EP0801138A2 - Préparation d'un alliage-mère titane-molybdène - Google Patents

Préparation d'un alliage-mère titane-molybdène Download PDF

Info

Publication number
EP0801138A2
EP0801138A2 EP97105999A EP97105999A EP0801138A2 EP 0801138 A2 EP0801138 A2 EP 0801138A2 EP 97105999 A EP97105999 A EP 97105999A EP 97105999 A EP97105999 A EP 97105999A EP 0801138 A2 EP0801138 A2 EP 0801138A2
Authority
EP
European Patent Office
Prior art keywords
molybdenum
titanium
powdered
master alloy
alloying
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.)
Withdrawn
Application number
EP97105999A
Other languages
German (de)
English (en)
Other versions
EP0801138A3 (fr
Inventor
Brian J. Higgins
James D. Kahl
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.)
Reading Alloys Inc
Original Assignee
Reading Alloys Inc
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 Reading Alloys Inc filed Critical Reading Alloys Inc
Publication of EP0801138A2 publication Critical patent/EP0801138A2/fr
Publication of EP0801138A3 publication Critical patent/EP0801138A3/fr
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys

Definitions

  • the invention relates to titanium base alloys, and more particularly to titanium base binary master alloys containing substantial amounts of refractory metals, such as molybdenum, which are suitable for further alloying into titanium base alloys.
  • This invention also relates to methods for producing alloys containing substantial amounts of refractory metals, such as high molybdenum (and other refractory)-containing titanium base master alloys.
  • Titanium metal and titanium base alloys are low weight, yet relatively strong metals, with high heat and corrosion resistance. These metals are in great demand today as preferred materials for use in aircraft, space shuttle, and military applications.
  • US-A 3,269,825 discloses vacuum, consumable electrode, arc melted homogeneous titanium base alloys containing between about 6% to 15% molybdenum with substantially complete dissolution of the molybdenum in the base alloy, thereby avoiding formation of molybdenum inclusions.
  • mentioned document also uses ternary additions to attain such results in the final alloy.
  • US-A 3,552,947 Patent at al. discloses vacuum, consumable electrode, arc melted titanium base alloys containing about 11,5% molybdenum having a homogeneous microstructure, but this method uses a low density, porous, sintered molybdenum agglomerates as the refractory alloying component to avoid segregation and ternary additions.
  • US-A 3,645,727 discloses a ternary titanium base alloy from master alloys containing high amounts of molybdenum, such as 30% to 75% molybdenum, in which the master alloy is a lower melting alloy than molybdenum alone through ternary additions which aids in its later dissolution in titanium.
  • US-A 4,634,478 discloses a vacuum arc melted and annealed titanium base alloy containing 0,2 to 3,0% molybdenum, the balance being substantially titanium.
  • US-A 5,316,723 discloses a thermite titanium base master alloy containing substantial amounts of molybdenum, such as 55% to 75% molybdenum, and which also contains ternary additions to aid in its later dissolution in titanium.
  • a method is provided of obtaining substantially complete dissolution and/or distribution of refractory metals, such as molybdenum, tantalum, niobium, tungsten, in a relatively lower melting point base alloy, such as titanium base alloy.
  • refractory metals such as molybdenum, tantalum, niobium, tungsten
  • a method is provided of producing titanium base binary master alloy compositions containing substantial quantities of refractory molybdenum or tantalum, in which the resultant alloy is homogeneous and, thus, available for subsequent alloying into an acceptable final titanium base alloy (claims 11 to 14).
  • the examples of present invention are directed to a method of producing homogeneous alloy compositions, and the alloys produced thereby, which comprise lower melting base alloys containing substantial quantities of refractory metals uniformly and homogeneously distributed throughout the alloys.
  • the present invention is not limited to a single, restricted class of alloys nor to any particular alloy composition.
  • the example of the method according to the invention is broadly useful in the production of nearly all alloys containing appreciable quantities of refractory metal, such as molybdenum, tantalum, niobium, tungsten, in a base metal having a melting point substantially lower than that of the refractory metal, such as titanium. It is especially useful in the production of titanium base alloys, in particular master alloys, containing high amounts of molybdenum, which for a variety of reasons are not commercially viable at this time.
  • refractory metal such as molybdenum, tantalum, niobium, tungsten
  • the present invention provides homogeneous titanium base binary alloys containing substantial quantities of refractory molybdenum, preferably high molybdenum-containing titanium base master alloys used for subsequent alloying with titanium and other metals to form a final titanium base alloy.
  • molybdenum, in powdered form preferably, pure molybdenum metal powder
  • titanium, in powdered form, preferably pure titanium metal powder is intimately mixed in appropriate proportions with titanium, in powdered form, preferably pure titanium metal powder.
  • the powder mixture is then pressed into a compact or briquette with application of pressures over about 7000 psi (490 kg/cm 2 ) and preferably between about 15000 and 30000 psi (1055 kg/cm 2 to 2110 kg/cm 2 ).
  • Usually such compacts are formed in an isostatic press and within cylindrical rubber bags of approximately 12 inches (30,5 cm) in diameter and 32 inches (81 cm) in height.
  • the compacts are preferably formed in the shape of discs weighing between about 4,5 kg to 22,7 kg.
  • the compacts are then stacked, one on top of the other, typically in a staggered overlapping array, in a furnace preferably having a controlled atmosphere, for example, a vacuum furnace with internal resistive heating elements or a vacuum induction furnace.
  • a furnace preferably having a controlled atmosphere, for example, a vacuum furnace with internal resistive heating elements or a vacuum induction furnace.
  • spacers can be made from rubber.
  • the spacers are constructed, typically with raised ridges on one side, so as to form grooves or scores in the compacts which facilitate subsequent breaking into pieces after alloying.
  • the stacked compacts are alloyed by a "solid state fusion" reaction which occurs substantially in a solid state. It is believed that the compaction of the metal powders under pressure results in a high degree of intermingling of the grain boundary layers of the individual elements, somewhat akin to melting conditions, and thus when exposed to elevated temperatures, but below the individual element melting points, the compacted charge unexpected goes into solid solution and forms an alloy substantially free of inclusions of the refractory metal.
  • the stacked compacts are preferably placed in the furnace under vacuum or inert gas, such as argon. It is preferred that the furnace is heated to between about 250°C and 350°C, typically about 300°C, while under vacuum to drive off any retained moisture and gases and held at that temperature until the furnace vessel and compacts reach equilibrium. At such point argon or other inert gases can, if desired, be introduced into the furnace, preferably introduced to a pressure of between about 5 psi and 15 psi (0,35 kg/cm 2 to 1,05 kg/cm 2 ).
  • the temperature is then increased to between about 800°C and 1400°C, typically about 900°C for Mo/Ti, and held until equilibrium is reached within the compacts, actual time is dependent on size of load, during which time solid state alloying occurs.
  • the alloying temperature and time will depend on the optimal solid state fusion temperature of the compact. No special pressure conditions are required for the alloying, which is usually carried out either in a vacuum or at about or slightly above atmospheric pressure.
  • the fused compacts are allowed to cool to ambient temperature, preferably also under vacuum or inert gas, such as argon. Once cooled the fused compacts can be further processed, such as size reduced into broken pieces, typically by crushing, milling, grinding or otherwise comminuting, to form a powdered master alloy.
  • the powdered master alloy can then be mixed with other alloying components, such as titanium, to form another charge and then subsequently alloyed to yield a final titanium base alloy.
  • the titanium-molybdenum binary master alloy produced comprises about 50% molybdenum, and the balance being titanium. In another embodiment, the titanium-molybdenum binary master alloy produced comprises between about 10% and 90% molybdenum, and the balance being titanium. In yet another embodiment, the titanium-molybdenum binary master alloy produced comprises between about 45 and 55% molybdenum, and the balance being titanium.
  • the master alloy composition contain low gas impurities, that is, less than 0,5% oxygen, 0,2% nitrogen, and 0,1% hydrogen.
  • Other impurities must be as low as possible and are directly dependent on raw material purity.
  • the titanium-molybdenum master alloy produced thereby will be substantially homogeneous and molybdenum inclusions in the ingot will predominately not be present.
  • a titanium base master alloy containing about 50% by weight molybdenum, the balance being titanium was prepared by the following process:
  • FIGURES 1, 1a and 2 represent the structural and compositional analysis of the master alloy produced in EXAMPLE 1.
  • the represented master alloy being substantially homogenous.
  • Example 2 was a scaled up repeat of Example 1 using 250 lbs. (113,4 kg) of molybdenum powder and 250 lbs. (113,4 kg) of Titanium powder.
  • the compositional analysis is provided below. (Table 2) RAI ANALYSIS VIM3-002 Element Weight % Mo 50,08 Ti 49,19 Al 0,01 C 0,027 H 0,002 Fe 0,041 N 0,130 O 0,243 S 0,001 W 0,0003
  • a titanium based master alloy containing approximately 50% Ta and 50% Ti was prepared by the following process. About 5 pounds (2,27 kg) of Ta powder was intimately mixed with about 5 pounds (2,27 kg) of Ti powder for about 15 minutes to form a powdered charge. The powdered charge was then packed into a cylindrical rubber bag (23 x 66 cm) with scored rubber spacers about every 20 lbs. (9 kg) apart and compacted at 25000 psi. (1760 kg/cm 2 ) in an isostatic press to form 5 compacted discs weighing about 20 lbs. (9 kg) each disc. The compacted discs were then loaded in a vacuum furnace, stacked one on top of each other and were heated to about 1400°C for several hours and then allowed to cool to ambient temperature.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
EP97105999A 1996-04-12 1997-04-11 Préparation d'un alliage-mère titane-molybdène Withdrawn EP0801138A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US63124496A 1996-04-12 1996-04-12
US631244 1996-04-12

Publications (2)

Publication Number Publication Date
EP0801138A2 true EP0801138A2 (fr) 1997-10-15
EP0801138A3 EP0801138A3 (fr) 1998-05-27

Family

ID=24530373

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97105999A Withdrawn EP0801138A3 (fr) 1996-04-12 1997-04-11 Préparation d'un alliage-mère titane-molybdène

Country Status (2)

Country Link
EP (1) EP0801138A3 (fr)
JP (1) JPH1046269A (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010018303A1 (de) * 2010-04-23 2011-10-27 W.C. Heraeus Gmbh Schmelzverfahren zur Herstellung einer einschlussfreien Ta-Basislegierung
US8394170B2 (en) 2009-12-02 2013-03-12 W. C. Heraeus Gmbh Use of powder-metallurgical pre-material for producing an NB alloy that is free of inclusions
US8414679B2 (en) 2009-08-06 2013-04-09 W. C. Heraeus Gmbh Producing an alloy with a powder metallurgical pre-material
CN110551919A (zh) * 2019-09-23 2019-12-10 西安赛特金属材料开发有限公司 钛钼合金的制备方法
CN113462904A (zh) * 2021-07-22 2021-10-01 西安汉唐分析检测有限公司 一种高Mo含量Ti-Mo合金真空自耗电极棒的压制方法
CN114855052A (zh) * 2022-05-13 2022-08-05 赵克中 一种钼-钛基合金材料及其制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4754415B2 (ja) * 2005-07-29 2011-08-24 東邦チタニウム株式会社 チタン合金の製造方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB788245A (en) * 1955-08-05 1957-12-23 Ass Elect Ind Improved alloys of titanium or zirconium intended for drawing into wire
US3645727A (en) * 1969-10-28 1972-02-29 Crucible Inc Method for melting titanium alloys
GB2155957A (en) * 1984-03-16 1985-10-02 Elektrometallurgie Gmbh Process and pre-alloy for production of titanium alloy
GB2155955A (en) * 1984-03-16 1985-10-02 Elektrometallurgie Gmbh Process and pre-alloy for production of titanium alloy
GB2155956A (en) * 1984-03-16 1985-10-02 Elektrometallurgie Gmbh Process and pre-alloy for production of titanium alloy
GB2182676A (en) * 1985-11-06 1987-05-20 Elektrometallurgie Gmbh Master alloy for titanium-based alloys

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB788245A (en) * 1955-08-05 1957-12-23 Ass Elect Ind Improved alloys of titanium or zirconium intended for drawing into wire
US3645727A (en) * 1969-10-28 1972-02-29 Crucible Inc Method for melting titanium alloys
GB2155957A (en) * 1984-03-16 1985-10-02 Elektrometallurgie Gmbh Process and pre-alloy for production of titanium alloy
GB2155955A (en) * 1984-03-16 1985-10-02 Elektrometallurgie Gmbh Process and pre-alloy for production of titanium alloy
GB2155956A (en) * 1984-03-16 1985-10-02 Elektrometallurgie Gmbh Process and pre-alloy for production of titanium alloy
GB2182676A (en) * 1985-11-06 1987-05-20 Elektrometallurgie Gmbh Master alloy for titanium-based alloys

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8414679B2 (en) 2009-08-06 2013-04-09 W. C. Heraeus Gmbh Producing an alloy with a powder metallurgical pre-material
US8394170B2 (en) 2009-12-02 2013-03-12 W. C. Heraeus Gmbh Use of powder-metallurgical pre-material for producing an NB alloy that is free of inclusions
US8778262B2 (en) 2009-12-02 2014-07-15 Heraeus Precious Metals Gmbh & Co. Kg Alloy having reduced inclusions
DE102010018303A1 (de) * 2010-04-23 2011-10-27 W.C. Heraeus Gmbh Schmelzverfahren zur Herstellung einer einschlussfreien Ta-Basislegierung
US8636825B2 (en) 2010-04-23 2014-01-28 W. C. Heraeus Gmbh Melting method for producing an inclusion-free Ta-base alloy
DE102010018303B4 (de) * 2010-04-23 2015-02-12 Heraeus Precious Metals Gmbh & Co. Kg Schmelzverfahren zur Herstellung einer einschlussfreien Ta-Basislegierung für eine implantierbare medizinische Vorrichtung
CN110551919A (zh) * 2019-09-23 2019-12-10 西安赛特金属材料开发有限公司 钛钼合金的制备方法
CN113462904A (zh) * 2021-07-22 2021-10-01 西安汉唐分析检测有限公司 一种高Mo含量Ti-Mo合金真空自耗电极棒的压制方法
CN113462904B (zh) * 2021-07-22 2022-12-09 西安汉唐分析检测有限公司 一种高Mo含量Ti-Mo合金真空自耗电极棒的压制方法
CN114855052A (zh) * 2022-05-13 2022-08-05 赵克中 一种钼-钛基合金材料及其制备方法

Also Published As

Publication number Publication date
JPH1046269A (ja) 1998-02-17
EP0801138A3 (fr) 1998-05-27

Similar Documents

Publication Publication Date Title
RU2572928C2 (ru) Порошковая смесь для получения титанового сплава, титановый сплав, полученный из такой смеси, и способы их получения
US4373947A (en) Process for the preparation of alloy powders which can be sintered and which are based on titanium
EP0244949B1 (fr) Préparation d'un alliage d'aluminium contenant un carbure stable par alliage mécanique
JP4894008B2 (ja) ＭｏＮｂ系焼結スパッタリングターゲット材の製造方法
EP1652945B1 (fr) Feuille en niobium ou en tantale recristallisée à grains fins à teneur en silicium, procédée par fondre suivi d'un procédé thermoméchanique
EP0801138A2 (fr) Préparation d'un alliage-mère titane-molybdène
US4595413A (en) Group IVb transition metal based metal and processes for the production thereof
US5422069A (en) Master alloys for beta 21S titanium-based alloys and method of making same
EP0577116A1 (fr) Procédé pour la fabrication d'un matériau composite, constitué par une matrice de beta aluminiure de titane avec une dispersion de diborure de titane comme élément de renforcement
JP2782665B2 (ja) チタンまたはチタン合金粉末の製造方法
US4655825A (en) Metal powder and sponge and processes for the production thereof
US5124122A (en) Titanium alloy containing prealloyed vanadium and chromium alloy
JP2821662B2 (ja) チタン系粉末およびその製造方法
JPS5935642A (ja) Ｍｏ合金インゴツトの製造方法
US5364587A (en) Nickel alloy for hydrogen battery electrodes
US5236661A (en) Chromium-based weld material
JP3625928B2 (ja) Ｔａ／Ｓｉ系焼結合金の製造方法
US5126106A (en) Chromium-based weld material and rolled article and process for producing the rolled article
US5209790A (en) Production of Ti-V-Cr homogeneous alloy without vanadium inclusions
WO1986000610A1 (fr) Metal a base de metaux de transition de groupe ivb et ses procedes de production
JP2668621B2 (ja) チタン系複合粉体の製造方法
Arunachalam Critical Review Powder Metallurgy of Titanium
JPS6364507B2 (fr)
EP0309479A1 (fr) Poudre et eponge metalliques et leurs procedes de production
AU3109484A (en) Group ivb transition metal based metal and processes for the production thereof

Legal Events

Date Code Title Description
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

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

AX Request for extension of the european patent

Free format text: AL PAYMENT 970509;LT PAYMENT 970509;LV PAYMENT 970509;SI PAYMENT 970509

PUAL Search report despatched

Free format text: ORIGINAL CODE: 0009013

AK Designated contracting states

Kind code of ref document: A3

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

AX Request for extension of the european patent

Free format text: AL PAYMENT 970509;LT PAYMENT 970509;LV PAYMENT 970509;SI PAYMENT 970509

17P Request for examination filed

Effective date: 19981116

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 19991001