EP0886683A1 - Thixotrope aluminium-silizium-küpfer legierung für formgebung in halbfesten zustand - Google Patents
Thixotrope aluminium-silizium-küpfer legierung für formgebung in halbfesten zustandInfo
- Publication number
- EP0886683A1 EP0886683A1 EP97914379A EP97914379A EP0886683A1 EP 0886683 A1 EP0886683 A1 EP 0886683A1 EP 97914379 A EP97914379 A EP 97914379A EP 97914379 A EP97914379 A EP 97914379A EP 0886683 A1 EP0886683 A1 EP 0886683A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- silicon
- alloy
- semi
- thixoforming
- alloys
- 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.)
- Granted
Links
- 239000007787 solid Substances 0.000 title claims description 8
- 229910000881 Cu alloy Inorganic materials 0.000 title description 6
- 238000007493 shaping process Methods 0.000 title description 3
- 230000009974 thixotropic effect Effects 0.000 title description 3
- -1 aluminium-silicon-copper Chemical compound 0.000 title 1
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 26
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 7
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 33
- 239000000956 alloy Substances 0.000 claims description 33
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 230000001747 exhibiting effect Effects 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 18
- 239000010949 copper Substances 0.000 description 22
- 230000005496 eutectics Effects 0.000 description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000011777 magnesium Substances 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003303 reheating Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 241000237858 Gastropoda Species 0.000 description 1
- 229910019018 Mg 2 Si Inorganic materials 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910004028 SiCU Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical group [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000009862 microstructural analysis Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000031070 response to heat Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012384 transportation and delivery Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
- C22C21/04—Modified aluminium-silicon alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
Definitions
- the invention relates to the field of aluinimum-sihcium-copper alloys, which may optionally contain other addition elements such as magnesium, cast in the form of billets having a globular solidification structure giving it thixotropic properties and intended to be used. shaped, by forging or injection under pressure, after reheating in the semi-solid state. Such shaping is known as thixoforming
- Thixoforming developed from the discovery made in the early 1970s by the team of Professor FLEMLNGS at MIT that a metal, produced under certain specific conditions, presents when it is heated to the semi- solid, an apparent viscosity which strongly depends on the shearing speed, so that it behaves as a solid during handling and as a viscous liquid when injected into a mold.
- This property leads, compared to traditional shaping processes, to a better metallurgical quality of the parts produced, higher production rates, less wear of tools and molds and energy savings.
- the solidification of the metal on thixoforming must lead to a globular, and not dendritic, structure which can be obtained either by mechanical stirring of the solid-liquid mixture as in US Pat. No.
- Billets and cast is cut into slugs corresponding to the quantity of metal required for the manufacture of the part to be formed, these plots being reheated to the semisolid state, generally by induction heating, and transferred to the processing equipment shaped (forging press or pressurized injection machine). This process s' was developed industrially primarily for aluminum alloys intended for the manufacture of parts for the automotive industry.
- alloys of the Al-Si7Mg type with 7% silicon and less than 1% magnesium for example the alloys Al-Si7MgO, 3 and Al- Si7Mg0,6 (A356 and 357 according to the nomenclature of the Aluminum Association for casting alloys). These alloys have good thixoforming ability. Indeed, when they are heated so as to obtain a liquid fraction rate of the order of 50%, corresponding to an optimum of the rheological properties of the metal, the eutectic phase is completely remelted while the fusion of the primary silicon phase is not started.
- the object of the invention is to find a field of composition of aluminum-silicon alloys with more than 5% of silicon and containing from 1 to 5% of copper making it possible to overcome the dilemma exposed above, that is to say of allow both problem-free thixoforming and obtain parts with high mechanical strength and good elongation.
- the subject of the invention is an aluminum alloy intended for thixoforming, of composition (% by weight): Si: 5% - 7.2% Cu: 1% - 5% Mg ⁇ 1% Zn ⁇ 3% Fe ⁇ 1 , 5% other elements ⁇ 1% each and 3% in total, such as:% Si ⁇ 7.5 -% Cu / 3, and having, when reheated in the semi-solid state to a rate liquid fraction between 35% and 55%, a structure free of polyhedral crystals of non-remelted silicon.
- compositions such as:
- the single figure represents, in a diagram having for abscissa the silicon content and for ordinate the copper content, the lines of equal eutectic fraction and the range of composition according to the invention.
- the alloys according to the invention remain in the usual composition ranges of AlSiCu molding alloys. We do not go below 5% silicon because the alloy becomes difficult to flow.
- the addition of copper has a significant effect on the mechanical strength and the machinability only from a content of approximately 1% and. beyond 5%, there is a very unfavorable effect on the elongation.
- Magnesium in a content of less than 1%, increases the response to heat treatment by the formation of hardening particles Mg 2 Si, but, beyond 1%, there is also an unfavorable effect on the elongation. Relatively high contents can be observed for zinc and iron in the case where one starts from secondary metal resulting from recycling. These contents are obviously much more reduced if Your share of primary metal.
- an agent for modifying the silicon of the eutectic such as sodium, strontium or antimony, which prevents the formation of excessively coarse grains of silicon.
- Sodium and strontium can be present alone or together, antimony being always alone.
- strontium for example, the content is between 0.005 and 0.05%.
- titanium up to 0.2% and / or boron up to 0.1%. allows a refinement of the grain and a better heat resistance.
- the composition of the alloy must be such that the Si and Cu contents satisfy the relationship: (2) 6.5 -% Cu / 3 ⁇ % Si ⁇ 7.5 -% Cu / 3 which corresponds to the fact that the rate of liquid fraction obtained with complete melting of the eutectic is between 45 and 55%, or that the eutectic fraction of the alloy is between 45 and 55%.
- the casting of thixotropic billets is done with difficulty, causing casting defects such as tears and breakthroughs. Furthermore, the thixoforming behavior is poor, as soon as the filling of the mold cavity begins, the heat loss by exchange with the mold wall leads to partial resolidification and an increase in the apparent viscosity which leads to defects in the part. injected, such as folds, shrinkage or non-arrival.
- the range corresponding to the compositions according to the invention comprises not only the band between the straight lines representing the eutectic fractions of 55% and 45%, i.e. the fringe surrounding the straight line representing 50%, but also the area between 45% and 35% which, taking into account the lower limit of Cu to 1 %, practically corresponds to the adjacent triangle.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Conductive Materials (AREA)
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Forging (AREA)
- Ceramic Products (AREA)
- Materials For Medical Uses (AREA)
- Chemically Coating (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Silicon Compounds (AREA)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9603703A FR2746414B1 (fr) | 1996-03-20 | 1996-03-20 | Alliage thixotrope aluminium-silicium-cuivre pour mise en forme a l'etat semi-solide |
FR9603703 | 1996-03-20 | ||
PCT/FR1997/000439 WO1997035040A1 (fr) | 1996-03-20 | 1997-03-12 | Alliage thixotrope aluminium-silicium-cuivre pour mise en forme a l'etat semi-solide |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0886683A1 true EP0886683A1 (de) | 1998-12-30 |
EP0886683B1 EP0886683B1 (de) | 1999-08-18 |
Family
ID=9490523
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97914379A Expired - Lifetime EP0886683B1 (de) | 1996-03-20 | 1997-03-12 | Thixotrope aluminium-silizium-kupfer legierung zur formgebung in halbfesten zustand |
Country Status (16)
Country | Link |
---|---|
US (1) | US5879478A (de) |
EP (1) | EP0886683B1 (de) |
JP (1) | JP2000506938A (de) |
AT (1) | ATE183549T1 (de) |
AU (1) | AU715447B2 (de) |
BR (1) | BR9708091A (de) |
CA (1) | CA2249464C (de) |
CZ (1) | CZ293598A3 (de) |
DE (2) | DE886683T1 (de) |
ES (1) | ES2136468T3 (de) |
FR (1) | FR2746414B1 (de) |
HU (1) | HUP9902156A3 (de) |
NO (1) | NO984366L (de) |
PL (1) | PL185416B1 (de) |
SK (1) | SK128098A3 (de) |
WO (1) | WO1997035040A1 (de) |
Families Citing this family (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100247143B1 (ko) * | 1998-02-04 | 2000-04-01 | 박호군 | 반응고 성형용 전신재 sic/(2xxx al+si)복합재료 및 그의 제조방법 |
FR2788788B1 (fr) * | 1999-01-21 | 2002-02-15 | Pechiney Aluminium | Produit en alliage aluminium-silicium hypereutectique pour mise en forme a l'etat semi-solide |
US6428636B2 (en) | 1999-07-26 | 2002-08-06 | Alcan International, Ltd. | Semi-solid concentration processing of metallic alloys |
DE50005101D1 (de) | 1999-07-28 | 2004-02-26 | Ruag Components Thun | Verfahren zur herstellung eines aus einer metall-legierung gebildeten werkstoffes |
US6446325B1 (en) | 1999-12-22 | 2002-09-10 | International Business Machines Corporation | Method of making a swagable metal arm tip for a ceramic actuator arm |
KR20020096279A (ko) * | 2001-06-19 | 2002-12-31 | 현대자동차주식회사 | 알루미늄 합금 |
US6719859B2 (en) | 2002-02-15 | 2004-04-13 | Northwest Aluminum Company | High strength aluminum base alloy |
US6908590B2 (en) * | 2002-03-19 | 2005-06-21 | Spx Corporation | Aluminum alloy |
CN100338248C (zh) * | 2003-11-20 | 2007-09-19 | 北京有色金属研究总院 | 一种Al-Mg-Si系合金半固态坯料的制备方法及其半固态坯料 |
US7165598B2 (en) * | 2004-03-15 | 2007-01-23 | Spx Corporation | Magnesium alloy and methods for making |
JP5069111B2 (ja) * | 2004-07-28 | 2012-11-07 | アルコア インコーポレイテッド | 航空宇宙及び自動車鋳物用Al−Si−Mg−Zn−Cu合金 |
FR2887182B1 (fr) * | 2005-06-15 | 2007-09-21 | Salomon Sa | Rayon pour une roue a rayons en traction et roue a rayons en traction |
GB0514751D0 (en) * | 2005-07-19 | 2005-08-24 | Holset Engineering Co | Method and apparatus for manufacturing turbine or compressor wheels |
US20080299001A1 (en) * | 2007-05-31 | 2008-12-04 | Alcan International Limited | Aluminum alloy formulations for reduced hot tear susceptibility |
CN100464898C (zh) * | 2007-06-18 | 2009-03-04 | 北京科技大学 | 用半固态技术制备SiC颗粒增强复合材料电子封装壳体方法 |
US8047258B1 (en) | 2008-07-18 | 2011-11-01 | Brunswick Corporation | Die casting method for semi-solid billets |
BRPI0918454A2 (pt) * | 2008-09-17 | 2015-11-24 | Cool Polymers Inc | carga de alimentação de liga metálica, e, métodos para moldar por injeção um metal em uma máquina de moldagem por injeção, e para selecionar ligas metálicas para uso em um processo de moldagem por injeção de metal |
CN102319876B (zh) * | 2011-08-31 | 2013-05-01 | 苏州有色金属研究院有限公司 | 汽车用铝合金零部件近终形铸造生产方法 |
US10174409B2 (en) | 2011-10-28 | 2019-01-08 | Alcoa Usa Corp. | High performance AlSiMgCu casting alloy |
EP2895284B1 (de) * | 2012-09-12 | 2019-01-02 | Aluminio Tecno Industriales Orinoco C.A. | Verfahren und anlage zur herstellung von bauteilen aus einer aluminiumlegierung für fahrzeuge und weisse waren sowie in diesem verfahren hergestellte bauteile |
CN105874090A (zh) | 2013-12-20 | 2016-08-17 | 美铝公司 | 高性能AlSiMgCu铸造合金 |
CN103831417A (zh) * | 2014-03-11 | 2014-06-04 | 扬州宏福铝业有限公司 | 一种高硅铝合金封装外壳半固态的连续成形方法 |
CN110592438A (zh) * | 2019-09-03 | 2019-12-20 | 滨州联信新材料科技有限公司 | 一种高性能a356铝合金的配方以及制备方法 |
CN112646993A (zh) * | 2020-12-15 | 2021-04-13 | 有研工程技术研究院有限公司 | 一种适用于高固相半固态流变压铸的铝合金材料 |
Family Cites Families (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1924725A (en) * | 1932-09-21 | 1933-08-29 | Aluminum Co Of America | Aluminum alloys |
GB555425A (en) * | 1942-02-18 | 1943-08-23 | Magnal Products Ltd | Improvements in and relating to aluminium alloys |
LU69788A1 (de) * | 1974-04-04 | 1976-03-17 | Pechiney Aluminium | |
SU523953A1 (ru) * | 1975-01-13 | 1976-08-05 | Ярославское Объединение "Автодизель" | Литейный сплав на основе аллюмини |
US4457355A (en) * | 1979-02-26 | 1984-07-03 | International Telephone And Telegraph Corporation | Apparatus and a method for making thixotropic metal slurries |
CA1235048A (en) * | 1983-05-23 | 1988-04-12 | Yoji Awano | Method for producing aluminum alloy castings and the resulting product |
FR2557144A1 (fr) * | 1983-12-22 | 1985-06-28 | Fonderie Alcoa Mg Sa | Alliage d'aluminium a proprietes ameliorees |
US4865808A (en) * | 1987-03-30 | 1989-09-12 | Agency Of Industrial Science And Technology | Method for making hypereutetic Al-Si alloy composite materials |
FR2634677B1 (fr) * | 1988-07-07 | 1990-09-21 | Pechiney Aluminium | Procede de fabrication par coulee continue de produits metalliques thixotropes |
FR2656552B1 (fr) * | 1990-01-04 | 1995-01-13 | Pechiney Aluminium | Procede de fabrication de produits metalliques thixotropes par coulee continue avec brassage electromagnetique en courant polyphase. |
GB2243620B (en) * | 1990-03-27 | 1994-06-29 | Atsugi Unisia Corp | Improvements in and relating to forming aluminium-silicon alloy |
JP2901218B2 (ja) * | 1992-07-16 | 1999-06-07 | 大同メタル工業 株式会社 | アルミニウム合金軸受 |
-
1996
- 1996-03-20 FR FR9603703A patent/FR2746414B1/fr not_active Expired - Fee Related
-
1997
- 1997-02-26 US US08/806,399 patent/US5879478A/en not_active Expired - Fee Related
- 1997-03-12 BR BR9708091A patent/BR9708091A/pt not_active Application Discontinuation
- 1997-03-12 CA CA002249464A patent/CA2249464C/fr not_active Expired - Fee Related
- 1997-03-12 SK SK1280-98A patent/SK128098A3/sk unknown
- 1997-03-12 AU AU21645/97A patent/AU715447B2/en not_active Ceased
- 1997-03-12 EP EP97914379A patent/EP0886683B1/de not_active Expired - Lifetime
- 1997-03-12 PL PL97329008A patent/PL185416B1/pl not_active IP Right Cessation
- 1997-03-12 ES ES97914379T patent/ES2136468T3/es not_active Expired - Lifetime
- 1997-03-12 JP JP9533188A patent/JP2000506938A/ja active Pending
- 1997-03-12 DE DE0886683T patent/DE886683T1/de active Pending
- 1997-03-12 HU HU9902156A patent/HUP9902156A3/hu unknown
- 1997-03-12 CZ CZ982935A patent/CZ293598A3/cs unknown
- 1997-03-12 DE DE69700436T patent/DE69700436T2/de not_active Expired - Fee Related
- 1997-03-12 WO PCT/FR1997/000439 patent/WO1997035040A1/fr not_active Application Discontinuation
- 1997-03-12 AT AT97914379T patent/ATE183549T1/de not_active IP Right Cessation
-
1998
- 1998-09-18 NO NO984366A patent/NO984366L/no not_active Application Discontinuation
Non-Patent Citations (1)
Title |
---|
See references of WO9735040A1 * |
Also Published As
Publication number | Publication date |
---|---|
CZ293598A3 (cs) | 1999-10-13 |
SK128098A3 (en) | 1999-05-07 |
HUP9902156A2 (hu) | 1999-11-29 |
DE69700436T2 (de) | 2000-02-03 |
DE69700436D1 (de) | 1999-09-23 |
JP2000506938A (ja) | 2000-06-06 |
AU2164597A (en) | 1997-10-10 |
CA2249464C (fr) | 2004-12-14 |
ES2136468T3 (es) | 1999-11-16 |
EP0886683B1 (de) | 1999-08-18 |
WO1997035040A1 (fr) | 1997-09-25 |
PL329008A1 (en) | 1999-03-01 |
ATE183549T1 (de) | 1999-09-15 |
NO984366L (no) | 1998-11-18 |
PL185416B1 (pl) | 2003-05-30 |
HUP9902156A3 (en) | 2001-11-28 |
BR9708091A (pt) | 1999-07-27 |
AU715447B2 (en) | 2000-02-03 |
CA2249464A1 (fr) | 1997-09-25 |
DE886683T1 (de) | 1999-05-06 |
FR2746414B1 (fr) | 1998-04-30 |
FR2746414A1 (fr) | 1997-09-26 |
NO984366D0 (no) | 1998-09-18 |
US5879478A (en) | 1999-03-09 |
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