IP Library Granted Patent US 8,518,319
Granted Patent B2
US 8,518,319 · App. 12/728,070 · Granted Aug 27, 2013

Process of making fibers by electric-field-driven spinning using low-conductivity fluid formulations

Inventors: Ashley S. Scott (Grove City, OH); Andrew L. Washington, Jr. (Pataskala, OH); John A. Robertson (Chillicothe, OH)
Assignee: Nanostatics Corporation
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Quick Facts
Patent No.
US 8,518,319
App. No.
12/728,070
Granted
Aug 27, 2013
Kind
B2
Abstract

A first method comprises: dissolving a polymer in a terpene, terpenoid, or aromatic solvent to form a polymer solution; dissolving a salt in a polar organic solvent to form a salt solution; and mixing the salt solution and the polymer solution to form a mixture. The salt and the polar organic solvent do not cause substantial precipitation of the polymer upon mixing with the polymer solution. A resulting terpene, terpenoid, or aromatic solvent phase of the mixture is suitable for forming fibers by electric-field-driven spinning from one or more spinning tips onto a target substrate. A composition comprises the terpene, terpenoid, or aromatic solvent phase of the mixture resulting from the method. A second method comprises forming fibers by electric-field-driven spinning of the first composition from one or more spinning tips onto a target substrate. A second composition comprises the fibers formed by the second method.

Claims (30)

1. A method comprising:

dissolving a polymer in a terpene, terpenoid, or aromatic solvent to form a polymer solution;

dissolving a salt in a polar organic solvent to form a salt solution;

mixing the salt solution and the polymer solution to form a mixture;

allowing a terpene, terpenoid, or aromatic solvent phase of the mixture to phase separate from the mixture;

removing the phase separated terpene, terpenoid, or aromatic solvent phase from the mixture; and

after removing the phase separated terpene, terpenoid, or aromatic solvent phase from the mixture, using the terpene, terpenoid, or aromatic solvent phase of the mixture to form fibers by electric-field-driven spinning from one or more spinning tips onto a target substrate,

wherein:

the salt and the polar organic solvent do not cause substantial precipitation of the polymer upon mixing with the polymer solution;

the terpene, terpenoid, or aromatic solvent phase of the mixture has an electrical conductivity less than 100 μS/cm; and

the terpene, terpenoid, or aromatic solvent phase of the mixture is suitable for forming the fibers by electric-field-driven spinning from the one or more spinning tips onto the target substrate.

2. The method of claim 1 wherein the polymer comprises polystyrene.

3. The method of claim 1 wherein the terpene, terpenoid, or aromatic solvent comprises D-limonene, p-cymene, terpinene, or terpinolene.

4. The method of claim 1 wherein the polar organic solvent comprises one or more of dimethyl formamide, methyl ethyl ketone, or N-methyl-2-pyrrolidone.

5. The method of claim 1 wherein the polar organic solvent includes a solvent having a dielectric constant greater than about 15.

6. The method of claim 1 wherein the polar organic solvent includes a solvent having a dielectric constant greater than about 30.

7. The method of claim 1 wherein the salt comprises an inorganic salt, an ionic liquid, or an ionic surfactant.

8. The method of claim 1 wherein the salt comprises a quaternary ammonium salt, an imidazolium salt, LiCl, AgNO 3 , CuCl 2 , or FeCl 3 .

9. The method of claim 1 wherein the polymer comprises polystyrene, the terpene, terpenoid, or aromatic solvent comprises D-limonene, the polar organic solvent comprises dimethyl formamide, and the salt comprises cetyl-trimethyl-ammonium bromide, 1-butyl-3-methyl-imidazolium hexafluorophosphate, LiCl, AgNO 3 , CuCl 2 , or FeCl 3 .

10. The method of claim 1 wherein the terpene, terpenoid, or aromatic solvent phase of the mixture has a viscosity less than about 1000 centipoise.

11. The method of claim 1 wherein the polymer solution is between about 15% and about 40% by weight of the polymer, the salt solution is between about 0.02% and about 5% by weight of the salt, and the mixture has a mole ratio between about 2:1 and about 1:4 of the polar organic solvent to the terpene, terpenoid, or aromatic solvent in the mixture.

12. The method of claim 1 wherein the spinning tips and the terpene, terpenoid, or aromatic solvent phase of the mixture are electrically isolated from a voltage source that drives the electric-field-driven spinning.

13. The method of claim 1 wherein the spinning tips or the terpene, terpenoid, or aromatic solvent phase of the mixture are in electrical contact with a voltage source that drives the electric-field-driven spinning.

14. The method of claim 1 wherein the target substrate is electrically insulating.

15. The method of claim 1 wherein the target substrate is electrically isolated.

16. The method of claim 1 wherein the terpene, terpenoid, or aromatic solvent phase of the mixture has an electrical conductivity less than about 75 μS/cm.

17. The method of claim 1 wherein the terpene, terpenoid, or aromatic solvent phase of the mixture has an electrical conductivity less than about 50 μS/cm.

18. The method of claim 1 wherein the terpene, terpenoid, or aromatic solvent phase of the mixture has an electrical conductivity less than about 20 μS/cm.

19. The method of claim 1 wherein the fibers formed have an average diameter less than about 500 nm.

20. The method of claim 1 wherein a magnitude of electrical current carried by the formed fibers is less than about 0.3 μA per spinning tip.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 6, 2017
From: NANOSTATICS CORPORATION
To: DROPLETECH, LLC
Reel/Frame 042920/0172 →
RELEASE OF SECURITY INTEREST Recorded Jun 29, 2015
From: INDEPENDENCE EQUITY I, LP
To: NANOSTATICS CORPORATION
Reel/Frame 035930/0729 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 10, 2013
From: SCOTT, ASHLEY S.; ROBERTSON, JOHN A.; WASHINGTON, ANDREW L., JR.
To: NANOSTATICS CORPORATION
Reel/Frame 030782/0734 →
SECURITY AGREEMENT Recorded May 11, 2012
From: NANOSTATICS CORPORATION
To: INDEPENDENCE EQUITY I, LP
Reel/Frame 028194/0792 →
Continuity (3)
Provisional Application 61161498 · Mar 19, 2009
Provisional Application 61256873 · Oct 30, 2009
Related Publication 20100239861A1 · Sep 23, 2010