US20090102100A1 - Fiber formation by electrical-mechanical spinning - Google Patents

Fiber formation by electrical-mechanical spinning Download PDF

Info

Publication number
US20090102100A1
US20090102100A1 US12/255,806 US25580608A US2009102100A1 US 20090102100 A1 US20090102100 A1 US 20090102100A1 US 25580608 A US25580608 A US 25580608A US 2009102100 A1 US2009102100 A1 US 2009102100A1
Authority
US
United States
Prior art keywords
rotating member
liquid material
fibers
target
periphery
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US12/255,806
Other languages
English (en)
Inventor
Stuart D. Hellring
Melanie S. Campbell
Calum H. Munro
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
PPG Industries Ohio Inc
Original Assignee
PPG Industries Ohio Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by PPG Industries Ohio Inc filed Critical PPG Industries Ohio Inc
Priority to US12/255,806 priority Critical patent/US20090102100A1/en
Assigned to PPG INDUSTRIES OHIO, INC. reassignment PPG INDUSTRIES OHIO, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CAMPBELL, MELANIE S., HELLRING, STUART D., MUNRO, CALUM H.
Publication of US20090102100A1 publication Critical patent/US20090102100A1/en
Abandoned legal-status Critical Current

Links

Images

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/098Melt spinning methods with simultaneous stretching
    • D01D5/0985Melt spinning methods with simultaneous stretching by means of a flowing gas (e.g. melt-blowing)
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/18Formation of filaments, threads, or the like by means of rotating spinnerets
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/18Monocomponent 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 unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide

Definitions

  • the present invention relates to fiber formation, particularly to fibers of nano dimensions.
  • Fibers of nano dimensions can be produced by streaming an electrostatically charged liquid such as a polymeric solution through a jet or needle with a very small orifice. Scaling up this process by using multiple needles suffers from the difficulty of electrically isolating these needles from each other. Consequently, needles typically must be at least one centimeter away from the nearest neighbor. In addition, the need to draw a Tailor cone from a single droplet on the end of each needle limits the maximum flow rate per needle and increases the number of needles that are needed to achieve large scale production.
  • the present invention provides a method of fiber production starting from a liquid material such as a polymer solution or a polymer melt.
  • the liquid material is fed to an annular rotating member such as a disk or cup rotating around an axis concentric therewith.
  • the rotating member has a relatively smooth continuous surface extending from the central area to a periphery.
  • the liquid material is directed by centrifugal force radially from the central area to the periphery and is expelled from the periphery towards a target.
  • Liquid material is electrically charged either by the rotating member or immediately after being expelled from the periphery of the rotating member by passing through an electric field.
  • the target to which the fibers are directed is electrically grounded.
  • the difference in electrical potential between the charged fibers and the target, the viscosity of the liquid material and the size and speed of the annular member, the liquid delivery rate and the optional use of shaping air are adjusted relative to one another so that the liquid material is expelled in fibrous form. Also adjusting these variables affects the quality and quantity of the fibers.
  • the continuous surface of the annular rotating member is the interior surface of a substantially cylindrical member such as a cup.
  • the sides of the cup may be divergent such that the cup is in the form of a truncated cone.
  • the annular spinning member rotates around an axis concentric therewith.
  • the rotating member may be electrically charged to impart an electrical charge to the liquid material being fed to the rotating member.
  • an electrical charge can be imposed on the liquid material as it is expelled from the rotating member in fibrous form by passing the fibers through an electric field.
  • the liquid material is centrifugally directed along the interior surface towards the periphery of the rotating member.
  • spinning points are located along the periphery of the rotating member.
  • spinning points are V-shaped serrations extending around the periphery, preferably extending outwardly and substantially parallel to the axis of rotation of the rotating member.
  • the liquid material passes over the spin points and is expelled from the rotating member towards the grounded target.
  • the rotating member may vary in size and geometry.
  • the rotating member may be as a disk or rotating bell.
  • the diameter of the rotating member may vary from 20 mm to 350 mm, such as 20 to 160, such as 30 to 80 mm.
  • the difference in electrical potential between the charged fibers and the target is preferably at least 5000 volts, such as within the range of 20,000 to 100,000 volts and 50,000 to 90,000 volts. If the electrical potential is insufficient, droplets and not fibers may be formed.
  • the fibers are directed towards a grounded target where the fibers are collected.
  • the grounded target can be positioned behind a moving belt or conveyor where the fibers can be collected and removed from the target area.
  • the distance to target can vary from 2 to 50 (5 to 130 cm), such as 2 to 30 inches (5 to 76 cm) such as 10 to 20 inches (25-51 cm).
  • an air stream is propelled normally and concurrently against the expelled fibers so as to shape the fibers into a flow pattern concentric with the axis of rotation and towards the target.
  • Air pressure measured at the entrance of the rotating member can typically be set at such as 1-80 PSIG (6.9 ⁇ 10 3 -5.5 ⁇ 10 5 Pascals), such as 1-60 PSIG (6.9 ⁇ 10 3 -4.1 ⁇ 10 5 Pascals) such as from 5 to 40 PSIG (3.4 ⁇ 10 4 -2.8 ⁇ 10 5 Pascals).
  • PSIG 6.9 ⁇ 10 3 -5.5 ⁇ 10 5 Pascals
  • 1-60 PSIG 6.9 ⁇ 10 3 -4.1 ⁇ 10 5 Pascals
  • PSIG 3.4 ⁇ 10 4 -2.8 ⁇ 10 5 Pascals
  • shaping air is usually not used.
  • the rotating member is connected to a drive means such as a rotating drive shaft connected to a member such as an electrical motor or air motor capable of spinning the rotary member at speeds of at least 500 rpm, such as 1000 to 100,000, and 3000 to 50,000 rpms typically with speeds of 10,000 to 100,000 rpms. If the speed of the rotating member is insufficient, fibers may not form and the liquid may be expelled from the rotary member as sheets or globs. If the speed of the rotating member is too high, droplets may form or fibers may break off.
  • a drive means such as a rotating drive shaft connected to a member such as an electrical motor or air motor capable of spinning the rotary member at speeds of at least 500 rpm, such as 1000 to 100,000, and 3000 to 50,000 rpms typically with speeds of 10,000 to 100,000 rpms. If the speed of the rotating member is insufficient, fibers may not form and the liquid may be expelled from the rotary member as sheets or globs. If the speed of the rotating member is too high, droplets may form or
  • the liquid material is passed through the interior of the drive shaft and fed to the rotating member.
  • the rotating member is cup-shaped, such as a rotating bell
  • the liquid material is fed through the closed end of the cup and in the central or base area of the cup.
  • the liquid enters the closed end of the cup through a supply nozzle that may range in size from 0.5 to 1.5 mm.
  • the liquid can then travel through the inside of the cup and exits on the surface of the cup through a center orifice or series of orifices onto the cup face.
  • the flow rate of liquid material to the rotating member is typically 1 ml/hour to 500 ml/minute, such as from 20 ml/hour to 50 ml/minute such as from 50 to 1000 ml/hour.
  • the liquid material that is spun into fibers in accordance with the invention is typically a polymer solution or melt.
  • the polymers can be organic polymers such as polyesters, polyamides, polymers of n-vinyl pyrrolidone polyacrylonitrile and acrylic polymers such as are described in published application U.S. 2008/0145655A1.
  • the liquid can be an inorganic polymer.
  • inorganic polymers are polymeric metal oxides that contain alkoxide groups and optionally hydroxyl groups.
  • the alkoxide groups contains from 1 to 4 carbon atoms such as methoxide and ethoxide.
  • polymeric metal oxides are polyalkylsilicates such as those of the following structure:
  • R is alkyl containing from 1 to 4, preferably from 1 to 2 carbon atoms, and n is 3 to 10.
  • hybrid organic/inorganic polymers such as acrylic polymers and polymeric metal oxides can be employed. Examples of such organic/inorganic hybrid polymers are described in published application U.S. 2008/0207798A1. Also, inorganic materials such as inorganic oxides or inorganic nitrides or carbon or ceramic precursors, such as silica, aluminia, Titania, or mixed metal oxides can be used.
  • the electrical conductivity of the liquid material can vary and should be sufficiently electrically conductive such that it can accept a charge build up but not to the point that electrical shorting occurs. With indirect charging, the electrical conductivity can be high since shorting is not a problem.
  • the electrical conductivity can be adjusted by using appropriate amounts of salts such as ammonium salts and electrically conductive solvents such as alcohol-water mixtures.
  • the surface tension of the liquid material can vary. If the surface tension is too high, atomization and droplets rather than fibers may be formed.
  • the liquid preferably thickens as polymer concentration increases or polymer crosslinking occurs.
  • the viscosity of the solution can be controlled by controlling the molecular weight of the polymer, the concentration of the polymer in the solution, the presence of crosslinking of the polymer in solution, or by adding a thickening agent to the polymer solution such as polyvinyl pyrrolidone, polyvinyl alcohol, polyvinyl acetate, polyamides and a cellulosic thickener. If the viscosity of the solution is too high, i.e., at its gel point or above, it behaves more like a solid material and may not form a fiber and may build up as solid polymer on the surface of the rotating member. If the viscosity of the liquid is too low, atomization and not fiber formation may result.
  • the fibers that are formed in accordance with the invention typically have diameters of up to 5,000 nanometers, such as 5 to 5,000 nanometers or within the range of 50 to 1200 nanometers such as 50 to 700 nanometers. Fibers can also have ribbon or flat face configuration and in this case the diameter is intended to mean the largest dimension of the fiber. Typically, the width of ribbon-shaped fibers is up to 5,000, such as 500 to 5,000 nanometers, and the thickness is up to 200, such as 5 to 200 nanometers.
  • the nanofibers can be twisted around each other in a yarn-like structure.
  • FIG. 1 is a schematic vertical cross-section through a centrifugal spinning apparatus in which the process of the invention may be practiced.
  • FIG. 2 is a bottom elevation of a spinning member in accordance with the process of the invention.
  • FIG. 3 is a section along line III-III of FIG. 2 .
  • FIG. 4 shows photomicrographs at various magnifications of nanofibers prepared in accordance with Example 1.
  • FIG. 4 a shows photomicrographs at various magnifications of droplets prepared in accordance with Example 1a (comparative).
  • FIG. 5 is a chart showing how the variables of rotating member speed, shaping air and liquid flow effect fiber formation for the polymer solutions of Examples 1 and 1a (comparative).
  • FIG. 6 shows photomicrographs at various magnifications of nanofibers prepared in accordance with Example 2.
  • FIG. 6 a shows photomicrographs at various magnifications of droplets prepared in accordance with Example 2a (comparative).
  • FIG. 7 is a chart showing how the variables of rotating member speed, shaping air and liquid flow effect fiber formation for the polymer solutions of Examples 2 and 2a (comparative).
  • FIG. 8 shows photomicrographs at various magnifications of nanofibers prepared in accordance with Example 3.
  • FIG. 8 a shows photomicrographs at various magnifications of droplets prepared in accordance with Example 3a (comparative).
  • FIG. 9 shows photomicrographs at various magnifications of nanofibers in the form of a twisted yarn prepared in accordance with Example 4.
  • FIG. 10 shows photomicrographs at various magnifications of nanofibers prepared in accordance with Example 5.
  • the apparatus 1 contains a cup-shaped rotating member 5 and an air plenum arrangement 7 through which air is directed to shape the fibrous stream 9 as it is directed towards the target 11 .
  • a conveyor 12 Positioned before the target is a conveyor 12 for removing the fibrous product from the apparatus 1 .
  • a container 13 for the liquid material 15 includes a suitable feed mechanism (not shown) for feeding the liquid material to the rotating cup 5 via a feed supply line 17 mounted concentrically with the axis 3 .
  • the supply line 17 has an exit in the rotating cup 5 adjacent to closed end.
  • the feed supply line is located within a rotating drive shaft for rotating the cup-shaped rotary member 5 .
  • a voltage is imposed on the rotating cup to impart a charge on the liquid material and the fibers that are expelled from the rotating cup.
  • the rotating member 5 is cup-shaped having a planar base or closed end 21 and divergent walls 23 extending from the base 21 .
  • the base 21 has a central aperture 25 through which the feed supply line extends and fixing elements 27 by which the rotating cup S is mounted on the drive means for rotation around the axis 3 .
  • the interior surface 29 of the wall 23 is relatively smooth over the region extending from the base 21 to the edge 31 of the cup 5 .
  • the edge of the cup 5 is serrated such that there are spinning points 33 defined by V-shaped serrations 35 on the external periphery of the cup 5 .
  • V-shaped serrations 35 lie in a plane parallel to the base of the cup 5 .
  • the cup 5 is spun at the desired rate and the liquid is fed to the rotating cup in the central area of the base of the cup and is directed to the periphery of the base 21 and across the interior surface 29 by centrifugal force.
  • the liquid that is electrically charged flows across the interior surface 29 of the rotating cup through the spinning points 33 from which the liquid is expelled in fibrous form towards the grounded target 11 .
  • An acrylic-silane polymer was prepared as follows.
  • a reaction flask was equipped with a stirrer, thermocouple, nitrogen inlet and a condenser.
  • Charge A was then added and stirred with heat to reflux temperature (75° C.-80° C.) under nitrogen atmosphere.
  • To the refluxing ethanol Charge B and Charge C were simultaneously added over three hours.
  • the reaction mixture was held at reflux condition for two hours.
  • Charge D was then added over a period of 30 minutes.
  • the reaction mixture was held at reflux condition for two hours and subsequently cooled to 30° C.
  • a hybrid organic-inorganic polymer was prepared as follows:
  • An acrylic-silane polymer was prepared as follows.
  • a reaction flask was equipped with a stirrer, thermocouple, nitrogen inlet and a condenser.
  • Charge A was then added and stirred with heat to reflux temperature (75° C.-80° C.) under nitrogen atmosphere.
  • To the refluxing ethanol Charge B and Charge C were simultaneously added over three hours.
  • the reaction mixture was held at reflux condition for two hours.
  • Charge D was then added over a period of 30 minutes.
  • the reaction mixture was held at reflux condition for two hours and subsequently cooled to 30° C.
  • Deionized water (30 grams) was pored into a jar, and polyvinylpyrrolidone (4 grams, Aldrich, Catalog 437190, CAS [9003-39-8], and MW 1,300,000) was added. The mixture was warmed on a hotplate to promote dissolution, and the resulting solution was allowed to stand at room temperature. The acrylic-silane polymer solution, 170 grams, was added to this aqueous polyvinylpyrrolidone solution. While heating the contents of the jar with warm water on a hot plate, the mixture was hand shaken until a homogeneous solution was obtained. This organic polymer solution was allowed to stand at room temperature to cool before use.
  • An inorganic sol gel polymer was prepared as follows.
  • Deionized water (36 grams) was placed in a jar, and polyvinyl alcohol (4 grams, Aldrich, Catalog 36311, CAS [9002-89-5], 96% hydrolyzed, and MW 85,000-100,000) was added to the water while stirring magnetically. This mixture was warmed to 80° C. in a hot water bath to affect dissolution. More deionized water (40 grams) was added to this warm aqueous polyvinyl alcohol solution while continuing to stir. To this warm, diluted aqueous polyvinyl alcohol solution was added colloidal silica dispersion (120 grams, MT-ST Silica, Nissan Chemical Industries, LTD., about 30% silica in methanol) while continuing to stir. Viscosity of this polyvinyl alcohol, silica solution was determined to be A ⁇ by the method of ASTM-D1545.
  • a solution of polyacrylonitrile was prepared by dissolving 12 weight percent of polyacrylonitrile resin (Aldrich, Catalog 181315, CAS [25014-41-9], MW 150,000) in dimethylformaldehyde solvent while warming on a hot plate.
  • polyacrylonitrile resin Aldrich, Catalog 181315, CAS [25014-41-9], MW 150,000
  • the polyacrylonitrile resin solution of Example D was loaded into a 300 ml positive pressure fluid delivery system.
  • a rate of 300 milliliters per hour was fed through a 3 ⁇ 8 inch (9.5 mm) outside diameter teflon tube system to a rotary spray applicator via a 1.1 mm diameter fluid nozzle.
  • the outlet of the nozzle was connected to a rotary bell cup 55 mm in diameter.
  • the fluid nozzle inserts to the back of the bell cup where approximately 80-100% of the fluid exits through a circular slit of approximately 40 mm diameter.
  • the fluid then forms a thin sheet across the bell cup and spins off the edge of the rotary bell cup to form fibers.
  • This rotary bell was set to spin at a rate of 12,000 rpms.
  • the bell cup edge geometry is configured with straight serrations.
  • the perpendicular distance from the circular slit to the edge of the bell cup is approximately 7.85 cm.
  • the bell cup referred to in this experiment is a Durr Behr Eco bell cup model N16010037 type.
  • the bell shaping air was set at 25 psig (1.72 ⁇ 10 5 Pascals) at the back of the bell via a 1 ⁇ 2 inch (12.7 mm) outside diameter nylon tube.
  • the rotary applicator was connected to a high voltage source with a 75,000 Volt indirect charge applied potential.
  • the entire delivery tube, rotary applicator and collector were in a booth that allowed the environmental condition to maintain a relative humidity of approximately 55% to 60% at a room temperature of 70° F. to 72° F. (21° C.-22° C.).
  • Nanofibers were collected on the grounded target onto aluminum panels set at a target/collection distance of 15 inches (38 cm) from the rotary bell and were characterized by optical microscopy and scanning electron microscopy.
  • the nanofibers were essentially cylindrical and had diameters of 600 to 1800 nanometers (nm). Some large diameter fibers were observed that appear to be assemblies of the smaller diameter fibers.
  • the scanning electron micrograph is shown in FIG. 4 and shows many fibers with little or no drops.
  • Example 1 A Design Analysis was completed for the solution of Example 1 to determine application factors with respect to this solution.
  • the application factors studied for this work were bell speed from 12K rpms to 28K rpms, target distance from 10 inches to 20 inches (25.4-50.8 cm), voltage from 60 KV to 90 KV, fluid delivery rate from 100 ml/hour to 300 ml/hour and bell shaping air from 15 psig to 35 psig (1.03 ⁇ 10 5 -2.41 ⁇ 10 5 Pascals).
  • the results reported in FIG. 5 showed that fluid delivery rate, shaping air, and bell speed were the most influential application factors followed by target distance and KV.
  • BS refers to Bell Speed”.
  • SA refers to Shaping Air.
  • FF Fluid Delivery Rate.
  • the values of the vertical axis are the product of the thickness of the nanofiber mat that is formed multiplied by the ratio of nanofiber to drops.
  • the thickness of the mat is given a subjective value of 1 to 10 and the ratio of nanofibers to drops is given a subjective value of 1 to 6.
  • Example 1 the procedure of Example 1 was repeated with the following differences:
  • Nanofibers were attempted to be collected on the grounded aluminum target onto aluminum panels set at a part/collection and were characterized by scanning electron microscopy as shown in FIG. 4 a.
  • the electron microscopy shows very little fiber formation and many wet drops.
  • Example A The hybrid organic—inorganic polymer solution of Example A was spun into nanofibers in accordance with the procedure of Example 1, but using a Dur Behr Eco bell cup model N16010033.
  • the nanofibers were characterized by optical microscopy and scanning electron microscopy.
  • the nanofibers were somewhat flat-faced with cross-sectional dimensions that ranged from 700 nanometers (nm) to 5000 nm.
  • the scanning electron micrograph is shown in FIG. 6 and shows many fibers with little or no wet drops.
  • Example 2 A Design Analysis as described in Example 1 was completed for the solution of Example 2.
  • the application factors studied for this work were bell speed from 12K rpms to 28K rpms, target distance from 10 inches to 20 inches (25.4-38.1 cm), voltage from 60 KV to 90 KV, fluid delivery rate from 100 ml/hour to 300 ml/hour and bell shaping air from 15 psig to 35 psig (1.03 ⁇ 10 5 -2.41 ⁇ 10 5 Pascals).
  • the results reported in FIG. 7 showed that fluid delivery rate, shaping air, bell speed and target distance were the most influential followed by KV.
  • FIG. 7 uses the same terminology as used in FIG. 5 .
  • Example C The inorganic sol gel polymer solution of Example C was spun into nanofibers in accordance with the procedure of Example 2 using a fluid delivery rate of 100 milliliters per hour, a spin rate of 28,000 rpms, a voltage of 90,000 volts and a target collector distance of 20 inches (50.8 cm).
  • the bell shaping air was set at 15 psig (1.03 ⁇ 10 5 Pascals) at the back of the bell. Nanofibers were collected on the grounded aluminum panel target and were characterized by optical microscopy and scanning electron microscopy.
  • the nanofibers were essentially cylindrical and had diameters of 100 to 700 nm. Some of the fibers appeared to have small beads along the linear axis that had not drawn into a fiber. The scanning electron micrograph is shown in FIG. 8 and shows many small fibers with little drop formation.
  • Nanofibers were attempted to be collected on the grounded aluminum target and were characterized by scanning electron microscopy as shown in FIG. 8A .
  • the electron microscopy shows little fibers with wet drops.
  • Example D The polyacrylonitrile resin solution of Example D was spun into fiber in accordance with the procedure of Example 1 using a voltage 86,000. Fibers were collected on the grounded aluminum panel target and were characterized by optical microscopy and scanning electron microscopy. Large fibers collected on the panel. One large fiber was removed from the panel and was evaluated microscopically as shown in FIG. 9 . A low resolution optical image (left-most image) indicated that the large fiber might be an assembly of smaller fibers. Scanning electron microscopy (center image) revealed that these large fibers are a twisted yarn 100 microns in diameter comprised of several much smaller fibers. The yarn is formed as the smaller fibers rotate from the spinning bell cup. Higher magnification (right-most image) revealed that these smaller fibers are nano-scale in diameter within the yarn.
  • Example B The organic polymer solution of Example B was spun into fibers in accordance with the procedure of Example 1 with the following differences:
  • the nanofibers were somewhat flat-faced with cross-sectional dimensions and had diameters of 300 to 700 nm.
  • the scanning electromicrograph is shown in FIG. 10 .
  • the micrograph shows many small fibers with little drop formation.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Nonwoven Fabrics (AREA)
  • Artificial Filaments (AREA)
US12/255,806 2007-10-23 2008-10-22 Fiber formation by electrical-mechanical spinning Abandoned US20090102100A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US12/255,806 US20090102100A1 (en) 2007-10-23 2008-10-22 Fiber formation by electrical-mechanical spinning

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US98184807P 2007-10-23 2007-10-23
US12/255,806 US20090102100A1 (en) 2007-10-23 2008-10-22 Fiber formation by electrical-mechanical spinning

Publications (1)

Publication Number Publication Date
US20090102100A1 true US20090102100A1 (en) 2009-04-23

Family

ID=40228078

Family Applications (1)

Application Number Title Priority Date Filing Date
US12/255,806 Abandoned US20090102100A1 (en) 2007-10-23 2008-10-22 Fiber formation by electrical-mechanical spinning

Country Status (9)

Country Link
US (1) US20090102100A1 (ko)
EP (1) EP2209933A1 (ko)
JP (1) JP2011501790A (ko)
KR (1) KR20100088141A (ko)
CN (1) CN101883882A (ko)
CA (1) CA2703958A1 (ko)
EA (1) EA201070516A1 (ko)
MX (1) MX2010004467A (ko)
WO (1) WO2009055413A1 (ko)

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080242171A1 (en) * 2007-03-29 2008-10-02 Tao Huang Production of nanofibers by melt spinning
US20090232920A1 (en) * 2008-03-17 2009-09-17 Karen Lozano Superfine fiber creating spinneret and uses thereof
US20090326128A1 (en) * 2007-05-08 2009-12-31 Javier Macossay-Torres Fibers and methods relating thereto
US20100072674A1 (en) * 2006-11-24 2010-03-25 Panasonic Corporation Method and apparatus for producing nanofibers and polymer web
US20100148405A1 (en) * 2007-05-21 2010-06-17 Hiroto Sumida Nanofiber producing method and nanofiber producing apparatus
US20100148404A1 (en) * 2007-05-29 2010-06-17 Hiroto Smida Nanofiber spinning method and device
CN102191568A (zh) * 2010-03-16 2011-09-21 北京化工大学 一种利用爬杆效应促进高黏度聚合物熔体静电纺丝的装置
WO2012009521A2 (en) 2010-07-14 2012-01-19 Ppg Industries Ohio, Inc. Filtration media and applications thereof
WO2012027659A2 (en) 2010-08-26 2012-03-01 Ppg Industries Ohio, Inc. Filtration media and applications thereof
CN102373513A (zh) * 2010-08-12 2012-03-14 华东师范大学 水平盘式旋转离心纺丝法
WO2012109240A2 (en) * 2011-02-07 2012-08-16 Fiberio Technology Corporation Split fiber producing devices and methods for the production of microfibers and nanofibers
CN102925995A (zh) * 2012-02-07 2013-02-13 南京理工大学 采用套装针头的新型静电纺丝方法
US8647541B2 (en) 2011-02-07 2014-02-11 Fiberio Technology Corporation Apparatuses and methods for the simultaneous production of microfibers and nanofibers
KR101426738B1 (ko) * 2013-09-11 2014-08-06 전북대학교산학협력단 원심력이 결합된 전기방사를 이용한 나노섬유의 제조방법
CN104060355A (zh) * 2014-06-12 2014-09-24 天津工业大学 一种连续纳米纤维纱的生产方法及装置
CN104862786A (zh) * 2015-05-11 2015-08-26 北京化工大学 一种熔体微分静电纺丝装置
CN105951195A (zh) * 2016-06-24 2016-09-21 武汉纺织大学 一种微重力悬浮式离心纺丝方法
US9644295B2 (en) 2012-08-16 2017-05-09 University Of Washington Through Its Center For Commercialization Centrifugal electrospinning apparatus and methods and fibrous structures produced therefrom
CZ306772B6 (cs) * 2015-12-21 2017-06-28 Technická univerzita v Liberci Způsob výroby polymerních nanovláken elektrickým zvlákňováním roztoku nebo taveniny polymeru, zvlákňovací elektroda pro tento způsob, a zařízení pro výrobu polymerních nanovláken osazené alespoň jednou touto zvlákňovací elektrodou
CN109594135A (zh) * 2018-12-19 2019-04-09 青岛科技大学 一种中心点电极静电纺丝装置及纺丝方法
CN114606583A (zh) * 2022-03-30 2022-06-10 广东工业大学 一种连续式离心静电纺丝装置
US11408096B2 (en) 2017-09-08 2022-08-09 The Board Of Regents Of The University Of Texas System Method of producing mechanoluminescent fibers
US11427937B2 (en) 2019-02-20 2022-08-30 The Board Of Regents Of The University Of Texas System Handheld/portable apparatus for the production of microfibers, submicron fibers and nanofibers
US11958308B1 (en) 2023-05-31 2024-04-16 G13 Innovation In Production Ltd Thermal paper, and methods and systems for forming the same

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5458280B2 (ja) * 2010-01-06 2014-04-02 パナソニック株式会社 ナノファイバ製造装置および製造方法
JP5322112B2 (ja) * 2010-01-18 2013-10-23 パナソニック株式会社 ナノファイバ製造装置および製造方法
CN102061530B (zh) * 2010-12-17 2013-03-13 多氟多化工股份有限公司 离心式静电纺丝装置
JP6118341B2 (ja) 2011-12-21 2017-04-19 イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニーE.I.Du Pont De Nemours And Company 遠心紡糸法によって繊維ウェブを積層する方法
WO2014025794A1 (en) * 2012-08-06 2014-02-13 Fiberio Technology Corporation Devices and methods for the production of microfibers and nanofibers in a controlled environment
CN102965743B (zh) * 2012-12-17 2016-01-27 厦门大学 一种带辅助电极的纳米纤维低压电纺装置
JP6577945B2 (ja) * 2013-10-22 2019-09-18 イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニーE.I.Du Pont De Nemours And Company 高分子ナノファイバ製造装置
CN103696025B (zh) * 2013-12-24 2015-09-02 北京化工大学 一种可控的叠加式双向纺丝装置
CN104099674A (zh) * 2014-05-19 2014-10-15 浙江大东南集团有限公司 一种气流助力式连续纳米纤维膜静电纺丝装置
CN104452109B (zh) * 2014-12-09 2016-01-06 东华大学 一种高透湿通量的纤维基防水透湿膜的静电纺丝方法及其装置
CN105350093B (zh) * 2015-11-13 2018-04-17 广东工业大学 一种负压阵列离心气电纺丝装置
JP6210422B2 (ja) * 2015-12-21 2017-10-11 パナソニックIpマネジメント株式会社 繊維集合体
WO2017110057A1 (ja) * 2015-12-21 2017-06-29 パナソニックIpマネジメント株式会社 繊維集合体
CN105568403B (zh) * 2016-01-27 2017-11-24 广东工业大学 一种具旋转吸气的离心静电纺丝装置
CN108035075A (zh) * 2017-12-14 2018-05-15 武汉纺织大学 一种纳米纤维无纺布的生产装置
CN109881270A (zh) * 2019-04-03 2019-06-14 中国恩菲工程技术有限公司 熔体静电纺丝方法
CN110144632A (zh) * 2019-06-24 2019-08-20 广东工业大学 一种离心静电纺丝装置
CN111441092B (zh) * 2020-05-15 2024-10-25 西安工程大学 一种静电纺丝喷头及具有其的静电纺丝系统及其工作方法

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4808097A (en) * 1986-01-22 1989-02-28 Sanei-Kisetsu Co., Ltd. Apparatus for manufacturing short inorganic fibers
US4937020A (en) * 1988-01-16 1990-06-26 Bayer Aktiengesellschaft Production of very fine polymer fibres
US5114631A (en) * 1990-04-12 1992-05-19 Bayer Aktiengesellschaft Process for the production from thermoplastic polymers of superfine fibre nonwoven fabrics
US5326241A (en) * 1991-04-25 1994-07-05 Schuller International, Inc. Apparatus for producing organic fibers
US5460498A (en) * 1990-08-03 1995-10-24 Imperial Chemicals Industries Plc Centrifugal spinning
US5462571A (en) * 1992-12-07 1995-10-31 Nitto Boseki Co., Ltd. Nozzle tip for spinning glass fiber having deformed cross-section and a plurality of projections
US5494616A (en) * 1993-05-11 1996-02-27 Basf Aktiengesellschaft Production of fibers by centrifugal spinning
US5693117A (en) * 1995-07-12 1997-12-02 Owens-Corning Fiberglas Technology Inc. Radial rotary fiberizer
US20040000604A1 (en) * 1998-03-27 2004-01-01 Kurt Vetter Rotary atomizer for particulate paints
US20050106391A1 (en) * 2001-11-14 2005-05-19 Lawrence Anthony C. Centrifugal spinning process
US20060012084A1 (en) * 2004-07-13 2006-01-19 Armantrout Jack E Electroblowing web formation process
US7105124B2 (en) * 2001-06-19 2006-09-12 Aaf-Mcquay, Inc. Method, apparatus and product for manufacturing nanofiber media
US7118698B2 (en) * 2003-04-03 2006-10-10 E. I. Du Pont De Nemours And Company Rotary process for forming uniform material
US20060228435A1 (en) * 2004-04-08 2006-10-12 Research Triangle Insitute Electrospinning of fibers using a rotatable spray head
US20060290031A1 (en) * 2003-09-08 2006-12-28 Oldrich Jirsak Method of nanofibres production from a polymer solution using electrostatic spinning and a device for carrying out the method
US20080029617A1 (en) * 2006-03-28 2008-02-07 Marshall Larry R Solution spun fiber process
US20080242171A1 (en) * 2007-03-29 2008-10-02 Tao Huang Production of nanofibers by melt spinning
US20080284055A1 (en) * 2003-04-03 2008-11-20 Jack Eugene Armantrout Process for forming uniformly distributed material

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005042813A1 (en) * 2003-10-30 2005-05-12 Clean Air Technology Corp. Electrostatic spinning equipment and method of preparing nano fiber using the same
PL1998798T3 (pl) * 2006-03-28 2013-08-30 Lnk Chemsolutions Llc Sposób wytwarzania włóknistych bandaży hemostatycznych
WO2008004712A2 (en) * 2006-07-05 2008-01-10 Panasonic Corporation Method and apparatus for producing nanofibers and polymeric webs
DE112007002799T5 (de) * 2006-11-24 2009-10-01 Panasonic Corp., Kadoma Verfahren und Vorrichtung zur Erzeugen von Nanofasern und eines Polymervlieses
US8088323B2 (en) 2007-02-27 2012-01-03 Ppg Industries Ohio, Inc. Process of electrospinning organic-inorganic fibers

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4808097A (en) * 1986-01-22 1989-02-28 Sanei-Kisetsu Co., Ltd. Apparatus for manufacturing short inorganic fibers
US4937020A (en) * 1988-01-16 1990-06-26 Bayer Aktiengesellschaft Production of very fine polymer fibres
US5114631A (en) * 1990-04-12 1992-05-19 Bayer Aktiengesellschaft Process for the production from thermoplastic polymers of superfine fibre nonwoven fabrics
US5460498A (en) * 1990-08-03 1995-10-24 Imperial Chemicals Industries Plc Centrifugal spinning
US5326241A (en) * 1991-04-25 1994-07-05 Schuller International, Inc. Apparatus for producing organic fibers
US5462571A (en) * 1992-12-07 1995-10-31 Nitto Boseki Co., Ltd. Nozzle tip for spinning glass fiber having deformed cross-section and a plurality of projections
US5494616A (en) * 1993-05-11 1996-02-27 Basf Aktiengesellschaft Production of fibers by centrifugal spinning
US5693117A (en) * 1995-07-12 1997-12-02 Owens-Corning Fiberglas Technology Inc. Radial rotary fiberizer
US20040000604A1 (en) * 1998-03-27 2004-01-01 Kurt Vetter Rotary atomizer for particulate paints
US7105124B2 (en) * 2001-06-19 2006-09-12 Aaf-Mcquay, Inc. Method, apparatus and product for manufacturing nanofiber media
US20050106391A1 (en) * 2001-11-14 2005-05-19 Lawrence Anthony C. Centrifugal spinning process
US7118698B2 (en) * 2003-04-03 2006-10-10 E. I. Du Pont De Nemours And Company Rotary process for forming uniform material
US20080284055A1 (en) * 2003-04-03 2008-11-20 Jack Eugene Armantrout Process for forming uniformly distributed material
US20060290031A1 (en) * 2003-09-08 2006-12-28 Oldrich Jirsak Method of nanofibres production from a polymer solution using electrostatic spinning and a device for carrying out the method
US20060228435A1 (en) * 2004-04-08 2006-10-12 Research Triangle Insitute Electrospinning of fibers using a rotatable spray head
US20060012084A1 (en) * 2004-07-13 2006-01-19 Armantrout Jack E Electroblowing web formation process
US20080029617A1 (en) * 2006-03-28 2008-02-07 Marshall Larry R Solution spun fiber process
US20080242171A1 (en) * 2007-03-29 2008-10-02 Tao Huang Production of nanofibers by melt spinning

Cited By (40)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8110136B2 (en) * 2006-11-24 2012-02-07 Panasonic Corporation Method and apparatus for producing nanofibers and polymer web
US20100072674A1 (en) * 2006-11-24 2010-03-25 Panasonic Corporation Method and apparatus for producing nanofibers and polymer web
US8277711B2 (en) 2007-03-29 2012-10-02 E I Du Pont De Nemours And Company Production of nanofibers by melt spinning
US20080242171A1 (en) * 2007-03-29 2008-10-02 Tao Huang Production of nanofibers by melt spinning
US20090326128A1 (en) * 2007-05-08 2009-12-31 Javier Macossay-Torres Fibers and methods relating thereto
US20100148405A1 (en) * 2007-05-21 2010-06-17 Hiroto Sumida Nanofiber producing method and nanofiber producing apparatus
US20100148404A1 (en) * 2007-05-29 2010-06-17 Hiroto Smida Nanofiber spinning method and device
US8163227B2 (en) * 2007-05-29 2012-04-24 Panasonic Corporation Nanofiber spinning method and device
US20090280207A1 (en) * 2008-03-17 2009-11-12 Karen Lozano Superfine fiber creating spinneret and uses thereof
US20090280325A1 (en) * 2008-03-17 2009-11-12 Karen Lozano Methods and apparatuses for making superfine fibers
US20090269429A1 (en) * 2008-03-17 2009-10-29 Karen Lozano Superfine fiber creating spinneret and uses thereof
US8231378B2 (en) 2008-03-17 2012-07-31 The Board Of Regents Of The University Of Texas System Superfine fiber creating spinneret and uses thereof
US8828294B2 (en) 2008-03-17 2014-09-09 Board Of Regents Of The University Of Texas System Superfine fiber creating spinneret and uses thereof
US20090232920A1 (en) * 2008-03-17 2009-09-17 Karen Lozano Superfine fiber creating spinneret and uses thereof
US8721319B2 (en) 2008-03-17 2014-05-13 Board of Regents of the University to Texas System Superfine fiber creating spinneret and uses thereof
CN102191568A (zh) * 2010-03-16 2011-09-21 北京化工大学 一种利用爬杆效应促进高黏度聚合物熔体静电纺丝的装置
WO2012009521A2 (en) 2010-07-14 2012-01-19 Ppg Industries Ohio, Inc. Filtration media and applications thereof
CN102373513A (zh) * 2010-08-12 2012-03-14 华东师范大学 水平盘式旋转离心纺丝法
WO2012027659A2 (en) 2010-08-26 2012-03-01 Ppg Industries Ohio, Inc. Filtration media and applications thereof
US8647541B2 (en) 2011-02-07 2014-02-11 Fiberio Technology Corporation Apparatuses and methods for the simultaneous production of microfibers and nanofibers
US8647540B2 (en) 2011-02-07 2014-02-11 Fiberio Technology Corporation Apparatuses having outlet elements and methods for the production of microfibers and nanofibers
US8658067B2 (en) 2011-02-07 2014-02-25 Fiberio Technology Corporation Apparatuses and methods for the deposition of microfibers and nanofibers on a substrate
US8709309B2 (en) 2011-02-07 2014-04-29 FibeRio Technologies Corporation Devices and methods for the production of coaxial microfibers and nanofibers
US8777599B2 (en) 2011-02-07 2014-07-15 Fiberio Technology Corporation Multilayer apparatuses and methods for the production of microfibers and nanofibers
US8778240B2 (en) 2011-02-07 2014-07-15 Fiberio Technology Corporation Split fiber producing devices and methods for the production of microfibers and nanofibers
WO2012109240A2 (en) * 2011-02-07 2012-08-16 Fiberio Technology Corporation Split fiber producing devices and methods for the production of microfibers and nanofibers
WO2012109240A3 (en) * 2011-02-07 2013-02-28 Fiberio Technology Corporation Split fiber producing devices and methods for the production of microfibers and nanofibers
US9394627B2 (en) 2011-02-07 2016-07-19 Clarcor Inc. Apparatuses having outlet elements and methods for the production of microfibers and nanofibers
CN102925995A (zh) * 2012-02-07 2013-02-13 南京理工大学 采用套装针头的新型静电纺丝方法
US9644295B2 (en) 2012-08-16 2017-05-09 University Of Washington Through Its Center For Commercialization Centrifugal electrospinning apparatus and methods and fibrous structures produced therefrom
KR101426738B1 (ko) * 2013-09-11 2014-08-06 전북대학교산학협력단 원심력이 결합된 전기방사를 이용한 나노섬유의 제조방법
CN104060355A (zh) * 2014-06-12 2014-09-24 天津工业大学 一种连续纳米纤维纱的生产方法及装置
CN104862786A (zh) * 2015-05-11 2015-08-26 北京化工大学 一种熔体微分静电纺丝装置
CZ306772B6 (cs) * 2015-12-21 2017-06-28 Technická univerzita v Liberci Způsob výroby polymerních nanovláken elektrickým zvlákňováním roztoku nebo taveniny polymeru, zvlákňovací elektroda pro tento způsob, a zařízení pro výrobu polymerních nanovláken osazené alespoň jednou touto zvlákňovací elektrodou
CN105951195A (zh) * 2016-06-24 2016-09-21 武汉纺织大学 一种微重力悬浮式离心纺丝方法
US11408096B2 (en) 2017-09-08 2022-08-09 The Board Of Regents Of The University Of Texas System Method of producing mechanoluminescent fibers
CN109594135A (zh) * 2018-12-19 2019-04-09 青岛科技大学 一种中心点电极静电纺丝装置及纺丝方法
US11427937B2 (en) 2019-02-20 2022-08-30 The Board Of Regents Of The University Of Texas System Handheld/portable apparatus for the production of microfibers, submicron fibers and nanofibers
CN114606583A (zh) * 2022-03-30 2022-06-10 广东工业大学 一种连续式离心静电纺丝装置
US11958308B1 (en) 2023-05-31 2024-04-16 G13 Innovation In Production Ltd Thermal paper, and methods and systems for forming the same

Also Published As

Publication number Publication date
CN101883882A (zh) 2010-11-10
CA2703958A1 (en) 2009-04-30
JP2011501790A (ja) 2011-01-13
EP2209933A1 (en) 2010-07-28
EA201070516A1 (ru) 2010-12-30
MX2010004467A (es) 2010-05-03
WO2009055413A1 (en) 2009-04-30
KR20100088141A (ko) 2010-08-06

Similar Documents

Publication Publication Date Title
US20090102100A1 (en) Fiber formation by electrical-mechanical spinning
Long et al. Electrospinning: the setup and procedure
KR101417142B1 (ko) 용액 방사 섬유 제조방법
KR101680908B1 (ko) 원심식 용액 방사 나노섬유 방법
Wang et al. Electrospun poly (methyl methacrylate) nanofibers and microparticles
JP4975613B2 (ja) 回転可能なスプレーヘッドを用いたファイバーのエレクトロスピニング
US8241537B2 (en) Method for manufacturing polymeric fibrils
US20050104258A1 (en) Patterned electrospinning
CN109537073B (zh) 一种利用溶液吹纺技术制备定向排列纤维的装置和方法
CN109097849B (zh) 纳米纤维发生装置
KR20180069118A (ko) 교류형 전자분무 제조 및 그의 생성물
BRPI0903844A2 (pt) método e aparelho para produzir mantas de micro e/ou nanofibras a partir de polìmeros, seu usos e método de revestimento
Sun et al. Research on parametric model for polycaprolactone nanofiber produced by centrifugal spinning
CN105350098A (zh) 一种具有三维结构的纳米纤维支架制备装置及方法
KR20150116492A (ko) 나노섬유 구조체의 제조방법
CN113913954B (zh) 一种基于溶液雾化和静电-气流接替牵伸的极细纳米纤维制备装置及方法
JP5253319B2 (ja) 不織布製造装置及び不織布の製造方法
Amith et al. Development of electrospinning system for synthesis of polyvinylpyrrolidone thin films for sensor applications
KR20100070203A (ko) 수직 기류 및 원심력을 이용한 나노섬유로 구성된 섬유집합체의 제조장치 및 제조방법
KR101102999B1 (ko) 수직기류를 이용한 전기방사장치
CN212655894U (zh) 纤维制备系统
JP4904083B2 (ja) 静電紡糸法により高分子化合物繊維構造体を製造する装置
Derch et al. Polymer nanofibers prepared by electrospinning
JP4954946B2 (ja) ナノファイバ製造装置
CN116180326B (zh) 加湿膜、加湿膜的制备方法和空气处理设备

Legal Events

Date Code Title Description
AS Assignment

Owner name: PPG INDUSTRIES OHIO, INC., OHIO

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:HELLRING, STUART D.;CAMPBELL, MELANIE S.;MUNRO, CALUM H.;REEL/FRAME:021999/0137

Effective date: 20081022

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION