WO2008106381A2 - Electrofilage de fibres polymères et de réseaux fibreux à l'aide du potentiel ca polarisé cc - Google Patents

Electrofilage de fibres polymères et de réseaux fibreux à l'aide du potentiel ca polarisé cc Download PDF

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Publication number
WO2008106381A2
WO2008106381A2 PCT/US2008/054829 US2008054829W WO2008106381A2 WO 2008106381 A2 WO2008106381 A2 WO 2008106381A2 US 2008054829 W US2008054829 W US 2008054829W WO 2008106381 A2 WO2008106381 A2 WO 2008106381A2
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Prior art keywords
polymer
potential
fibers
electrospinning
polymer fibers
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PCT/US2008/054829
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English (en)
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WO2008106381A3 (fr
Inventor
Gary Tepper
Soumayajit Sarkar
Seetharama Deevi
Supriyo Bandyopadhyay
Mohamed Samy Sayed Ahmed El-Shall
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Virginia Commonwealth University
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Publication of WO2008106381A2 publication Critical patent/WO2008106381A2/fr
Publication of WO2008106381A3 publication Critical patent/WO2008106381A3/fr

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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
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/20—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of cyclic compounds with one carbon-to-carbon double bond in the side chain
    • D01F6/22—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of cyclic compounds with one carbon-to-carbon double bond in the side chain from polystyrene
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/66—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyethers

Definitions

  • the invention is directed to electrospinning polymer fibers and fiber arrays and, more particularly, to processes which ensure the production of spun fibers which are aligned and which have very little variation in fiber diameter, as well as to polymer fibers and fiber arrays which include one or more polymer fibers together with one or more secondary materials which impart a chemical, physical, optical, magnetic or other functionality to the fibers, or fibrous mat or other array which includes the fibers.
  • Electrospinning polymers typically involves generating a high voltage, DC, electric field between a polymer fluid and a substrate where the polymer fluid and substrate have opposite charges. Once the voltage reaches a critical value, the surface tension of the polymer is overcome by the charge and a jet of ultrafine fibers is produced. Because electrostatic forces, rather than mechanical forces, are used to draw polymer fibers from the solution, the mean fiber diameter can be quite small such as on the order of 10 nm to 1000 nm. However, electrospun fibers are electrically charged during formation, and are inherently unstable, and the mats produced from the fibers usually exhibit a random, non- woven microstructure.
  • Electrospinning processes may have utility in a wide variety of applications including the fabrication of electronic devices such as sensors, actuators, and Schottky junctions; the fabrication of materials having corrosion resistance, materials having microwave or radar absorbing capabilities, and materials having magnetic or electrical conductivity capabilities; the fabrication of biological scaffolds for tissue engineering, controlled drug delivery devices, and devices which may exhibit selective antibody-antigen binding or DNA hybridization; the production of mats or fiber arrays with catalytic activity; the production of functional filters; the production of coatings with embedded intelligence; and in a wide variety of other applications. See, for example, U.S. Patent 6,800,155 to Senecal, U.S.Patent 7,267,789 to Chhabra, U.S. Patent 7,264,762 to Ko, U.S.
  • a DC biased AC potential is used to produce submicron fibers, such as fibers having a diameter in the 300-500 nm range, which are aligned in a fibrous mat or array, i.e., the polymer fibers are generally parallel to one another and are not in the form of a random, non-woven microstructure.
  • the fiber instability in DC based polymer electrospinning processes was eliminated through the use of a DC biased AC potential.
  • Figure 1 shows a schematic of an exemplary electrospinning apparatus
  • Figure 2 shows a schematic of an exemplary DC biased AC waveform
  • Figure 3 is a graph showing the stable frequency range for each of six different electrospun fiber arrays
  • Figures 4a-f are scanning electron micrographs of various experimentally produced fiber arrays produced under different conditions
  • Figures 5a-b are scanning electron micrographs of electrospun fibers deposited in a crisscross mesh pattern
  • Figures 6a-c are scanning electron micrographs of PEO/FeAl nanoparticle fibers produced using biased AC, unbiased AC, and DC electrospinning; and Figures 7a-c are plots of magnetic properties curves measured at a temperature of 10 0 K for three different concentrations of magnetic nanoparticles
  • FIG. 1 provides a schematic diagram of an electrospinning apparatus.
  • a source of polymer solution is provided in a syringe 10.
  • the polymer solution is charged with an AC potential from AC source 12, and is biased with a DC potential from high voltage source 14.
  • a conductor 16, in the form of a collecting drum, is grounded 18 and has a substrate 20 positioned thereon.
  • the conductor 16 is rotatable and maybe moveable up and down to allow fiber strands to be deposited in a precise array.
  • the conductor 16 serves to take up the jet of electrospun fiber emerging from the tip of syringe 10.
  • the configuration of the electrospinning apparatus can be varied considerably within the practice of the invention.
  • the collector could be charged and the polymer solution could be grounded, or the fiber jet could be produced from a device other than a syringe, etc.
  • a waveform generator was used to provide the AC signal in the form of a square wave with adjustable amplitude, duty cycle, and frequency.
  • a high voltage amplifier having a maximum output of -10,000 to +10,000 V ac and frequency range of DC to 30 kHz was used to amplify the output of the waveform generator.
  • the high voltage amplifier (source 14), had a biasing feature which was used to bias the AC voltage to a desired DC value.
  • the liquid flow rat to the electrospinning needle was controlled using a syringe pump.
  • the electrospinning source was a syringe with a 27 gauge tip.
  • the AC potential, frequency, biasing value, flow rate, and distance between the needle (on syringe 10) and the target (substrate 20), were adjusted to obtain a stable fiber, and the resulting fiber mater were characterized by a JOEL scanning electron microscope (SEM), LEO SEM, and an optical microscope (Olympus BX60).
  • the DC biased AC electrospinning can be practiced with a wide variety of polymers, hi the experiments reported herein poly(ethylene oxide) (PEO), polyisobutylene (PIB), and poly(styrene) (PS), commercially obtained from Aldrich chemicals were used as prototypical polymers.
  • PEO poly(ethylene oxide)
  • PIB polyisobutylene
  • PS poly(styrene)
  • electrospinning processes can be used with a wide range of organic and synthetic polymers including, without limitation, biological polymers (e.g., proteins, carbohydrates, DNA, and RNA), conducting polymers (e.g., polyanilines, polypyrroles, polythiophenes, polyphenols, polyacetylenes, and polyphenylenes), and matrix polymers (e.g., polyurethanes, PEO, polyacrylonitriles, polylactic acids, polyvinyl acetates, and cellulose acetates).
  • biological polymers e.g., proteins, carbohydrates, DNA, and RNA
  • conducting polymers e.g., polyanilines, polypyrroles, polythiophenes, polyphenols, polyacetylenes, and polyphenylenes
  • matrix polymers e.g., polyurethanes, PEO, polyacrylonitriles, polylactic acids, polyvinyl acetates, and cellulose acetates.
  • the polymer solution can include a single polymer, two or more polymers, one or more polymers plus one or more solvents (e.g., deionized water, tetrahydrofuran, dimethyl formamide, et), or a combination of one or more polymers plus one or more secondary materials to provide a functionality of interest tot he fiber array produced.
  • a secondary material is a material that has a chemical, physical, optical, or magnetic functionality different from the polymer or polymers which are being electrospun.
  • the secondary material may be a flavor ingredient or drug or nutriceutical ingredient which is slowly released from the fiber mat, a metallic or other catalyst which will permit the mat to be used in a filtering and catalytic function, a magnetic or magnetizable compound or a compound with conductive properties which permits the mat to have embedded intelligence.
  • PEO composite fibers comprising PEO blended with single walled carbon nanotubes (SWCNT), gold nanoparticles, and FeAl nanoparticles have been prepared.
  • the SWCNT were obtained commercially from Carbon Solutions.
  • the gold nanoparticles were obtained commercially from Aldrich Chemicals.
  • the FeAl nanoparticles were produced using a laser ablation process as described in Mo et al., Macromol. Symp. 2004, 217, 413, and Pithawalla et al., Mat. Set. Eng. A: Struct. Mat.: Properties, Microstruct., Processing 2002, A329, 92.
  • Table 1 presents exemplary experimental conditions for obtaining aligned fibers using an AC voltage with a biased DC component under a range of experimental electrospinning conditions.
  • PEO + Au nanoparticles 10 9.3 4.2 500-1000 1.0 7.0 PEO + FeAl nanoparticles 6 9.5 3.8 550-1000 0.7 7.0 PS 20 11 5.2 300-700 0.6 7.0 PB 15 12 5.5 400-700 1.2 7.0
  • a solution of 8 wt% PEO in DI water was prepared and was used for electrospinning, and as a base for the SWNCT composite.
  • the SWCNTs were added to a water solution with sodium dodecyl benzene sulfonate, which acts as a surfactant.
  • the SWCNT solution was then mixed in a homegenizer for 5h and the 8 wt% PEO solution was added to the resulting solution to produce a homogenous dispersion.
  • the final solution was a composition of 8wt% PEO solution in water with w.b wt% SWCNT.
  • a solution of 6wt% PEO in DI water was prepared and 2.4wt% of FeAl nanoparticles were added after 5 hours in a homogenizer.
  • the resulting solution included a 6 wt% PEO solution with 2.4 wt% FeAl nanoparticles by weight with respect to the polymer.
  • a 10 wt% solution of PEO was prepared in DI water.
  • Figure 2 shows an exemplary DC biased AC waveform according to the invention.
  • the magnitude of the DC bias is set such that the bottom edge of the negative half- cycle of the AC voltage just crosses zero and becomes negative.
  • a high degree of fiber uniformity and alignment was achieved for each polymer/solvent system investigated when the magnitude of the DC bias is less than half the amplitude of the AC potential.
  • the DC bias of 5.64 kV is slightly less than half the 11.55 kV amplitude of the AC waveform.
  • the DC bias may be between 10-49% of the AC potential. This allows a slight negative voltage every other cycle to be imparted to the fiber.
  • the AC potential should have a frequency sufficiently high to produce positively and negatively charged regions on a fiber before it traverses a distance from a source to a substrate on a collecting electrode.
  • the minimum frequency limit is related to the fiber production (draw) rate. That is, the AC frequency should be sufficient high such that the multiple positively and negatively charged regions are produced on the fiber before it traverses the distance between the source (e.g., needle) and collecting electrode. For example, for a flow rate of 1 ⁇ L-min "1 and assuming that the diameter of the jet of liquid emerging from the tip of the Taylor cone is approximately 10 ⁇ m, the fiber production rate is on the order of 20 cm-s "1 .
  • the AC potential has a frequency ranging from 100 to 1500 Hz, or more preferably 200 to 1200 Hz, or still more preferably from 300 to 1000 Hz. Excellent results were obtained with a number of different polymers when the AC potential had a frequency ranging from 500 to 1000 Hz.
  • Figure 3 shows the stable frequency range for each of six different systems.
  • Pl is PEO
  • P2 is PEO with SWCNT
  • P3 is PEO with Au
  • P4 is PEO with FeAl
  • P5 is PS
  • P6 is PIB.
  • the minimum and maximum stable frequencies are defined as the frequency where the first visible onset of instability was observed. Instability onset was determined by visually monitoring the fibers as they are drawn from the needle to the collector and documenting the frequency when mechanical oscillations first become visible. A high speed digital camera with a microscopic lens was used to monitor the stability of the small diameter fibers. The minimum and maximum stable frequencies varied for each polymer solution. However, the maximum frequency for PEO and PEO composites was consistent at about 1,000 Hz. The maximum frequency for the PS and PIB polymer solutions was relatively lower at around 700 Hz.
  • the rotational speed of the collecting drum was not shown to influence the stability of the electrospun fibers; however, it could impact the morphology of the collected fiber mat.
  • stable fibers can be collected at a variety of different rotating speeds, hi addition, stable fibers can be deposited onto a non-rotating substrate, but in such a process they would accumulate at one location. In contrast, unstable fibers generally cannot be forced into an aligned array even under very high rotational speeds of the collecting substrate.
  • Figures 4a and 4b show SEM images of PEO fiber mats collected, respectively, under pur AC and pure DC potentials, hi Figure 4a the AC electrospun PEO was produced at 5,000 V p _ p and 60 Hz. In Figure 4b the CD electrospun PEO was produced at 6,000 V. While use of the AC potential significantly increased the degree of fiber alignment in comparison to that which was obtained with a pure DC potential, the AC spun fibers exhibited a relatively large variation in diameter which can be attributed to the very low overall drawing force on the fiber.
  • Figure 4c-f show SEM images of mats of pure PEO and three PEO composite fibers produced using DC biased AC electrospinning under the processing conditions shown in Table 1.
  • hi Figure 4c electrospun fibers of PEO with SWCNT were produced at a biased voltage of 4,100 V and AC voltages of 9300 V ⁇ and 600 Hz.
  • Figure 4d is a high magnification image of a section from the image in Figure 4c.
  • electrospun fibers of PEO were poduced at a bias voltage of 4000V and an AC voltage of 9500 V p . p and 600 Hz.
  • Figures 6a-c show submicron PEO/FeAl nanoparticle fibers produced using DC bias AC electrospinning (Figure 6a), AC electrospinning without a DC bias ( Figure 6b), and DC electrospinning ( Figure 6c).
  • the DC biased AC electrospinning yields markedly better alignment and uniformity in the fiber diameter compared to AC electrospinning without a DC bias. Electrospining with only a DC potential yields a fibrous mat with effectively no fiber alignment.
  • Figures 7a-c are plots of magnetic properties ( Magnetic Hysteresis curves or "M-H" curves) for the aligned fabrics at three different concentrations of magnetic nanoparticles at a temperature of 1 OK.
  • Figure 7a shows measurements with a PEO nano fiber containing 8 wt% FeAl.
  • Figure 7b shows measurements with a PEO nanofiber containing 4-5 wt% FeAl.
  • Figure 7c shows measurements with a PEO nanofiber containing 2.5 wt% FeAl. All of the curves illustrate classic ferromagnetic behavior with magnetic hysteresis.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

L'électrofilage est un procédé pratique et très courant pour produire des fibres polymères nanométriques et des fibres composites polymères destinées à différentes applications. Malheureusement, les fibres électrofilées chargées sont instables de façon inhérente et il est difficile de produire des matériaux présentant une morphologie fibreuse contrôlée. L'électrofilage à l'aide d'un potentiel CA, au lieu d'un potentiel CC, et l'application d'une polarisation CC, de telle sorte qu'il en résulte un électrofilage CA polarisé CC, permettent de produire des réseaux fibreux alignés avec des diamètres de fibres hautement contrôlés. En démarrant avec une solution polymère contenant un ou plusieurs polymères et un ou plusieurs matériaux secondaires qui confèrent des propriétés chimiques, physiques, optiques, magnétiques ou autres, un réseau fibreux peut être formé à l'aide de l'électrofilage CA polarisé CC.
PCT/US2008/054829 2007-02-28 2008-02-25 Electrofilage de fibres polymères et de réseaux fibreux à l'aide du potentiel ca polarisé cc WO2008106381A2 (fr)

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US89211707P 2007-02-28 2007-02-28
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
EP2456911A2 (fr) * 2009-07-22 2012-05-30 Corning Inc. Procédé d électrofilage et appareil de production de fibres alignées
US20120219772A9 (en) * 2009-03-03 2012-08-30 The Johns Hopkins University System and method for precision transport, positioning, and assembling of longitudinal nano-structures
CN102912458A (zh) * 2012-11-08 2013-02-06 厦门大学 一种具有加热功能的电纺纳米纤维膜制备装置
CN103741231A (zh) * 2013-01-30 2014-04-23 上海洁晟环保科技有限公司 应用于静电纺丝装置中的绝缘系统
JP2016503838A (ja) * 2012-12-17 2016-02-08 テクニカ ユニヴェルズィタ ヴェー リベルシー 電場中でポリマーの溶媒液または溶融液を紡糸することによるポリマー・ナノファイバーの製造方法、およびこの方法によって作成されたポリマー・ナノファイバーの線状形成体
JP2016141041A (ja) * 2015-02-02 2016-08-08 キヤノン株式会社 光沢部材及びその製造方法
US10870928B2 (en) 2017-01-17 2020-12-22 Ian McClure Multi-phase, variable frequency electrospinner system

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120219772A9 (en) * 2009-03-03 2012-08-30 The Johns Hopkins University System and method for precision transport, positioning, and assembling of longitudinal nano-structures
US9044808B2 (en) * 2009-03-03 2015-06-02 The Johns Hopkins University System and method for precision transport, positioning, and assembling of longitudinal nano-structures
US9718683B2 (en) 2009-03-03 2017-08-01 The Johns Hopkins University System and method for precision transport, positioning, and assembling of longitudinal nano-structures
EP2456911A2 (fr) * 2009-07-22 2012-05-30 Corning Inc. Procédé d électrofilage et appareil de production de fibres alignées
US8211352B2 (en) 2009-07-22 2012-07-03 Corning Incorporated Electrospinning process for aligned fiber production
CN102575385A (zh) * 2009-07-22 2012-07-11 康宁股份有限公司 用于形成有序排列纤维的电纺丝工艺和设备
EP2456911A4 (fr) * 2009-07-22 2013-04-17 Corning Inc Procédé d électrofilage et appareil de production de fibres alignées
CN102912458A (zh) * 2012-11-08 2013-02-06 厦门大学 一种具有加热功能的电纺纳米纤维膜制备装置
JP2016503838A (ja) * 2012-12-17 2016-02-08 テクニカ ユニヴェルズィタ ヴェー リベルシー 電場中でポリマーの溶媒液または溶融液を紡糸することによるポリマー・ナノファイバーの製造方法、およびこの方法によって作成されたポリマー・ナノファイバーの線状形成体
CN103741231A (zh) * 2013-01-30 2014-04-23 上海洁晟环保科技有限公司 应用于静电纺丝装置中的绝缘系统
JP2016141041A (ja) * 2015-02-02 2016-08-08 キヤノン株式会社 光沢部材及びその製造方法
US10870928B2 (en) 2017-01-17 2020-12-22 Ian McClure Multi-phase, variable frequency electrospinner system

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