EP0285741A1 - Procédé de fabrication d'un produit semi-fini à bonne ductilité à base de tantale - Google Patents

Procédé de fabrication d'un produit semi-fini à bonne ductilité à base de tantale Download PDF

Info

Publication number: EP0285741A1
Authority: EP; European Patent Office
Prior art keywords: melting; slab; semi; block; mbar
Prior art date: 1987-04-10
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

Application number

EP88100151A

Other languages

German (de)

English (en)

Other versions

EP0285741B1 (fr

Inventor

Michael Dr. Hörmann

Otto Bach

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.)

WC Heraus GmbH and Co KG

Original Assignee

WC Heraus GmbH and Co KG

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.)

1987-04-10

Filing date

1988-01-08

Publication date

1988-10-12

1988-01-08 Application filed by WC Heraus GmbH and Co KG filed Critical WC Heraus GmbH and Co KG

1988-10-12 Publication of EP0285741A1 publication Critical patent/EP0285741A1/fr

1990-10-10 Application granted granted Critical

1990-10-10 Publication of EP0285741B1 publication Critical patent/EP0285741B1/fr

2008-01-08 Anticipated expiration legal-status Critical

Status Expired - Lifetime legal-status Critical Current

Links

238000000034 method Methods 0.000 title claims abstract description 17
GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 15
238000004519 manufacturing process Methods 0.000 title claims abstract description 11
229910052715 tantalum Inorganic materials 0.000 title claims abstract description 9
238000002844 melting Methods 0.000 claims abstract description 33
230000008018 melting Effects 0.000 claims abstract description 33
238000010894 electron beam technology Methods 0.000 claims abstract description 10
239000011265 semifinished product Substances 0.000 claims abstract description 9
238000010438 heat treatment Methods 0.000 claims abstract description 4
238000005097 cold rolling Methods 0.000 claims description 10
239000000155 melt Substances 0.000 claims description 8
238000000137 annealing Methods 0.000 claims description 7
238000003825 pressing Methods 0.000 claims description 7
239000000843 powder Substances 0.000 claims description 4
238000005096 rolling process Methods 0.000 claims description 4
ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
238000001816 cooling Methods 0.000 claims description 3
GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
238000001953 recrystallisation Methods 0.000 claims description 3
238000007493 shaping process Methods 0.000 claims description 3
WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
229910052750 molybdenum Inorganic materials 0.000 claims description 2
239000011733 molybdenum Substances 0.000 claims description 2
229910052758 niobium Inorganic materials 0.000 claims description 2
239000010955 niobium Substances 0.000 claims description 2
230000001590 oxidative effect Effects 0.000 claims description 2
229910052721 tungsten Inorganic materials 0.000 claims description 2
239000010937 tungsten Substances 0.000 claims description 2
230000001939 inductive effect Effects 0.000 claims 1
238000009499 grossing Methods 0.000 abstract 1
238000003754 machining Methods 0.000 abstract 1
239000000463 material Substances 0.000 description 5
239000000047 product Substances 0.000 description 3
KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
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
229910052708 sodium Inorganic materials 0.000 description 2
239000011734 sodium Substances 0.000 description 2
RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
229910001141 Ductile iron Inorganic materials 0.000 description 1
GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
239000002253 acid Substances 0.000 description 1
QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
238000009694 cold isostatic pressing Methods 0.000 description 1
229910052802 copper Inorganic materials 0.000 description 1
239000010949 copper Substances 0.000 description 1
238000005242 forging Methods 0.000 description 1
230000006698 induction Effects 0.000 description 1
238000010309 melting process Methods 0.000 description 1
238000003801 milling Methods 0.000 description 1
239000000203 mixture Substances 0.000 description 1
229910017604 nitric acid Inorganic materials 0.000 description 1
230000035515 penetration Effects 0.000 description 1
230000000930 thermomechanical effect Effects 0.000 description 1
XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1

Classifications

- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/15—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using vacuum
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon

Definitions

the invention relates to a method for producing highly ductile semi-finished tantalum products for use in the field of high-speed forming.
the object of the present invention is to provide a method for producing highly ductile semi-finished tantalum product which is suitable for use in the field of high-speed forming, in particular for projectiles.
the melting block obtained by melting the body made of powder by pressing is advantageously melted in the electron beam furnace at a higher melting rate (kg / h) than the aforementioned body.
the melt rate for the melt block has proven to be at least twice as large as the melt rate for the body produced by pressing the powder.
the melting block obtained from the last remelting cycle is first cold-forged into a blank, which is divided into block-shaped individual pieces. Then each individual piece is heated to a temperature of about 650 ° in a slightly oxidizing atmosphere and, after removal from the oven, if the individual piece still has a temperature in the range from 450 to 600 ° C., is compressed. After cooling completely to room temperature, the compressed body is cold forged into a slab.
the tantalum semi-finished products produced according to the invention are texture-free and have a grain size that is finer than 30 ⁇ m (according to ASTM E 112). Their tensile strength is less than 200 N / mm2, their elongation is greater than 60%.
the overall purity of the materials according to the invention is calculated by determining the residual resistance ratio (electrical resistance at the temperature of 273 K: by electrical resistance at the temperature of 4.2 K). It is at least 200 for materials according to the invention.
a method for producing a highly ductile tantalum semi-finished product according to the invention is described with the aid of the exemplary embodiment below.
Sodium-reduced tantalum powder was used to produce the rod-shaped body produced by pressing.
a rod-shaped body was produced from this tantalum powder by cold isostatic pressing.
This body was used as a melting electrode in an electron beam furnace and melted at a melting rate in the range from 25 to 35 kg / h.
a pressure of 2 ⁇ 10 ⁇ 4 mbar was maintained during the melting process.
the melt was collected in a water-cooled mold and a melting block (ingot) with a diameter of 150 mm was formed. This melting block was then three times in the Electron beam furnace remelted by melting, the melt block formed in each case being used again as the melting electrode.
a pressure of 8 ⁇ 10 ⁇ 5 mbar was maintained in the electron beam furnace, the melting rate was in the range of 70 to 100 kg / h.
the corresponding values for the second remelting process were 6 ⁇ 10 ⁇ 5 mbar, the melting rate was again in the range from 70 to 100 kg / h, while during the last remelting process the pressure in the electron beam furnace was reduced to 3 ⁇ 10 ⁇ 5 mbar and the melting rate was 120 Kg / h.
the diameter of the melting block obtained from the last remelting cycle was 175 mm.
the melting block was first cold forged on 150 mm octagon, after which it was cut into block-shaped individual pieces of 350 mm length. Each individual piece was then heated to 650 ° C. in a slightly oxidized atmosphere in a gas-heated hearth furnace and held at this temperature for a period of about 2 to 3 hours. After removal from the hearth furnace, the individual pieces were compressed at a temperature of approx. 550 ° C on a forging hammer. After it had completely cooled to room temperature, the compressed individual piece was cold-forged into a slab, down to dimensions in mm of approx. 160 ⁇ 65 ⁇ 800.
the smoothed slab was degreased and first pickled in aqua regia and then in an acid mixture consisting of one part by volume of concentrated hydrofluoric acid, two parts by volume of concentrated nitric acid and two parts by volume of water.
the degree of deformation was ⁇ ⁇ 1.3 ( ⁇ ⁇ 75%). After this cold rolling process, the cold-rolled part was degreased and pickled.
a relaxation annealing was carried out in an inductively heated furnace, in which a pressure of 2 ⁇ 10bar mbar was maintained during the heat treatment.
the annealed part was subjected to several cold rolling steps, in which case rolling was again carried out in the direction along and transversely to the axis of the last melting block obtained.
This cold rolling process was also carried out with a high number of individual passes.
the degree of deformation was ⁇ ⁇ 1.9 ( ⁇ ⁇ 85%).
the workpiece was again cold-rolled, as described above, ground, degreased and pickled and then subjected to recrystallization annealing at 875 ° C. in a resistance-heated vacuum oven.
the highly ductile tantalum semi-finished product thus obtained was texture-free and had a grain size finer than 30 ⁇ m according to (ASTM E 112). Its tensile strength was 192 N / mm2, its elongation was 65%, the residual resistance ratio was found to be 220.

Landscapes

Chemical & Material Sciences (AREA)
Engineering & Computer Science (AREA)
Mechanical Engineering (AREA)
Physics & Mathematics (AREA)
Thermal Sciences (AREA)
Crystallography & Structural Chemistry (AREA)
Materials Engineering (AREA)
Metallurgy (AREA)
Organic Chemistry (AREA)
Manufacture And Refinement Of Metals (AREA)
Forging (AREA)

EP88100151A 1987-04-10 1988-01-08 Procédé de fabrication d'un produit semi-fini à bonne ductilité à base de tantale Expired - Lifetime EP0285741B1 (fr)

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
DE3712281		1987-04-10
DE19873712281 DE3712281A1 (de)	1987-04-10	1987-04-10	Verfahren zur herstellung von hochduktilem tantal-halbzeug

Publications (2)

Publication Number	Publication Date
EP0285741A1 true EP0285741A1 (fr)	1988-10-12
EP0285741B1 EP0285741B1 (fr)	1990-10-10

Family

ID=6325394

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP88100151A Expired - Lifetime EP0285741B1 (fr)	1987-04-10	1988-01-08	Procédé de fabrication d'un produit semi-fini à bonne ductilité à base de tantale

Country Status (3)

Country	Link
US (1)	US4844746A (fr)
EP (1)	EP0285741B1 (fr)
DE (2)	DE3712281A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
WO2000031310A1 (fr) *	1998-11-25	2000-06-02	Cabot Corporation	Tantale de grande purete et produits le contenant, tels que les cibles pulverisees
CN1066367C (zh) *	1998-11-12	2001-05-30	北京有色金属研究总院	一种制造用于生产钼电极坯和钼流口坯的金属钼棒的方法
CN120628214A (zh) *	2025-08-08	2025-09-12	四川省第七地质大队	一种基于地质分析的地质灾害位移监测装置

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
US5411611A (en) *	1993-08-05	1995-05-02	Cabot Corporation	Consumable electrode method for forming micro-alloyed products
US6323055B1 (en) *	1998-05-27	2001-11-27	The Alta Group, Inc.	Tantalum sputtering target and method of manufacture
US6348139B1 (en) *	1998-06-17	2002-02-19	Honeywell International Inc.	Tantalum-comprising articles
US20040072009A1 (en) *	1999-12-16	2004-04-15	Segal Vladimir M.	Copper sputtering targets and methods of forming copper sputtering targets
US6878250B1 (en)	1999-12-16	2005-04-12	Honeywell International Inc.	Sputtering targets formed from cast materials
US7517417B2 (en) *	2000-02-02	2009-04-14	Honeywell International Inc.	Tantalum PVD component producing methods
US6331233B1 (en)	2000-02-02	2001-12-18	Honeywell International Inc.	Tantalum sputtering target with fine grains and uniform texture and method of manufacture
CN1257998C (zh) *	2001-01-11	2006-05-31	卡伯特公司	钽和铌的坯料及其制造方法
RU2205248C2 (ru) *	2001-02-19	2003-05-27	Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара"	Способ изготовления танталовой ленты
US7416697B2 (en)	2002-06-14	2008-08-26	General Electric Company	Method for preparing a metallic article having an other additive constituent, without any melting
US7897103B2 (en) *	2002-12-23	2011-03-01	General Electric Company	Method for making and using a rod assembly
US7228722B2 (en) *	2003-06-09	2007-06-12	Cabot Corporation	Method of forming sputtering articles by multidirectional deformation
CN1836307A (zh) *	2003-06-20	2006-09-20	卡伯特公司	溅镀靶安装到垫板上的方法和设计
US7531021B2 (en)	2004-11-12	2009-05-12	General Electric Company	Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix
US7819079B2 (en)	2004-12-22	2010-10-26	Applied Materials, Inc.	Cartesian cluster tool configuration for lithography type processes
US7798764B2 (en)	2005-12-22	2010-09-21	Applied Materials, Inc.	Substrate processing sequence in a cartesian robot cluster tool
US7699021B2 (en)	2004-12-22	2010-04-20	Sokudo Co., Ltd.	Cluster tool substrate throughput optimization
US7651306B2 (en)	2004-12-22	2010-01-26	Applied Materials, Inc.	Cartesian robot cluster tool architecture
US20060130767A1 (en)	2004-12-22	2006-06-22	Applied Materials, Inc.	Purged vacuum chuck with proximity pins
US7998287B2 (en)	2005-02-10	2011-08-16	Cabot Corporation	Tantalum sputtering target and method of fabrication
US20070084527A1 (en) *	2005-10-19	2007-04-19	Stephane Ferrasse	High-strength mechanical and structural components, and methods of making high-strength components
EE05493B1 (et)	2006-03-07	2011-12-15	Cabot Corporation	Meetod l?pliku paksusega metallesemete valmistamiseks, saadud metallplaat ja selle valmistamiseks kasutatav BCC- metall
US20070251818A1 (en) *	2006-05-01	2007-11-01	Wuwen Yi	Copper physical vapor deposition targets and methods of making copper physical vapor deposition targets

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Publication number	Priority date	Publication date	Assignee	Title
DE1141794B (de) *	1958-06-13	1962-12-27	Nat Res Corp	Verfahren zur Herstellung von Tantalpulver
US3497402A (en) *	1966-02-03	1970-02-24	Nat Res Corp	Stabilized grain-size tantalum alloy
WO1982001677A1 (fr) *	1980-11-14	1982-05-27	Oproiu Margareta	Procede et installation de fusion-coulee pour metaux et alliages a haut point de fusion et forts reactifs

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US2825641A (en) *	1955-09-21	1958-03-04	Robert A Beall	Method for melting refractory metals for casting purposes
US3285716A (en) *	1964-07-20	1966-11-15	Kawecki Chemical Company	Etched tantalum foil
JPS6066425A (ja) *	1983-09-22	1985-04-16	Nippon Telegr & Teleph Corp <Ntt>	Ｌｓｉ電極用の高純度モリブデンタ−ゲツトならびに高純度モリブデンシリサイドタ−ゲツトおよびその製造方法
JPS60124452A (ja) *	1983-12-07	1985-07-03	Hitachi Ltd	高純度金属スリ−ブの製造方法
US4722756A (en) *	1987-02-27	1988-02-02	Cabot Corp	Method for deoxidizing tantalum material

1987
- 1987-04-10 DE DE19873712281 patent/DE3712281A1/de active Granted
1988
- 1988-01-08 EP EP88100151A patent/EP0285741B1/fr not_active Expired - Lifetime
- 1988-01-08 DE DE8888100151T patent/DE3860768D1/de not_active Expired - Lifetime
- 1988-03-23 US US07/172,201 patent/US4844746A/en not_active Expired - Fee Related

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
DE1141794B (de) *	1958-06-13	1962-12-27	Nat Res Corp	Verfahren zur Herstellung von Tantalpulver
US3497402A (en) *	1966-02-03	1970-02-24	Nat Res Corp	Stabilized grain-size tantalum alloy
WO1982001677A1 (fr) *	1980-11-14	1982-05-27	Oproiu Margareta	Procede et installation de fusion-coulee pour metaux et alliages a haut point de fusion et forts reactifs

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
CN1066367C (zh) *	1998-11-12	2001-05-30	北京有色金属研究总院	一种制造用于生产钼电极坯和钼流口坯的金属钼棒的方法
WO2000031310A1 (fr) *	1998-11-25	2000-06-02	Cabot Corporation	Tantale de grande purete et produits le contenant, tels que les cibles pulverisees
US6348113B1 (en)	1998-11-25	2002-02-19	Cabot Corporation	High purity tantalum, products containing the same, and methods of making the same
US6893513B2 (en)	1998-11-25	2005-05-17	Cabot Corporation	High purity tantalum, products containing the same, and methods of making the same
US7431782B2 (en)	1998-11-25	2008-10-07	Cabot Corporation	High purity tantalum, products containing the same, and methods of making the same
US7585380B2 (en)	1998-11-25	2009-09-08	Cabot Corporation	High purity tantalum, products containing the same, and methods of making the same
CN120628214A (zh) *	2025-08-08	2025-09-12	四川省第七地质大队	一种基于地质分析的地质灾害位移监测装置

Also Published As

Publication number	Publication date
US4844746A (en)	1989-07-04
DE3860768D1 (de)	1990-11-15
DE3712281A1 (de)	1988-10-27
EP0285741B1 (fr)	1990-10-10
DE3712281C2 (fr)	1989-09-14

Legal Events

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1988-08-27	PUAI	Public reference made under article 153(3) epc to a published international application that has entered the european phase	Free format text: ORIGINAL CODE: 0009012
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Publication	Publication Date	Title
EP0285741B1 (fr)	1990-10-10	Procédé de fabrication d'un produit semi-fini à bonne ductilité à base de tantale
DE3621671C2 (fr)	1989-05-11
DE69419176T2 (de)	2000-01-05	Co-cr-mo pulvermetallurgischen gegenstände und verfahren deren herstellung
DE1935329A1 (de)	1970-01-22	Verfahren zur Herstellung dispersionsverstaerkter Metalle oder Metallegierungen und Verwendung der nach diesem Verfahren hergestellten Metalle oder Metallegierungen
DE2542094A1 (de)	1976-04-08	Metallpulver, verfahren zur behandlung losen metallpulvers und verfahren zur herstellung eines verdichteten presslings
DE2630141C2 (de)	1986-02-20	Verwendung einer Wolfram, Silizium und/oder Titan enthaltenden Eisenlegierung zur Herstellung von Teilen mit hoher Dämpfungsfähigkeit
DE2751623C2 (de)	1982-08-05	Verfahren zur Herstellung von warmverformten Fertigprodukten auf Molybdänbasis
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EP0035601A1 (fr)	1981-09-16	Procédé de fabrication d'un alliage-mémoire
DE2543893C2 (de)	1987-04-30	Verfahren zur Herstellung eines warmverformten Produktes aus Titan bzw. einer Titanlegierung
DE3326554C2 (de)	1994-06-30	Auskleidung für Hohlladungen und Verfahren zum Herstellen einer solchen Auskleidung
DE1558632A1 (de)	1970-04-23	Korrosionsbestaendige Kobalt-Nickel-Molybdaen-Chromlegierungen
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