Heated solution electrospinning

Patent metadata

Field	Value
Publication number	US-12540420-B2
Application number	US-202318500960-A
Country	US
Kind code	B2
Filing date	Nov 2, 2023
Priority date	Nov 2, 2023
Publication date	Feb 3, 2026
Grant date	Feb 3, 2026

Abstract

Certain aspects of the disclosure concern a device including a nozzle configured to receive a heated polymer solution from a reservoir and a power supply configured to generate an electrostatic field between a tip portion of the nozzle and a substrate so as to draw a charged jet of the heated polymer solution out of the tip portion of the nozzle toward a substrate situated at an operating distance from the tip portion of the nozzle and form a polymer fiber on the substrate. The heated polymer solution is at an operating temperature that is greater than or equal to 40° C.

First claim

We claim:

1 . A device comprising:
a nozzle configured to receive a heated polymer solution from a reservoir; and a power supply configured to generate an electrostatic field between a tip portion of the nozzle and a substrate so as to draw a charged jet of the heated polymer solution out of the tip portion of the nozzle toward a substrate situated at an operating distance from the tip portion of the nozzle and form a polymer fiber on the substrate, wherein the heated polymer solution is at an operating temperature that is greater than or equal to 40° C., wherein the nozzle is one of a plurality of nozzles configured to receive the heated polymer solution which is electrospun into charged jets escaping from the plurality of nozzles to form respective polymer fibers on the substrate, wherein a distance between two adjacent nozzles is between 50% and 250%, inclusive, of the operating distance.

2 . The device of claim 1 , further comprising a heating container situated to provide the heated polymer solution to the nozzle.

3 . The device of claim 2 , wherein the heating container encloses the reservoir and a body portion of the nozzle, wherein the tip portion of the nozzle extends out of the heating container.

4 . The device of claim 2 , wherein the tip portion of the nozzle extending out of the heating container has an axial length between 0.5 mm and 3 mm, inclusive.

5 . The device of claim 2 , wherein the heated polymer solution comprises a solvent and a polymer dissolved in the solvent, wherein the heating container is configured to maintain the heated polymer solution at the operating temperature, wherein the operating temperature is below a boiling temperature of the solvent.

6 . The device of claim 5 , wherein the operating temperature is below a melting point of the polymer.

7 . The device of claim 5 , wherein the polymer comprises polycaprolactone and the solvent comprises dimethylformamide, wherein the operating temperature is between 40° C. and 100° C., inclusive.

8 . The device of claim 5 , wherein the polymer has a concentration between 10-50 wt. %, inclusive, in the heated polymer solution at the operating temperature.

9 . The device of claim 1 , wherein the tip portion of the nozzle has an opening with an inner diameter between 50 μm and 1 mm, inclusive.

10 . The device of claim 1 , wherein the operating distance is between 5 mm and 30 mm, inclusive.

11 . A method comprising:
heating a polymer solution to an operating temperature that is greater than or equal to 40° C.; electrospinning the polymer solution as a charged jet escaping from a nozzle; and collecting a polymer fiber on a substrate situated at an operating distance from a tip portion of the nozzle, wherein the polymer solution comprising a polymer dissolved in a solvent at the operating temperature, wherein the polymer fiber is formed from the charged jet after evaporation of at least some of the solvent, wherein the nozzle is one of a plurality of nozzles configured to receive the heated polymer solution which is electrospun into charged jets escaping from the plurality of nozzles to form respective polymer fibers on the substrate, wherein a distance between two adjacent nozzles is between 50% and 250%, inclusive, of the operating distance.

12 . The method of claim 11 , further comprising varying the operating temperature of the polymer solution while electrospinning the polymer solution so as to change evaporation rate of the solvent.

13 . The method of claim 11 , wherein collecting the polymer fiber comprises moving the substrate relative to the nozzle.

14 . The method of claim 13 , wherein moving the substrate relative to the nozzle comprises varying translation path of the substrate while electrospinning the polymer solution so as to adjust thickness of a membrane formed by the polymer fiber collected on the substrate.

15 . A method comprising:
preparing a polymer solution comprising polycaprolactone dissolved in dimethylformamide; heating the polymer solution to an operating temperature that is between 40° C. and 100° C., inclusive; feeding the polymer solution to a nozzle; applying an electrostatic field between a tip portion of the nozzle and a substrate spaced apart from the tip portion of the nozzle by an operating distance, wherein the electrostatic field is configured to draw a charged jet of the polymer solution out of the tip portion of the nozzle toward the substrate; and collecting a fiber on the substrate, wherein the fiber is formed from the charged jet after evaporation of at least some of the dimethylformamide, wherein the nozzle is one of a plurality of nozzles configured to receive the heated polymer solution which is electrospun into charged jets escaping from the plurality of nozzles to form respective polymer fibers on the substrate, wherein a distance between two adjacent nozzles is between 50% and 250%, inclusive, of the operating distance.

16 . The method of claim 11 , wherein at least one of the plurality of nozzles was at least partially clogged by a polymer precipitate, the method further comprising:
heating the at least one nozzle to a melting temperature sufficient to melt the polymer precipitate into a polymer melt; and pressurizing the polymer melt out of the at least one nozzle through an opening so that the at least one nozzle is unclogged.

17 . The method of claim 11 , wherein the operating distance is between 10 mm and 20 mm, and an accelerating voltage applied between the tip portion of the nozzle and the substrate is between 10 kV and 20 kV.

18 . The method of claim 11 , wherein the charged jet remains substantially straight with no whipping along its trajectory until within about 1 mm above the substrate.

19 . The method of claim 11 , wherein the electrospinning is controlled such that the polymer fiber is deposited on the substrate in one or more localized spots each having a diameter between about 1 mm and about 10 mm.

20 . The method of claim 14 , wherein varying translation path of the substrate while electrospinning the polymer solution comprises depositing the polymer fiber along a plurality of parallel deposition lines having progressively reduced spacing, thereby producing the membrane whose local thickness progressively increases as the spacing between the deposition lines decreases.

Assignees

• Univ Oregon

Inventors

• Dalton Paul D
• Liashenko Ievgenii

Classifications

• D10B2331/041

  derived from hydroxy-carboxylic acids, e.g. lactones · CPC title

• D01D5/0069 Primary

  characterised by the spinning section, e.g. capillary tube, protrusion or pin · CPC title

• D01D5/0061

  characterised by the electro-spinning apparatus · CPC title

• D01D5/0038 Primary

  the fibre formed by solvent evaporation, i.e. dry electro-spinning · CPC title

• D01D7/00

  Collecting the newly-spun products ({D01D5/0076 takes precedence;} collecting newly-spun products with the imparting of twist D01H) · CPC title