IP Library Granted Patent US 9,321,675
Granted Patent B2
US 9,321,675 · App. 13/617,293 · Granted Apr 26, 2016

Fabrication of porous glass bioscaffolds by sol-gel and polymer sponge methods

Inventor: Himanshu Jain (Bethlehem, PA)
Assignee: Lehigh University
C03C11/00C03B19/06C03B19/12C03C1/006C03C3/078C03C4/0007C04B35/622C04B38/0625C04B2111/00836C04B2235/36C04B2235/616
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Quick Facts
Patent No.
US 9,321,675
App. No.
13/617,293
Granted
Apr 26, 2016
Kind
B2
Abstract

Provided herein are biocompatible scaffolds and methods of preparing such bioscaffolds. The methods provide a superior high surface area, interconnected nanomacroporous bioactive glass scaffold, by combining a sol-gel process and polymer sponge replication methods. The formation of a uniformly nanoporous and interconnected macroporous bioscaffold is demonstrated using a starting material comprising a 70 mol % SiO2—30 mol % CaO glass composition as an example. The bioscaffold includes a series of open, interconnected macropores with size from 300 to 600 μm, as desired for tissue ingrowth and vascularization. At the same time, coexisting nanopores provide high-specific surface area (>150 m2/g), which is needed for enhancing the structure's degradation rate. These bioscaffolds hold promise for applications in hard tissue engineering.

Claims (27)

1. A method of producing a biocompatible scaffold, the method comprising the steps of:

a) infiltrating a sponge template with a slurry composition, the slurry composition comprising at least one glass precursor material, wherein the glass precursor material comprises at least one nanoporous xerogel glass powder;

b) optionally removing excess slurry from the sponge template; and

c) heating the sponge template to a temperature and for a time sufficient to convert the slurry composition into the biocompatible scaffold comprising at least a glass, the scaffold comprises interconnected macropores, and interconnected nanopores, wherein the nanopores have an average diameter less than about 100 nm.

2. The method of claim 1 , wherein the nanoporous xerogel glass powder is made by a sol-gel process.

3. The method of claim 2 , wherein the xerogel glass powder comprises particles comprising about 70 mol % SiO 2 and about 30 mol % CaO.

4. The method of claim 1 , wherein the slurry composition further comprises an aqueous medium, containing about 1 wt % of a binder and about 0.5 wt % of a dispersant.

5. The method of claim 1 , wherein the series of interconnected macropores comprise macropores and interconnections each having an average diameter of between about 300 to about 600 μm.

6. The method of claim 1 , wherein the scaffold has a specific surface area that is between about 50 to about 160 m 2 /g.

7. The method of claim 1 , wherein the step of providing a slurry composition comprising at least one glass precursor material further comprises preparing the slurry composition by adding about 25 wt % of dried xerogel powder to about 75 wt % aqueous medium, the medium optionally further comprising about 1 wt % binder and about 0.5 wt % dispersant.

8. The method of claim 1 , wherein the optional step of adjusting the amount of the slurry composition in the sponge to a desired amount comprises at least one of wringing, squeezing, compressing, or drying the sponge.

9. The method of claim 8 , wherein step of adjusting the amount of the slurry composition in the sponge comprises drying the sponge by a temperature at least about 200 degrees below the glass transition temperature of the glass precursor material.

10. The method of claim 1 , wherein the step of heating the soaked sponge for a time sufficient at a temperature comprises gradually heating by increasing the temperature by less than about 5° C. per minute up to a desired temperature sufficient to convert the composition to yield a scaffold, wherein said heating thermally degrades the sponge.

11. The method of claim 10 , further comprising the step of sintering the scaffold at a time and temperature sufficient to produce a hardened, stabilized scaffold.

12. The method of claim 11 , wherein the step of sintering is performed at a temperature of at least about 700° C.

13. The method of claim 12 , wherein the step of sintering is performed by increasing the temperature from the desired temperature of claim 12 up to the sintering temperature at a rate of about rate 2° C. per minute.

14. The method of claim 13 , wherein the step of sintering comprises holding the sintering temperature for at least about 2 hours, before cooling down to room temperature.

15. The method of claim 1 , wherein the step of providing a slurry composition comprising at least one glass precursor material further comprises the steps of:

a) dissolving calcium nitrate tetrahydrate (Ca(NC 3 ) 2 .4H 2 O) in a catalyst solution;

b) adding tetramethylorthosilicate (TMOS) to the acetic acid solution;

c) stirring, followed by aging at 40° C. to yield a gelled sample;

d) crushing and drying the gelled samples to yield xerogel particles;

e) grinding the xerogel particles in an attrition mill with a solvent to form a fine xerogel powder; and

f) optionally, drying the fine xerogel powder for use in preparing the slurry composition.

16. The method of claim 15 , wherein the catalyst solution comprises at least one of an acid or a base.

17. The method of claim 15 , wherein the step of attrition milling comprises using Y 2 O 3 -stabilized ZrO 2 milling media and a solvent.

18. The method of claim 15 , wherein the step of adding TMOS comprises accomplishing a molar ratio of TMOS to Ca(NO 3 ) 2 4H 2 O of about 7:3.

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 12, 2016
From: WANG, SHAOJIE
To: LEHIGH UNIVERSITY
Reel/Frame 039669/0979 →
CONFIRMATORY LICENSE Recorded Apr 7, 2016
From: LEHIGH UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 038380/0308 →
CONFIRMATORY LICENSE Recorded Oct 2, 2015
From: LEHIGH UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 036745/0869 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 1, 2014
From: JAIN, HIMANSHU
To: LEHIGH UNIVERSITY
Reel/Frame 033860/0616 →
CONFIRMATORY LICENSE Recorded Jul 29, 2014
From: LEHIGH UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 033433/0291 →
Continuity (3)
Continuation PCTUS2011028695 · Mar 16, 2011
Provisional Application 61314377 · Mar 16, 2010
Related Publication 20140075993A1 · Mar 20, 2014