WO2000007759A1 - Alloyed, non-oxidising metal powder - Google Patents

Alloyed, non-oxidising metal powder Download PDF

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Publication number
WO2000007759A1
WO2000007759A1 PCT/SE1999/001293 SE9901293W WO0007759A1 WO 2000007759 A1 WO2000007759 A1 WO 2000007759A1 SE 9901293 W SE9901293 W SE 9901293W WO 0007759 A1 WO0007759 A1 WO 0007759A1
Authority
WO
WIPO (PCT)
Prior art keywords
alloyed
metal powder
powder
weight
atomised
Prior art date
Application number
PCT/SE1999/001293
Other languages
French (fr)
Inventor
Rutger Larsson
Erik Axmin
Original Assignee
Rutger Larsson Konsult Ab
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 Rutger Larsson Konsult Ab filed Critical Rutger Larsson Konsult Ab
Priority to DE69939230T priority Critical patent/DE69939230D1/en
Priority to AU50778/99A priority patent/AU5077899A/en
Priority to EP99935265A priority patent/EP1742753B1/en
Publication of WO2000007759A1 publication Critical patent/WO2000007759A1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid

Definitions

  • the present invention relates to an atomised, non-oxidising, alloyed metal powder based on iron enriched with carbide-bound carbon in the surface layer, and also to the use of the atomised, non-oxidising, alloyed metal powder.
  • metal powders are produced by means of atomising, electrolysis or through chemical or oxide reduction. Powder is used in mixtures for producing alloy compositions that are bound metallurgically upon sintering. Metallic and non-metallic powders can be combined to produce composite material having special properties.
  • the powder metallurgical composition most frequently used is iron powder, which is used in the manufacture of various structured parts. Iron powder is sometimes used alone or, which is more usual, together with various additives in order to improve the mechanical properties of compacted sintered products. Powder additives include carbon, copper, nickel and molybdenum.
  • US, A, 5,522,914 reveals an alloyed metal powder composed of 0.80 to 3.00 per cent by weight carbon, 0.20 to 2.00 per cent by weight manganese, 0.20 to 1.50 per cent by weight silicon, as well as 3.0 to 12.0 per cent by weight chromium, 0.20 to 0.30 per cent by weight sulphur, up to 0.04 per cent by weight phosphorous, 0.25 to 10.0 per cent by weight vanadium, up to 11.0 per cent by weight molybdenum, up to 18.00 per cent by weight mercury, up to 10 per cent by weight cobalt and up to 0.10 per cent by weight nitrogen, besides the iron.
  • the oxygen content in the powder is less than 0.025 per cent by weight.
  • the powder is produced by atomisation in nitrogen gas atmosphere in order to achieve a low oxygen content.
  • the problem in the production of metal powder is the oxygen content.
  • hydrocarbon which is partially carbonised during the atomisation process.
  • hydrocarbon is known through Swedish patent application 9601482- 4.
  • the atomised steel powder obtained has acquired enriched carbide- bound carbon in the surface layer, and a low oxygen content.
  • alloyed powder particles can be produced that include oxidation- sensitive alloying substances such as chromium, manganese, silicon.
  • nitrogen gas atmosphere can be avoided since the atmosphere in the atomising equipment is saturated with vaporised or carbonised atomising medium.
  • the present invention thus solves the problems of added oxygen and undesired nitrogen.
  • the atomised, alloyed metal powder according to the invention is non-oxidising as well as preventing oxidation. It has improved powder-metallurgical properties such as strength and toughness.
  • the carbide-bound carbon in the surface layer of the powder particles is enriched.
  • the non-oxidising, alloyed metal powder in accordance with the invention comprises oxidation-sensitive alloying metals such as chromium, manganese and/ or silicon, besides iron and carbide-bound carbon. These alloying metals are also capable of carbide-binding carbon.
  • Atomising medium used in the producion of the non-oxidising alloyed metal powder consists of hydrocarbons selected from the group comprising paraffin, diesel oils, or other cyclic or acyclic hydrocarbons that have been partially carbonised during the atomisation. Hydrogen gas is formed during the carbonisation of the hydrocarbons, as well as the carbides that are bound to the metals in the powder particles.
  • the atmosphere in the atomising vessel is saturated with vaporised or carbonised atomising medium consisting of hydrocarbons and hydrogen gas. The atmosphere is thus reducing, thereby protecting the powder particles produced.
  • the alloyed metal powder may also include other alloying substances such as vanadium, molybdenum, tungsten, aluminium, copper, nickel, titanium.
  • a preferred embodiment of the invention constitutes atomised, alloyed, non-oxidising metal powder based on iron with enriched carbide-bound carbon in the surface layer, that has been carbide-bound to the metal in the powder particles by carbonised atomising medium selected from the group comprising paraffin, diesel oils, or other cyclic or acyclic hydrocarbons during the atomising, wherein, besides iron and the carbide-bound carbon, the alloyed powder particles comprise one or more of the following alloying substances: 0.1 to 16 % by weight chromium, preferably 0.5 to 12 % by weight, 0.1 to 12 % by weight manganese, preferably 0.5 to 10 % by weight, or 0.1 to 5.0 % by weight silicon, preferably 0.5 to 4.5 % by weight, wherein the carbon content is 0.02 to 3.0 % by weight of the total contents in the metal powder, and wherein the oxygen content is less than 200 ppm.
  • Another preferred embodiment of the invention comprises the addition of extra alloying substances to said alloyed non-oxidising metal powder mentioned above.
  • extra alloying substances may be, for example, vanadium, molybdenum, tungsten, aluminium, copper, nickel, titanium.
  • Preferred contents of the extra alloying substances are within the range 0.1 to 5.0 % by weight.
  • the size distribution in the powder particles is mainly 10 to 350 ⁇ m, preferably 45 to 200 ⁇ m.
  • Producing the atomised, alloyed, non-oxidising metal powder, based on iron with enriched carbide-bound carbon in the surface layer enables the manufacture of compacted sintered products such as toothed wheels, ball-bearings and tool steel. These products require high mechanical strength and toughness, and these properties are achieved since the alloying additives increase tempering quality and strength.
  • the products are manufactured by means of conventional powder metallurgical compressing, hot compacting and sintering, hot isostatic pressing and sinter forging.
  • the metal powder produced is non-oxidising and prevents oxidation it can be mixed with other powder produced from oxidation- sensitive metals. This enables the manufacture of composite material having completely new qualities.
  • the present invention thus also relates to the use of the atomised, alloyed, non-oxidising metal powder as claimed in any of claims 1 to 6 for the manufacture of compressed, sintered products, such as toothed wheels, ball-bearings, tool steel, manufactured by means of conventional powder-metallurgical compression, hot compacting and sintering, hot isostatic compacting and sinter forging.
  • Alloyed metal powder of type US32CrMn was produced, with the difference that the powder produced has metal carbide in the surface layer.
  • the powder comprises 0.9 to 1.2 per cent by weight chromium,
  • Alloyed metal powder of "Case Hardening Steel” type was produced with metal carbides in the surface layer.
  • the powder comprises 0.8 to 1.3 per cent by weight chromium and 1.1 per cent by weight manganese.
  • An alloyed metal powder with metal carbides in the surface layer was produced having 8.0 to 10 per cent by weight chromium, 8.0 to 10 per cent by weight manganese, 0.8 to 1.2 per cent by weight carbon and the remainder iron.
  • the powder produced is spherical and has a size distribution of between 45 and 200 ⁇ m.

Abstract

The present invention relates to an atomised, non-oxidising, alloyed metal powder based on iron, that has been enriched with carbide-bound carbon in the surface layer of the powder particle. Besides iron and the carbide-bound carbon, the powder particles comprise one or more of the alloying substances, chromium, manganese or silicon. The oxygen content in the atomised, non-oxidising alloyed metal powder is less than 200 ppm. The invention also relates to the use of the atomised, non-oxidising, alloyed metal powder.

Description

Alloyed, non-oxidising metal powder
The present invention relates to an atomised, non-oxidising, alloyed metal powder based on iron enriched with carbide-bound carbon in the surface layer, and also to the use of the atomised, non-oxidising, alloyed metal powder.
Most metal powders are produced by means of atomising, electrolysis or through chemical or oxide reduction. Powder is used in mixtures for producing alloy compositions that are bound metallurgically upon sintering. Metallic and non-metallic powders can be combined to produce composite material having special properties.
The powder metallurgical composition most frequently used is iron powder, which is used in the manufacture of various structured parts. Iron powder is sometimes used alone or, which is more usual, together with various additives in order to improve the mechanical properties of compacted sintered products. Powder additives include carbon, copper, nickel and molybdenum.
US, A, 5,522,914 reveals an alloyed metal powder composed of 0.80 to 3.00 per cent by weight carbon, 0.20 to 2.00 per cent by weight manganese, 0.20 to 1.50 per cent by weight silicon, as well as 3.0 to 12.0 per cent by weight chromium, 0.20 to 0.30 per cent by weight sulphur, up to 0.04 per cent by weight phosphorous, 0.25 to 10.0 per cent by weight vanadium, up to 11.0 per cent by weight molybdenum, up to 18.00 per cent by weight mercury, up to 10 per cent by weight cobalt and up to 0.10 per cent by weight nitrogen, besides the iron. The oxygen content in the powder is less than 0.025 per cent by weight. The powder is produced by atomisation in nitrogen gas atmosphere in order to achieve a low oxygen content.
The problem in the production of metal powder is the oxygen content.
A high oxygen content is unsuitable when metal powder is to be used for tools or other articles requiring high mechanical strength. In US, A, 5,522,914 the problem has been solved by atomising the powder in nitrogen gas atmosphere. This is expensive and results in undesired nitrogen being included in the alloyed powder produced.
The problem of the added nitrogen is solved by using hydrocarbon which is partially carbonised during the atomisation process. Such use of hydrocarbon is known through Swedish patent application 9601482- 4. The atomised steel powder obtained has acquired enriched carbide- bound carbon in the surface layer, and a low oxygen content.
It has now surprisingly been found that oxidation can be prevented by enriching the carbide-bound carbon in the surface layer. This means that alloyed powder particles can be produced that include oxidation- sensitive alloying substances such as chromium, manganese, silicon. Furthermore, the use of nitrogen gas atmosphere can be avoided since the atmosphere in the atomising equipment is saturated with vaporised or carbonised atomising medium.
The present invention thus solves the problems of added oxygen and undesired nitrogen. The atomised, alloyed metal powder according to the invention is non-oxidising as well as preventing oxidation. It has improved powder-metallurgical properties such as strength and toughness. The carbide-bound carbon in the surface layer of the powder particles is enriched.
Detailed description of the invention
The non-oxidising, alloyed metal powder in accordance with the invention comprises oxidation-sensitive alloying metals such as chromium, manganese and/ or silicon, besides iron and carbide-bound carbon. These alloying metals are also capable of carbide-binding carbon.
Atomising medium used in the producion of the non-oxidising alloyed metal powder consists of hydrocarbons selected from the group comprising paraffin, diesel oils, or other cyclic or acyclic hydrocarbons that have been partially carbonised during the atomisation. Hydrogen gas is formed during the carbonisation of the hydrocarbons, as well as the carbides that are bound to the metals in the powder particles. The atmosphere in the atomising vessel is saturated with vaporised or carbonised atomising medium consisting of hydrocarbons and hydrogen gas. The atmosphere is thus reducing, thereby protecting the powder particles produced.
The alloyed metal powder may also include other alloying substances such as vanadium, molybdenum, tungsten, aluminium, copper, nickel, titanium.
A preferred embodiment of the invention constitutes atomised, alloyed, non-oxidising metal powder based on iron with enriched carbide-bound carbon in the surface layer, that has been carbide-bound to the metal in the powder particles by carbonised atomising medium selected from the group comprising paraffin, diesel oils, or other cyclic or acyclic hydrocarbons during the atomising, wherein, besides iron and the carbide-bound carbon, the alloyed powder particles comprise one or more of the following alloying substances: 0.1 to 16 % by weight chromium, preferably 0.5 to 12 % by weight, 0.1 to 12 % by weight manganese, preferably 0.5 to 10 % by weight, or 0.1 to 5.0 % by weight silicon, preferably 0.5 to 4.5 % by weight, wherein the carbon content is 0.02 to 3.0 % by weight of the total contents in the metal powder, and wherein the oxygen content is less than 200 ppm.
Another preferred embodiment of the invention comprises the addition of extra alloying substances to said alloyed non-oxidising metal powder mentioned above. Such extra alloying substances may be, for example, vanadium, molybdenum, tungsten, aluminium, copper, nickel, titanium. Preferred contents of the extra alloying substances are within the range 0.1 to 5.0 % by weight. The size distribution in the powder particles is mainly 10 to 350 μm, preferably 45 to 200 μm.
Producing the atomised, alloyed, non-oxidising metal powder, based on iron with enriched carbide-bound carbon in the surface layer enables the manufacture of compacted sintered products such as toothed wheels, ball-bearings and tool steel. These products require high mechanical strength and toughness, and these properties are achieved since the alloying additives increase tempering quality and strength. The products are manufactured by means of conventional powder metallurgical compressing, hot compacting and sintering, hot isostatic pressing and sinter forging.
Since the metal powder produced is non-oxidising and prevents oxidation it can be mixed with other powder produced from oxidation- sensitive metals. This enables the manufacture of composite material having completely new qualities.
The present invention thus also relates to the use of the atomised, alloyed, non-oxidising metal powder as claimed in any of claims 1 to 6 for the manufacture of compressed, sintered products, such as toothed wheels, ball-bearings, tool steel, manufactured by means of conventional powder-metallurgical compression, hot compacting and sintering, hot isostatic compacting and sinter forging.
The embodiments described above, and other preferred embodiments of the invention are defined in the subordinated claims.
The present invention will be further illustrated with concrete examples which should not, however, be considered as limiting the scope of protection of the invention otherwise than as defined in the appended claims.
In the following, examples of alloyed, non-oxidising metal powder according to the invention were produced in accordance with the procedure described in Swedish patent application No. 9601482-4. Paraffin was used as atomising medium in the experiments.
Example 1
Alloyed metal powder of type US32CrMn was produced, with the difference that the powder produced has metal carbide in the surface layer. The powder comprises 0.9 to 1.2 per cent by weight chromium,
1.5 per cent by weight manganese and 0.15 to 0.25 per cent by weight molybdenum.
Example 2
Alloyed metal powder of "Case Hardening Steel" type was produced with metal carbides in the surface layer. The powder comprises 0.8 to 1.3 per cent by weight chromium and 1.1 per cent by weight manganese.
Example 3
An alloyed metal powder with metal carbides in the surface layer was produced having 8.0 to 10 per cent by weight chromium, 8.0 to 10 per cent by weight manganese, 0.8 to 1.2 per cent by weight carbon and the remainder iron. The powder produced is spherical and has a size distribution of between 45 and 200 μm.

Claims

1. An atomised, alloyed, non-oxidising metal powder based on iron enriched with carbide-bound carbon in the surface layer, that has been carbide-bound to the metals in the powder particles by carbonised atomising medium selected from the group comprising paraffin, diesel oils, or other cyclic or acyclic hydrocarbons characterized in that besides iron and the carbide-bound carbon, the powder particles comprise one or more of the alloying substances chromium, manganese or silicon in contents of in the range of 0.1 to 16 % by weight for chromium, in contents of in the range of 0.1 to 12 % by weight for manganese or in contents of in the range of 0.1 to 5.0 % by weight for silicon, in that the carbon content is 0.02 to 3.0 % by weight of the total contents in the metal powder, and in that the oxygen content is less than 200 ppm.
2. An atomised, alloyed, non-oxidising metal powder as claimed in claim 1, characterized in that the alloying substances have contents in the ranges of 0.5 to 12 % by weight for chromium, 0.5 to 10 % by weight for manganese or 0.5 to 4.5 % by weight for silicon.
3. An atomised, alloyed, non-oxidising metal powder as claimed in claim 1 or claim 2, characterized in that the atomised, alloyed, non-oxidising metal powder also includes one or more other alloying metals, such as vanadium, molybdenum, tungsten, aluminium, copper, nickel, titanium.
4. An atomised, alloyed, non-oxidising metal powder as claimed in any of claims lto3, characterized in that the powder particles mainly have a size of between 10 and 350 ╬╝m.
5. An atomised, alloyed, non-oxidising metal powder as claimed in claim 4, characterized in that the powder particles have a size of between 45 and 200 ╬╝m.
6. An atomised, alloyed, non-oxidising metal powder as claimed in any of the preceding claims, c h a r a c t e r i z e d i n t h a t the powder particles are spherical and have high mechanical strength and toughness.
7. The use of alloyed, non-oxidising metal powder as claimed in any of claims 1 to 6 for the manufacture of compressed, sintered products, such as toothed wheels, ball-bearings, tool steel, manufactured by means of conventional powder-metallurgical compression, hot compacting and sintering, hot isostatic compacting and sinter forging.
8. The use of alloyed, non-oxidising metal powder as claimed in any of claims 1 to 6 for the manufacture of compressed, sintered, alloyed products, such as toothed wheels, ball-bearings, tool steel, together with iron powder.
PCT/SE1999/001293 1998-08-06 1999-07-19 Alloyed, non-oxidising metal powder WO2000007759A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE69939230T DE69939230D1 (en) 1998-08-06 1999-07-19 ALLOY, NONOXIDING METAL POWDER
AU50778/99A AU5077899A (en) 1998-08-06 1999-07-19 Alloyed, non-oxidising metal powder
EP99935265A EP1742753B1 (en) 1998-08-06 1999-07-19 Alloyed, non-oxidising metal powder

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE9802682-6 1998-08-06
SE9802682A SE521053C2 (en) 1998-08-06 1998-08-06 Use of an alloy non-oxidizing metal powder

Publications (1)

Publication Number Publication Date
WO2000007759A1 true WO2000007759A1 (en) 2000-02-17

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Application Number Title Priority Date Filing Date
PCT/SE1999/001293 WO2000007759A1 (en) 1998-08-06 1999-07-19 Alloyed, non-oxidising metal powder

Country Status (7)

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EP (2) EP2163331A1 (en)
AT (1) ATE402773T1 (en)
AU (1) AU5077899A (en)
DE (1) DE69939230D1 (en)
ES (1) ES2310427T3 (en)
SE (1) SE521053C2 (en)
WO (1) WO2000007759A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7875134B2 (en) * 2007-03-12 2011-01-25 IUCF-HYU (Industry-University Cooporation Foundation Hanyang University) Fe-based alloy having corrosion resistance and abrasion resistance and preparation method thereof
US20130039796A1 (en) * 2010-02-15 2013-02-14 Gilles L'Esperance Master alloy for producing sinter hardened steel parts and process for the production of sinter hardened parts

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6229277B2 (en) * 2013-03-01 2017-11-15 日立化成株式会社 Sintered alloy and method for producing the same

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2220673B2 (en) * 1972-04-27 1974-11-21 Bayrisches Leichtmetallwerk Graf Bluecher Von Wahlstatt Kg, 8000 Muenchen Metallic sintered alloys, in particular sintered steel alloys
WO1996005007A1 (en) * 1994-08-10 1996-02-22 Höganäs Ab Iron-based powder containing chromium, molybdenum and manganese
US5522914A (en) * 1993-09-27 1996-06-04 Crucible Materials Corporation Sulfur-containing powder-metallurgy tool steel article
WO1997041986A1 (en) * 1996-04-18 1997-11-13 Rutger Larsson Konsult Ab A process and plant for producing atomized metal powder, metal powder and the use of the metal powder
US9302818B2 (en) * 2011-11-22 2016-04-05 Robert Beadles Reusable envelope

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61276949A (en) * 1985-05-29 1986-12-06 Sumitomo Metal Ind Ltd Manufacture of sintered parts
US5435827A (en) * 1991-08-07 1995-07-25 Erasteel Kloster Aktiebolag High speed steel manufactured by power metallurgy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2220673B2 (en) * 1972-04-27 1974-11-21 Bayrisches Leichtmetallwerk Graf Bluecher Von Wahlstatt Kg, 8000 Muenchen Metallic sintered alloys, in particular sintered steel alloys
US5522914A (en) * 1993-09-27 1996-06-04 Crucible Materials Corporation Sulfur-containing powder-metallurgy tool steel article
WO1996005007A1 (en) * 1994-08-10 1996-02-22 Höganäs Ab Iron-based powder containing chromium, molybdenum and manganese
WO1997041986A1 (en) * 1996-04-18 1997-11-13 Rutger Larsson Konsult Ab A process and plant for producing atomized metal powder, metal powder and the use of the metal powder
US9302818B2 (en) * 2011-11-22 2016-04-05 Robert Beadles Reusable envelope

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7875134B2 (en) * 2007-03-12 2011-01-25 IUCF-HYU (Industry-University Cooporation Foundation Hanyang University) Fe-based alloy having corrosion resistance and abrasion resistance and preparation method thereof
US20130039796A1 (en) * 2010-02-15 2013-02-14 Gilles L'Esperance Master alloy for producing sinter hardened steel parts and process for the production of sinter hardened parts
US10618110B2 (en) * 2010-02-15 2020-04-14 Tenneco Inc. Master alloy for producing sinter hardened steel parts and process for the production of sinter hardened parts

Also Published As

Publication number Publication date
SE9802682D0 (en) 1998-08-06
SE9802682L (en) 2000-02-07
EP2163331A1 (en) 2010-03-17
ES2310427T3 (en) 2009-01-01
SE521053C2 (en) 2003-09-23
AU5077899A (en) 2000-02-28
EP1742753A1 (en) 2007-01-17
ATE402773T1 (en) 2008-08-15
EP1742753B1 (en) 2008-07-30
DE69939230D1 (en) 2008-09-11

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