US20150079337A1 - Films comprising an array of openings and methods of making the same - Google Patents
Films comprising an array of openings and methods of making the same Download PDFInfo
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- US20150079337A1 US20150079337A1 US14/387,332 US201314387332A US2015079337A1 US 20150079337 A1 US20150079337 A1 US 20150079337A1 US 201314387332 A US201314387332 A US 201314387332A US 2015079337 A1 US2015079337 A1 US 2015079337A1
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- openings
- polymeric layer
- micrometers
- polymeric
- major surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/222—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length characterised by the shape of the surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/24—Calendering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/12—Articles with an irregular circumference when viewed in cross-section, e.g. window profiles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D28/00—Producing nets or the like, e.g. meshes, lattices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/911—Cooling
- B29C48/9135—Cooling of flat articles, e.g. using specially adapted supporting means
- B29C48/914—Cooling of flat articles, e.g. using specially adapted supporting means cooling drums
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2028/00—Nets or the like
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24273—Structurally defined web or sheet [e.g., overall dimension, etc.] including aperture
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24273—Structurally defined web or sheet [e.g., overall dimension, etc.] including aperture
- Y10T428/24298—Noncircular aperture [e.g., slit, diamond, rectangular, etc.]
- Y10T428/24314—Slit or elongated
Definitions
- Macroporous, perforated films are commonly used for vapor and liquid permeable applications, whereas microporous perforated films are useful for vapor permeable applications, but not liquid permeable applications.
- Macroporous perforated films are commonly used as components in personal care garments (e.g., diapers and feminine hygiene products). Perforated films are also used in filtering, and acoustic applications.
- Macroporous permeable films are commonly made by first producing a continuous film and then subjecting the film to a perforation process.
- Mechanical perforating devices include intermeshing rollers, die punching, or needlepunching. Films can also be perforated using perforated rollers having thermal zones or lasers that melt perforations into the film.
- Other techniques for providing the perforations include casting a film on to a porous quench roll that has vacuum on the holes to pull the melt into the hole and produce an aperture, using electrical corona treatment to create perforations by localized energy treatment, and creating perforations is by blending immiscible materials followed by film stretching to create perforations by generation of film voids. It is also known that after quenching polypropylene in to beta phase crystals, upon orientation, the film will become porous.
- the present disclosure describes a polymeric layer having first and second, generally opposed major surfaces, comprising an array of openings extending between the first and second major surfaces, wherein the openings each have a series of areas through the openings from the first and second major surfaces ranging from minimum to maximum areas, wherein there is a total area and a total open area for each of the first and second major surfaces, wherein the total open area for each of the first and second major surfaces is not greater than 50 (in some embodiments, not greater than 45, 40, 35, 30, 25, 20, 15, 10, 5, 4, 3, 2, 1, 0.75, 0.5, 0.25, or even not greater than 0.1; in some embodiments, in a range from 0.1 to not greater than 50, 0.1 to not greater than 45, 0.1 to not greater than 40, 0.1 to not greater than 35, 0.1 to not greater than 30, 0.1 to not greater than 25, 0.1 to not greater than 20, 0.1 to not greater than 15, 0.1 to not greater than 10, or even 0.1 to not greater than 5) percent of the total area of the respective major surface,
- the area of each opening is not greater than 5 (in some embodiments, not greater than 2.5, 2, 1, 0.5, 0.1, 0.05, 0.01, 0.075, or even not greater than 0.005) mm 2 .
- the present disclosure describes a polymeric layer having first and second, generally opposed major surfaces, comprising an array of openings extending between the first and second major surfaces, wherein the openings each have a series of areas through the openings from the first and second major surfaces ranging from minimum to maximum areas, wherein for at least a majority of the openings, the area of each opening is not greater than is 5 (in some embodiments, not greater than 2.5, 2, 1, 0.5, 0.1, 0.05, 0.01, 0.075, or even not greater than 0.005) mm 2 , and wherein for at least a majority of the openings, the minimum area is not at either major surface.
- the present disclosure describes a method of making a polymeric layer described herein, the method comprising at least one of passing through a nip or calendaring netting comprising an array of polymeric strands periodically joined together at bond regions throughout the array.
- the present disclosure describes a method of making a polymeric layer having openings therein, the method comprising at least one of passing through a nip or calendaring a netting comprising an array of polymeric strands periodically joined together at bond regions throughout the array, wherein the netting has a thickness up to 2 mm (in some embodiments, up to 1.5 mm, 1 mm, 750 micrometers, 500 micrometers, 250 micrometers, 100 micrometers, 75 micrometers, 50 micrometers, or even up to 25 micrometers; in a range from 10 micrometers to 2 mm, 10 micrometers to 1.5 mm, 10 micrometers to 1 mm, 10 micrometers to 750 micrometers, 10 micrometers to 750 micrometers, 10 micrometers to 500 micrometers, 10 micrometers to 250 micrometers, 10 micrometers to 100 micrometers, 10 micrometers to 75 micrometers, 10 micrometers to 50 micrometers, or even 10 micrometers to 25 micrometers).
- Polymeric layers described herein are useful, for example, as components in personal care garments such as diapers and feminine hygiene products. They can also be useful for filtering (including liquid filtering) and acoustic applications.
- FIG. 1 is a schematic view of an apparatus for making forming polymeric layers having openings therein as described herein;
- FIG. 2 is a cross-section view of the forming polymeric layer having openings therein as described herein taken along section lines 2 - 2 in FIG. 1 ;
- FIG. 3 is an exploded perspective view of an exemplary embodiment of a set of extrusion die elements suitable for use in the apparatus of FIG. 1 , including a plurality of shims, a set of end blocks, bolts for assembling the components, and inlet fittings for the materials to be extruded;
- FIG. 4 is a plan view of one of the shims of FIG. 3 ;
- FIG. 5 is a plan view of a different one of the shims of FIG. 3 ;
- FIG. 6 is a plan view of a different one of the shims of FIG. 3 ;
- FIG. 7 is a schematic perspective view of a portion of the extrusion die of FIG. 3 , supplied with polymeric material and forming a netting;
- FIG. 7 a is a schematic perspective view of an alternate arrangement of the extrusion die relative to the nip;
- FIG. 7 b is a schematic perspective view of an alternate nip roll
- FIG. 8 is a close up front view of the dispensing surface of an extrusion die used in certain of the Examples.
- FIG. 9 is an optical digital photo of Example 1 polymeric layer having openings therein;
- FIG. 10 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 9 ;
- FIG. 11 is an optical digital photo of Example 2 polymeric layer having openings therein;
- FIG. 12 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 11 ;
- FIG. 13 is an optical digital photo of Example 3 polymeric layer having openings therein;
- FIG. 14 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 13 ;
- FIG. 15 is an optical digital photo of Example 4 polymeric layer having openings therein;
- FIG. 16 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 15 ;
- FIG. 17 is an optical digital photo of Example 5 polymeric layer having openings therein;
- FIG. 18 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 17 ;
- FIG. 19 is an optical digital photo of Example 6 polymeric layer having openings therein;
- FIG. 20 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 19 ;
- FIG. 21 is a close up front view of the dispensing surface of an extrusion die used in certain of the Examples.
- FIG. 22 is an optical digital photo of Example 7 polymeric layer having openings therein;
- FIG. 23 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 22 ;
- FIG. 24 is a close up front view of the dispensing surface of an extrusion die used in certain of the Examples.
- FIG. 25 is an optical digital photo of Example 8 polymeric layer having openings therein;
- FIG. 26 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 22 ;
- FIG. 27 is an optical digital photo of Example 9 polymeric layer having openings therein;
- FIG. 28 is a scanning electron digital photomicrograph of the cross-section of one of the holes of the polymeric layer having openings therein shown in FIG. 27 ;
- FIG. 29 is a close up front view of the dispensing surface of an extrusion die used in Example 10.
- FIG. 30 is an optical digital photo of Example 10 polymeric layer having openings therein.
- Apparatus 20 has extruder 22 extruding polymeric netting 24 comprising first strands 26 and second strands 28 joined together at bond regions 30 .
- Any of a variety of nettings comprising an array of polymeric strands periodically joined together at bond regions throughout the array including those known in the art (see, e.g., U.S. Pat. No. 4,038,008 (Larsen)) may be used.
- Useful polymeric netting is also described in copending applications having U.S. Serial Nos. 61/526,001, filed Aug. 22, 2011 and 61/530,521, filed Sep. 2, 2011, the disclosures of which are incorporated herein by reference.
- Nip 40 includes backup roll 42 , and nip roll 44 .
- backup roll 42 is a smooth, chrome-plated steel roll and nip roll 44 is a silicone rubber roll.
- both backup roll 42 and nip roll 44 are temperature controlled with, for example, internal water flow.
- polymeric netting 24 passes directly into nip 40 , and nip 40 is a quench nip. However, this is not considered necessary, and the extrusion of the netting and the entry into the nip need not be immediately sequential.
- polymeric netting 24 After passing through nip 40 , polymeric netting 24 has been transformed into polymeric layer having openings therein 50 .
- polymeric layer 50 it may be advantageous to allow polymeric layer 50 to remain wrapped around backup roll 42 for at least a portion of its circumference.
- Polymeric layer 50 has first major surface 52 on the side towards the viewer, and second major surface 54 on the side opposite from the viewer. Numerous openings 56 pass through polymeric layer 50 from first major surface 52 to second major surface 54 .
- openings 56 have well-formed, smooth edges 58 . Further, in some embodiments, openings 56 taper inwards from both first major surface 52 and second major surface 54 so that opening 56 has a minimum area 60 somewhere in the interior of polymeric layer 50 .
- openings 56 can be better appreciated in FIG. 2 , which is a cross-section view of polymeric layer 50 taken along section lines 2 - 2 in FIG. 1 .
- openings 56 have well-formed, smooth edges 58 .
- Openings 56 taper inwards from both first major surface 52 and second major surface 54 .
- the point where opening 56 tapers down to a minimum area 60 is shown to be in the interior of polymeric layer 50 .
- individual openings 56 range from 0.005 mm 2 to 5 mm 2 , and further, for at least a majority of openings 56 , the minimum area is not at either major surface 52 or 54 .
- Extrusion die 22 includes plurality of shims 70 .
- shims 40 there will be a large number of very thin shims 40 (typically several thousand shims; in some embodiments, at least 1000, 2000, 3000, 4000, 5000, 6000, 7000, 8000, 9000, or even at least 10,000), of diverse types (e.g., shims 70 a , 70 b , and 70 c ), compressed between two end blocks (e.g., 74 a and 74 b ).
- fasteners e.g., through bolts 76 threaded onto nuts 78 ) are used to assemble the components for extrusion die 22 by passing through holes 79 .
- Inlet fittings 80 a and 80 b are provided on end blocks 74 a and 74 b respectively to introduce the materials to be extruded into extrusion die 22 .
- inlet fittings 80 a and 80 b are connected to melt trains of conventional type.
- cartridge heaters 82 are inserted into receptacles 84 in extrusion die 22 to maintain the materials to be extruded at a desirable temperature while in the die.
- Shim 70 a has first aperture 90 a and second aperture 90 b .
- first apertures 90 a in shims 70 together define at least a portion of first cavity 92 a .
- second apertures 90 b in shims 70 together define at least a portion of second cavity 92 b .
- Material to be extruded conveniently enters first cavity 92 a via inlet port 80 a
- material to be extruded conveniently enters second cavity 92 b via inlet port 80 b .
- Shim 70 a has duct 94 ending in first dispensing orifice 96 a in a dispensing surface 97 .
- Shim 70 a further has passageway 98 a affording a conduit between first cavity 92 a and duct 94 .
- the dimensions of duct 94 , and especially first dispensing orifice 96 a at its end, are constrained by the dimensions desired in the polymer strands extruded from them. Since the strand speed of the strand emerging from first dispensing orifice 96 a is also of significance, manipulation of the pressure in cavity 92 a and the dimensions of passageway 98 a can be used to set the desired strand speed.
- shim 70 b is a reflection of shim 70 a , having a passageway instead affording a conduit between second cavity 92 b and second dispensing orifice 96 .
- Shim 70 c has no passageway between either of first or second cavities 92 a and 92 b , respectively, and no duct opening onto dispensing surface 97 .
- FIG. 7 a schematic perspective view of a portion of extrusion die 22 is illustrated, supplied with polymeric material and forming a net.
- Polymer from first cavity 92 a emerges as first strands 100 a from first dispensing orifices 96 a
- second strands 100 b are emerging from second dispensing orifices 96 b .
- Passageways 98 a hidden behind the nearest shim in this view
- 98 b and the pressures in cavities 92 a and 92 b are typically selected so that the strand speed of first strands 100 a are between about 2 and 6 times greater than the strand speed of second strands 100 b .
- this allows polymeric netting 24 to be formed.
- FIG. 7 a a schematic perspective view of another exemplary apparatus 20 a with a different arrangement of extrusion die 22 relative to the nip 40 is shown.
- extrusion die 22 is positioned so that the polymeric netting 24 is dispensed onto nip roller 44 and carried on that roller into the nip between nip roller 44 and backup roller 42 .
- extrusion die 22 By positioning extrusion die 22 quite close to nip roller 44 , there is little time for the strands that make up polymeric netting 24 to sag and extend under the force of gravity.
- An advantage provided by this positioning is that openings 56 a in polymeric layer 50 a tend to be rounder. More in this regard can be achieved by extruding not only very close to one of the rolls forming nip 40 , but also at an extrusion speed similar to the circumferential speed of that roll.
- FIG. 7 b a schematic perspective view of another exemplary apparatus 20 b with an alternate nip roll 44 b is shown.
- the surface of alternate nip roll 44 b includes raised areas 44 b ′ which apply more nipping force on polymeric netting 24 against backup roll 42 than the other areas of nip roll 44 b .
- enough force has been applied by raised areas 44 b ′ that openings 56 in polymeric layer 50 b are separated by longitudinal bands 50 b ′ of solid layer where the potential openings have been crushed completely closed within nip 40 .
- one or both of the rolls comprising the nip may have zones of different temperature, giving rise to longitudinal bands having no openings or different sized openings.
- the relative thickness of the extruded polymeric netting has been found to affect the range of hole sizes; with a relatively thick netting it is easier to nip the melt to form longitudinal bands 50 b ′ of solid film.
- Exemplary polymeric materials from which the netting can be made includes thermoplastic resins comprising polyolefins (e.g., polypropylene and polyethylene), polyvinyl chloride, polystyrene, nylons, polyesters (e.g., polyethylene terephthalate) and copolymers and blends thereof; elastomeric materials (e.g., ABA block copolymers, polyurethanes, polyolefin elastomers, polyurethane elastomers, metallocene polyolefin elastomers, polyamide elastomers, ethylene vinyl acetate elastomers, and polyester elastomers); adhesives such as acrylate copolymer pressure sensitive adhesives, rubber based adhesives (e.g., those based on natural rubber, polyisobutylene, polybutadiene, butyl rubbers, and styrene block copolymer rubbers), adhesives based on silicone polyureas or silicone
- Other desirable materials include, for example, styrene-acrylonitrile, cellulose acetate butyrate, cellulose acetate propionate, cellulose triacetate, polyether sulfone, polymethyl methacrylate, polyurethane, polyester, polycarbonate, polyvinyl chloride, polystyrene, polyethylene naphthalate, copolymers or blends based on naphthalene dicarboxylic acids, polyolefins, polyimides, mixtures and/or combinations thereof.
- netting used to make polymeric layers described herein include alternating first and second polymeric strands, wherein the second polymeric strands comprise a second, different polymer.
- polymeric materials of nettings used to make polymeric layers described herein comprise a colorant (e.g., pigment and/or dye) for functional (e.g., optical effects) and/or aesthetic purposes (e.g., each has different color/shade).
- a colorant e.g., pigment and/or dye
- Suitable colorants are those known in the art for use in various polymeric materials. Exemplary colors imparted by the colorant include white, black, red, pink, orange, yellow, green, aqua, purple, and blue.
- the amount of colorant(s) to be used in specific embodiments can be readily determined by those skilled in the (e.g., to achieve desired color, tone, opacity, transmissivity, etc.).
- the polymeric materials may be formulated to have the same or different colors.
- colored strands are of a relatively fine (e.g., less than 50 micrometers) diameter, the appearance of the web may have a shimmer reminiscent of silk.
- the polymeric strands have an average width in a range from 10 micrometers to 500 micrometers (in a range from 10 micrometers to 400 micrometers, or even 10 micrometers to 250 micrometers).
- nettings used to make polymeric layers described herein have a basis weight in a range from 5 g/m 2 to 400 g/m 2 (in some embodiments, 10 g/m 2 to 200 g/m 2 ).
- nettings used to make polymeric layers described herein have a strand pitch in a range from 0.5 mm to 20 mm (in some embodiments, in a range from 0.5 mm to 10 mm).
- strands of netting used to make polymeric layers described herein do not substantially cross over each other (i.e., at least 50 (at least 55, 60, 65, 70, 75, 80, 85, 90, 95, 99, or even 100) percent by number).
- nettings used to make polymeric layers described herein have alternating first and second polymeric strands exhibiting at least one of diamond-shaped or hexagonal-shaped openings.
- polymeric strands of netting used to make polymeric layers described herein have an average width in a range from 10 micrometers to 500 micrometers (in a range from 10 micrometers to 400 micrometers, or even 10 micrometers to 250 micrometers).
- polymeric strands of netting used to make polymeric layers described herein are elastic
- nettings used to make polymeric layers described herein are made of, or coated with, hydrophilic material to make them absorbent.
- nettings described herein are useful as wound absorbants to remove excess exudate from wounds, and in some embodiments, nettings described herein are made of bioresorbable polymers.
- Polymeric layers described herein can be made, for example, at least one of passing through a nip or calendaring netting comprising an array of polymeric strands periodically joined together at bond regions throughout the array.
- polymeric layers described herein have a total open area for each of the first and second, generally opposed major surfaces is not greater than 50 (in some embodiments, not greater than 45, 40, 35, 30, 25, 20, 15, 10, 5, 4, 3, 2, 1, 0.75, 0.5, 0.25, or even not greater than 0.1) percent of the total area of the respective major surface. In some embodiments, for at least a majority of the openings, the area of each opening is not greater than is 5 (in some embodiments, not greater than 2.5, 2, 1, 0.5, 0.1, 0.05, 0.01, 0.075, or even not greater than 0.005) mm 2 .
- polymeric layers described herein have in a range from 50,000 to 6,000,000 (in some embodiments, 100,000 to 6,000,000, 500,000 to, 6,000,000, or even 1,000,000 to 6,000,000) openings/m 2 .
- the openings have widths in a range from 5 micrometers to 1 mm (in some embodiments, 10 micrometers to 0.5 mm). In some embodiments, for polymeric layers described herein the openings have lengths in a range from 100 micrometers to 10 mm (in some embodiments, 100 micrometers to 1 mm). In some embodiments, for polymeric layers described herein the openings have a length to width ratio in a range from 1:1 to 100:1, (in some embodiments, 1:1 to 1.9:1, 2:1 to 100:1, 2:1 to 75:1, 2:1 to 50:1, 2:1 to 25:1, or even, 2:1 to 10:1).
- the openings have at least two pointed ends. In some embodiments, at least some of the openings are elongated with two pointed ends. In some embodiments, at least some of the openings are elongated with two opposed pointed ends. In some embodiments, at least some of the openings are ovals.
- for polymeric layers described herein have a thickness up to 2 mm (in some embodiments, up to 1 mm, 500 micrometers, 250 micrometers, 100 micrometers, 75 micrometers, 50 micrometers, or even up to 25 micrometers; in a range from 10 micrometers to 750 micrometers, 10 micrometers to 750 micrometers, 10 micrometers to 500 micrometers, 10 micrometers to 250 micrometers, 10 micrometers to 100 micrometers, 10 micrometers to 75 micrometers, 10 micrometers to 50 micrometers, or even 10 micrometers to 25 micrometers.
- for polymeric layers described herein are films having an average thickness not greater than 5 mm.
- the openings have a first side on the first major surface comprising a first polymeric material and a second, opposed side on the first major surface comprising a second, different polymeric material.
- at least one of the first or second polymeric materials are thermoplastic (e.g., nylons, polyesters, polyolefins, polyurethanes, elastomers (e.g., styrenic block copolymers), and blends thereof).
- polymeric layers described herein have a basis weight in a range from 25 g/m 2 to 500 g/m 2 (in some embodiments, 50 g/m 2 to 250 g/m 2 )
- Polymeric layers described herein are useful, for example, for as components in personal care garments such as diapers and feminine hygiene products. They can also be useful for filtering (including liquid filtering) and acoustic applications.
- the polymeric layer of Embodiment 1A wherein the total open area for each of the first and second major surfaces is in a range from 0.1 percent to not greater than 50 percent (in some embodiments, in a range from 0.1 percent to not greater than 45 percent, 0.1 percent to not greater than 40 percent, 0.1 percent to not greater than 35 percent, 0.1 percent to not greater than 30 percent, 0.1 percent to not greater than 25 percent, 0.1 percent to not greater than 20 percent, 0.1 percent to not greater than 15 percent, 0.1 percent to not greater than 10 percent, or even 0.1 percent to not greater than 5 percent) of the total area of the respective major surface.
- 0.1 percent to not greater than 50 percent in some embodiments, in a range from 0.1 percent to not greater than 45 percent, 0.1 percent to not greater than 40 percent, 0.1 percent to not greater than 35 percent, 0.1 percent to not greater than 30 percent, 0.1 percent to not greater than 25 percent, 0.1 percent to not greater than 20 percent, 0.1 percent to not greater than 15 percent, 0.1 percent to not greater than 10 percent
- the polymeric layer of Embodiment 1A wherein the total open area for each of the first and second major surfaces is not greater than 1 percent of the total area of the respective major surface.
- 4A The polymeric layer of any preceding Embodiment A, wherein for at least a majority of the openings, the area of each opening is not greater than is 5 (in some embodiments, not greater than 2.5, 2, 1, 0.5, 0.1, 0.05, 0.01, 0.075, or even not greater than 0.005) mm 2 .
- 5A The polymeric layer of any preceding Embodiment A, wherein the openings have at least two pointed ends. 6A.
- the polymeric layer of Embodiment 17A wherein at least one of the first or second polymeric materials are thermoplastic (e.g., nylons, polyesters, polyolefins, polyurethanes, elastomers (e.g., styrenic block copolymers), and blends thereof).
- 19A The polymeric layer of any preceding Embodiment A having a basis weight in a range from 25 g/m 2 to 500 g/m 2 (in some embodiments, 50 g/m 2 to 250 g/m 2 ).
- 20A The polymeric layer of any preceding Embodiment A comprising at least one of a dye or pigment therein. 21A.
- the polymeric layer of any preceding Embodiment A further comprising a layer of adhesive thereon.
- 22A A method of making a polymeric layer of any preceding Embodiment A, the method comprising at least one of passing through a nip or calendaring a netting comprising an array of polymeric strands periodically joined together at bond regions throughout the array. 1B.
- 9B. The polymeric layer of any preceding Embodiment B, wherein the openings have widths in a range from 5 micrometers to 1 mm (in some embodiments, 10 micrometers to 0.5 mm) 10B.
- the polymeric layer of Embodiment 14B wherein at least one of the first or second polymeric materials are thermoplastic (e.g., nylons, polyesters, polyolefins, polyurethanes, elastomers (e.g., styrenic block copolymers), and blends thereof).
- thermoplastic e.g., nylons, polyesters, polyolefins, polyurethanes, elastomers (e.g., styrenic block copolymers), and blends thereof.
- 16B The polymeric layer of any preceding Embodiment B having a basis weight in a range from 25 g/m 2 to 500 g/m 2 (in some embodiments, 50 g/m 2 to 250 g/m 2 ).
- 17B The polymeric layer of any preceding Embodiment B comprising at least one of a dye or pigment therein. 18B.
- the polymeric layer of any preceding Embodiment B further comprising a layer of adhesive thereon.
- 19B A method of making a polymeric layer of any preceding Embodiment B, the method comprising at least one of passing through a nip or calendaring netting comprising an array of polymeric strands periodically joined together at bond regions throughout the array. 1C.
- a method of making a polymeric layer having openings therein comprising at least one of passing through a nip or calendaring netting comprising an array of polymeric strands periodically joined together at bond regions throughout the array, wherein the netting has a thickness up to 2 mm (in some embodiments, up to 1.5 mm, 1 mm, 750 micrometers, 500 micrometers, 250 micrometers, 100 micrometers, 75 micrometers, 50 micrometers, or even up to 25 micrometers; in a range from 10 micrometers to 2 mm, 10 micrometers to 1.5 mm, 10 micrometers to 1 mm, 10 micrometers to 750 micrometers, 10 micrometers to 750 micrometers, 10 micrometers to 500 micrometers, 10 micrometers to 250 micrometers, 10 micrometers to 100 micrometers, 10 micrometers to 75 micrometers, 10 micrometers to 50 micrometers, or even 10 micrometers to 25 micrometers).
- Embodiment 2C The method of Embodiment 1C, wherein the polymeric strands do not cross each other.
- 3C The method of either Embodiment 1C or 2C, wherein the polymeric layer has a basis weight in a range from 25 g/m 2 to 500 g/m 2 (in some embodiments, 50 g/m 2 to 250 g/m 2 or 10 g/m 2 to 200 g/m 2 ).
- 4C The method of any preceding Embodiment C, wherein the netting has a strand pitch in a range from 0.5 mm to 20 mm (in some embodiments, in a range from 0.5 mm to 10 mm) 5C.
- 7C The method of any preceding Embodiment C, wherein the plurality of strand of the netting include alternating first and second polymeric strands, wherein the second polymeric strands comprise a second, different polymer.
- 8C. The method of any preceding Embodiment C, wherein the nip or calendar has at least one of at least one raised area or at least two zones of different temperatures.
- the thickness of the shims in the repeat sequence was 4 mils (0.102 mm) for shims 70 with connection to the first cavity, the second cavity, and for the spacers which had no connection to either cavity ( 70 a , 70 b and 70 c , respectively).
- Shims 70 were formed from stainless steel, with perforations cut by a wire electron discharge machining.
- the height of dispensing orifices 96 a fed by the first cavity was cut to 15 mils (0.381 mm)
- the height of dispensing orifices 96 b fed by the second cavity was cut to 5 mils (0.127 mm)
- the extrusion orifices were aligned in a collinear, alternating arrangement, and resulting dispensing surface 97 was as shown in FIG. 8 .
- the total width of the shim setup was 15 cm.
- the inlet fittings on the two end blocks were each connected to a conventional single-screw extruder.
- a chill roll was positioned adjacent to the distal opening of the co-extrusion die to receive the extruded material.
- the extruder feeding the first cavity was loaded with thirty-five melt flow index polypropylene pellets (obtained under the trade designation “EXXONMOBIL 3155 PP” from ExxonMobil, Irving Tex.).
- the extruder feeding the second cavity was also loaded with thirty-five melt flow index polypropylene pellets (“EXXONMOBIL 3155 PP”).
- the melt was extruded vertically into an extrusion quench takeaway nip.
- the quench nip was a smooth temperature controlled chrome plated 20 cm diameter steel roll and an 11 cm diameter silicone rubber roll. The rubber roll was about 60 durometer. Both were temperature controlled with internal water flow.
- the nip pressure was generated with 2 pressurized air cylinders.
- the web path wrapped 180 degrees around the chrome steel roll and then to a windup roll.
- a schematic of the quench process is shown in FIG. 1 .
- Orifice width for the first cavity 0.102 mm Orifice height for the first cavity: 0.381 mm Orifice width of the second cavity: 0.102 mm Orifice height of the second cavity: 0.127 mm Land spacing between orifices 0.102 mm
- Flow rate of first polymer 0.60 kg/hr.
- Flow rate of second polymer 0.64 kg/hr.
- Quench roll temperature 65° C. Quench takeaway speed 3.1 m/min. Melt drop distance 5 cm Nip Pressure 0.1 kg/cm
- FIG. 9 An optical digital photo at 10 ⁇ of the resulting polymeric layer is shown in FIG. 9 .
- FIG. 10 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 10 .
- Example 2 was made as described for Example 1, except the quench takeaway speed was 1.5 m/min.
- FIG. 11 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 11 .
- FIG. 12 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 12 .
- Example 3 was made as described for Example 1, except the quench roll temperature was 24° C.
- FIG. 13 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 13 .
- FIG. 14 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 14 .
- Example 4 was made the same as Example 2 except the quench roll temperature was 24° C.
- FIG. 15 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 15 .
- FIG. 16 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 16 .
- Example 5 was made the same as Example 4 except the polymer melt temperature was raised to 260° C.
- FIG. 17 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 17 .
- FIG. 18 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 18 .
- Example 6 was made the same as Example 5 except the quench takeaway speed was 3.1 m/min.
- FIG. 19 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 19 .
- FIG. 20 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 20 .
- the thickness of the shims in the repeat sequence was 4 mils (102 mm) for shims 70 ′ with connection to the first cavity, the second cavity, and for the spacers which had no connection to either cavity ( 70 a ′, 70 b ′ and 70 c ′, respectively).
- the shims were formed from stainless steel, with perforations cut by a wire electron discharge machining.
- first and second extrusion orifices 96 a ′ and 96 b ′ was cut to 30 mils (0.762 mm)
- the extrusion orifices were aligned in a collinear, alternating arrangement, and resulting dispensing surface 97 ′ was as shown generally in FIG. 21 .
- Two spacer shims followed by two shims with connection to the first cavity, followed by two spacer shims, followed by 4 shims with connection to the second cavity comprises the shim stack sequence.
- the total width of the shim setup was 15 cm.
- the inlet fittings on the two end blocks were each connected to a conventional single-screw extruder.
- a chill roll was positioned adjacent to the distal opening of the co-extrusion die to receive the extruded material.
- the extruder feeding the first cavity was loaded with thirty-five melt flow index polypropylene pellets (“EXXONMOBIL 3155 PP”).
- the extruder feeding the second cavity was also loaded with thirty-five melt flow index polypropylene pellets (“ExxonMobil 3155PP”).
- the melt was extruded vertically into an extrusion quench takeaway nip.
- the quench nip was a smooth temperature controlled chrome plated 20 cm diameter steel roll and an 11 cm diameter silicone rubber roll. The rubber roll was about 60 durometer. Both were temperature controlled with internal water flow.
- the nip pressure was generated with 2 pressurized air cylinders.
- the web path wrapped 180 degrees around the chrome steel roll and then to a windup roll.
- a schematic view of the quench process in shown in FIG. 1 .
- Orifice width for the first cavity 0.204 mm Orifice height for the first cavity: 0.762 mm Orifice width of the second cavity: 0.408 mm Orifice height of the second cavity: 0.762 mm Land spacing between orifices 0.204 mm
- Flow rate of first polymer 1.9 kg/hr.
- Flow rate of second polymer 1.5 kg/hr.
- Quench roll temperature 15° C. Quench takeaway speed 6.1 m/min. Melt drop distance 10 cm.
- FIG. 22 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 22 .
- FIG. 23 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 23 .
- the thickness of shims 70 ′′ in the repeat sequence was 4 mils (102 mm) for the shims with connection to the first cavity, the second cavity, and for the spacers which had no connection to either cavity ( 70 a ′′, 70 b ′′ and 70 c ′′, respectively).
- the shims were formed from stainless steel, with perforations cut by a wire electron discharge machining.
- first and second extrusion orifices 96 a ′′ and 96 b ′′ was cut to 30 mils (0.762 mm)
- Four spacer shims followed by four shims with connection to the first cavity, followed by four spacer shims, followed by eight shims with connection to the second cavity comprises the shim stack sequence.
- the extrusion orifices were aligned in a collinear, alternating, arrangement, and resulting dispensing surface 97 ′′ was as shown generally in FIG. 24 .
- the total width of the shim setup was 15 cm.
- the inlet fittings on the two end blocks were each connected to a conventional single-screw extruder.
- a chill roll was positioned adjacent to the distal opening of the co-extrusion die to receive the extruded material.
- the extruder feeding the first cavity was loaded with thirty-five melt flow index polypropylene pellets (“EXXONMOBIL 3155 PP”).
- the extruder feeding the second cavity was also loaded with thirty-five melt flow index polypropylene pellets (“ExxonMobil 3155PP”).
- the melt was extruded vertically into an extrusion quench takeaway nip.
- the quench nip was a smooth temperature controlled chrome plated 20 cm diameter steel roll and an 11 cm diameter silicone rubber roll. The rubber roll was about 60 durometer. Both were temperature controlled with internal water flow.
- the nip pressure was generated with 2 pressurized air cylinders.
- the web path wrapped 180 degrees around the chrome steel roll and then to a windup roll.
- a schematic view of the quench process in shown in FIG. 1 .
- Orifice width for the first cavity 0.408 mm Orifice height for the first cavity: 0.762 mm Orifice width of the second cavity: 0.816 mm Orifice height of the second cavity: 0.762 mm Land spacing between orifices 0.408 mm
- Flow rate of first polymer 2.1 kg/hr.
- Flow rate of second polymer 2.6 kg/hr.
- FIG. 25 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 25 .
- FIG. 26 A scanning electron digital photomicrograph of a cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 26 .
- Example 9 was made the same as Example 8 except the quench takeaway speed was 2.4 m/min.
- FIG. 27 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 27 .
- FIG. 28 A cross-section of one of the holes in the resulting polymeric layer is shown in FIG. 28 .
- the thickness of the shims in the repeat sequence was 4 mils (102 mm) for the shims with connection to the first cavity, the second cavity, and for the spacers which had no connection to either cavity ( 70 a ′′′, 70 b ′′′ and 70 c ′′′, respectively).
- the shims were formed from stainless steel, with perforations cut by a wire electron discharge machining.
- first and second extrusion orifices, 96 a ′′′ and 96 b ′′′ was cut to 30 mils (0.762 mm)
- the extrusion orifices were aligned in a collinear, alternating arrangement, and resulting dispensing surface 97 ′′′ was as shown generally in FIG. 29 .
- Four spacer shims 70 c ′′′ followed by eight shims with connection to second cavity 96 b ′′, followed by four spacer shims 70 c ′′′, followed by twenty shims with connection to first cavity 96 a ′′′ comprises the shim stack sequence.
- the total width of the shim setup was 15 cm.
- the inlet fittings on the two end blocks were each connected to a conventional single-screw extruder.
- a chill roll was positioned adjacent to the distal opening of the co-extrusion die to receive the extruded material.
- the extruder feeding the first cavity was loaded with thirty-five melt flow index polypropylene pellets (“EXXONMOBIL 1024 PP”).
- the extruder feeding the second cavity was also loaded with thirty-five melt flow index polypropylene pellets (“ExxonMobil 1024 PP”).
- the melt was extruded vertically into an extrusion quench takeaway nip.
- the quench nip was a smooth temperature controlled chrome plated 20 cm diameter steel roll and an 11 cm diameter silicone rubber roll. The rubber roll was About 60 durometer. Both were temperature controlled with internal water flow.
- the nip pressure was generated with 2 pressurized air cylinders.
- the web path wrapped 180 degrees around the chrome steel roll and then to a windup roll.
- a schematic view of the quench process in shown in FIG. 1 .
- Orifice width for the first cavity 0.408 mm Orifice height for the first cavity: 0.762 mm Orifice width of the second cavity: 2.032 mm Orifice height of the second cavity: 0.762 mm Land spacing between orifices 0.306 mm Flow rate of first polymer 0.95 kg/hr. Flow rate of second polymer 0.9 kg/hr. Extrusion temperature 218° C. Quench roll temperature 15° C. Quench takeaway speed 1.4 m/min. Melt drop distance 10 cm. Nip Pressure 0.1 kg/cm
- FIG. 30 An optical photograph at 10 ⁇ of the resulting polymeric layer is shown in FIG. 30 .
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US14/387,332 US20150079337A1 (en) | 2012-03-26 | 2013-03-11 | Films comprising an array of openings and methods of making the same |
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US201261615676P | 2012-03-26 | 2012-03-26 | |
PCT/US2013/030143 WO2013148128A1 (en) | 2012-03-26 | 2013-03-11 | Films comprising an array of openings and methods of making the same |
US14/387,332 US20150079337A1 (en) | 2012-03-26 | 2013-03-11 | Films comprising an array of openings and methods of making the same |
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US14/387,332 Abandoned US20150079337A1 (en) | 2012-03-26 | 2013-03-11 | Films comprising an array of openings and methods of making the same |
US15/269,223 Active 2034-01-15 US10449700B2 (en) | 2012-03-26 | 2016-09-19 | Methods of making films comprising an array of openings |
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EP (1) | EP2830863B1 (de) |
JP (1) | JP2015516900A (de) |
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KR20130018778A (ko) | 2010-03-25 | 2013-02-25 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | 복합 층 |
KR101812822B1 (ko) | 2010-03-25 | 2017-12-27 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | 복합 층 |
WO2011119327A1 (en) | 2010-03-25 | 2011-09-29 | 3M Innovative Properties Company | Composite layer |
CN105399971B (zh) | 2010-03-25 | 2019-03-01 | 3M创新有限公司 | 复合层 |
KR101831461B1 (ko) | 2010-03-25 | 2018-02-22 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | 다중 스트라이프 압출물을 제조하기 위한 압출 다이 요소, 압출 다이 및 방법 |
TWI616195B (zh) | 2011-02-16 | 2018-03-01 | 3M新設資產公司 | 製造一機械式緊固件之方法、網狀機械式緊固件、及網狀機械式緊固層壓物 |
WO2013028654A2 (en) * | 2011-08-22 | 2013-02-28 | 3M Innovative Properties Company | Netting, arrays, and dies, and methods of making the same |
CN103764367B (zh) | 2011-09-02 | 2017-05-31 | 3M创新有限公司 | 股线、结网、模头及其制造方法 |
EP2763843B1 (de) | 2011-10-05 | 2018-11-07 | 3M Innovative Properties Company | Dreidimensionales polymerfasernetz, matrizen und verfahren zu ihrer herstellung |
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US8889243B2 (en) | 2012-08-16 | 2014-11-18 | 3M Innovative Properties Company | Mechanical fastening nets and methods of making the same |
-
2013
- 2013-03-11 EP EP13712041.6A patent/EP2830863B1/de active Active
- 2013-03-11 JP JP2015503242A patent/JP2015516900A/ja active Pending
- 2013-03-11 WO PCT/US2013/030143 patent/WO2013148128A1/en active Application Filing
- 2013-03-11 US US14/387,332 patent/US20150079337A1/en not_active Abandoned
- 2013-03-11 CN CN201380016502.7A patent/CN104321186B/zh not_active Expired - Fee Related
- 2013-03-11 KR KR1020147029909A patent/KR20140139075A/ko not_active Application Discontinuation
-
2016
- 2016-09-19 US US15/269,223 patent/US10449700B2/en active Active
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Cited By (9)
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US10449700B2 (en) | 2012-03-26 | 2019-10-22 | 3M Innovative Properties Company | Methods of making films comprising an array of openings |
US9591896B2 (en) | 2012-05-16 | 2017-03-14 | 3M Innovative Properties Company | Method of making a mechanical fastener using diverging disks |
US9687048B2 (en) | 2012-05-16 | 2017-06-27 | 3M Innovative Properties Company | Method of making a mechanical fastener using a crowned surface |
US10327967B2 (en) | 2012-05-16 | 2019-06-25 | 3M Innovative Properties Company | Method of making a mechanical fastener using a crowned surface |
US9475205B2 (en) | 2012-05-18 | 2016-10-25 | 3M Innovative Properties Company | Method of making a mechanical fastener and apparatus including a roller with protrusions |
US10000028B2 (en) | 2012-08-16 | 2018-06-19 | 3M Innovative Properties Company | Mechanical fastening nets and methods of making the same |
US9314962B2 (en) | 2013-05-10 | 2016-04-19 | 3M Innovative Properties Company | Method of separating strands on a stretching surface |
US9630359B2 (en) | 2013-05-10 | 2017-04-25 | 3M Innovative Properties Company | Method of separating strands on a stretching surface |
US11220085B2 (en) * | 2017-08-31 | 2022-01-11 | Kimberly-Clark Worldwide, Inc. | Apertured elastic film laminates |
Also Published As
Publication number | Publication date |
---|---|
KR20140139075A (ko) | 2014-12-04 |
EP2830863B1 (de) | 2016-05-25 |
US20170001342A1 (en) | 2017-01-05 |
JP2015516900A (ja) | 2015-06-18 |
CN104321186B (zh) | 2017-09-08 |
US10449700B2 (en) | 2019-10-22 |
EP2830863A1 (de) | 2015-02-04 |
WO2013148128A1 (en) | 2013-10-03 |
CN104321186A (zh) | 2015-01-28 |
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