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US20080070463A1 - Nanowebs - Google Patents

Nanowebs Download PDF

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Publication number
US20080070463A1
US20080070463A1 US11/523,827 US52382706A US2008070463A1 US 20080070463 A1 US20080070463 A1 US 20080070463A1 US 52382706 A US52382706 A US 52382706A US 2008070463 A1 US2008070463 A1 US 2008070463A1
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US
United States
Prior art keywords
nanoweb
web
nonwoven
roll
less
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
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US11/523,827
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English (en)
Inventor
Pankaj Arora
Guanghui Chen
Simon Frisk
David Keith Graham
Robert Anthony Marin
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.)
EIDP Inc
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Individual
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 Individual filed Critical Individual
Priority to US11/523,827 priority Critical patent/US20080070463A1/en
Assigned to E. I. DU PONT DE NEMOURS AND COMPANY reassignment E. I. DU PONT DE NEMOURS AND COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MARIN, ROBERT ANTHONY, CHEN, GUANGHUI, FRISK, SIMON, GRAHAM, DAVID KEITH, JR., ARORA, PANKAJ
Priority to EP07852413.9A priority patent/EP2064379B1/fr
Priority to KR1020097005356A priority patent/KR101516436B1/ko
Priority to BRPI0715159-4A2A priority patent/BRPI0715159A2/pt
Priority to CN2007800345429A priority patent/CN101558194B/zh
Priority to PCT/US2007/020334 priority patent/WO2008036332A2/fr
Priority to JP2009529230A priority patent/JP5615547B2/ja
Assigned to E. I. DU PONT DE NEMOURS AND COMPANY reassignment E. I. DU PONT DE NEMOURS AND COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SUH, HAGEUN
Publication of US20080070463A1 publication Critical patent/US20080070463A1/en
Priority to US12/496,242 priority patent/US8697587B2/en
Abandoned legal-status Critical Current

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    • D—TEXTILES; PAPER
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    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
    • B01D39/163—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin sintered or bonded
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    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
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    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/411—Organic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/44—Fibrous material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
    • H01M50/494—Tensile strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/025—Types of fibres, filaments or particles, self-supporting or supported materials comprising nanofibres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/27—Web or sheet containing structurally defined element or component, the element or component having a specified weight per unit area [e.g., gms/sq cm, lbs/sq ft, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/298—Physical dimension
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T442/10—Scrim [e.g., open net or mesh, gauze, loose or open weave or knit, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T442/608—Including strand or fiber material which is of specific structural definition
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T442/608—Including strand or fiber material which is of specific structural definition
    • Y10T442/614—Strand or fiber material specified as having microdimensions [i.e., microfiber]
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    • Y10T442/647—Including a foamed layer or component
    • Y10T442/651—Plural fabric layers
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    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/659—Including an additional nonwoven fabric

Definitions

  • the present invention is directed towards an improved nonwoven web comprising nanofibers and a process for consolidating and stabilizing such a web.
  • Nanowebs are nonwoven webs comprising primarily, or even exclusively, fibers that have a number average diameter of less than one micrometer. Due to their extremely small pore dimensions and high surface area to volume ratio, nanowebs have been expected to be utilized as substrates for many applications such as, for example, high performance air filtration, waste water filtration, filtration membranes for biological contaminants, separators for batteries and other energy storage devices. However, one disadvantage of nanowebs for these applications is their poor mechanical integrity.
  • Nanowebs made for example by electrospinning or electroblowing also tend to have low solids volume content (solidity), typically less than about 20%.
  • Unsupported nanowebs also exhibit an excessive reduction in width (“necking”) when tension is applied in the machine direction (MD), such as when winding or post processing, for example, when applying surface treatments and laminating for some product applications. Where the material is unwound and wound again, varying tensions can result in different widths and potentially create variations in sheet properties. A material is desired which is more robust with regard to applied tension.
  • necking when tension is applied in the machine direction (MD), such as when winding or post processing, for example, when applying surface treatments and laminating for some product applications.
  • the low surface stability of electrospun and electroblown nanowebs also creates problems when handling the sheet or when the sheet goes over rolls or other surfaces. Fibers are removed from the sheet and collect on various contact surfaces, such as hands, rolls, guides, etc., and sheet properties can be potentially changed and/or process equipment contaminated with fibers. A material with a more stable surface is desired.
  • as-spun nanowebs typically yields structures with a solidity in the range of 20% to 10% or even lower. This open structure provides low resistance to fluid flow and/or ion flow due to the low solidity, which conversely can be reported as large total pore volume percent or “porosity”.
  • as-spun nanowebs typically have maximum pore sizes between fibers of in the range of about 0.5 to 10 micrometers, even as high as 20 micrometers, and mean flow pore size ranges between about 0.05 to 10 micrometers.
  • Some fabric applications require smaller pore size and hence higher web solidity, approaching or even within the 40% to 90% range. These fabrics exhibit higher filtration efficiency and in general better overall barrier properties for fluids, and resistance to “short-circuit” in battery separator and other energy storage applications. Other applications require low air flow and low liquid flow while yielding a low resistance to moisture vapor transmission and require the higher % solidity materials or small pores.
  • Conventional nanowebs are currently excluded from these applications that require higher solidity, since there is typically not enough nanoweb material to modify to smaller pore size and higher solidity. Instead, nonwoven webs which can be produced in commercially acceptable sizes and basis weights, such as meltblown webs, are often used in such applications.
  • meltblown webs consist of much larger fibers, typically between about 2 to 10 micrometers in diameter, and modification of as-spun meltblown webs to meet the small pore size limitations necessary for high filtration efficiency requires high solidifies, even as high as about 80%, and results in dramatic decreases in fluid flow rates through such modified meltblown webs.
  • “As-spun” nanowebs also exhibit relatively high surface drag or friction, a surface coefficient of friction as high as about 2.5. Some material applications require smoother or softer, low friction hand. Other applications require a smooth outer surface for filter cake release, or low liquid flow resistance. For a material to be used in these applications, it requires a “smooth” surface which promotes low friction and high wear resistance.
  • calendering is the process of passing a sheet material through a nip between rolls or plates to impart a smooth, glossy appearance to the sheet material or otherwise improving selected physical properties.
  • U.S. Pat. No. 4,606,264 provides a method and apparatus for temperature gradient calendering, wherein paper or like material is passed into at least one nip formed by an iron roll and a soft roll. The iron roll is heated to at least the temperature at which the fibers in the web begin to deform; for paper, that temperature is approximately 350° F. As therein disclosed, it is preferred that the web is passed through two successive nips, one for glazing one face of the web and the other for glazing the opposite face.
  • Poisson's Ratio times basis weight is disclosed to be limited to less than 1.2, but Poisson's Ratios of the order of 2.5 to 4 are exemplified.
  • a bonding pattern is described that strengthens a web but at the cost of a considerable reduction in open area or porosity.
  • the present invention is directed to increasing the utility of nanowebs by improving their physical properties while maintaining a high open area and hence porosity, and to the webs produced thereby.
  • the product of the invention is a nonwoven nanoweb comprising a web of polymer nanofibers having a Poisson Ratio of less than about 0.8, a solidity of at least about 20%, a basis weight of at least about 1 gram per square meter (gsm), and a thickness of at least about 1 ⁇ m.
  • the invention is also directed to a nonwoven web formed by calendering a polymeric nanoweb through a nip between a first roll and a second roll and applying a pressure to the web across the thickness of the web, wherein one of the first roll and the second roll is a hard roll, the other roll being a soft roll having a hardness less than Rockwell B 70, and heating the web to a temperature between the T g and T om of the nanoweb polymer, where T om is defined as the temperature of the onset of melting, wherein the nanoweb has less than about 15% by area in the plane of the web comprising melted regions.
  • the invention is also directed to a process for stabilizing the surface of an electroblown or electrospun polymeric nanoweb comprising calendering the web through a nip between a first roll and a second roll and applying pressure to the web across the thickness of the web, wherein one of the first roll and the second roll is a hard roll, the other roll being a soft roll, and heating the web to between its T g and its T om .
  • the invention is directed to a nonwoven nanoweb comprising polymer nanofibers having a solidity of at least about 20%, a basis weight of at least about 1 gsm, a thickness of between about 1 ⁇ m and 400 ⁇ m and a maximum pore size of about 5 micrometers, wherein the nanoweb has less than about 15% by area in the plane of the web comprising melted regions.
  • FIG. 1 is a photomicrograph of an as-spun nanoweb derived from the electroblowing process, described herein as Comparative Example 1.
  • FIG. 2 is a photomicrograph of a nanoweb calendered between two hard rolls, showing melted regions in the nanoweb.
  • FIGS. 3 a and 3 b are photomicrographs of a nanoweb calendered in the manner of the present invention.
  • nonwoven means a web including a multitude of randomly distributed fibers.
  • the fibers generally can be bonded to each other or can be unbonded.
  • the fibers can be staple fibers or continuous fibers.
  • the fibers can comprise a single material or a multitude of materials, either as a combination of different fibers or as a combination of similar fibers each comprised of different materials.
  • “Calendering” is the process of passing a web through a nip between two rolls.
  • the rolls may be in contact with each other, or there may be a fixed or variable gap between the roll surfaces.
  • the nip is formed between a soft roll and a hard roll.
  • the “soft roll” is a roll that deforms under the pressure applied to keep two rolls in a calender together.
  • the “hard roll” is a roll with a surface in which no deformation that has a significant effect on the process or product occurs under the pressure of the process.
  • An “unpatterned” roll is one which has a smooth surface within the capability of the process used to manufacture them. There are no points or patterns to deliberately produce a pattern on the web as it passed through the nip, unlike a point bonding roll.
  • a “scrim” is a support layer and can be any planar structure with which the nanoweb can be bonded, adhered or laminated.
  • the scrim layers useful in the present invention are spunbond nonwoven layers, but can be made from carded webs of nonwoven fibers and the like. Scrim layers useful for some filter applications require sufficient stiffness to hold pleats and dead folds.
  • machine direction means the direction in which the length of a fabric is produced on the machine that produces it.
  • cross direction means the width of a fabric, i.e., a direction generally perpendicular to the MD and the thickness direction of the web.
  • Poisson Ratio is a measurement of the dimensional stability of the fabric in the cross direction. The lower the Poisson Ratio, the better the dimensional stability of the fabric. In particular, the Poisson Ratio is a measurement of the relative change in width with a change in length. The better the dimensional stability of the fabric, the lesser the tendency of the fabric to “neck in” during the converting process.
  • the Poisson Ratio (PR) is a dimensionless number calculated by the following formula:
  • PR ⁇ ( W 0 ⁇ W i )/ W 0 ⁇ / ⁇ ( L i ⁇ L 0 )/ L 0 ⁇ ;
  • W 0 is the initial sample width
  • W i is the sample width at an extended length L i
  • L 0 is the initial sample length
  • the value of L 0 is a minimum of four (4) times the value of W 0
  • L i is the sample length at a given extension.
  • the “footprint” is the area of the web that is compressed as it passes between the two calendar rolls.
  • the footprint can be measured by the length that the web is compressed in the MD at any point along the CD of the web.
  • melted region is meant a region of the web, whether or not traversing the entire web, which is visible to the naked eye or in a micrograph and which comprises fibers that have been fused into each other and lost their individual shape.
  • photomicrographs of nanowebs calendered between two hard, stainless steel rolls show spots where fibers have been fused into each other to form a bond and the fibers have lost their fibrous character.
  • FIG. 2 shows an example of such a photomicrograph, in which areas of melting can be seen, wherein the fibers are essentially merged into each other.
  • adheresively bonded is meant that a material is introduced into the web that bonds fibers together in selected areas upon action of heat or removal of solvent.
  • discrete discontinuous bonded areas regions in the plane of the web in which separate fibers are bonded to each other at some point, said regions not forming one continuous region that extends from any one edge of the web to another edge.
  • discrete discontinuous unbonded areas regions in the plane of the web in which separate fibers are not bonded to each other at any point, said regions not forming one continuous region that extends from any one edge of the web to another edge.
  • nanofiber refers to fibers having a number average diameter or cross-section less than about 1000 nm, even less than about 800 nm, even between about 50 nm and 500 nm, and even between about 100 and 400 nm.
  • diameter as used herein includes the greatest cross-section of non-round shapes.
  • the invention is a nonwoven web comprising polymeric nanofibers, said web having a Poisson's Ratio of less than about 0.8, even less than about 0.3, even less than about 0.2 and even less than about 0.1.
  • the invention is directed to a nonwoven web optionally having discrete discontinuous either bonded or unbonded areas and having less than about 15% of the area in the plane of the web comprising melted regions and being not adhesively bonded.
  • the nonwoven web comprises less than about 10%, even less than about 5% or even less than about 1% melted regions by area in the plane of the web.
  • the improved nanowebs of the invention resist Necking, such that when a tension of 100 g/cm is applied in the MD, the improved nanowebs demonstrate Necking of less than about 10%, or even less than about 5%, or even less than about 2%, or even less than about 1%.
  • the nonwoven web of the invention can have a solidity of between about 10% to about 80%, even between about 20% to about 60% and even between about 20% to about 40%, and the basis weight of the web can be at least about 1 gsm, even at least about 2 gsm, even at least about 5 gsm and even at least about 20 gsm. In still further embodiment, the nonwoven web has a basis weight of less than about 50 gsm.
  • the nonwoven web of the invention has a minimum thickness of about 1 micrometer, and no maximum thickness. In alternative embodiments the thickness can be a maximum of about 800 micrometers or even about 400 micrometers.
  • the nonwoven web can be any of the above mentioned webs which has a MD tensile stress at break of at least about 600 psi (4.1 MPa), even at least about 1000 psi (6.9 MPa), and even at least about 2000 psi (13.8 MPa), or a MD tensile modulus of at least about 10,000 psi (69 MPa), even at least about 20,000 psi (138 MPa), and even at least about 40,000 psi (276 MPa), or both.
  • a MD tensile stress at break of at least about 600 psi (4.1 MPa), even at least about 1000 psi (6.9 MPa), and even at least about 2000 psi (13.8 MPa), or a MD tensile modulus of at least about 10,000 psi (69 MPa), even at least about 20,000 psi (138 MPa), and even at least about 40,000 psi (276 MPa), or both.
  • the nonwoven web can be any of the above mentioned webs and which has a Surface Stability Index of greater than about 100 lbf/inch (17,513 N/m), or a surface coefficient of friction of less than about 0.9, or both.
  • the improved nanowebs of the present invention can demonstrate maximum pore sizes, measured as Bubble Point (BP), in the range of about 0.1 micrometer to about 15 micrometers, even between about 0.5 micrometer to about 2.5 micrometers, and mean flow pore sizes (MFP) in the range of between about 0.01 micrometer to about 5 micrometers, even between about 0.2 micrometer to about 3 micrometers, or even between about 0.2 micrometer and 1.5 micrometers.
  • An indication of the pore size distributions of the improved nanowebs of the invention can be determined by the ratio of the BP/MFP, which can be in the range of about 1.1 to about 6, even from about 1.1 to about 4.
  • the as-spun nonwoven web comprises primarily or exclusively nanofibers that are produced by electrospinning, such as classical electrospinning or electroblowing, and in certain circumstances, by meltblowing processes.
  • Classical electrospinning is a technique illustrated in U.S. Pat. No. 4,127,706, incorporated herein in its entirety, wherein a high voltage is applied to a polymer in solution to create nanofibers and nonwoven mats.
  • total throughput in electrospinning processes is too low to be commercially viable in forming heavier basis weight webs.
  • a stream of polymeric solution comprising a polymer and a solvent is fed from a storage tank to a series of spinning nozzles within a spinneret, to which a high voltage is applied and through which the polymeric solution is discharged. Meanwhile, compressed air that is optionally heated is issued from air nozzles disposed in the sides of, or at the periphery of the spinning nozzle. The air is directed generally downward as a blowing gas stream which envelopes and forwards the newly issued polymeric solution and aids in the formation of the fibrous web, which is collected on a grounded porous collection belt above a vacuum chamber.
  • the electroblowing process permits formation of commercial sizes and quantities of nanowebs at basis weights in excess of about 1 gsm, even as high as about 40 gsm or greater, in a relatively short time period.
  • a substrate or scrim can be arranged on the collector to collect and combine the nanofiber web spun on the substrate, so that the combined fiber web is used as a high-performance filter, wiper and so on.
  • the substrate may include various nonwoven cloths, such as meltblown nonwoven cloth, needle-punched or spunlaced nonwoven cloth, woven cloth, knitted cloth, paper and the like, and can be used without limitations so long as a nanofiber layer can be added on the substrate.
  • the following electroblowing process conditions can be used to manufacture the web of the invention.
  • Voltage applied to the spinneret is preferably in the range of about 1 to 300 kV and more preferably of about 10 to 100 kV.
  • the polymer solution can be discharged in a pressure ranging from about 0.01 to 200 kg/cm 2 and in preferably about 0.1 to 20 kg/cm 2 . This allows the polymer solution to be discharged in large quantity in an adequate manner for mass production.
  • the process of the invention can discharge the polymer solution with a discharge rate of about 0.1 to 5 cc/min-hole.
  • Compressed air injected via the air nozzle has a flow rate of about 10 to 10,000 m/min and preferably of about 100 to 3,000 m/min.
  • Air temperature is preferably in the range of about 300° C. and more preferably of about 100° C.
  • the die to collector distance (DCD), i.e. the distance between the lower end of the spinning nozzle and the suction collector, is preferably about 1 to 200 cm and more preferably 10 to 50 cm.
  • Polymer materials that can be used in forming the nanowebs of the invention are not particularly limited and include both addition polymer and condensation polymer materials such as, polyacetal, polyamide, polyester, polyolefins, cellulose ether and ester, polyalkylene sulfide, polyarylene oxide, polysulfone, modified polysulfone polymers and mixtures thereof.
  • Preferred materials that fall within these generic classes include, poly(vinylchloride), polymethylmethacrylate (and other acrylic resins), polystyrene, and copolymers thereof (including ABA type block copolymers), poly(vinylidene fluoride), poly(vinylidene chloride), polyvinylalcohol in various degrees of hydrolysis (87% to 99.5%) in crosslinked and non-crosslinked forms.
  • Preferred addition polymers tend to be glassy (a T g greater than room temperature). This is the case for polyvinylchloride and polymethylmethacrylate, polystyrene polymer compositions or alloys or low in crystallinity for polyvinylidene fluoride and polyvinylalcohol materials.
  • polyamide condensation polymers are nylon materials, such as nylon-6, nylon-6,6, nylon 6,6-6,10 and the like.
  • any thermoplastic polymer capable of being meltblown into nanofibers can be used, including polyolefins, such as polyethylene, polypropylene and polybutylene, polyesters such as poly(ethylene terephthalate) and polyamides, such as the nylon polymers listed above.
  • plasticizers can be added to the various polymers described above, in order to reduce the T g of the fiber polymer.
  • Suitable plasticizers will depend upon the polymer to be electrospun or electroblown, as well as upon the particular end use into which the nanoweb will be introduced.
  • nylon polymers can be plasticized with water or even residual solvent remaining from the electrospinning or electroblowing process.
  • the Handbook of Plasticizers edited by George Wypych, 2004 Chemtec Publishing, incorporated herein by reference, discloses other polymer/plasticizer combinations which can be used in the present invention.
  • the as-spun nanoweb of the present invention can be calendered in order to impart the desired improvements in physical properties.
  • the as-spun nanoweb is fed into the nip between two unpatterned rolls in which one roll is an unpatterned soft roll and one roll is an unpatterned hard roll, and the temperature of the hard roll is maintained at a temperature that is between the T g , herein defined as the temperature at which the polymer undergoes a transition from glassy to rubbery state, and the T om , herein defined as the temperature of the onset of melting of the polymer, such that the nanofibers of the nanoweb are at a plasticized state when passing through the calendar nip.
  • the composition and hardness of the rolls can be varied to yield the desire end use properties.
  • one roll is a hard metal, such as stainless steel, and the other a soft-metal or polymer-coated roll or a composite roll having a hardness less than Rockwell B 70.
  • the residence time of the web in the nip between the two rolls is controlled by the line speed of the web, preferably between about 1 m/min and about 50 m/min, and the footprint between the two rolls is the MD distance that the web travels in contact with both rolls simultaneously.
  • the footprint is controlled by the pressure exerted at the nip between the two rolls and is measured generally in force per linear CD dimension of roll, and is preferably between about 1 mm and about 30 mm.
  • the nonwoven web can be stretched, optionally while being heated to a temperature that is between the T g and the lowest T om of the nanofiber polymer.
  • the stretching can take place either before and/or after the web is fed to the calender rolls, and in either or both of the MD or CD.
  • SMI Surface Stability Index
  • MTS QUESTTM 5 An extensometer
  • a steel plate approximately 4′′ ⁇ 6′′ was placed on top of the magnet.
  • a piece of 2-sided tape was firmly attached, the tape being about 2.5′′ wide and about 3′′ long.
  • a piece of the material to be tested, at least 2′′ ⁇ 2′′ was laid gently, but smoothly atop the 2-sided tape. Care was taken not to disrupt the surface of the material being tested; wrinkles and folds were avoided.
  • the probe was allowed to travel downward (toward the sample) at a continuous rate of 0.050 in/min. The probe continued down until a normal force of 0.5 lbs was established between the sample and the probe. The probe remained in this position for 10 seconds. The probe direction was then reversed and it traveled away from the sample at a continuous rate of 0.010 in/min. This motion continued until the crosshead reached its starting point.
  • the end point was chosen along the linear portion of the unloading curve, at a point more than 10 ⁇ m (in extension) from the start point.
  • the test software automatically fitted a least squares linear trendline to the data between the start point and end point and the slope of the trend line was reported in lb/in (N/m).
  • the absolute value of the slope was reported as SSI.
  • Basis Weight was determined by ASTM D-3776, which is hereby incorporated by reference and reported in g/m 2 (gsm).
  • Fiber Diameter was determined as follows. Ten scanning electron microscope (SEM) images at 5,000 ⁇ magnification were taken of each fine fiber layer sample. The diameter of eleven (11) clearly distinguishable fine fibers were measured from the photographs and recorded. Defects were not included (i.e., lumps of fine fibers, polymer drops, intersections of fine fibers). The average (mean) fiber diameter for each sample was calculated.
  • Thickness was determined by ASTM D-645 (or ISO 534), which is hereby incorporated by reference, under an applied load of 50 kPa and an anvil surface area of 200 mm 2 . The thickness is reported in mils and converted to micrometers.
  • Ionic Resistance in organic electrolyte is a measure of a separator's resistance to the flow of ions, and was determined as follows. Samples were cut into small pieces (1.5 cm diameter) and soaked in 2 M solution of LiCl in methanol electrolyte. The separator resistance was measured using Solartron 1287 Electrochemical Interface along with Solartron 1252 Frequency Response Analyzer and the Zplot software. The test cell had a 0.3165 square cm electrode area that contacts the wetted separator.
  • MacMullin Number is a dimensionless number and is a measure of the ionic resistance of the separator, and is defined as the ratio of the resistivity of a separator sample filled with electrolyte to the resistivity of an equivalent volume of the electrolyte alone. It is expressed by:
  • Nm ( R separator ⁇ A electrode )/( ⁇ electrolyte ⁇ t separator ),
  • R separator is the resistance of the separator in ohms
  • a electrode is the area of electrode in cm 2
  • ⁇ electrolyte is the resistivity of electrolyte in ohms-cm
  • t separator is the thickness of separator in cm.
  • the resistivity of 2 M solution of LiCl in methanol electrolyte at 25° C. is 50.5 ohms-cm.
  • Tensile Modulus was measured on an extensometer (MTS QUESTTM 5) at a constant rate of elongation of 2 inches per minute. Samples were cut to a size of 1 inch ⁇ 8 inches, being longer in the direction of loading. The gage length of samples was 6 inches and the starting width of samples was 1 inch.
  • the Tensile Modulus (aka Modulus of Elasticity, Young's Modulus) is defined as the slope of a line tangential to the low-strain part of a graph of Stress(s) vs. Strain(e). Samples were tested in both the machine and cross directions.
  • the static coefficient of friction was measured in accordance with TAPPI Method T 503, using a Testing Machines Incoroporated (Amityville, N.Y.) Coefficient of Friction Tester model no. 32-25.
  • a sample was mounted on an inclined plane, with a matching sample mounted to the bottom of a 2.5′′ square metal sled.
  • the metal sled had a conductive flap attached, which mounted into a circuit at the left end of the inclined plane.
  • At the right end of the plane there was an electric motor which increased the angle of elevation of the plane compared to level at a rate of 1.5 ⁇ 0.5 degrees per second.
  • the switch at the left end of the plane was broken, and the electric motor stopped. The angle at which the plane rested was recorded.
  • the static coefficient of friction was the tangent of this angle.
  • the examples were spun from polyamide (Nylon-6,6) with a T om of about 215° C.
  • as-spun nanofiber sheets with number average fiber diameters of about 717 microns and target basis weights of about 18 gsm were calendered, by delivering a nanofiber sheet to a two roll calender nip from an unwind.
  • a device for spreading the sheet prior to the nip was used to maintain a flat, wrinkle free sheet upon entering the nip.
  • the hard roll was a 9.76 inch (24.79 cm) diameter steel roll
  • the soft roll was a nylon-surfaced roll having a Shore D hardness of about 85, and about 10.5 inches (26.67 cm) in diameter.
  • FIG. 3 a shows a photomicrograph of an example of a typical web obtained by the process of the invention, in which individual fibers, while flattened ( FIG. 3 b ), are not melted into each other into a non-fibrous mass, but retain their fibrous nature.
  • Comparative example 1 was an uncalendered nanoweb ( FIG. 1 ). It had a maximum pore size of about 7 micrometers, and a mean flow pore size of about 3 micrometers.
  • the winding speed of the sheet was 10 ft/min (3.05 m/min), and the temperature of the hard roll was 80° C. Pressure in the nip was documented via the nip footprint of 12.64 mm.
  • the sheet was stretched after calendering with a tension of 62.5 g/cm at the exit of the nip.
  • the processed nanoweb had a maximum pore size of about 2.6 micrometers and a mean flow pore size of about 1.0 micrometer.
  • a nanoweb was made and calendered in accordance with Example 2, but was stretched with a tension of 198 g/cm tension at the exit of the nip.
  • the processed nanoweb had a maximum pore size of about 2.3 micrometers and a mean flow pore size of about 0.9 micrometer.
  • a 17 gsm meltblown web with a mean fiber diameter of 0.85 ⁇ m was prepared from polypropylene (Basell, Wilmington, Del.) X11292-36-6 of 1200 g/10 minutes Melt Flow Rate (MFR).
  • a 17 gsm meltblown web with a mean fiber diameter of 0.94 ⁇ m was prepared from polypropylene (Basell, Wilmington, Del.) PF017 (2000 MFR, peroxide coated).
  • Table 1 shows results obtained from Examples 1 through 3 and Comparative Example 1.
  • the data in Table 1 demonstrate that nanowebs subjected to the calendering process of the present invention are greatly improved in Poisson Ratio and resistance to Necking, as compared to the as-spun nanowebs of Comparative Example 1.
  • Example 4 In Table 4 is shown the ionic resistance of the product of the invention. Of significance is the fact that the resistance is not increased, or is only insignificantly increased, by the process of the invention as shown by Example 1 and 2 as compared to Comparative Example 1. Also of significance is that the ionic resistance can be significantly altered by stretching the web before or after calendaring as shown by Example 3 and Comparative Example 1. The web of this invention is stronger, has better surface stability, and still has lower ionic resistance as shown by Example 3 in comparison with CE1.

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JP2009529230A JP5615547B2 (ja) 2006-09-20 2007-09-19 改良されたナノウェブ
CN2007800345429A CN101558194B (zh) 2006-09-20 2007-09-19 改进的纳米纤网
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EP07852413.9A EP2064379B1 (fr) 2006-09-20 2007-09-19 Nanotoiles perfectionnées
PCT/US2007/020334 WO2008036332A2 (fr) 2006-09-20 2007-09-19 Nanotoiles perfectionnées
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US8697587B2 (en) 2014-04-15
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KR101516436B1 (ko) 2015-04-30
KR20090068320A (ko) 2009-06-26
CN101558194A (zh) 2009-10-14
EP2064379A2 (fr) 2009-06-03
WO2008036332A3 (fr) 2008-06-12
US20090261035A1 (en) 2009-10-22
WO2008036332A2 (fr) 2008-03-27
EP2064379B1 (fr) 2020-01-15
JP2010504444A (ja) 2010-02-12

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