EP1038059B1 - Fil comprenant un materiau de liaison active par la chaleur et procede de production de ce fil - Google Patents

Fil comprenant un materiau de liaison active par la chaleur et procede de production de ce fil Download PDF

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Publication number
EP1038059B1
EP1038059B1 EP98948411A EP98948411A EP1038059B1 EP 1038059 B1 EP1038059 B1 EP 1038059B1 EP 98948411 A EP98948411 A EP 98948411A EP 98948411 A EP98948411 A EP 98948411A EP 1038059 B1 EP1038059 B1 EP 1038059B1
Authority
EP
European Patent Office
Prior art keywords
yarn
fiber
binder material
binder
bundle
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.)
Expired - Lifetime
Application number
EP98948411A
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German (de)
English (en)
Other versions
EP1038059B2 (fr
EP1038059A1 (fr
Inventor
Charles Edward Bowers
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.)
Honeywell International Inc
Original Assignee
AlliedSignal Inc
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Filing date
Publication date
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Priority claimed from US08/933,822 external-priority patent/US6682618B1/en
Application filed by AlliedSignal Inc filed Critical AlliedSignal Inc
Publication of EP1038059A1 publication Critical patent/EP1038059A1/fr
Application granted granted Critical
Publication of EP1038059B1 publication Critical patent/EP1038059B1/fr
Publication of EP1038059B2 publication Critical patent/EP1038059B2/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
    • D02G3/40—Yarns in which fibres are united by adhesives; Impregnated yarns or threads
    • D02G3/402—Yarns in which fibres are united by adhesives; Impregnated yarns or threads the adhesive being one component of the yarn, i.e. thermoplastic yarn
    • D—TEXTILES; PAPER
    • D05—SEWING; EMBROIDERING; TUFTING
    • D05C—EMBROIDERING; TUFTING
    • D05C17/00—Embroidered or tufted products; Base fabrics specially adapted for embroidered work; Inserts for producing surface irregularities in embroidered products
    • D05C17/02—Tufted products
    • D05C17/026—Tufted products characterised by the tufted pile surface

Definitions

  • the invention relates to yarn suitable for tufting, especially to form carpet face fiber, and other applications.
  • the yarn comprises a blend of fibers including a first, preferably synthetic, base fiber, ring spun or wrap spun with a second fiber that at least partially comprises a heat-activated adhesive material having a melting point substantially below that of the base fiber.
  • U.S. Patent 3,494,819 to McAlister discloses a blend of fusible and non-fusible polyethylene terephthalate fibers incorporated into fabric, wherein the finished fabric is heated to fusion temperatures to provide improved pill resistance.
  • U.S. Patent 3,978,267 to Selwood, issued August 31, 1976 discloses a substantially twistless compact yarn comprising a proportion of potentially adhesive fiber which has been activated to bond contacting fibers.
  • Cut-pile carpet is customarily produced from staple yarns or bulked continuous filament yarns.
  • staple fiber is conventionally carded, pinned, and spun or wrap spun into a singles yarn, which typically is twisted and plied with similar yarn to form a 2-ply or 3-ply yarn construction.
  • This yarn is twist set by utilizing one of several commercially available twist setting processes such as the Suessen or Superba processes.
  • the yarn is passed through a heated chamber, while in a relaxed condition.
  • the temperature of this process step is crucial to the proper twist setting of the base fiber, to obtain desired properties of the final carpet product.
  • the conditions for this step are typically 190-200°C with a residence time of about 60 seconds for the Suessen process and about 125-140°C with a residence time of about 60 seconds for the Superba process.
  • the Superba process utilizes saturated steam and thus the yarn is subjected to a much higher level of humidity than in the Suessen process.
  • bulked continuous filament yarn is produced according to various conventional methods. Twisting, entangling, or direct cabling may be utilized in various processes. For example, a 2-ply twisted yarn combining 2 ends of 1185 denier 70 filament nylon-6 yarn is prepared and subjected to conventional twist setting conditions, such as that for the staple yarn above, or in an autoclave at 132°C in saturated steam with a residence time of about 40 to 60 minutes.
  • twist set yarns Multiple ends of the twist set yarns are tufted into cut pile carpet and conventionally finished to obtain the desired carpet product.
  • WO-A-94/09196 discloses a synthetic yarn made from a blend of base fibers selected from polyester, nylon 6 and nylon 6,6 and 1 to 12 weight % of a heat-activated binder fiber having a melting point within the range of 165°C to 190°C.
  • the blended fiber may be processed in conventional ways, including spinning.
  • WO-A-94/20657 discloses ply-twisted yarns comprising blends of 70 to 90 weight % base fiber which is preferably nylon 6,6 or nylon 6, and 10 to 30 weight % of a non-melt compatible polyolefin fiber having a melting point of 130°C to 170°C.
  • yarn preferably synthetic, comprises at least one bundle of fiber, the fiber bundle being ring spun or wrap spun with a second fiber (either an insert fiber in the case of ring spun or a wrapping fiber in the case of wrap spun) comprising a heat-activated binder material, preferably a fiber, having a melting point range of about 105 to 190°C, preferably 165 to 190°C, under ambient humidity conditions, such that the yarn comprises a total of 0.1 to 12, preferably 0.25 to 10, more preferably 0.5 to 8, weight percent binder material.
  • the preferred fiber bundle comprise staple fibers, preferably in the form of a sliver. Alternatively the bundle of fibers may be continuous filaments.
  • the preferred second, binder fiber is a copolyamide, more preferably a copolyamide of the nylon 6/nylon 6,6 type.
  • the preferred bundle of fiber is nylon 6.
  • the present invention is also an article, preferably tufted, more preferably a carpet, made from this yarn.
  • the present invention is also a process of producing a yarn suitable for tufting, the process comprising the steps of:
  • the insert fiber is inserted before the front delivery roll into a continuous bundle of base fibers, preferably staple fibers in a sliver.
  • This invention also relates to yarn made in accordance with the aforesaid process,
  • the yarn When the yarn is twisted, plied and twist set by conventional processes, for example 190-200°C Suessen twistsetting with a residence time of about 60 seconds, and the treated yarn tufted into cut-pile carpet, the resulting carpet displays enhanced carpet tuft appearance, improved resilience, and reduced change of appearance with use.
  • conventional processes for example 190-200°C Suessen twistsetting with a residence time of about 60 seconds
  • the base fiber is selected from known synthetic fibers suitable for carpet use; such as, polyamides, nylon-6 and nylon-6,6, polyesters, and polyolefins, as well as material fibers, such as cotton and wool.
  • the binder fiber is selected to provide good adhesion to the base fiber. It is important that the melting point of the binder fiber be in the range of 105-190°C, preferably 165-190°C, under ambient humidity conditions. This range ensures that the binder fiber will melt during the conventional twist setting process yet will provide adequate adhesive properties during any subsequent dyeing steps and final use. A saturated steam environment, such as in an autoclave, reduces the fiber melting point of polyamide binder fibers dramatically.
  • a preferred class of binder fiber for use with polyamide base fibers are copolyamides within the specified melting point ranges. Suitable copolyamides of the 6/66/12 type and a process for their production are disclosed in U.K. Patent 1,168,404, issued October 22,1969 to Inventa A. G.
  • a melt bonding copolyamide adhesive fiber is commercially available from EMS as GRILON® type K 140 (melting range 130-140°C) and type K 115 (melting range 110-117°C) copolyamides of the 6/66 Type as in U.S. Patent 5,478,624 to Lofquist.
  • thermally activated binder fiber within the weight percent ranges and melting point ranges specified it is possible to modify end-use properties of the finished carpet to improve wear resistance, resilience, reduced change of appearance over time and with use, and to increase hand, lustre and apparent value.
  • Denier per filament, cut length, fiber cross-section, crimp type and frequency, surface finish, melt viscosity, softening point, melting point, dye affinity, and other properties are crucial to achieving ideal properties in the final product.
  • a proper selection of the binder fiber must be made to obtain the desired, or optimum results from the finished carpet product. This will depend on numerous factors including the denier, length, crimp, finish, and other properties of the base fiber product.
  • twist setting conditions normally used are sufficient to activate the binder fiber, to create bind points which strengthen the final product, thereby imparting other characteristics which are desirable.
  • the twisted yarn is subjected to a temperature of 190-205°C for a residence time of 50-60 seconds.
  • motion of the fiber while in the relaxed state caused by vibration or air currents, sufficiently motivates the molten binder fiber to flow to the intersecting "touch points" of the base fiber, as a function of the melt flow properties of the binder fiber and surface characteristics.
  • the binder solidifies and encapsulates or bonds two or more base fibers together at intersecting points in a durable bond.
  • the resultant carpet can be of many forms, but a typical style would be cut-pile carpet with about 1.4 kg/m 2 (40 ounces per square yard) of face yarn including the binder, with an attached backing.
  • Carpet construction would be typically 0.06cm (5/32") gauge, 1.9cm (3/4") pile height, and the carpet would be dyed, dryed, backcoated, and sheared using normal processing techniques.
  • the yarn of the invention would also provide important property improvements in the production of loop-pile carpet.
  • Carpets also may be produced by introducing a binder yarn as the wrapper yarn that is placed uniformly around a continuous bundle of base staple fibers at wrap (hollow spindle) spinning to produce a wrap spun yarn.
  • the binder yarn can consist of 100% heat-activated adhesive fibers or consist of a blend of heat activated adhesive fibers and non-adhesive fibers. Binder yarns as such can be either continuous filament yarn or spun staple yarn produced by conventional manufacturing methods.
  • the carpet When the resulting wrap spun yarn is twisted into a plied yarn, twist set by conventional process, and the treated yarn tufted into cut-pile carpet, the carpet displays enhanced carpet tuft appearance, more resilience, and better wear resistance than similar carpets not containing the binder yarn.
  • These carpet improvements can be further enhanced by the continuous bundle of base staple fibers being a blend with a low weight percent of heat activated adhesive fibers and a high weight percent of non-adhesive fibers that is wrapped with a binder yarn as described above.
  • the continuous bundle (sliver) of base staple fibers is 100% 1.9 tex (17 denier) per filament AlliedSignal T317 nylon-6 staple fibers that is wrapped with a 3.3 tex (30 denier) 12 filament yarn at wrap spinning to produce a 5.4/1 mm/kg (3.35/1) cotton count yarn containing 2"Z" wraps per cm (5.2 "Z" wraps per inch).
  • This singles yarn is then plied with another singles end of the same yarn to produce 5.4/2 mm/kg (3.35/2 cotton count) 2 Z wraps per cm x 2.1 s twists cm (5.2 Z wraps per inch x 5.4 S twists per inch) final yarn.
  • This final yarn contains a binder yarn, which is the 3.3 tex (30 denier) 12 filament yarn wrapped around each end of the 2 plies.
  • This 3.3 tex (30 denier) yarn is a copolyamide nylon having a melt point range of 105-180°C.
  • the remainder of the 5.4/2 mm/kg (3.35/2 cotton count) yarn is AlliedSignal T317 nylon-6 staple fibers having a melt point range of 215-225°C, which results in a blend of about 2.0 percent binder.
  • This ratio can be increased by using a larger denier binder yarn, or by a low weight percent of heat-activated adhesive fibers and a high weight percent of non-adhesive AlliedSignal T317 nylon-6 staple fibers blend being in the continuous bundle (sliver) of base staple fibers, before wrap spinning, that is wrapped with the 3.3 tex (30 denier) 12 filament binder yarn.
  • This final 5.4/2 mm/kg (3.35/2 cotton count) yarn was twist set by a conventional stuffer box Suessen twist setting process.
  • the yarn was passed through a heated chamber at 190°C, while in a relaxed condition, with a residence time of 60 seconds. Multiple ends of this yarn were tufted into cut-pile carpet and conventionally finished to obtain the improved product.
  • the resulting carpet was compared to a control carpet prepared in the same manner from 100 percent non-adhesive AlliedSignal T317 nylon-6 base staple fibers.
  • the carpet containing the 2.0 percent wrapper yarn binder displayed tighter and more defined individual pile tufts, a more resilient, stiffer hand, enhanced carpet surface appearance with significantly less hairiness, and better wear resistance.
  • Carpets also may be produced by introducing a binder yarn at ring spinning before the front delivery roll into a continuous bundle of base staple fibers being drafted to produce a ring spun yarn.
  • the binder yarn can consist of 100% heat-activated adhesive fibers or consist of a blend of heat-activated adhesive fibers and non-adhesive fibers.
  • Binder yarns as such can be either continuous filament yarn or spun staple yarn produced by conventional manufacturing methods. This ring spun yarn has greater strength due to the added strength of the inserted yarn in the total spun yarn structure, which results in improved operating performance at spinning by reducing single end breakouts.
  • the resulting ring spun yarn when later twisted into a plied yarn and twist set by conventional processes results in a treated yarn with altered, unique performance properties.
  • the unique properties are produced by the heat activated adhesive fibers in the inserted binder yarn being intermingled within the continuous bundle (sliver) of non-adhesive base staple fibers during the ring spinning process, melting during conventional twist setting processes, and then solidifying when emerging from the elevated temperature forming a durable crossbonding with the non-adhesive base staple fibers within the individual ends of the plied yarn and between the individual ends of the plied yarn.
  • the treated plied twist set yarn has a more resilient, stiffer hand, significantly improved ply twist retention, and a less hairy surface.
  • the hand of the pile is significantly firmer, the individual tufts are tighter and more defined, and the pile surface is cleaner with less hairiness.
  • These carpet improvements can be further enhanced by the continuous bundle of base staple fibers being a blend with a low weight percent of heat-activated adhesive fibers and a high weight percent of non-adhesive fibers in which the binder yarn is inserted as described above.
  • a 3.3 tex (30 denier) 12 filament yarn is inserted before the front delivery roll into the continuous bundle of base staple fibers (sliver) being drafted at ring spinning.
  • the sliver is 100% 1.9 tex (17 denier) per filament AlliedSignal T317 nylon-6 staple fibers, which is spun into a (3.0/1 cotton count) yarn containing 1.9 "z" twists per cm (4.8 "Z” twists per inch).
  • This singles yarn is then plied with another singles end of the same yarn to produce 5.2/2 mm/kg (3.0/2 cotton count )1.9 Z twists per cm x 1.6 twists per cm (4.8 Z twists per inch x 4.1 S twists per inch) final yarn.
  • This final yarn contains a binder yarn, which is the 3.3 tex (30 denier) 12 filament yarn inserted in each end of the 2 plies.
  • This 3.3 tex (30 denier yarn) is a copolyamide nylon having a melt point range of 105-180°C.
  • the remainder of the 5.2/2 mm/kg (3.0/2 cotton count) yarn is AlliedSignal T317 nylon-6 staple fibers having a melt point range of 215-225°C, which results in a blend of about 1.7 percent binder.
  • This ratio can be increased by inserting a larger denier binder yarn at the front delivery roll, or by a low weight percent of heat activated adhesive fibers and a high weight percent of non-adhesive AlliedSignal T317 nylon-6 staple fibers blend being in the continuous bundle (sliver) of base staple fibers, before ring spinning, in which the 3.3 tex (30 denier) 12 filament binder yarn is inserted at the front delivery roll of ring spinning.
  • This final 5.2/2 mm/kg (3.0/2 cotton count) yarn was twist set by a conventional Suessen twist setting process.
  • the yarn was passed through a heated chamber at 190°C, while in a relaxed condition, with a residence time of 60 seconds. Multiple ends of this yarn were tufted into cut-pile carpet and conventionally finished to obtain the improved product.
  • the resulting carpet was compared to a control carpet prepared in the same manner from 100 percent non-adhesive AlliedSignal T317 nylon-6 base staple fibers.
  • the carpet containing the 1.7 percent inserted binder yarn displayed more defined individual pile tufts, a more resilient, stiffer hand, and a cleaner, enhanced carpet surface appearance which is more like a BCF cut pile carpet.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Carpets (AREA)

Claims (8)

  1. Fil comprenant :
    a. au moins un faisceau de fibres, et
    b. une seconde fibre comprenant une matière liante activée par la chaleur ayant un intervalle de point de fusion d'environ 105°C à 190°C dans des conditions d'humidité ambiante, ledit fil comprenant un total de 0,1 à 12% en poids de matière liante, caractérisé en ce que ledit faisceau est filé en continu avec un anneau ou filé avec enveloppement par ladite seconde fibre.
  2. Fil selon la revendication 1 comprenant 0,25 à 10% en poids de matière liante et de préférence 0,5 à 8% en poids de matière liante.
  3. Fil selon la revendication 1 ou la revendication 2 dans lequel le faisceau de fibres est sélectionné parmi le groupe constitué de fibres discontinues ; un ruban ; et des filaments continus.
  4. Fil selon l'une quelconque des revendications précédentes dans lequel la seconde fibre comprend une fibre de liaison activée par la chaleur.
  5. Fil selon la revendication 4 dans lequel ladite fibre de liaison est sélectionnée parmi le groupe constitué de Nylon 6 et d'un copolyamide du type Nylon 6/Nylon 6,6.
  6. Fil selon la revendication 1 dans lequel le faisceau de fibres comprend des fibres discontinues filées avec enveloppement par une fibre d'enveloppement et la fibre d'enveloppement forme essentiellement toute la matière liante activée par la chaleur.
  7. Procédé de production d'un fil adéquat pour le tuftage, ledit procédé comprenant les étapes de :
    a. formation d'un faisceau de fibres ;
    b. filage continu avec un anneau ou filage avec enveloppement du faisceau de fibres avec une seconde fibre comprenant une matière liante activée par la chaleur ayant un intervalle de point de fusion d'environ 105°C à 190°C dans des conditions d'humidité ambiante, pour former un fil comprenant 0,1 à 12% en poids de matière liante ;
    c. chauffage du fil suffisamment pour faire fondre la matière liante, et enfin
    d. refroidissement du fil pour solidifier la matière liante.
  8. Procédé selon la revendication 7, dans lequel le faisceau de fibres est formé par filage de fibres discontinues.
EP98948411A 1997-09-19 1998-09-18 Fil comprenant un materiau de liaison active par la chaleur et procede de production de ce fil Expired - Lifetime EP1038059B2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US933822 1997-09-18
US08/933,822 US6682618B1 (en) 1986-11-24 1997-09-19 Yarn with heat-activated binder material and process of making
PCT/US1998/019745 WO1999014408A1 (fr) 1997-09-18 1998-09-18 Fil comprenant un materiau de liaison active par la chaleur et procede de production de ce fil

Publications (3)

Publication Number Publication Date
EP1038059A1 EP1038059A1 (fr) 2000-09-27
EP1038059B1 true EP1038059B1 (fr) 2003-07-30
EP1038059B2 EP1038059B2 (fr) 2008-01-02

Family

ID=25464560

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98948411A Expired - Lifetime EP1038059B2 (fr) 1997-09-19 1998-09-18 Fil comprenant un materiau de liaison active par la chaleur et procede de production de ce fil

Country Status (5)

Country Link
EP (1) EP1038059B2 (fr)
AU (1) AU741990B2 (fr)
DE (1) DE69816860T3 (fr)
WO (1) WO1999014408A1 (fr)
ZA (1) ZA988628B (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6682618B1 (en) 1986-11-24 2004-01-27 Alliedsignal Inc. Yarn with heat-activated binder material and process of making
US6969437B1 (en) 1997-01-30 2005-11-29 Alliedsignal Inc. Yarn with heat-activated binder material and process of making
WO2000012796A1 (fr) * 1998-08-31 2000-03-09 Alliedsignal Inc. Fil comprenant un materiau de liaison active par la chaleur et procede de production de ce fil
US6658835B1 (en) * 2000-11-28 2003-12-09 Honeywell International Inc. Untwisted wrapped singles yarns and carpets manufactured therefrom
US6755366B2 (en) 2002-09-30 2004-06-29 Solutia Inc. Device for direct insertion of yarn in automatic winder
US20040175534A1 (en) * 2002-12-23 2004-09-09 Bridges James C. Enhanced surface coverings, yarns and methods

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2252999A (en) * 1937-05-24 1941-08-19 Sylvania Ind Corp Article and process for the manufacture thereof
CH220994A (fr) * 1937-05-24 1942-05-15 Sylvania Ind Corp Procédé de fabrication d'un produit textile.
GB568675A (en) * 1943-03-12 1945-04-16 George Frederick Rayner Process of making composite yarns, and the composite yarns so produced
DD240918A1 (de) * 1985-09-16 1986-11-19 Ver Baumwollspinnereien Und Zw Verfahren und vorrichtung zum verfestigen von faserbaendchen
US4644741A (en) * 1984-06-11 1987-02-24 Golden Star, Inc. Mop yarns made by fiber bonding process
US4668552A (en) * 1986-07-28 1987-05-26 Collins & Aikman Corporation Wrap yarns having low-melt binder strands and pile fabrics formed therefrom and attendant processes
WO1988003969A1 (fr) * 1986-11-24 1988-06-02 Allied Corporation Fil synthetique avec fibre de liaison thermoactivee

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NZ220444A (en) * 1987-05-26 1991-06-25 Wool Res Organisation Yarn pile fabrics with fusible fibre bonding agent
US5032333A (en) * 1990-02-27 1991-07-16 E. I. Du Pont De Nemours And Company One-line interlacing of bulked continuous filament yarns and low-melting binder fibers
FR2664621B1 (fr) * 1990-07-13 1994-08-26 Schappe Sa Fil hybride pour materiaux composites a matrice thermoplastique et procede pour son obtention.
DE69304929T2 (de) * 1992-10-14 1997-01-30 Allied Signal Inc Sythethetisches, durch wärme aktivierbare fasern gebundenes garn
US5284009A (en) * 1993-03-09 1994-02-08 E. I. Du Pont De Nemours And Company Fiber blends for improved carpet texture retention
EP0760875B1 (fr) * 1994-04-29 2004-06-23 Kleentex Industries, Inc. Paillasson ameliore et procede de fabrication
JPH09119034A (ja) * 1995-10-26 1997-05-06 Unitika Ltd バインダー繊維含有紡績糸

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2252999A (en) * 1937-05-24 1941-08-19 Sylvania Ind Corp Article and process for the manufacture thereof
CH220994A (fr) * 1937-05-24 1942-05-15 Sylvania Ind Corp Procédé de fabrication d'un produit textile.
GB568675A (en) * 1943-03-12 1945-04-16 George Frederick Rayner Process of making composite yarns, and the composite yarns so produced
US4644741A (en) * 1984-06-11 1987-02-24 Golden Star, Inc. Mop yarns made by fiber bonding process
DD240918A1 (de) * 1985-09-16 1986-11-19 Ver Baumwollspinnereien Und Zw Verfahren und vorrichtung zum verfestigen von faserbaendchen
US4668552A (en) * 1986-07-28 1987-05-26 Collins & Aikman Corporation Wrap yarns having low-melt binder strands and pile fabrics formed therefrom and attendant processes
WO1988003969A1 (fr) * 1986-11-24 1988-06-02 Allied Corporation Fil synthetique avec fibre de liaison thermoactivee

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Encyclopedia of polymer science and technology Vol. 13, p.692-699 (John Wiley & Sons, Inc. 1970) *

Also Published As

Publication number Publication date
DE69816860D1 (de) 2003-09-04
EP1038059B2 (fr) 2008-01-02
AU741990B2 (en) 2001-12-13
WO1999014408A1 (fr) 1999-03-25
EP1038059A1 (fr) 2000-09-27
DE69816860T3 (de) 2008-06-26
ZA988628B (en) 1999-06-29
AU9498898A (en) 1999-04-05
DE69816860T2 (de) 2004-06-03

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