} · CPC title

• C03C4/0007

  for biologically-compatible glass · CPC title