US20230038283A1 - Hybrid electrospinner for core-shell fiber fabrication - Google Patents
Hybrid electrospinner for core-shell fiber fabrication Download PDFInfo
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- US20230038283A1 US20230038283A1 US17/739,602 US202217739602A US2023038283A1 US 20230038283 A1 US20230038283 A1 US 20230038283A1 US 202217739602 A US202217739602 A US 202217739602A US 2023038283 A1 US2023038283 A1 US 2023038283A1
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- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 239000011258 core-shell material Substances 0.000 title description 3
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- 238000010438 heat treatment Methods 0.000 claims abstract description 18
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- 238000001523 electrospinning Methods 0.000 abstract description 48
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- 108010010803 Gelatin Proteins 0.000 abstract description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract description 2
- 229920000159 gelatin Polymers 0.000 abstract description 2
- 239000008273 gelatin Substances 0.000 abstract description 2
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 229920001610 polycaprolactone Polymers 0.000 description 1
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Images
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/04—Melting filament-forming substances
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
- D01D13/02—Elements of machines in combination
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/0023—Electro-spinning characterised by the initial state of the material the material being a polymer melt
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
Definitions
- FIG. 9 is a photograph of the split block melt chamber attached to the side of the coaxial block spinneret.
- heater cartridges have been inserted into the melt chamber as well as the spinneret to provide heat at multiple points along the polymer path prior to extrusion from the spinneret and ES.
- FIG. 11 is a far field micrograph of monoaxial electrospun fibers produced from polypropylene melt in the hybrid electrospinner. During ES, polypropylene melt was subjected to an electric field strength of 367 kV/m. The resulting fibers had an average diameter of 20 ⁇ m and presented a smooth, consistent surface.
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
Electrospinning (ES) provides the technical community with a readily available method to produce polymer fibers ranging from nanoscale to microscale. Here, we present a novel “hybrid electrospirming apparatus,” whereby, modifications to a melt electrospinner have allowed fabrication of core-sheath fibers with polymer sheaths and solution-based cores. These modifications include a split polymer melt heating block, coaxial block spinneret equipped with heaters and multiple feed ports for core and sheath material, and a wiring system for heat which requires multiple switches for safety and on-demand heat activation. Successful demonstration of coaxial fiber fabrication is demonstrated using polycaprolactone-polyethylene oxide blend shell and fluorescent gelatin core materials.
Description
- This continuation application claims the benefit of U.S. Nonprovisional Application No. 16/402,881 filed on May 3, 2019, which claims the benefit of U.S. Provisional Application No. 62/666,475 filed on May 3, 2018, the disclosures of which are hereby incorporated by reference in their entirety to provide continuity of disclosure.
- Research was sponsored by the Army Research Laboratory and was accomplished under Cooperative Agreement Number W911NF-15-2-0020. The views and conclusions contained in this document are those of the authors and should not be interpreted as representing the official policies, either expressed or implied, of the Army Research Laboratory or the U.S. Government.
- Not applicable.
- Not applicable.
- Electrospinning (ES) provides the technical community with a readily available method to produce polymer fibers ranging from nanoscale to microscale. ES produces fibers with small cross-sections and high surface area, making them ideal for a multitude of applications. Structures produced using ES methods exhibit a high surface-to-volume ratio, tunable porosity, and controllable composition. ES is of interest to the technical community in areas involving novel ES methods and materials including enhanced filtration [D. Aussawasathien, et al., Journal of Membrane Science, 2008, R. Gopal et al., Journal of Membrane Science, 2007. K. M. Yun, et al., Chemical Engineering Science, 2007. X. H. Qin, et al., Journal of Applied Polymer Science, 2006] augmented biomedical tissue regeneration [D. Liang, et al., Advanced Drug Reviews, 2007, Kim et al., Biomaterials, 2003], and advanced fabrication of liquid crystal polarizers [Y. YF, et al., Advanced Materials, 2007]. Although ES is the common term today, it was initially described by Formhals in a series of patents as an experimental setup for the production of polymer filaments using electrostatic force. The first patent filed by Formhals in 1934 on ES was issued for the production of textile yarns, with a process consisting of a movable thread collecting device that gathered threads in a stretched condition. He was granted related patents in 1938, 1939, and 1940[K. J. Pawlowski, et al., Materials Research Society Symposia, 2004]. ES was first observed in 1897 by Rayleigh, with related electrospraying studied in detail in 1914 and a patent issued to Antonin Formhals in 1934 [J. Zeleny, Physical Reviews, 1914, A. Formhals, Patent US1975504A, 1934]. In 1969, the published work of Taylor set the foundation for ES [G. Taylor, Proceedings “Electrically driven jets,” Proceedings of the Royal Society of London A: Mathematical, Physical, and Engineering Sciences, 1969].
- ES involves the delivery of a liquid polymer to a spinneret (sometimes referred to as a capillary or needle) [I. S. Chronakis, Journal of Materials Processing Technology, 2005, Z. M. Huang, et al. Journal of Composites Science, 2003, J. Doshi et al., Journal of Electrostatics, 1995] that is held at a high voltage relative to a collection plate [J. L. Skinner et al., Proceedings of SPIE—The International Society for Optical Engineering, 2015]. Polymer is pumped to the tip of the spinneret, and electric charge is initiated in the collection plate. The initiated voltage creates an electrostatic force that pulls polymer from the spinneret to an electrode deposition surface. An initial short region (microns to millimeters) where the fiber is essentially straight is called the stable region. At the point where lateral perturbations cause transverse fiber velocities, the instability region starts. The instability region consists of polymer fiber moving in a whipping motion from the stable region toward the collection plate, while solvent evaporates off the polymer jet. Polymer fibers are then deposited onto the collection surface. Fiber size depends largely on solution flow rate, supplied electric current, and fluid surface tension [S. V. Fridrikh, et al., Physical Reviews Letters, V. Beachley et al., Materials Science Engineering C, 2009, A. Koski, et al., Materials Letters, 2004]. Given the time scales associated with fiber deposition by ES, charges on the metallic collection plate move instantaneously. Motion of charge in the polymer (much slower than motion of charge in metals) is dictated by ionic mobility in the polymer [D. H. Reneker, et al., Journal of Applied Physics]. Any effort to control the electric field within ES must take into account the high-frequency cutoff enforced by polymer limitations. The low-frequency cut-off for dynamic field control relates to the spatial fiber deposition rate and time constants associated with the instability region.
- In solution ES, polymers which are pre-dissolved in solvent are used. Although solution ES is more common, melt ES can also be performed, in which, solid polymers are used. Melt-ES does not require solvent evaporation, instead creating a liquid polymer from a solid, in which phase transition of the polymer is associated with increased temperature [P.D. Dalton, et al., Biomacromolecules, 2006, J.S. Kim et al., Polymer Journal, 2000, L. Larrondo et al., Journal of Polymer Science and Polymer Physics, 1981, S. Lee et al., Journal of Applied Polymer Science, 2006, J. Lyons, et al., Polymer, 2004]. Lack of solvent in melt ES is beneficial for two reasons. First, the lack of harsh solvent requires less precaution during polymer preparation, and second, the instability region caused by solvent evaporation is a non-issue. Melt-ES was first patented by Norton in 1936 [C. L. Norton, US Patent 2048651,1936] but it was not until 1981 that a three-paper series describing electrostatics and polymer melts was published by Larrondo and Manley [L. Larrondo, et al., Journal of Polymer Science Part B, 1981].
- An apparatus designed for hybrid ES, whereby, materials which consist of core-sheath fibers can be fabricated is disclosed herein. The hybrid electrospinner designed allows a polymer melt to encase a solution-based (solution or solution-based) core, forming coaxial or core-sheath structured fibers. ES in the dual feed system designed will force polymer shell and core solution into a high voltage electric field generated between the spinneret and the collection plate. The electric field described is initiated by an externally applied voltage. The electric field used during ES creates a force on polymer shell and core solution, which results in deformation of the polymer/solution stream to lower surface area. Polymer shell and core solution are then pulled by the electrostatic force from spinneret to collection plate, forming core-shell fibers with a solid shell and liquid core.
- For core-shell or coaxial structures to be fabricated on melt ES, a novel ES spinneret had to be designed. Because melt ES involves dry polymers, the spinneret had to be equipped not only with concentric spinneret configuration, but also heaters to melt the dry polymer used for the shell, prior to ES. The novel ES spinneret designed is comprised of an outer and inner annulus contained within a block spinneret. The block spinneret also contains two channels for cartridge heaters and a channel that incorporates a feed control mechanism for the outer annulus region.
- The hybrid electrospinner heating design will include cartridge heaters and a Proportional-Integral-Derivative (PID) controller. In the heating design, two safety switches were added to require the main power input controller and also a secondary control switch on the heaters. The secondary control switch enables powering of the PM controller, but not activating the heaters until desired.
- The fiber sheath created during ES with the hybrid electrospinner is delivered to the outer annular region of the coaxial block spinneret from a split block used to melt the polymer prior to ES. The split block design allows polymer to be molded to the correct shape for the hybrid electrospinner, and also for easy cleaning. The split block melt chamber contains a threaded fitting to attach to the sheathing feed of the spinneret, and an isolated heater cartridge holder to maintain the heat input but separate fed polymer from the cartridge heater.
- The core (solution) feed for the hybrid electrospinner was designed to provide control over flow rate and provide consistent flow through the coaxial block spinneret within the applied electric field without damaging any electronics. This was accomplished by feeding the core solution through a syringe regulated by a commonly used syringe pump.
- The hybrid electrospinner was designed and fabricated to electrospin monoaxial polymer fibers, or coaxial (core-sheath/shell) fibers with a solution-based core and polymer shell.
-
FIG. 1 is a schematic of the design used for the hybrid ES apparatus. The set-up shown is designed to enable production of materials which contain fibers composed of a polymer melt sheath and a solution- based core, although monoaxial polymer fibers can be electrospun as well. -
FIG. 2 is a schematic plan view of a coaxial (core-sheath) spinneret design incorporating two heaters to melt polymer prior to ES. -
FIG. 3 is a perspective view of a coaxial (core-sheath) spinneret design incorporating two heaters to melt polymer prior to ES. -
FIG. 4 : is a photograph of a coaxial block spinneret prototype. Image shows two ports for heater cartridges as well as two feed ports. Side port allows polymer feed for fiber sheath, while top port is used for solution, core feed. -
FIG. 5 is a wiring schematic for a PID heater controller. The control loop shown has two main power controls, one for overall power, and a second for heater power. The separated control design allows the PID controller to be activated and set without activating the heaters until desired. -
FIG. 6 is a photograph of a PID controller and power switch control panel. -
FIG. 7 is a perspective transparent view of the polymer melting chamber design with split block. -
FIG. 8 is a perspective view of the split block design of the melting chamber, which allows for polymer melt to be molded for delivery into the outer annulus of the coaxial block spinneret for sheath material delivery, as well as for easy cleaning. -
FIG. 9 is a photograph of the split block melt chamber attached to the side of the coaxial block spinneret. Here, heater cartridges have been inserted into the melt chamber as well as the spinneret to provide heat at multiple points along the polymer path prior to extrusion from the spinneret and ES. -
FIG. 10 is a photograph of a syringe pump used to deliver solution core to the coaxial block spinneret. The syringe pump allows for control over the core solution delivery to the spinneret using a stepper motor for calibrated flow rate set by the user. -
FIG. 11 is a far field micrograph of monoaxial electrospun fibers produced from polypropylene melt in the hybrid electrospinner. During ES, polypropylene melt was subjected to an electric field strength of 367 kV/m. The resulting fibers had an average diameter of 20 μm and presented a smooth, consistent surface. -
FIG. 12 is another far field micrograph of monoaxial electrospun fibers produced from polypropylene melt in the hybrid electrospinner. During ES, polypropylene melt was subjected to an electric field strength of 367 kV/m. The resulting fibers had an average diameter of 20 μm and presented a smooth, consistent surface. -
FIG. 13 is a photograph taken during ES. Photo shows polymer/solution jet deforming into a cone shape. This is typical during ES, where deformation incurs as a mechanism to reduce surface area during electric field exposure. Solution core can be seen pulling into the polymer stream, while polymer sheath material maintains the overall structure of the stream, which will result in coaxial fiber formation. -
FIG. 14 is an epifluorescent micrograph showing coaxial electrospun fiber containing a polycaprolactone/polyethylene oxide blend polymer shell and fluorescent gelatin core. The fiber produced was fabricated in an electric field strength of 400 kV/m, and a diameter of approximately 20 μm with a core diameter of 9 to 15 μm. - A schematic of a hybrid electrospinner is shown in
FIG. 1 . Said hybrid electrospinner is comprised of: aheating block 30, which is further comprised of apolymer melt chamber 1, and at least oneheater cartridge 2; ahybrid spinneret 3; asyringe pump 4; a thermocouple 5; atemperature controller 6; a highvoltage power supply 7; and acollection plate 9. Whereby saidheating block 30 is further comprised of acommunication 10 between saidpolymer melt chamber 1 and saidhybrid spinneret 3 for delivery of polymer melt 11. Said at least oneheater cartridge 2 is designed to be inserted and removable from saidheating block 30. Saidsyringe pump 4 deliverscore solution 13 to thehybrid spinneret 3. The design shown allows a polymer melt 11 to encase acore 14, where said core can be solution-based or solution, forming coaxial fibers or core-sheath structuredfibers 15. ES in this dual feed system will forcepolymer shell 17 andcore solution 13 into a high voltageelectric field 18 generated between thehybrid spinneret 3 and thecollection plate 9. Theelectric field 18 described is initiated by an externally applied highvoltage power supply 7. Theelectric field 18 used during ES creates a force onpolymer shell 17 andcore solution 13, which results in deformation of the polymer/solution stream to lower surface area. Polymer shell and core solution are then pulled by the electrostatic force from thehybrid spinneret 3 to thecollection plate 9, forming core-sheath structuredfibers 15 with a solid shell and liquid core as shown inFIGS. 13 and 14 . - For coaxial or core-sheath structured
fibers 15 to be fabricated by melt ES, a novelES hybrid spinneret 3 had to be designed. Solution ES of coaxial structures involves a simple change of the spinneret to contain one instead of two concentric spinnerets, which are each fed a separate polymer or solution. Because melt ES involves dry polymers, thehybrid spinneret 3 had to be equipped not only with concentric spinneret configuration, but alsoheater cartridges 2 to melt the dry polymer used for the shell, prior to ES. The novelES hybrid spinneret 3 designed contains an outerannular wall 19 and innerannular wall 20 contained within the hybrid spinneret. Melted polymer enters thehybrid spinneret 3 through acommunication 10 comprising apolymer entry port 21, allowing polymer flow and fiber sheath formation within the space created between the outerannular wall 19 and innerannular wall 20. Core solution-basedmaterial entry 22 occurs via acore solution feed 31, which allows core solution to flow into the space enclosed by the innerannular wall 20. The outerannular wall 19 and innerannular wall 20 terminate at anextrusion port 23 where the polymer and solution-based material are subjected to theelectric field 18 for ES of core-sheath structuredfibers 15. Thehybrid spinneret 3 also contains twochannels 24 forcartridge heaters 2 to be removably inserted, and a channel that incorporates a feed control mechanism for the outer annular region. - A schematic model of the coaxial melt
ES hybrid spinneret 3 is shown inFIGS. 2 and 3 , while a photograph of thehybrid spinneret 3 is shown inFIG. 4 . - The hybrid electrospinner heating design includes
heater cartridges 2 and atemperature controller 6 comprising a Proportional-Integral-Derivative (PID)controller 25. The wiring diagram for the heating mechanism designed is shown inFIG. 5 . InFIG. 5 , a completed heater control loop is shown, excluding the thermocouple 5 that thePID controller 25 collects data from.FIG. 5 schematic contains two 144Ohm heater cartridges 2, aPID controller 25, aheater power switch 26, amain power switch 27 and a highvoltage power supply 7 comprising a 120-volt power source. Theheater cartridges 2 are comprised of HDC0031 heaters that are matched up to anOmega PID controller 25 for temperature control. Also seen in the wiring schematic are the two switches added as a safety precaution, requiring not only the main power input controller, but also a secondary control switch on the heaters. The secondary control switch enables powering of the PID controller, but not activating the heaters until desired. Controller switches 26 and 27 on the panel are shown inFIG. 6 . - The feed mechanism for the fiber sheath creating during ES is shown in
FIGS. 7 and 8 . The design shown is comprised of aheating block 30 with apolymer melt chamber 1, which provides afeed 28 to theouter annulus 19 region of thehybrid spinneret 3. Saidfeed 28 can be threaded to accommodate a threadedfitting 33, for attachment to thepolymer entry port 21 of thehybrid spinneret 3. Theheating block 30 design comprises a split block shown inFIG. 8 so that melt polymer mold can be prepared in themelt chamber 1 mold, and also for ease of cleaning. Theheating block 30 is also comprised of an isolated melt chamberheater cartridge channel 29 to accept a melt chamber heater cartridge, which maintains heat input, but is separate from the fed polymer. InFIG. 9 , a photograph of theheating block 30 is shown attached to the side of thehybrid spinneret 3. Active control or gravity feed are both possible with the feed mechanism designed. - The core solution feed 31 for the hybrid electrospinner was designed to provide control over flow rate and provide consistent flow through the
hybrid spinneret 3 within the appliedelectric field 18 without damaging any electronics. This was accomplished by feeding the core solution through a syringe 32 regulated by a commonly usedsyringe pump 4 shown inFIG. 10 . - The hybrid electrospinner was designed and fabricated to electrospin monoaxial polymer fibers, or coaxial (core-sheath/shell) fibers with a solution core and polymer shell. In
FIGS. 11 and 12 , an example of monoaxial fibers electrospun with the hybrid electrospinner are shown. InFIGS. 13 and 14 , an example of coaxial fibers electrospun with the hybrid electrospinner are shown. - It is understood that the foregoing examples are merely illustrative of the present invention. Certain modifications of the articles and/or methods may be made and still achieve the objectives of the invention. Such modifications are contemplated as within the scope of the claimed invention.
Claims (6)
1. A Hybrid ES apparatus comprising:
a. a heating block, comprised of a polymer melt chamber further comprised of a feed at a bottom end of said polymer melt chamber, and at least one heating block heater cartridge channel isolated from said polymer melt chamber to accept at least one removable heating block heater cartridge;
b. a hybrid spinneret comprised of a concentric spinneret further comprising an outer annular wall and an inner annular wall, where a space is created between said outer annular wall and inner annular wall to accept a melted polymer from said polymer melt chamber feed through a polymer entry port of said hybrid spinneret where said melted polymer enters said space between said outer annular wall and inner annular wall, and
a space is created inside said inner annular wall isolated from said space between said outer annular wall and inner annular wall, which accepts a core solution from a core solution feed located at a first end of said hybrid spinneret;
where said outer annular wall and inner annular wall terminate at a polymer extrusion port located at a second end of said hybrid spinneret; and
whereby said hybrid spinneret is further comprised of at least one removable spinneret heater cartridge channel isolated from said outer annular wall, which accepts at least one removable spinneret heater cartridge.
2. The Hybrid ES apparatus of claim 1 where said feed and said polymer entry port are threaded to accommodate a threaded fitting for attachment of said heating block to said hybrid spinneret.
3. The Hybrid ES apparatus of claim 1 where a syringe and a syringe pump delivers core solution to the space created by said inner annular wall.
4. The Hybrid ES apparatus of claim 1 where said heating block comprises a split block to facilitate cleaning.
5. The Hybrid ES apparatus of claim 1 further comprising a temperature controller comprised of a Proportional-Integral-Derivative (PID) controller, which controls the temperature of said heating block and said hybrid spinneret.
6. The Hybrid ES apparatus of claim 5 further comprising a main power input controller, and a secondary control switch for said heater cartridges to enable powering of said PID controller without activating said heater cartridges until desired.
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US17/739,602 US20230038283A1 (en) | 2018-05-03 | 2022-05-09 | Hybrid electrospinner for core-shell fiber fabrication |
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US201862666475P | 2018-05-03 | 2018-05-03 | |
US201916402881A | 2019-05-03 | 2019-05-03 | |
US17/739,602 US20230038283A1 (en) | 2018-05-03 | 2022-05-09 | Hybrid electrospinner for core-shell fiber fabrication |
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US3936262A (en) * | 1973-07-28 | 1976-02-03 | Karl Hehl | Multi-orifice injector nozzle for injection molding machine |
US20050287239A1 (en) * | 2004-06-29 | 2005-12-29 | Cornell Research Foundation Inc. | Apparatus and method for elevated temperature electrospinning |
US7134857B2 (en) * | 2004-04-08 | 2006-11-14 | Research Triangle Institute | Electrospinning of fibers using a rotatable spray head |
US20120292795A1 (en) * | 2011-02-07 | 2012-11-22 | Ed Peno | Apparatuses and methods for the simultaneous production of microfibers and nanofibers |
US20140332733A1 (en) * | 2011-08-30 | 2014-11-13 | Cornell University | Pure metal and ceramic nanofibers |
US20150240388A1 (en) * | 2012-09-17 | 2015-08-27 | Cornell University | Reinforcing nanofiber additives |
-
2022
- 2022-05-09 US US17/739,602 patent/US20230038283A1/en not_active Abandoned
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3936262A (en) * | 1973-07-28 | 1976-02-03 | Karl Hehl | Multi-orifice injector nozzle for injection molding machine |
US7134857B2 (en) * | 2004-04-08 | 2006-11-14 | Research Triangle Institute | Electrospinning of fibers using a rotatable spray head |
US20050287239A1 (en) * | 2004-06-29 | 2005-12-29 | Cornell Research Foundation Inc. | Apparatus and method for elevated temperature electrospinning |
US20120292795A1 (en) * | 2011-02-07 | 2012-11-22 | Ed Peno | Apparatuses and methods for the simultaneous production of microfibers and nanofibers |
US20140332733A1 (en) * | 2011-08-30 | 2014-11-13 | Cornell University | Pure metal and ceramic nanofibers |
US20150240388A1 (en) * | 2012-09-17 | 2015-08-27 | Cornell University | Reinforcing nanofiber additives |
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