EP2382343A1 - Structure fibreuse consolidée - Google Patents

Structure fibreuse consolidée

Info

Publication number
EP2382343A1
EP2382343A1 EP09796157A EP09796157A EP2382343A1 EP 2382343 A1 EP2382343 A1 EP 2382343A1 EP 09796157 A EP09796157 A EP 09796157A EP 09796157 A EP09796157 A EP 09796157A EP 2382343 A1 EP2382343 A1 EP 2382343A1
Authority
EP
European Patent Office
Prior art keywords
polymer
core
fibers
fibrous
melting temperature
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.)
Withdrawn
Application number
EP09796157A
Other languages
German (de)
English (en)
Inventor
Sujith Nair
Sasha Stankovich
Yunzhang Wang
Venkatkrishna Raghavendran
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.)
Milliken and Co
Original Assignee
Milliken and Co
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
Priority claimed from US12/360,553 external-priority patent/US8119549B2/en
Priority claimed from US12/360,576 external-priority patent/US8114507B2/en
Application filed by Milliken and Co filed Critical Milliken and Co
Publication of EP2382343A1 publication Critical patent/EP2382343A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/022—Non-woven fabric
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    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/024—Woven fabric
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    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/026—Knitted fabric
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    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/08—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
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    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/42—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
    • D01D5/426—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by cutting films
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
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    • B32B2255/00—Coating on the layer surface
    • B32B2255/02—Coating on the layer surface on fibrous or filamentary layer
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    • B32B2255/26—Polymeric coating
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
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Definitions

  • the present application is directed to consolidated fibrous structures, fibrous layers, and fibers making up the fibrous structures. Also disclosed are methods of making the same.
  • Consolidation of thermoplastic fibers into a fibrous structure such as the consolidation of polypropylene fibers for molded parts and other applications is typically accomplished by hot pressing under pressure at typically high temperatures (about 300 0 F or more) and typically high pressures of (about 300 psi or more) to obtain consolidated fibrous structures having the desired performance attributes.
  • the high temperature requirement hinders the ability to co-process the polypropylene fibers with other materials such as polymer fibers that are compromised at or above 250 0 F.
  • the high pressure requirements prevent these materials from being processed in cost-effective autoclavable processes where the maximum application pressure is often about 45-100 psi. Due to the existing method of high temperature-high pressure consolidation, manufacturability of large parts requires large metal moulds which significantly add to the cost of the machinery and finished parts.
  • thermoplastic fibrous layers and structures that are able to be processed at lower temperatures, pressures, and/or dwell times while having the same or better performance characteristics than the prior art materials processed at much higher temperatures and pressures.
  • the present disclosure provides a consolidated fibrous structure of fibrous layers in cohesive adjoined relation.
  • a consolidated fibrous structure comprising a multiplicity of fibrous layers.
  • Each fibrous layer contains fibers.
  • the fibers of each fibrous layer contain a core and a skin layer.
  • the core has an exterior surface portion containing polypropylene.
  • the skin layer is disposed on at least a portion of the core and contains a first polymer and a second polymer.
  • the first polymer contains a polymer having at least 70% ⁇ -olefin units and is characterized by a melting temperature lower than the melting temperature of the exterior surface portion of the core.
  • the second polymer contains a co-polymer having at least 50% ⁇ -olefin units and is characterized by a number-average molecular weight of about 7,000 g/mol to 50,000 g/mol, a viscosity of between about 2,500 and 150,000 cP measured at 170 0 C, and a melting temperature lower than the melting temperature of the exterior surface portion of the core.
  • the viscosity of the second polymer is not ; greater than 10% of the viscosity of the first polymer measured at 170 0 C. At least a portion of the skin layers of the fibers within each fibrous layer are fused to at least a portion of other skin layers of fibers within the same fibrous layer, at least a portion of the skin layers of the fibers of each fibrous layer are fused with at least a portion of the skin layers of the fibers in an adjacent fibrous layer, and the stiffness of the consolidated fibrous structure is at least 1 N-m measured by ASTM D 790.
  • a multi-layered fiber comprising a core and a skin layer.
  • the core has an exterior surface portion containing polypropylene.
  • the skin layer is disposed on at least a portion of the core and contains a first polymer and a second polymer.
  • the first polymer contains a polymer having at least 70% ⁇ -olefin units and is characterized by a melting temperature lower than the melting temperature of the exterior surface portion of the core.
  • the second polymer contains a co-polymer having at least
  • the second polymer is not greater than 10% of the viscosity of the first polymer measured at 170 0 C.
  • Figure 1 illustrates schematically a cross-section of an exemplary consolidated fibrous structure.
  • Figure 2 illustrates schematically a cross-section of an exemplary fiber of tape construction having a skin layer on one side of a core.
  • Figure 3 illustrates schematically a cross-section of an exemplary fiber of tape construction having a skin layer on both sides of a core.
  • Figure 4 illustrates schematically a cross-section of an exemplary fiber of tape construction having a skin layer on both sides of a core where the core has an inner portion and an exterior surface portion.
  • Figure 5 illustrates schematically a cross-section of an exemplary fiber of circular cross-section having a skin layer surrounding a core.
  • Figure 6 illustrates schematically a cross-section of an exemplary fiber of oval cross-section having a skin layer surrounding a core.
  • Figure 7 illustrates schematically a cross-section of an exemplary fiber of oval cross-section having a skin layer surrounding a core where the core has an inner portion and an exterior surface portion of the core.
  • Figure 8 illustrates schematically a cross-section of an exemplary fibrous layer having a woven construction.
  • Figure 9 illustrates schematically a cross-section of an exemplary fibrous layer having a unidirectional construction.
  • Figure 10 illustrates schematically a cross-section of an exemplary fibrous layer having a knit construction.
  • Figure 11 illustrates schematically a cross-section of an exemplary fibrous layer having a non-woven construction.
  • Figure 12 illustrates schematically a consolidated fibrous structure in a three-dimensional shape.
  • Figure 13 illustrates schematically a cross-section of two fibrous layers consolidated together showing polymer at least partially filling the interstices of the fibrous layers.
  • Figure 14 illustrates schematically a cross-section of an exemplary fibrous layer having a unidirectional construction where the fibers have one continuous skin layer and one discontinuous skin layer.
  • Figure 15 illustrates schematically a cross-section of a fibrous layer showing 2 fibers fused together.
  • Figure 16 is a 100x image of a fibrous layer as illustrated in Figure 15 illustrating the peeling failure mode.
  • Figure 17 is an illustrative version of the image of Figure 16.
  • Figure 18 is a 20Ox image of fibers peeled apart having the interface between the skin layer and the skin layer fail.
  • Figure 19 is an illustrative version of the image of Figure 18.
  • each fibrous layer 100 contains fibers 10 having a core 12 with an exterior surface portion comprising polypropylene and skin layers 14 and 14' comprising a first polymer and a second polymer.
  • the stiffness of the consolidated fibrous structure is at least about 1 N-m, more preferably at least 5 N-m measured by ASTM D 790.
  • Figures 2-7 illustrate different configurations of the fibers 10.
  • fiber is defined as an elongated body, the length at least 100x the square root of the cross-sectional area.
  • the term "fiber” as used herein includes a monofilament elongated body, a multifilament elongated body, ribbon, strip, tape, and the like.
  • the term fibers include a plurality of any one or combination of the above.
  • Figure 2 shows a fiber 10 having a tape construction with a core 12 and a skin layer 14 on one side of the core 12.
  • Figure 3 shows a fiber 10 being tape elements having a core 12 and two skin layers 14, 14' sandwiching the core 12.
  • Figure 4 illustrates an embodiment where the core has an inner portion 12" and an exterior surface portion 12' including polypropylene.
  • the inner portion 12" may be, but is not limited to, polypropylene, polyethylene, polyester, polyamides, polyethers, or copolymers thereof; glass fiber, aramid, carbon fiber, ceramic fiber, nylon, polyetherimide, polyamide-imide, polyphenylene sulfide, polysulfones, polyimide, conjugated polymers, mineral fiber, natural fibers, metallic fiber or mixtures thereof.
  • the inner portion 12" of the core 12 has a tensile modulus of greater than 15 grams per denier as measured by ASTM method
  • the inner portion 12" and exterior surface portion 12' of the core may be of the same or similar chemical composition or may be of different chemical composition with or without the use of surfactants, copolymers, or other means of reducing the surface energy difference between the inner portion 12" and exterior surface portion 12' of the core 12.
  • the fiber 10 is a high modulus fiber, being defined as fibers having a tensile modulus of greater than 10 grams per denier as measured by ASTM method 3811-07 and preferably have a tensile strength of at least 100 MPa.
  • Figure 5 shows a fiber 10 being a fiber having a circular cross- section with a core 12 and a skin layer 14 surrounding the core.
  • Figure 6 shows a fiber 10 being a fiber having an oval or oblong cross-section having a core 12 and a skin layer 14 surrounding a section of the core, the skin layer 14 being discontinuous at least in the direction around the circumference of the core 12.
  • Figure 7 illustrates the embodiment where the core has an inner portion 12" and an exterior surface portion 12' being polypropylene. The exterior surface portion
  • the inner portion 12" of the core 12 may be continuous or discontinuous.
  • the inner portion 12" may be, but is not limited to, polypropylene, polyethylene, polyester, polyamides, polyethers, or copolymers thereof; glass fiber, aramid, carbon fiber, ceramic fiber, nylon, polyetherimide, polyamide-imide, polyphenylene sulfide, polysulfones, polyimide, conjugated polymers, mineral fiber, natural fibers, metallic fiber or mixtures thereof.
  • the inner portion 12" of the core 12 has a tensile modulus of greater than 15 grams per denier as measured by ASTM method 3811-07.
  • the inner portion 12" and exterior surface portion 12' of the core may be of the same or similar chemical composition or may be of different chemical composition with or without the use of surfactants, copolymers, or other means of reducing the surface energy difference between the inner portion 12" and exterior surface portion 12' of the core.
  • the interface between the inner portion 12" and the exterior surface portion 12' should have sufficient physical interlocking as to prevent delamination between the inner portion 12" and the exterior surface portion 12' of the fiber 12 in the final product.
  • the core 12 of the fiber 10 has a high modulus (greater than 10 grams per denier) to provide stiffness for the fiber 10. It is contemplated that the core 12 of the fibers 10 is preferably made up of a molecularly-oriented thermoplastic polymer. The core 12 may account for about 50-99 wt. % of the fiber 10. Preferably, the core 12 of the fiber 10 has a tensile modulus of at least greater than 10 grams per denier as measured by ASTM method 3811-07, and more preferably greater than 40 grams per denier. According to one practice, the core 12 of the fiber 10 is polypropylene and is highly drawn with a draw ratio greater than 10:1.
  • the core 12 (inner portion 12" and exterior surface portion 12') of fiber 10 has a peak melting temperature equal to or higher than the all the skin layers 14, 14'.
  • the core 12 (inner portion 12" and exterior surface portion 12') of the fiber 10 has a peak melting temperature of at least 5°F greater than the skin layers 14, 14', more preferably at least 10 0 F greater than the skin layers 14, 14'.
  • the fibers 10 are tape elements having a core 12 and at least one skin layer 14, 14'.
  • the tape fibers 10 may be formed by slitting a film.
  • the film may be formed by any conventional means of extruding such multilayer polymeric films. By way of example, and not limitation, the film may be formed by blown film or cast film extrusion.
  • the film is then cut into a multiplicity of longitudinal strips of a desired width by slitting the film to yield tape fibers 10 having cross-sections in the thickness dimension as shown in Figures 2-4.
  • the tape fibers 10 are then preferably drawn in order to increase the orientation of the core 12 so as to provide increased strength and stiffness of the material. After the drawing process is complete, in one embodiment the resulting strips are in the range of about 1 to about 5 millimeters wide.
  • Fiber elements being tape elements, core-shell elements, and their textile layer constructions are believed to be more fully described in U.S. Patent Publication No. 2007/0071960 (Eleazer et al.), US Patent Application No. 11/519,134 (Eleazer et al.), and US Patents 7,300,691 (Eleazer et al.),
  • the core 12 (or exterior surface portion 12' of the core 12) is compatibly bonded to each of skin layers 14, 14' along their respective surfaces.
  • the skin layers 14, 14' contain a first polymer and a second polymer.
  • the skin layers 14, 14' may be continuous or discontinuous on the core 12.
  • the skin layers 14, 14' account for about 1-50 vol. % of the fiber 10.
  • the core 12 and skin layer(s) 14, 14' may be co-extruded together, or the skin layer(s) layer 14, 14' may be applied to the core 12 after the core 12 has been formed. Additionally, a portion of the skin layer(s) may be applied during or after core formation with the balance of the skin layer(s) being introduced at a later point.
  • the fiber 10 may be drawn or oriented before or after the skin layer(s) 14, 14' are formed in order to increase the orientation of the core 12 so as to provide increased strength and stiffness or achieve a targeted core dimension.
  • the first polymer comprises a polymer having at least about 70% ⁇ -olefin units and is compatible with the polypropylene of the exterior surface portion 12' of the core 12.
  • the first polymer is a co-polymer having at least about 70% ⁇ -olefin units.
  • "Compatible”, in this application, is defined as two or more polymers that are inherently or enhanced to remain mixed without objectionable separation over the range of processing conditions that will form the final product.
  • ⁇ -olefin in this application, is defined as 1-alkene olefin monomer units other than ethylene such as propylene, butylene, 4-methyl-1- pentene, pentene, 1-octene, and the like.
  • the first polymer may have an ethylene content of about 1-25 mol. %, and a propylene content of about 75-99 mol. %. It may be further preferred for the first polymer to have a ratio of about 95 mol. % propylene to about 5 mol. % ethylene.
  • the first polymer is a terpolymer, one example being a terpolymer of ethylene, propylene, and butylene.
  • the first polymer has a viscosity of greater than 150,000 cP measured at 17O 0 C and a melting temperature lower than the melting temperature of the exterior surface portion of the core.
  • the first polymer has a viscosity of greater than 1,000,000 cP measured at 170 0 C.
  • the first polymer has at least ten times the viscosity of the second polymer, measured at 170 0 C.
  • the first polymer has a melting temperature of between about 120 and 140 0 C, a weight average molecular weight of between about 300,000 and 350,000, a viscosity of about 4,000,000 to 7,000,000 cP at 170 0 C, a melt flow index of between about 4 and 8 grams/10 minutes measured at 230 0 C 1 and a polydispersity of between about 3 and 6.
  • Melting temperature in this application, is defined to be the lower of the peak melting temperature or the temperature at which 50% of the polymer has melted from the solid state as measured by Differential Scanning Calorimetry (DSC).
  • DSC Differential Scanning Calorimetry
  • the first polymer as a melting temperature of at least about 10 0 C lower than that of the exterior surface portion 12' of the core 12, and preferably between about 15- 4O 0 C lower.
  • the tensile modulus of the first polymer is greater than about 100 MPa, preferably greater than about 500 MPa and most preferably greater than about 1 GPa.
  • the skin layer(s) 14, 14' also contain a second polymer.
  • the second polymer comprises a co-polymer having at least 50% ⁇ -olefin units.
  • the second polymer comprises a co-polymer having at least 50% propylene units, more preferably 80% propylene units, most preferably more than 82% propylene units.
  • the second polymer comprises a number-average molecular weight of between about 7,000 g/mol and 50,000 g/mol, a viscosity of between about 2,500 and 150,000 cP measured at 170°C, and a melting temperature lower than the melting temperature of the exterior surface portion of the core.
  • the second polymer has a viscosity not greater than about 10% of the viscosity of the first polymer measured at 170 0 C. If the polymer has a number- average molecular weight lower than 7,000 g/mol or a viscosity lower than 2500 cP, the molecular chains of the second polymer are too short to entangle with one another and are too weak to effectively fuse with the first polymers. A polymer with a viscosity of greater than 150,000 cP has a reduced ability to flow into the interstices of the fibrous layers under lower temperature and pressure consolidation conditions.
  • the melting temperature of the second polymer is preferably lower than the core in order to fuse the layers together without compromising the integrity of the core. In one embodiment, the second polymer has a weight average molecular weight of between about 20,000 and 40,000 g/mol, a number average molecular weight of between about 7,000 and 22,000.
  • the viscosity of the second polymer is between about 4,000 and 120,000 cP measured at 170 0 C, more preferably between about 4,000 and 16,000 cP. In one embodiment, elongation at break is greater than about 200%, more preferably greater than about 400%. In one potentially preferred embodiment, the second polymer has a lower melting temperature than the first polymer. This aids in allowing the second polymer to flow into the interstices. In one embodiment, the second polymer has a cohesion strength of at least about 1 MPa, more preferably greater than about 4 MPa. Having a cohesion strength in this range provides a polymer that resists tearing.
  • the viscosity of the second polymer is between about 0.005 to 10% the viscosity of the first polymer measured at 170 0 C 1 more preferably about 0.1 and 10%.
  • the large difference in viscosity is believed to help facilitate the structural adhesion between the first polymer and the core and the filling of the interstices of the fibrous layers by the second polymer.
  • an increase in the molecular weight leads to an increase in the cohesion strength and the viscosity of the polymer.
  • the first polymer provides the strength of the reinforcement and is expected to have a high molecular weight and hence a higher cohesion strength and viscosity.
  • the second polymer aids in processing of the skin layer and also fills the interstices of the fibrous layers to provide additional reinforcement.
  • the tensile modulus of the second polymer is greater than about 0.1 MPa 1 preferably greater than about 0.5 MPa and most preferably greater than 1 MPa.
  • the percentage by weight of the second polymer to the total weight of the fiber is between about 0.25%wt and 50%wt, more preferably between about 1%wt and 25%wt.
  • the second polymer comprises a metallocene catalyzed propylene-ethylene co-polymer.
  • the skin layers 14, 14' have an interior margin adjacent the core 12 and an exterior margin in the skin layer 14, 14' remote from the core 12.
  • the interior margin of the skin layer comprises the first polymer and the exterior margin of the skin layer comprises the second polymer.
  • the first polymer contributes significantly to the adhesion between the core and the skin layer and the second polymer contributes significantly to the adhesion of the skin layer to skin layer of adjacent fibers 10.
  • the skin layers 14, 14' contain a generally homogenous blend of the first and second polymers. However, in one embodiment, the first and second polymers form concentration gradients through the thickness of the skin layer 14, 14'.
  • the first polymer has a higher concentration at the inner margin, decreasing concentration through the skin layer to a lower concentration at the exterior margin of the skin layer.
  • the second polymer forms a concentration gradient from a higher concentration at the outer margin decreasing through the thickness of the skin layer to the inner margin.
  • the first polymer is a majority component by weight of the skin layer 14, 14' at the inner margin and the second polymer is a majority component by weight of the skin at the exterior margin.
  • This gradient may be formed, for example, by co-extruding the skin layer and core together having the second polymer bloom towards the surface of the skin layer or applying the first and second polymers as discrete layers then heating them to form one layer where a portion of the first polymer migrates into the second and a portion of the second polymer migrates into the first.
  • the fibers 10 are in fibrous layers 100. These fibrous layers 100 may contain fibers in woven, non-woven, knit, or unidirectional constructions (or mixtures of these constructions). Referring now to Figure 8, there is shown fibers 10 in a woven construction. While the fibers 10 shown in Figures 8 are tape fibers having a core 12 and two skin layers 14 and 14', other fiber types or shapes may be utilized.
  • the fibrous layer 100 preferably includes a multiplicity of fibers 10 running in the warp direction interwoven with fibers 10 running in the fill direction in transverse relation to the warp fibers.
  • the fill fibers are interwoven with the warp fibers such that a given fill extends in a predefined crossing pattern above and below the warp.
  • the fill fibers and the warp fibers are formed into a so called plain weave wherein each fill fiber passes over a warp fiber and thereafter passes under the adjacent warp fiber in a repeating manner across the full width of the fibrous layer 100.
  • any number of other weave constructions as will be well known to those of skill in the art may likewise be utilized.
  • the fill fibers may pass over two or more adjacent warp fibers before transferring to a position below one or more adjacent warp fibers thereby forming a twill weave.
  • the term "interwoven" is meant to include any construction incorporating interengaging formation fibers.
  • Figure 9 illustrates a fibrous layer 100 having a unidirectional construction formed from a multiplicity of fibers 10 being tape elements.
  • the fibers are aligned parallel along a common fiber direction of the fibrous layer 100.
  • the fibers 10 in the fibrous layer 100 do not overlap one another, and may have gaps between the fibers 10.
  • the fibers overlap one another up to 90% in the fibrous layer 100.
  • One approach for aligning the fibers is to align the fibers into a sheet by pulling the fibers from a creel. Using a roll-off creel is helpful to reduce twist in the fibers.
  • the common fiber direction of the fibers 10 in one fibrous layer 100 is the same (parallel to) as the common fiber direction of the fibers 10 of the adjacent fibrous layer.
  • the common fiber direction of the fiber 10 in one layer 100 may be parallel, perpendicular, or have any other rotational degree relative to the fiber direction in the adjacent fibrous layers 100.
  • Figure 10 illustrates a fibrous layer 100 having a knit construction.
  • the warp and weft fibers are circular cross-section fibers 10.
  • the knit fibrous layer 100 may be any known knit, including, but not limited to circular knit, warp knit, weft-inserted warp knit, double needle bar, and jacquard knit fabrics.
  • Figure 11 illustrates a fibrous layer 100 having a non-woven construction.
  • the fibers 10 are tape fibers.
  • non-woven refers to structures incorporating a mass of fiber elements that are entangled and/or heat fused so as to provide a coordinated structure with a degree of internal coherency.
  • Non- woven fibrous layers or webs may be formed from many processes such as for example, meltspun processes, hydroentangling processes, mechanically entangled processes, needle punched processes, air-laying processes and wet laying processes, laid scrims and the like.
  • the fibers 10 may be unattached from one another or fused to one another.
  • the fused configuration at least a portion of the skin layers 14, 14' of the fibers 10 within the fibrous layer 100 are fused to one another.
  • the fibrous layer 100 is heated, preferably under pressure, to a softening temperature below that of the core 12. In so doing, the skin layers 14, 14' will melt while the core 12 will remain substantially solid and highly oriented. As the fibrous layer 100 then cools, the skin layers 14, 14" will fuse together, thereby forming a solid matrix. Fused or un-fused individual fibrous layers 100 may be stacked and reheated to form the consolidated fibrous structure 200.
  • At least 3 of the fibrous layers 100 are stacked together and consolidated using heat and/or pressure to form a consolidated fibrous structure 200 such as shown in Figure 1. While the consolidated fibrous structure 200 has been depicted in Figure 1 as including three (3) fibrous layers 100, those of ordinary skill in the art will readily appreciate that the consolidated fibrous structure 200 can comprise any suitable number of fibrous layers 100. In one embodiment, at least two (2) fibrous layers are consolidated together. In other embodiments, the consolidated fibrous structure 200 can comprise greater than three fibrous layers. By way of example only and not limitation, such structures may have ten fibrous layers, twelve fibrous layers, eighteen fibrous layers, twenty fibrous layers, thirty fibrous layers, or forty fibrous layers. While Figure 1 shows each of the fibrous layers 100 containing the same type of fibers 10 and layer construction (woven in the case of Figure 1), the consolidated fibrous structure 200 may contain many different fibrous layer 100 constructions and fibers 10 in the structure 200.
  • Several layers of fibrous layers 100 may be stacked in layered relation prior to the application of heat and pressure in order to form the consolidated fibrous structure 100.
  • the layers of the fibrous layer 100 may be formed from a single sheet of a fibrous layer that is repeatedly folded over itself, or from several discrete overlaid fibrous layers.
  • the structure 200 may be formed by reheating several previously fused fibrous layers 100. Any of these methods may be employed to form a structure 200 with any desired thickness or number of layers.
  • Consolidation of multiple fibrous layers 100 is preferably carried out at suitable temperature and pressure conditions to facilitate both interface bonding fusion and partial migration of the melted skin layer material between the layers. It has been found that having a both the first polymer and the second polymer in the skin layer aids in the ability to use lower temperature, lower pressure, and/or shorter dwell time consolidation conditions with the same or better properties as compared to a fiber having only a first polymer in the skin layer.
  • Heated batch or platen presses may be used for multi-layer consolidation. In one exemplary practice, autoclaves or vacuum bags may be used to provide the pressure during consolidation. Continuous consolidation methods such as calendaring or use of a single or double belt laminator may likewise be employed.
  • any other suitable press may likewise be used to provide appropriate combinations of temperature, pressure, and residence time.
  • heating is carried out at a temperature of about 195-325 0 F and a pressure of about 15-400 psi.
  • the skin layers 14, 14' When exposed to such an elevated temperature and pressure, the skin layers 14, 14' will melt while the core 12 will remain substantially solid. Upon cooling, the skin layers 14, 14' will fuse thereby forming a matrix through which the stiff core 12 are distributed. "Fuse" is defined as being joined as if by melting together.
  • cooling is carried out under pressure to a temperature lower than about 100 0 F. It is contemplated that maintaining pressure during the cooling step tends to inhibit shrinkage of the core and ensures no loss of consolidation. Without being limited to a specific theory, it is believed that higher pressures may facilitate polymer flow at lower temperatures. Thus, at the higher end of the pressure range, (greater than about 200 psi) the processing temperature may be about 80-140°C.
  • the consolidated fibrous structure 200 may thereafter be subjected to three-dimensional molding under heat and pressure at temperatures above the softening point of the skin layers 14, 14' so as to yield complex shapes.
  • the fibrous structures may also be consolidated and molded in a single step forming structure 200 simultaneous with the formation of a subtle or complex shape.
  • An example of a plurality of fibrous layers 100 formed into a consolidated fibrous structure 200 having a three-dimensional shape is shown in Figure 12.
  • the fibrous layers 100 contain interstices 22, or voids, between the fibers as shown, for example, in Figure 13. It has been found that the second polymer is more mobile during the fusing process and more easily migrates into the interstices 22 of the fibrous layer 100. In some embodiments, there are also interstices formed between fibers of adjacent fibrous layers. Preferably, when the interstices are at least partially filled with the first and second polymer, the filled interstices contain at least about 80% by weight the second polymer. At least partially filling the interstices 22 of the fibrous layers 100 creates better adhesion between the fibrous layers 100 and a better performing end product.
  • a portion of the second polymer and first polymer intermix forming a blend of the first and second polymers.
  • Semicrystalline polymers like the polyolefins involved in this patent comprise oriented crystallites separated by amorphous chains.
  • the amorphous chains migrate towards the interface to maximize the entropy. Due to the accumulations of short amorphous chains, the strength of the interface can be very weak.
  • the first polymer and second polymer can be found to co-crystallize with one another resulting in a polymer blend with a higher crystallinity than either polymer alone.
  • the complementary crystallization is believed to enhance the physical properties of the skin yielding an improved skin layer. This is achieved through the second polymer increasing the mobility of the first polymer chains and allowing a more extensive crystallization.
  • the second polymer, being compatible with the first is also able to incorporate into the crystal structure of the first without the introduction of significant additional defects.
  • the degree of co-crystallization is dependent on the molecular chain length of the amorphous segments of the first polymer and on the crystallizable chain length of the second polymer. Another phenomenon that could control the degree of co-crystallization is the rate of cooling. The rate of cooling is dependent on the consolidation conditions.
  • the skin layers 14, 14 may be applied to the core 12 of the fibers 10 in any known method.
  • the skin layers may be co-extruded or otherwise formed at the same time as the core of the fibers or may be applied to a core after the core are formed.
  • the skin layers 14, 14' may be applied to individual cores or onto cores that have already been formed into a fibrous layer.
  • the skin layers may be continuous or discontinuous.
  • Figure 14 illustrates a fibrous layer 100 being a unidirectional layer having a continuous skin layer 14 on one side of core and a discontinuous skin layer 14' on the opposite side of the core. These discontinuous regions may be along a single fiber 10 or across multiple fibers 10.
  • This application may be conducted by any known means including, but not limited to, solvent coating, curtain coating, extrusion coating, inkjet printing, gravure printing, solvent coating, powder coating, covering the core with a spunbond skin layer, or covering the core with a separate film layer comprising the skin polymers.
  • One contemplated practice to form multi-layered fiber comprises providing an elongated core having an exterior surface portion comprising polypropylene and applying a skin layer to at least a portion of the core, where the skin layer comprises a first polymer and a second polymer.
  • the first polymer contains a co-polymer having at least 70% ⁇ -olefin units and is characterized by a viscosity of greater than 1 ,000,000 cP measured at 170 0 C and a melting temperature lower than the melting temperature of the exterior surface portion of the core.
  • the second polymer contains a propylene co-polymer having at least 80% propylene units and is characterized by a number-average molecular weight of about 7,000 g/mol to 50,000 g/mol, a viscosity of between about 4,000 and 10,000 cP measured at 170 0 C, and a melting temperature lower than the melting temperature of the first polymer.
  • the ratio by weight of the second polymer to the first polymer is between about 1 : 20 to 20: 1.
  • a section of the consolidated fibrous structure has two interfaces as shown in Figure 15.
  • the core-skin layer adhesion is fixed by the method at which the skin layer was applied to the core (for example, co-extruded or coated on).
  • the skin layer contains the first and second polymers
  • the skin layer- skin layer interface is strong resulting in a failure between the core and the skin layer or within the core itself. This indicates a very strong bond between the skin layers.
  • FIG. 17 An illustration of the image is shown in Figure 17.
  • One is able to determine where in the structure the failure mode happened by the appearance, or lack thereof, of oriented fibers at the split. These oriented fibers are parts of the oriented core stripping away from the core.
  • the skin layer-skin layer cohesion is not stronger than the core- skin layer adhesion, the failure will occur between the skin layers and resulting in a smooth split as can been seen in the 20Ox micrograph of Figure 18 and as an illustration of the micrograph in Figure 19. This indicates a poor bond between the fibers within fibrous layers or between fibrous layers.
  • the skin layer-skin layer adhesion may be influenced by various material and processing parameters.
  • the fibrous layers 100 and consolidated fibrous structure 200 may contain additional fibers or layers.
  • additional fibers that may be incorporated include, but are not limited to fibers made from highly oriented polymers, such as gel-spun ultrahigh molecular weight polyethylene fibers, melt- spun polyethylene fibers, melt-spun nylon fibers, melt-spun polyester fibers, sintered polyethylene fibers, rigid-rod polymers, carbon fibers, aramid fibers, glass fibers, polylactic acid fibers, and natural fibers such as cotton.
  • Additional films such as polycarbonate films, polyester films, polyethylene films, and polypropylene films may be included into the structure 200.
  • additional panels may be included with the structure 200 such as ballistics panels or the like.
  • the fibers, fibrous layers, and consolidated fibrous structures may be used for many purposes in many different applications that would be unavailable to fibers having a core and a skin having only the first polymer.
  • Having the skin layer contain both the first polymer and the second polymer allows for the same or better performance of the element or structure as fibers with only the first polymer, but processed at much lower temperatures, pressures, and/or dwell times.
  • Stiffness was measured by ASTM D 790.
  • the areal density of the specimen is adjusted to 0.21 psf (Typically 10 layer consolidated stacks are used). The samples are cut to 2" width strips.
  • the peel specimens are prepared by leaving a 1" wedge at one end in the center of the stack (between layers 5 and 6) to grip the ends using fixtures mounted on the cross-head of an Instron.
  • a 180 degree peel test is conducted with a crosshead speed fixed at 127min. The initial gauge length is 1". The peel start point is 1" and the end point is 9".
  • the peel strength is calculated by measuring the average peel force divided by the sample width. Melting temperatures were measured by DSC using a scanning rate of 20°C/min.
  • the tensile modulus of Licocene ® 2602 is measured to be approximately 0.7 MPa; has an elongation at break of 760% and cohesion strength of 9 MPa.
  • the crystallinity of the polymer is ⁇ 17%.
  • the coating solution was padded on uniformly onto ten 12" x 12" woven tape layers.
  • the percent add-on on the fibrous layers was approximately 2% dry add on.
  • the layers were then dried overnight at room temperature. After drying the woven tape fibrous layers they were stacked and consolidated by being placed between heated aluminum platens at a temperature of 300 0 F and a pressure of 300 psi for 10 minutes of heating time. The sample was then subsequently cooled to 100 0 F. The cooling rate was approximately 20°F/minute.
  • Licocene ® 2602 had a viscosity of 6000 cP measured at 17O 0 C and a melting temperature of 75 0 C.
  • the tensile modulus of Licocene ® 2602 is measured to be approximately 0.7 MPa; has an elongation at break of
  • Woven fibrous layers were formed as described in Control Example 1.
  • the Vestoplast ® 708 had a number average molecular weight of 11 ,500 g/mol, a viscosity of 8,000 cP measured at 170°C, and a melting temperature of 56 0 C.
  • the coating solution was padded on uniformly onto ten 12" x 12" woven tape layers.
  • the percent add-on on the fibrous layers was approximately 2% dry.
  • the layers were then dried overnight at room temperature. After drying the woven fibrous layers they were stacked and consolidated by being placed between heated aluminum platens at a temperature of 300 0 F and a pressure of 300 psi for 10 minutes of heating time. The sample was then subsequently cooled to 100 0 F. The cooling rate was approximately 20°F/minute.
  • a peel strength of "No consolidation" indicates that fibrous layers did not hold together well enough to perform the peel strength test.
  • Working Examples 1 and 3 had at least 85% greater peel strength processed at lower conditions (300 0 F, 300 psi) than Control Example 1 processed at much higher conditions (320°F, 2,500 psi). Control Example 1 would not even consolidate at the lower temperatures and pressures. Additionally, stiffness was measured for all samples and the Working Examples were at least as stiff as or stiffer than the Control Examples processed at the same conditions.
  • Having a skin layer containing a first polymer and a second polymer enables the working examples to be consolidated at much lower temperatures, pressures and/or dwell time saving time and energy over prior art materials.

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Abstract

La présente invention porte sur une structure fibreuse consolidée comprenant une multiplicité de couches fibreuses. Les fibres de chaque couche fibreuse contiennent une âme et une couche de revêtement. L'âme présente une partie surface extérieure contenant du polypropylène. La couche de revêtement est disposée sur au moins une partie de l'âme et contient un premier polymère et un second polymère. Au moins une partie des couches de revêtement des fibres dans chaque couche fibreuse sont fusionnées à au moins une partie d'autres couches de revêtement de fibres à l'intérieur de la même couche fibreuse, au moins une partie des couches de revêtement des fibres de chaque couche fibreuse sont fusionnées à au moins une partie des couches de revêtement des fibres dans une couche fibreuse adjacente, et la rigidité de la structure fibreuse consolidée est au moins de 1 N-m. L'invention porte également sur une couche fibreuse.
EP09796157A 2009-01-27 2009-12-21 Structure fibreuse consolidée Withdrawn EP2382343A1 (fr)

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US12/360,553 US8119549B2 (en) 2009-01-27 2009-01-27 Consolidated fibrous structure
US12/360,576 US8114507B2 (en) 2009-01-27 2009-01-27 Multi-layered fiber
PCT/US2009/006624 WO2010087811A1 (fr) 2009-01-27 2009-12-21 Structure fibreuse consolidée

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JP3819440B2 (ja) * 1996-12-25 2006-09-06 チッソ株式会社 熱接着性複合繊維およびそれを用いた不織布
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US7300691B2 (en) 2005-09-27 2007-11-27 Milliken & Company Moldable construction incorporating non-olefin bonding interface
US7294384B2 (en) 2005-09-27 2007-11-13 Milliken & Company Moldable construction incorporating bonding interface
US20070071960A1 (en) 2005-09-27 2007-03-29 Eleazer Howell B Moldable fabric with variable constituents

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