EP1438452A1 - Non-tisses a un ou des sections de filaments - Google Patents
Non-tisses a un ou des sections de filamentsInfo
- Publication number
- EP1438452A1 EP1438452A1 EP02794942A EP02794942A EP1438452A1 EP 1438452 A1 EP1438452 A1 EP 1438452A1 EP 02794942 A EP02794942 A EP 02794942A EP 02794942 A EP02794942 A EP 02794942A EP 1438452 A1 EP1438452 A1 EP 1438452A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- filaments
- nonwoven fabric
- fabric
- nylon
- cross sections
- 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- Withdrawn
Links
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
Definitions
- This invention relates to new nonwoven fabrics made with two or more filament cross sections.
- the mixed filament cross sections give these new fabrics advantageous properties.
- Nonwoven fabrics and numerous uses thereof are well known to those skilled in the textiles art. Such fabrics can be prepared by forming a web of continuous filaments and/or staple fibers and bonding the fibers at points of fiber-to-fiber contact to provide a fabric of requisite strength.
- the term "bonded nonwoven fabric” is used herein to denote nonwoven fabrics wherein a major portion of the fiber-to-fiber bonding referred to is adhesive bonding accomplished via incorporation of adhesives in the web to "glue" fibers together or autogenous bonding such as obtained by heating the web or by the use of liquid or gaseous bonding agents (usually in conjunction with heating) to render the fibers cohesive or mechanical bonding, particularly autogenous bonding, the web may be subjected to mechanical compression to facilitate obtaining adequate bonding.
- Nonwoven fabrics are determined by several factors, including but not limited to, the method used to produce the fabrics, the polymer or polymer combinations used, the bonding method, the bond pattern, the fabrics, the structure of the fabric, the filament cross section, the filament denier (dpf) and the basis weight of the fabric.
- Nonwoven fabrics made with filaments with all round, all trilobal or all hollow cross sections are commonly found. These filament cross sections impart specific properties to the fabrics such as opacity or coverage, thickness, loft, strength, hand or softness, luster, fiber surface area to facilitate coating, tensile strength, water absorption and other properties.
- Spunbonded nonwoven fabrics formed of nylon, polyester, polypropylene, or other man-made polymers are widely used commercially for a number of purposes. Such fabrics exhibit excellent strength, coverage, hand and permeability properties and accordingly are desirable for use in construction fabrics, filtration material, mattress pads, mattress pad skirts, medical fabrics and furniture and bedding backing materials.
- the fabric can be produced via the well-known spunbonding process in which molten polymer is extruded through one or more spinnerets into filaments. Bicomponent or multicomponent spinning methods as described in U.S.
- Patent numbers 3,968,307; 4,052,146; 4,406,850; 4,424,257; 4,424,258; 4,830,904; 5,534,339; 5,783,503; 5,895,710; 6,074,590; and 6,207,276, incorporated by reference, can also be used to make multiconstituent filaments of different cross sections.
- the filaments are attenuated and drawn pneumatically and deposited onto a collection surface to form a web.
- the web is then bonded together to produce a strong, coherent fabric. Filament bonding is typically accomplished either thermally or chemically, i.e., autogenously.
- Thermal bonding is accomplished by compression of the web of filaments between the nip of a pair of cooperating heating calender rolls thereby setting the thickness.
- the web of filaments In autogenous bonding of nylon filaments, the web of filaments is transported to a chemical bonding station or "gashouse" which exposes the filaments to an activating agent (i.e., HCl) and water vapor. Water vapor enhances the penetration of the HCl into the filaments and causes them to become tacky and thus amenable to bonding.
- the web passes between rolls which compress and bond the web thereby setting the thickness.
- Adequate bonding is necessary to minimize fabric fuzzing (i.e., the presence of unbonded filaments) and to impart good strength properties to the fabric.
- Autogenous bonding has been especially used in forming spunbonded nylon industrial fabrics. Mechanical compression normally sets the loft or thickness of fabrics with similar basis weights. It is common practice to increase thickness and strength by increasing the basis weight, or the mass per square area.
- the lightest nonwoven fabric that meets the product property requirements is used due to cost factors.
- a nonwoven fabric that would meet the requirements by yielding the desired properties at lighter basis weights would reduce costs.
- a process that makes such fabrics would also be beneficial.
- Thickness or loft and coverage or opacity of nonwoven fabrics is normally determined by the basis weight. Increasing the basis weight adds cost due to the use of more raw materials. It is desirable to have increased thickness or coverage in some applications where these fabrics are used without increasing the basis weight. Thickness, coverage and strength can sometimes be affected by the filament cross section. Lighter weight fabrics with higher strength, loft or coverage would be more desirable and less costly.
- Nonwoven fabrics are also used in a variety of coating applications. Coating materials will be captured and held more effectively onto a fabric that contains more fiber surface area. Fabrics that use less coating to effect the same desired results would be more cost effective and desirable.
- the subject invention concerns nonwoven fabrics containing filaments of at least two different cross sections.
- the subject invention further pertains to methods used to produce these fabrics.
- the nonwoven fabric of the subject invention is made of nylon.
- the non- woven fabric can be made by, for example, altering the filament cross section in a portion of the capillaries in the same spinneret or by using spinnerets with different filament cross sections on opposing sides of a spunbond beam.
- the subject invention also provides advantageous processes for providing lighter fabrics that have the same properties as fabrics having higher basis weights.
- an improved nonwoven nylon fabric is produced by using filaments with at least two different cross sectional shapes.
- the nonwoven fabric can be produced by mechanically blending staple yarn with filaments of different cross sections into a web. This web is then formed into a bonded nonwoven fabric using adhesives or mechanical methods such as, but not limited to, carding, needle punching, air laying, wet laying, hydroentangling, powder or adhesive bonding, air bonding, thermal bonding and chemical bonding.
- the fabrics of the subject invention have filaments with two or more cross sections that are round, crescent, multilobal, oval, diamond or a cross section with voids (hollow filaments).
- the multilobal filaments have at least two lobes and, preferably, three or more lobes. In a preferred embodiment, the multilobal filaments are trilobal.
- the use of multilobal filaments is particularly advantageous for maximizing coatings since these filaments have more surface area.
- the fabrics may have a dpf ranging from about 0.5 dpf to about 20 dpf.
- the present invention concerns nonwoven fabrics with filaments of two or more different cross sections that provide properties better than fabrics with filaments of a single cross section.
- reference to two or more cross sections refers to the shape of the cross sections.
- the subject invention further concerns methods used to produce these fabrics.
- the fabrics of the subject invention have, for example, increased coverage or opacity compared to conventional nonwoven fabrics and have higher thickness while maintaining softness and strength at the same basis weight and dpf.
- round filaments are mixed with trilobal filaments to produce nonwoven fabrics. These fabrics have more opacity, stronger tensile properties and hold more coating material than fabrics made with only round cross section filaments because the trilobal filaments add strength by the way they pack in the fabric and add opacity by the way they reflect light. They also hold more coating material since trilobal filaments have more surface area.
- the nonwoven fabrics of the subject invention have basis weights from 0.1 ounce per square yard up to 7 ounces per square yard.
- the weight of the fabric produced as described herein is between about 0.5 and about 2.5 ounces per square yard. In a specific embodiment, the fabric is about 1.15 ounces per square yard.
- the characteristics of the fabrics of the subject invention are achieved utilizing filaments having, for example, round, crescent, diamond, oval, hollow, and/or multilobal cross- sections.
- the predominant fiber cross section is selected from the group consisting of round, multi-lobal, cresent, hollow, diamond and oval.
- reference to the "predominant" cross section means that, by number, that cross section makes up a greater percentage of the filaments than any other single cross section.
- the predominant cross section comprises at least about 10% by number of the filaments. More preferably the filaments with the predominant cross section comprise at least 15%.
- the filament with the predominant cross section may comprise up to 95% of the filaments by number.
- the filaments with the predominant cross section may comprise from about 10% to about 95% of the filaments by number.
- the percentage can be any percentage between 10 and 95 and every such percentage between 10 and 95 is specifically contemplated by the subject matter.
- the remaining filaments are preferably selected from the group consisting of round, multilobal, crescent, hollow, diamond and oval.
- reference to hollow filaments contemplates one or more voids within the filaments.
- the subject invention further concerns methods to produce these fabrics that contain filaments with at least two different cross sections.
- Any man-made (synthetic) polymer can be used, such as, but not limited to, polycaprolactum, polyamide, polyester, polyethylene, polypropylene, polylactic acid, nylon 10, nylon 11 and nylon 12. Blends and mixtures of man-made polymers can also be used.
- Conjugate spinning or multicomponenet spinning methods can be employed to make filaments of at least two different polymer types with two or more different cross sections.
- the fabrics can be produced by, for example, installing spinnerets with capillaries of different cross sections on different positions, sides or beams of a spunbond machine. Spinnerets with different capillary cross sections or capillary sizes within the same spinneret can also be used.
- the fabrics can also be produced by blending fiber with filaments of different cross sections using carding methods and then using dispersing methods to produce a nonwoven web such as, but not limited to, air laying or wet laying methods, needle punching or hydoentangling. This web is then formed into a nonwoven fabric using adhesives or mechanical methods such as, but not limited to, powder or adhesive bonding, air bonding, thermal bonding or chemical bonding. Discrete bonds between the filaments may account for 5% to 50% of the area of the fabric and, more preferably, 16% to 24% of the area.
- the fabrics of the subject invention can also be produced by extruding a plurality of continuous filaments, directing the filaments through an attenuation device, such as slots or jets, to draw the filaments, depositing the filaments onto a collection surface such that a web is formed, and bonding the filaments together either autogenously or thermally to form a coherent, strong fabric.
- the fibers (filaments) of the fabric of the subject invention need not be crimpled.
- the fibers are not melt blown.
- the filaments are continuous.
- reference herein to the molecular orientation of a filament pertains to the alignment or arrangement of polymer chains in the filament.
- fabrics with two or more filament cross sections can be made using a nylon spunbond method utilizing a slot drawing mechanism or attenuation jets.
- the nylon compound will be nylon 6, 6 and/or nylon 6; however, other man-made fibers from polymers such as, but not limited to, polyester, polypropylene, polyethylene or other polyamides or combinations of such can be used. Also, mixtures, blends or copolymers can be used as taught in U.S. Patents 5,431,986 and 5,913,993 both of which are incorporated herein by reference.
- polyethylene, polypropylene, and/or polyester can be added to the nylon material. This produces a softer feel and increases water repellency.
- the polyethylene should have a melt index between about 5 grams/10 min and about 200 grams/10 min and a density between about 0.85 grams/cc and about 1.1 grams/cc.
- the polyethylene can be added at a concentration of about 0.05% to about 20%.
- Nylon filaments produced during the process of the subject invention may be bonded chemically, ultrasonically, or thermally.
- HCl gas and water vapor can be applied to achieve boding as described in U.S. Patent 3,853,659 incorporated herein by reference.
- the filaments may be heated to, for example, between 180°C and about 250°C. Preferably, the filaments are heated to between about 200°C and 235°C.
- Nonwoven fabric samples with two or more filament cross sections can be made using nylon 6,6 polymer by installing a spinneret with round capillaries on one side and a spinneret with trilobal capillaries on the other side of a dual spinning beam. Other combinations of cross sections can be used as shown in Table 1 below.
- the number of spinneret holes can be adjusted to produce fabrics with filaments that are less than 1.5 times larger than the smallest filaments in the fabric. Spinnerets with the same number of holes and the same spinneret throughput will yield the same dpf for all filaments.
- the nylon 6,6 polymer can be melted and extruded at a temperature of about 295°C.
- Filaments can then be attenuated and drawn pneumatically using aspirating jets or a slot device and deposited onto a laydown or forming box.
- the resulting webs can then be directed to a calender where about 20% of the surface area is bonded at discrete points at a temperature of about 216°C. It is expected that fabrics with some trilobal filaments will have higher opacity at the same basis weight than fabrics containing only round filaments.
- Nonwoven fabric samples can be made using nylon 6,6 polymer by installing a spinneret or spinnerets where more than 50% but less that 95% of the capillaries are of a round cross section and the remaining are of a trilobal cross section. Placing the different cross sections in the same spinneret will yield the same dpf for all filaments.
- the nylon 6,6 polymer can be melted and extruded at a temperature of about 295°C.
- Filaments can then be attenuated and drawn pneumatically using aspirating jets or a slot device and deposited onto a laydown or forming box.
- the resulting webs can then be directed to a calender where about 20% of the surface area is bonded at discrete points at a temperature of about 216°C.
- Combinations of two different cross sections as shown in Table 1 can also be used to produce sample fabrics.
- Combinations of three or more filament cross sections can be created by adding one or more different cross sections in any possible combination to the items in Table 1 above. Filaments from each different cross section must comprise at least five or more percent of the total number of filaments. Filaments from any of the cross sections can make up the largest percentage of the total filaments in the web.
- a fabric can be comprised of 40% hollow filaments, 25% round filaments, 25% trilobal filaments, 5% diamond filaments and 5% oval filaments.
- Nonwoven fabric samples can be made using nylon 6,6 or nylon 6 polymer or a combination of both as in example 1, except, the resulting web can be autogeneously bonded by directing the web to a chemical bonding station where the web filaments are bonded using HCl gas and water vapor at a temperature around 39°C.
- the fabrics are produced by chemically bonding the filaments together in a gas house.
- the web is then subjected to a roll treatment in which the web is compacted and further bonded.
- Nonwoven fabric samples can be made using nylon 6,6 or nylon 6 polymer or a combination of both as in Example 2, except, the resulting web can be autogeneously bonded by directing the web to a chemical bonding station where the web filaments are bonded using HCl gas and water vapor at a temperature around 39°C. The fabrics are produced by chemically bonding the filaments together in a gas house. The web is then subjected to a roll treatment in which the web is compacted and further bonded.
- Nonwoven fabric samples can be made using polyester, polypropylene or polyethylene by installing spinnerets on respective sides of a spin beam as described in Example 1.
- the specific polymer must be melted and extruded at the appropriate temperature to achieve satisfactory spinning performance.
- Filaments can then be attenuated and drawn pneumatically using aspirating jets or a slot device and deposited onto a laydown or forming box.
- the resulting web can then be directed to a calender where about 20% of the surface area is bonded at discrete points at the appropriate temperature required to bond the web based on the polymer.
- Nonwoven fabric samples can be made as described in Examples 1 through 5 above using mixtures, blends or copolymers of man made polymers.
- Nonwoven fabric samples can be made as described in Examples 1 through 6 above using conjugate spinning or bicomponent spinning methods.
- Example 8 A web of filaments can be produced with a blend of filaments with different cross sections in combinations listed in Table 1. Filaments with different cross sections can comprise at least one and, preferably, at least five or more percent of the total number of filaments.
- the web can then be formed into a bonded nonwoven fabric using adhesives or mechanical methods using the processes commonly referred to as carding, needle punching, wet laying, air laying, hydroentagling, powder or adhesive bonding, through air bonding, thermal bonding or chemical bonding.
- Fabrics can be produced as described in Examples 1 through 8 above with mixed filaments of different cross sections. Certain cross sections can cause spectral reflection which is not desirable in some applications. Small amounts of titanium dioxide can be added if spectral reflection is objectionable.
- Example 10
- Nonwoven fabric samples can be made using nylon 6,6 polymer by installing a spinneret or spinnerets where at least 14.5% of the capillaries are of a round cross section, 5% are of a trilobal cross section and the remaining capillaries are a combination of oval, multilobal, hollow, crescent or diamond cross sections. Placing the different cross sections in the same spinneret will yield the same dpf for all filaments.
- the nylon 6,6 polymer can be melted and extruded at a temperature of about 295°C. Filaments can then be attenuated and drawn pneumatically using aspirating jets or a slot device and deposited onto a lay down or forming box.
- the resulting webs can then be directed to a calender where about 20% of the surface area is bonded at discrete points at a temperature of about 216°C.
- Other percentages of different cross sections can be used to produce sample fabrics. Filaments from any of the cross sections can make up the largest percentage of the total filaments in the web.
- a fabric can be comprised of 40% hollow filaments, 25% multilobal, 10%) round filaments, 10% trilobal filaments, 2% diamond filaments, 8% crescent, and 5% oval filaments.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
Abstract
La présente invention concerne des non-tissés contenant des filaments d'au moins deux sections transversales différentes. L'invention concerne également des procédés mis en oeuvre pour produire de tels tissus. Dans un mode de réalisation spécifiquement illustré de l'invention, le non-tissé est en nylon.
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US31320001P | 2001-08-17 | 2001-08-17 | |
US313200P | 2001-08-17 | ||
US33181201P | 2001-11-20 | 2001-11-20 | |
US331812P | 2001-11-20 | ||
PCT/US2002/027182 WO2003016606A1 (fr) | 2001-08-17 | 2002-08-19 | Non-tisses a un ou des sections de filaments |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1438452A1 true EP1438452A1 (fr) | 2004-07-21 |
Family
ID=26978735
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02794942A Withdrawn EP1438452A1 (fr) | 2001-08-17 | 2002-08-19 | Non-tisses a un ou des sections de filaments |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP1438452A1 (fr) |
JP (2) | JP4430932B2 (fr) |
WO (1) | WO2003016606A1 (fr) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10252414B4 (de) * | 2002-11-12 | 2007-04-26 | Corovin Gmbh | Nichtrunde Spinnplattenbohrung |
US20050227563A1 (en) * | 2004-01-30 | 2005-10-13 | Bond Eric B | Shaped fiber fabrics |
US20050215155A1 (en) * | 2004-03-23 | 2005-09-29 | The Procter & Gamble Company | Absorbent article with improved opacity |
US20060012072A1 (en) * | 2004-07-16 | 2006-01-19 | Hagewood John F | Forming shaped fiber fabrics |
US11274384B2 (en) | 2011-08-08 | 2022-03-15 | Avintiv Specialty Materials Inc. | Liquid barrier nonwoven fabrics with ribbon-shaped fibers |
JP2018523021A (ja) | 2015-07-13 | 2018-08-16 | アビンティブ・スペシャルティ・マテリアルズ・インコーポレイテッドAVINTIV Specialty Materials Inc. | 活性成分への親和性を有する処理済不織布 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4868031A (en) * | 1987-06-22 | 1989-09-19 | Hercules Incorporated | Soft water-permeable polyolefins nonwovens having opaque characteristics |
WO2000015891A1 (fr) * | 1998-09-14 | 2000-03-23 | Cerex Advanced Fabrics, L.P. | Non-tisses |
WO2000048478A1 (fr) * | 1999-02-17 | 2000-08-24 | Filtrona Richmond, Inc. | Procede et appareil permettant de filer une bande de fibres melangees et les produits ainsi obtenus |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4963298A (en) * | 1989-02-01 | 1990-10-16 | E. I. Du Pont De Nemours And Company | Process for preparing fiber, rovings and mats from lyotropic liquid crystalline polymers |
JPH03249255A (ja) * | 1990-02-21 | 1991-11-07 | Unitika Ltd | スパンボンド不織布及びその製造方法 |
JPH08260323A (ja) * | 1995-03-28 | 1996-10-08 | Unitika Ltd | 生分解性長繊維不織布及びその製造方法 |
FR2749860B1 (fr) * | 1996-06-17 | 1998-08-28 | Freudenberg Spunweb Sa | Nappe non tissee formee de filaments continus tres fins |
-
2002
- 2002-08-19 WO PCT/US2002/027182 patent/WO2003016606A1/fr active Application Filing
- 2002-08-19 JP JP2003520887A patent/JP4430932B2/ja not_active Expired - Lifetime
- 2002-08-19 EP EP02794942A patent/EP1438452A1/fr not_active Withdrawn
-
2009
- 2009-11-16 JP JP2009261186A patent/JP2010065376A/ja active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4868031A (en) * | 1987-06-22 | 1989-09-19 | Hercules Incorporated | Soft water-permeable polyolefins nonwovens having opaque characteristics |
EP0364979A2 (fr) * | 1988-10-21 | 1990-04-25 | Hercules Incorporated | Non tissés en polyoléfines, doux, imperméables et présentant des caractéristiques d'opacité |
WO2000015891A1 (fr) * | 1998-09-14 | 2000-03-23 | Cerex Advanced Fabrics, L.P. | Non-tisses |
WO2000048478A1 (fr) * | 1999-02-17 | 2000-08-24 | Filtrona Richmond, Inc. | Procede et appareil permettant de filer une bande de fibres melangees et les produits ainsi obtenus |
Non-Patent Citations (1)
Title |
---|
See also references of WO03016606A1 * |
Also Published As
Publication number | Publication date |
---|---|
JP2010065376A (ja) | 2010-03-25 |
JP4430932B2 (ja) | 2010-03-10 |
JP2004538388A (ja) | 2004-12-24 |
WO2003016606A1 (fr) | 2003-02-27 |
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