WO1998012448A1 - Friction material, method of preparing same and friction lining - Google Patents

Friction material, method of preparing same and friction lining Download PDF

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Publication number
WO1998012448A1
WO1998012448A1 PCT/DK1997/000391 DK9700391W WO9812448A1 WO 1998012448 A1 WO1998012448 A1 WO 1998012448A1 DK 9700391 W DK9700391 W DK 9700391W WO 9812448 A1 WO9812448 A1 WO 9812448A1
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WO
WIPO (PCT)
Prior art keywords
iron
particles
friction material
vol
graphite particles
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.)
Ceased
Application number
PCT/DK1997/000391
Other languages
French (fr)
Inventor
Ole Kraemer
Niels BRAMSØ
Erik Simonsen
Noel De Leon
Knud Strande
Rolf TÖRNBERG
Claes Kuylenstierna
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.)
Roulunds Fabriker AS
Volvo Truck Corp
Original Assignee
Roulunds Fabriker AS
Volvo Truck Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Roulunds Fabriker AS, Volvo Truck Corp filed Critical Roulunds Fabriker AS
Priority to US09/254,653 priority Critical patent/US6143051A/en
Priority to AT97939988T priority patent/ATE230830T1/en
Priority to CA002265718A priority patent/CA2265718C/en
Priority to BR9712054-5A priority patent/BR9712054A/en
Priority to EP97939988A priority patent/EP0944782B1/en
Priority to AU42006/97A priority patent/AU4200697A/en
Priority to DK97939988T priority patent/DK0944782T3/en
Priority to JP10514198A priority patent/JP2001501650A/en
Priority to DE69718346T priority patent/DE69718346T2/en
Publication of WO1998012448A1 publication Critical patent/WO1998012448A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02—Composition of linings ; Methods of manufacturing
    • F16D69/027—Compositions based on metals or inorganic oxides
    • F16D69/028—Compositions based on metals or inorganic oxides containing fibres

Definitions

  • Friction material method of preparing same and friction lining
  • the present invention relates to a friction material and in particular a brake lining material comprising a sintered mass of iron in which graphite particles are dispersed.
  • a number of commercially available brake lining materials comprise particles, such as iron particles and graphite particles, bonded together by an organic binder, such as a phenol-formaldehyde resin.
  • brake linings consisting of such a material are exposed to severe energy loads and consequently high temperatures, such as temperatures of the order of 700 °c, which e.g. arise when they are used in brakes for trucks, a decomposition of the organic binder occurs under formation of gaseous decomposition products.
  • high temperatures such as temperatures of the order of 700 °c, which e.g. arise when they are used in brakes for trucks, a decomposition of the organic binder occurs under formation of gaseous decomposition products.
  • the useful life of the brake linings is reduced.
  • Metal bonded brake lining materials are also known, viz. materials comprising a sintered iron matrix containing comparatively small amounts of dispersed graphite particles. These known metal bonded lining materials suffer from the disadvantage that at severe energy loads melting may occur of parts of the iron matrix, whereby an incipient welding together of the brake pads and the brake drum or the brake disc occurs.
  • EP 0 093 673 discloses a friction material comprising a ma or amount (72-85 weight-..) of iron powder, graphite (3-14 weight-?,), coke (2-12 weight-'), low melting material (3-10 weight-?), such as tin, and a friction modifying agent (up to 3 weight-' ) , some of the iron powder being optionally replaced with ron fibres.
  • the friction material according to the invention is characterized in that the sintered mass is formed from between 13 and 22 vol.-' of iron fibres, between 13 and 22 vol.-?, of iron particles having a particle size of 10- 400 ⁇ m, between 40 and 70 vol.- of graphite particles having a particle size of 25-3000 ⁇ m, and between 10 and 15 vol.-. of a metallic binder having a melting point of 800-1140 °C.
  • the invention is based on the discovery that by using comparatively large graphite particles, the graphite particles normally used in metallurgical processes typically have a particle size of 0.1-10 ⁇ m, and a metallic binder having a melting point within the temperature range m which the sintering takes place, a strong and stable iron framework is formed in which the graphite particles are embedded, and from where they can be released under the influence of friction and form a film between brake pad and brake drum or brake disc.
  • the iron fibres, the iron particles and the metallic binder are thus the sintering active and consequently strength imparting components, while the graphite particles are the friction controlling components of the sintering mass.
  • the iron fibres present in the friction material are preferably steel fibres, i.e. fibres of an iron alloy having a carbon content of up to 2%.
  • the iron fibres preferably have a length between 0.5 and 5 mm and a thickness within the range 10-100 ⁇ m.
  • the iron particles have a particle size from 10 to 400 ⁇ m, and preferably a particle size from 20 to 200 ⁇ m.
  • the graphite particles have a particle size from 25 to 3000 ⁇ m, and preferably a particle size from 90 to 1000 ⁇ m.
  • metallic binder preferably a metallic material selected from Cu, Sn and Zn is used.
  • the friction material according to the invention may in addition to the components mentioned above contain from 0.1 to 15 vol.-% of additional components, such as A1 2 0-., FeSi, Fe 3 Si ? , FeSi 2 , Fe 2 Si ⁇ , MgCO-., Si0 2 , BN, Caj(PO . ) 2 ,
  • BaS0 4 Fe 2 0 3 , CuAl 2 , Si, Al, Cu, P, and sulphides of Mo, Mn, Sb, Cu, Sn and .
  • Admixing of a ceramic material into the sintered mass causes a stabilization of the friction at fluctuating temperatures.
  • a particularly good stabilization is obtained by using a ceramic material having two different grain sizes.
  • a particularly preferred additive is Al 2 0 ( , which serves to increase the function coefficient and keep the friction coefficient constant.
  • the present invention further relates to a method of preparing a friction material, which method is characterized m that a mixture of 13-22 vol.-? of iron fibres, 13-22 vol.- 0 , of iron particles having a particle size between 10 and 400 ⁇ m, 40-70 vol.-' of graphite particles having a particle size between 25 and 3000 ⁇ m, and 10-15 vol.-? of metallic binder is compressed at a pressure of at least 100 MPa so as to form a compact having a desired form and size, and that the compact formed is sintered at a temperature between 800 and
  • iron fibres, iron particles and metallic binder can be mixed prior to these components being mixed with the graphite particles.
  • Al-O When Al-O, is to form part of the mixture of starting materials, it is preferred to disperse Al-O. m water and to mix the dispersion thus formed with the graphite particles, and to remove the water from the mixture prior to it being mixed with the other components.
  • the mixture of graphite particles and Al 0. may expediently be added with a minor amount, e.g. 1-3 weight-?, of an oil, such as a vegetable oil, prior to the mixing with the other components.
  • an oil such as a vegetable oil
  • A1 2 0 3 particles were added to 100 cm 3 of water, and the mixture thus formed was subjected to an ultrasonic treatment so as to form a homogeneous dispersion.
  • the dispersion was mixed with 40 cm 3 of graphite particles having an average particle size of 300 ⁇ m, following which the water was removed by evaporation in an oven.
  • the mixture of graphite and Al 2 0 3 particles thus obtained was added with 2 weight-% of vegetable oil, and the composition was mixed until an even distribution of the A1 2 0. particles on the graphite particles had been obtained.
  • the mixture of graphite particles, Al ? Oj particles and vegetable oil, and the mixture of iron fibres, iron particles and bronze powder were mixed in a V-mixer, internal rotor not being used for the first 5 min, and internal rotor being used for the succeeding 2 min.
  • the mixture thus obtained was pressed into briquettes having the dimensions 4 x 9 x 2 in a single-axis press and at a pressure of 300 MPa.
  • the green compacts obtained were then sintered in an oven in an atmosphere of H 2 and N 2 .
  • the compacts were first sintered at 700 °C for 0.5 h, and then at 1100 °C for 0.75 h. Finally, the sintered compacts were cooled to room temperature in an atmosphere of H 2 and N.. for a period of time of 0.75 h.
  • the sintered compacts thus obtained were mounted on a steel plate, and the product thus obtained could hereafter be used for brake lining.

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  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Braking Arrangements (AREA)
  • Powder Metallurgy (AREA)

Abstract

A friction material comprising a sintered mass of iron in which graphite particles are dispersed, which sintered mass is formed from between 13 and 22 vol.% of iron fibres, between 13 and 22 vol.% of iron particles having a particle size of 10-400 νm, between 40 and 70 vol.% of graphite particles having a particle size of 25-3000 νm, and between 10 and 15 vol.% of a metallic binder having a melting point of 800-1140 °C, and a method of preparing such a friction material, wherein a mixture of these components is compressed at a pressure of at least 100 MPa so as to form a compact having a desired form and size, and where the compact thus formed is sintered at a temperature between 800 and 1140 °C for a period of time which is sufficiently long for achieving concretion of iron fibres, iron particles and metallic binder.

Description

Friction material, method of preparing same and friction lining
The present invention relates to a friction material and in particular a brake lining material comprising a sintered mass of iron in which graphite particles are dispersed.
A number of commercially available brake lining materials comprise particles, such as iron particles and graphite particles, bonded together by an organic binder, such as a phenol-formaldehyde resin.
If brake linings consisting of such a material are exposed to severe energy loads and consequently high temperatures, such as temperatures of the order of 700 °c, which e.g. arise when they are used in brakes for trucks, a decomposition of the organic binder occurs under formation of gaseous decomposition products. Hereby the useful life of the brake linings is reduced.
Metal bonded brake lining materials are also known, viz. materials comprising a sintered iron matrix containing comparatively small amounts of dispersed graphite particles. These known metal bonded lining materials suffer from the disadvantage that at severe energy loads melting may occur of parts of the iron matrix, whereby an incipient welding together of the brake pads and the brake drum or the brake disc occurs.
It is known to use brake linings which essentially consist of graphite in brakes for Formel I racers. Such brakes are very efficient, but they are worn down very rapidly and normally only last one race. It has been attempted to prepare metal bonded brake lining materials having a large content of graphite particles, but these attempts have run up against the difficulty that increasing content of graphite particles m the iron matrix entails decreasing strength and consequently reduced wear resistance.
EP 0 093 673 discloses a friction material comprising a ma or amount (72-85 weight-..) of iron powder, graphite (3-14 weight-?,), coke (2-12 weight-'), low melting material (3-10 weight-?), such as tin, and a friction modifying agent (up to 3 weight-' ) , some of the iron powder being optionally replaced with ron fibres.
It is the object of the present invention to provide a friction material having higher wear resistance than the friction material according to EP 0 093 673.
The friction material according to the invention is characterized in that the sintered mass is formed from between 13 and 22 vol.-' of iron fibres, between 13 and 22 vol.-?, of iron particles having a particle size of 10- 400 μm, between 40 and 70 vol.- of graphite particles having a particle size of 25-3000 μm, and between 10 and 15 vol.-. of a metallic binder having a melting point of 800-1140 °C.
The invention is based on the discovery that by using comparatively large graphite particles, the graphite particles normally used in metallurgical processes typically have a particle size of 0.1-10 μm, and a metallic binder having a melting point within the temperature range m which the sintering takes place, a strong and stable iron framework is formed in which the graphite particles are embedded, and from where they can be released under the influence of friction and form a film between brake pad and brake drum or brake disc. The iron fibres, the iron particles and the metallic binder are thus the sintering active and consequently strength imparting components, while the graphite particles are the friction controlling components of the sintering mass.
The iron fibres present in the friction material are preferably steel fibres, i.e. fibres of an iron alloy having a carbon content of up to 2%. The iron fibres preferably have a length between 0.5 and 5 mm and a thickness within the range 10-100 μm.
As mentioned, the iron particles have a particle size from 10 to 400 μm, and preferably a particle size from 20 to 200 μm.
As mentioned, the graphite particles have a particle size from 25 to 3000 μm, and preferably a particle size from 90 to 1000 μm.
As metallic binder, preferably a metallic material selected from Cu, Sn and Zn is used.
Bronze in powder form and of a type in which the content of copper is from 85 to 99 %, and the content of tin is from 1 to 15 %, is particularly useful.
The friction material according to the invention may in addition to the components mentioned above contain from 0.1 to 15 vol.-% of additional components, such as A120-., FeSi, Fe3Si?, FeSi2, Fe2Si^, MgCO-., Si02, BN, Caj(PO.)2,
BaS04, Fe203, CuAl2, Si, Al, Cu, P, and sulphides of Mo, Mn, Sb, Cu, Sn and .
Admixing of a ceramic material into the sintered mass causes a stabilization of the friction at fluctuating temperatures. A particularly good stabilization is obtained by using a ceramic material having two different grain sizes.
A particularly preferred additive is Al20(, which serves to increase the function coefficient and keep the friction coefficient constant.
The present invention further relates to a method of preparing a friction material, which method is characterized m that a mixture of 13-22 vol.-? of iron fibres, 13-22 vol.-0, of iron particles having a particle size between 10 and 400 μm, 40-70 vol.-' of graphite particles having a particle size between 25 and 3000 μm, and 10-15 vol.-? of metallic binder is compressed at a pressure of at least 100 MPa so as to form a compact having a desired form and size, and that the compact formed is sintered at a temperature between 800 and
1140 °C for a sufficiently long period of time to achieve concretion of iron fibres, iron particles and metallic binder .
Optionally, iron fibres, iron particles and metallic binder can be mixed prior to these components being mixed with the graphite particles.
When Al-O, is to form part of the mixture of starting materials, it is preferred to disperse Al-O. m water and to mix the dispersion thus formed with the graphite particles, and to remove the water from the mixture prior to it being mixed with the other components.
The mixture of graphite particles and Al 0. may expediently be added with a minor amount, e.g. 1-3 weight-?, of an oil, such as a vegetable oil, prior to the mixing with the other components. In the following the invention is described in more detail with reference to the example below.
EXAMPLE
22 cm3 of iron fibres, 22 cm3 of iron particles having an average particle size of 100 μm, and 15 cm3 of bronze powder having a melting point of 1040 °C were mixed in a V-mixer with internal rotor for about 10 min.
1 cm3 of A1203 particles were added to 100 cm3 of water, and the mixture thus formed was subjected to an ultrasonic treatment so as to form a homogeneous dispersion. The dispersion was mixed with 40 cm3 of graphite particles having an average particle size of 300 μm, following which the water was removed by evaporation in an oven.
The mixture of graphite and Al203 particles thus obtained was added with 2 weight-% of vegetable oil, and the composition was mixed until an even distribution of the A120. particles on the graphite particles had been obtained. The mixture of graphite particles, Al?Oj particles and vegetable oil, and the mixture of iron fibres, iron particles and bronze powder were mixed in a V-mixer, internal rotor not being used for the first 5 min, and internal rotor being used for the succeeding 2 min.
The mixture thus obtained was pressed into briquettes having the dimensions 4 x 9 x 2 in a single-axis press and at a pressure of 300 MPa.
The green compacts obtained were then sintered in an oven in an atmosphere of H2 and N2. The compacts were first sintered at 700 °C for 0.5 h, and then at 1100 °C for 0.75 h. Finally, the sintered compacts were cooled to room temperature in an atmosphere of H2 and N.. for a period of time of 0.75 h.
The sintered compacts thus obtained were mounted on a steel plate, and the product thus obtained could hereafter be used for brake lining.

Claims

C l a i m s
1. A friction material comprising a sintered mass of iron in which graphite particles are dispersed, c h a r a c t e r i z e d in that the sintered mass is formed from between 13 and 22 vol.-% of iron fibres, between 13 and 22 vol.-% of iron particles having a particle size from 10 to 400 μm, between 40 and 70 vol.-% of graphite particles having a particle size from 25 to 3000 μm, and between 10 and 15 vol.-?. of a metallic binder having a melting point from 800 to 1140 °C .
2. A friction material according to claim 1, c h a r ¬ a c t e r i z e d in that the iron fibres are steel fibres .
3. A friction material according to claim 1 or 2, c h a r a c t e r i z e d in that the iron fibres have a length from 0.5 to 5 mm and a thickness from 10 to 100 μm.
4. A friction material according to any of the preceding claims, c h a r a c t e r i z e d in that the iron particles have a particle size from 20 to 200 μm.
5. A friction material according to any of the preceding claims, c h a r a c t e r i z e d in that the graphite particles have a particle size from 90 to 1000 μm.
6. A friction material according to any of the preceding claims, c h a r a c t e r i z e d in that the metallic binder is selected from a group consisting of Cu, Sn and Zn.
7. A friction material according to claim 6, c h a r a c t e r i z e d in that the metallic binder is bronze containing from 85 to 99 ° of copper and from 1 to 15 . of tin.
8. A friction material according to any of the preceding claims, c h a r a c t e r i z e d in that the sintered mass is formed from a mixture which additionally contains from 0.1 to 15 vol.-?, of additional components.
9. A friction material according to claim 8, c h a r a c t e r i z e d in that the additional component (s) is/are selected from a group consisting of Al2Oι, FeSi, Fe.Sι2, FeSi , Fe-Si-., MgCO,, SiO , BN, Ca4(PO„) , BaS0„, Fe2Oj, CuAl , Si, Al, Cu, P, and sulphides of Mo, Mn, Sb, Cu, Sn and W.
10. A friction material according to claim 8, c h a r a c t e r i z e d in that the additional component (s) is/are a ceramic material.
11. A friction material according to claim 10, c h a r - a c t e r i z e d in that the ceramic material is present m the sintered mass m two different grain sizes .
12. A method of preparing a friction material in the form of a sintered mass of iron in which graphite particles are dispersed, c h a r a c t e r i z e d in that a mixture of 13-22 vol.-? of iron fibres, 13-22 vol.-?. of iron particles having a particle size between 10 and 400 μm, 40-70 vol.-?, of graphite particles having a particle size between 25 and 3000 μm, and 10-15 vol.-? of metallic binder is compressed at a pressure of at least 100 MPa so as to form a compact having a desired form and size, and that the compact thus formed is sintered at a temperature between 800 and 1140 °C for a sufficiently long period of time to achieve concretion of iron fibres, iron particles and metallic binder.
13. A method according to claim 12, c h a r a c t e r i z e d m that iron fibres, iron particles and metallic binder are mixed prior to these components being mixed with the graphite particles.
14. A method according to claim 13, c h a r a c t e r i z e d in that the graphite particles are used in mixture with A1203 particles.
15. A method according to claim 14, c h a r a c t e r i z e d in that the mixture of graphite particles and A1203 particles is prepared by dispersing A1203 particles in water, mixing the dispersion thus formed with graphite particles, and removing the water by evaporation.
16. A method according to claim 14, c h a r a c t e r i z e d in that the mixture of graphite particles and A1203 particles additionally contains oil in an amount of 1-3 weight- .
17. A brake lining, c h a r a c t e r i z e d in that it comprises a friction material according to any of the claims 1-11.
PCT/DK1997/000391 1996-09-17 1997-09-17 Friction material, method of preparing same and friction lining Ceased WO1998012448A1 (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US09/254,653 US6143051A (en) 1996-09-17 1997-09-17 Friction material, method of preparing same and friction lining
AT97939988T ATE230830T1 (en) 1996-09-17 1997-09-17 FRICTION MATERIAL, METHOD FOR THE PRODUCTION THEREOF AND FRICTION LINING
CA002265718A CA2265718C (en) 1996-09-17 1997-09-17 Friction material, method of preparing same and friction lining
BR9712054-5A BR9712054A (en) 1996-09-17 1997-09-17 Friction material, preparation process, and brake lining.
EP97939988A EP0944782B1 (en) 1996-09-17 1997-09-17 Friction material, method of preparing same and friction lining
AU42006/97A AU4200697A (en) 1996-09-17 1997-09-17 Friction material, method of preparing same and friction lining
DK97939988T DK0944782T3 (en) 1996-09-17 1997-09-17 Friction material and method for making same and brake lining
JP10514198A JP2001501650A (en) 1996-09-17 1997-09-17 Friction material, method of preparing the friction material and friction lining
DE69718346T DE69718346T2 (en) 1996-09-17 1997-09-17 FRICTION MATERIAL, METHOD FOR THEIR PRODUCTION AND FRICTION COATING

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DK101296A DK101296A (en) 1996-09-17 1996-09-17 Brake lining material and method for making the same as well as brake lining
DK1012/96 1996-09-17

Publications (1)

Publication Number Publication Date
WO1998012448A1 true WO1998012448A1 (en) 1998-03-26

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Application Number Title Priority Date Filing Date
PCT/DK1997/000391 Ceased WO1998012448A1 (en) 1996-09-17 1997-09-17 Friction material, method of preparing same and friction lining

Country Status (12)

Country Link
US (1) US6143051A (en)
EP (1) EP0944782B1 (en)
JP (1) JP2001501650A (en)
AT (1) ATE230830T1 (en)
AU (1) AU4200697A (en)
BR (1) BR9712054A (en)
CA (1) CA2265718C (en)
DE (1) DE69718346T2 (en)
DK (2) DK101296A (en)
ES (1) ES2189973T3 (en)
RU (1) RU2194200C2 (en)
WO (1) WO1998012448A1 (en)

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US6648941B2 (en) * 2001-05-17 2003-11-18 Kawasaki Steel Corporation Iron-based mixed powder for powder metallurgy and iron-based sintered compact
US6863968B2 (en) * 2001-07-30 2005-03-08 Nisshinbo Industries, Inc. Non-asbestos-based friction materials

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US20040146702A1 (en) * 2003-01-29 2004-07-29 Xinming Shao Pure iron fiber based friction material product
US20060151268A1 (en) * 2005-01-12 2006-07-13 Sunil Kesavan Copper-free non-asbestos organic friction material
DE112007001402A5 (en) * 2006-07-21 2009-03-12 Luk Lamellen Und Kupplungsbau Beteiligungs Kg friction system
JP5405725B2 (en) * 2007-06-19 2014-02-05 曙ブレーキ工業株式会社 Sintered friction material
KR101453446B1 (en) 2008-12-24 2014-10-23 재단법인 포항산업과학연구원 Sintered friction material having good stability and manufacturing method of the same
JP2010222635A (en) * 2009-03-23 2010-10-07 Akebono Brake Ind Co Ltd Friction material for brake
US9039825B2 (en) 2009-06-01 2015-05-26 Hitachi Chemical Co., Ltd. Friction material composition, friction material using the same, and friction member
CN102352899B (en) * 2011-09-22 2013-02-13 山东金麒麟股份有限公司 Low-noise powder metallurgy brake pad and preparation method thereof
DE102012112643A1 (en) * 2012-12-19 2014-06-26 Ald Vacuum Technologies Gmbh Graphite matrix, useful for the preparation of a molded body to store radioactive waste, comprises graphite and a metallic binder
RU2665651C2 (en) * 2016-12-08 2018-09-03 Сергей Михайлович Романов Romanit-fuvlhch friction composite material and method of production thereof
EP3597718B1 (en) * 2017-03-14 2022-06-15 Sunstar Engineering Inc. Sintered friction material for brake
JP6920928B2 (en) * 2017-08-31 2021-08-18 曙ブレーキ工業株式会社 Friction material manufacturing method
DE102023106699A1 (en) 2023-03-17 2024-09-19 Tmd Friction Services Gmbh Silicone resin-based friction lining compounds and friction linings with metal fibers

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US6863968B2 (en) * 2001-07-30 2005-03-08 Nisshinbo Industries, Inc. Non-asbestos-based friction materials

Also Published As

Publication number Publication date
EP0944782A1 (en) 1999-09-29
JP2001501650A (en) 2001-02-06
CA2265718A1 (en) 1998-03-26
AU4200697A (en) 1998-04-14
DK101296A (en) 1998-03-18
DK0944782T3 (en) 2003-02-17
US6143051A (en) 2000-11-07
EP0944782B1 (en) 2003-01-08
RU2194200C2 (en) 2002-12-10
ES2189973T3 (en) 2003-07-16
DE69718346D1 (en) 2003-02-13
BR9712054A (en) 2000-01-18
CA2265718C (en) 2006-05-16
ATE230830T1 (en) 2003-01-15
DE69718346T2 (en) 2003-10-30

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