WO2013086010A1 - Procédé d'amélioration de la résistance mécanique d'un alliage de titane par vieillissement - Google Patents

Procédé d'amélioration de la résistance mécanique d'un alliage de titane par vieillissement Download PDF

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Publication number
WO2013086010A1
WO2013086010A1 PCT/US2012/067969 US2012067969W WO2013086010A1 WO 2013086010 A1 WO2013086010 A1 WO 2013086010A1 US 2012067969 W US2012067969 W US 2012067969W WO 2013086010 A1 WO2013086010 A1 WO 2013086010A1
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WIPO (PCT)
Prior art keywords
article
aging
alloy
titanium
phase
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Application number
PCT/US2012/067969
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English (en)
Inventor
Chien-Ping Ju
Jiin-Huey Chern Lin
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Chien-Ping Ju
Jiin-Huey Chern Lin
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Application filed by Chien-Ping Ju, Jiin-Huey Chern Lin filed Critical Chien-Ping Ju
Publication of WO2013086010A1 publication Critical patent/WO2013086010A1/fr

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    • 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
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium

Definitions

  • the present invention is related to a method for enhancing mechanical properties of a titanium-molybdenum alloy having a" phase as a major phase by aging, and in particular to a method for enhancing mechanical properties of a medical implant of a titanium-molybdenum alloy by aging .
  • Titanium and titanium alloys have been popularly used in many medical applications due to their light weight, excellent mechanical performance and corrosion resistance.
  • the relatively low strength commercially pure titanium c.p. Ti
  • Other examples for use of commercially pure titanium include pacemaker case, heart valve cage and reconstruction devices.
  • c.p. Ti may not be used for high load-bearing applications.
  • Ti-6AI-4V alloy the "work-horse” titanium alloy. With a much higher strength than c.p. Ti, Ti-6AI-4V alloy has been widely used in a variety of stress-bearing orthopedic applications, such as hip prosthesis and artificial knee joint.
  • the lower elastic modulus allows the titanium/titanium alloy to more closely approximate the stiffness of bone for use in orthopedic devices compared to alternative stainless steel and cobalt-chrome alloys in orthopedic implants.
  • devices formed from the titanium alloy produce less bone stress shielding and consequently interfere less with bone viability.
  • US 6,726,787 B2 provides a process for making a biocompatible low modulus high strength medical device from a titanium alloy, which comprises preparing a titanium alloy having a composition consisting essentially of at least one isomorphous beta stabilizing element selected from the group consisting of Mo, Nb, Ta and W; and the balance Ti, wherein said composition has a Mo equivalent value from about 6 to about 9; casting or metal working the titanium alloy to form a work piece; and quenching the work piece which is the resulting hot cast having a temperature higher than 800°C at a cooling rate greater than 1 0°C per second, or heating the work piece resulted from said metal working to a temperature higher than 800°C and quenching the work piece having a temperature higher than 800°C at a cooling rate greater than 1 0°C per second, so that the cooled work piece contains an a" phase as a major phase, and can be used as a medical device which is biocompatible, and has a low modulus and high strength .
  • a typical quenching method used in the process of the present application is water quenching; however, any methods known in the art which have a cooling rate greater than 1 0°C, preferably 20°C, per second, can also be used .
  • One disadvantage for an a" phase titanium alloy is that the alloy generally has a relatively low strength (e.g ., compared to Ti-6AI-4V ELI).
  • a primary objective of the present invention is to provide an article made of a titanium-molybdenum alloy with enhanced mechanical properties.
  • Another primary objective of the present invention is to provide a method for enhancing mechanical properties of a titanium-molybdenum alloy having a" phase as a major phase by aging .
  • a method for enhancing mechanical properties of a titanium-molybdenum alloy having a" phase as a major phase by aging disclosed in the present invention comprises providing an article of a titanium-molybdenum alloy having a" phase as a major phase;
  • the yield strength of said aged article is increased by at least 20%, preferably at least 50%, and more preferably at least 75%, based on the yield strength of said article, with elongation to failure of said aged article being not less than about 7.0%.
  • the titanium-molybdenum alloy consists essentially of 7-9 wt% of molybdenum and the balance titanium . More preferably, the
  • titanium-molybdenum alloy consists essentially of about 7.5 wt% of
  • the article provided is an as-cast article.
  • the article provided is a hot-worked or cold-worked article.
  • the article provided is a solution-treated article.
  • the article provided is a hot-worked and then
  • the article provided is a cold-worked and then
  • the article provided is a
  • the article provided is an as-cast
  • said aging is conducted at a temperature of 150-850°C, more preferably 200-800°C, and most preferably 250-750°C.
  • said aging is conducted for a period of time depending on the temperature as follows:
  • 450°C > 1 m; preferably >3 m; more preferably >3 m and ⁇ 960 m; most preferably >3 m and ⁇ 480 m;
  • 500°C >30 m; preferably > 60 m; more preferably >1 20 m;
  • 550°C >1 5 m; preferably > 30 m; more preferably >60 m;
  • 650°C >1 m; preferably > 5 m; more preferably >1 5 m;
  • the strength of a" phase Ti alloys can be dramatically increased while other important properties (e.g ., a reasonable elongation) of the alloys are maintained .
  • the a" phase Ti-7.5Mo alloy samples for aging treatment may be prepared from directly casting the alloy into a mold from the molten state, from solution-treating (heated to beta-phase regime) a cast alloy followed by fast cooling, e.g., water quenching, or from solution-treating a mechanically or thermomechanically worked (e.g., through rolling, drawing, forging, extrusion, etc. at a room temperature or a high temperature) alloy followed by fast cooling, e.g.
  • the aging treatment can also be directly conducted on a mechanically or thermomechanically worked (e.g., through rolling, drawing, forging, extrusion, etc. at a room temperature or a high temperature) alloy followed by water quenching without first solution-treating said alloy.
  • a mechanically or thermomechanically worked e.g., through rolling, drawing, forging, extrusion, etc. at a room temperature or a high temperature
  • A aged (Note: Aging was carried out in a quartz tube, which had been evacuated, followed by purging with inert (argon) gas. All aged samples were air-cooled to room temperature from the aging temperature.)
  • the various Ti alloys were prepared from grade-2 commercially pure titanium (c.p. Ti) bars (Northwest Institute for Non-ferrous Metal Research, China) and molybdenum wire of 99.95% purity (Alfa Aesar, USA) by using a commercial arc-melting vacuum-pressure type casting system (Castmatic, Iwatani Corp., Japan). Prior to melting/casting, the melting chamber was evacuated and purged with argon . An argon pressure of 1 .5 kgf/cm2 was maintained during melting . Appropriate amounts of metals were melted in a U-shaped copper hearth with a tungsten electrode. The ingots were re-melted at least three times to improve chemical homogeneity of the alloys. After each melting/casting, the alloys were pickled using H NO3/HF (3: 1 ) solution to remove surface oxide.
  • H NO3/HF 3: 1
  • X-ray diffraction (XRD) for phase analysis was conducted using a Rigaku diffractometer (Rigaku D-max 11 IV, Rigaku Co., Tokyo, Japan) operated at 30 kV and 20 mA with a scanning speed of 3 min .
  • XRD X-ray diffraction
  • Ni-filtered CuKa radiation was used for the study.
  • a silicon standard was used for the calibration of diffraction angles.
  • the various phases were identified by matching each characteristic peak in the diffraction patterns with JCPDS files.
  • a servo-hydraulic type testing machine (EHF-EG, Shimadzu Co., Tokyo, Japan) was used for tensile tests.
  • the tensile testing was performed at room temperature at a constant crosshead speed of 8.33x 1 0-6 m s-1 .
  • the average ultimate tensile strength (UTS), yield strength (YS) at 0.2% offset, modulus of elasticity (Modulus) and elongation to failure (Elongation) were taken from five tests under each process condition .
  • Cold rolling (rolling conducted at room temperature)
  • AC-A (650°C/15m) 921 1037 120 13.4
  • AC-A (650°C/30m) 927 1035 118 12.2
  • Aging treatment can sign ificantly increase the strength level of Ti-7.5Mo alloy.
  • the YS and UTS values of Ti-7.5Mo samplecoded "AC-A(450°C/30m)” are higher than those of Ti-6AI-4V(ELI)(ASTM F136) by 22% and 32%, respectively.
  • the YS and UTS values of Ti-7.5Mo sample coded "AC-A(600°C/480m)” are higher than those of Ti-6AI-4V(ELI)(ASTM F1 36) by 30% and 32%, respectively.
  • a mild aging treatment (with a temperature lower than about 250°C and time less than about 30m) can significantly increase the strength level while maintaining low modulus and reasonable elongation values of the alloy.
  • the YS and UTS values of Ti-7.5Mo sample coded "ST-CR 50%-A (200°C/1 5m)" are higher than those of Ti-6AI-4V (ELI) (ASTM F1 36) by 27% and 39%, respectively, while maintaining an elongation higher than Ti-6AI-4V(ELI) (ASTM F1 36) by 46% and a modulus lower than Ti-6AI-4V (ELI) (ASTM
  • the best aging temperature range 1 50-850°C; preferably 200-800°C; more preferably 250-750°C;
  • 450°C > 1 m; preferably >3 m; more preferably >3 m and ⁇ 960 m; most preferably >3 m and ⁇ 480 m;
  • 500°C >30 m; preferably > 60 m; more preferably >1 20 m;
  • 550°C >1 5 m; preferably > 30 m; more preferably >60 m;
  • 650°C >1 m; preferably > 5 m; more preferably >1 5 m;

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials For Medical Uses (AREA)

Abstract

L'invention concerne un alliage de titane et de molybdène présentant une phase α" en tant que phase principale, soumis à un traitement de vieillissement, de sorte que la limite d'élasticité de l'alliage vieilli est augmentée de 10 % à 120 %, l'allongement dudit alliage jusqu'à sa rupture n'étant pas inférieur à environ 5,0 %.
PCT/US2012/067969 2011-12-06 2012-12-05 Procédé d'amélioration de la résistance mécanique d'un alliage de titane par vieillissement WO2013086010A1 (fr)

Applications Claiming Priority (2)

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US201161567170P 2011-12-06 2011-12-06
US61/567,170 2011-12-06

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WO2013086010A1 true WO2013086010A1 (fr) 2013-06-13

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US (1) US20130139933A1 (fr)
TW (1) TW201331380A (fr)
WO (1) WO2013086010A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109371347A (zh) * 2018-12-11 2019-02-22 陕西宏远航空锻造有限责任公司 一种Ti-6242钛合金三态组织锻件的制备方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11111571B2 (en) 2016-11-14 2021-09-07 Fort Wayne Metals Research Products Ni-free beta Ti alloys with shape memory and super-elastic properties
CN115896497B (zh) * 2022-11-21 2024-08-13 西安圣泰金属材料有限公司 一种弹性模量自调节固溶态Ti-xCr合金棒的制备方法及Ti-xCr合金棒

Citations (5)

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Publication number Priority date Publication date Assignee Title
US5281285A (en) * 1992-06-29 1994-01-25 General Electric Company Tri-titanium aluminide alloys having improved combination of strength and ductility and processing method therefor
US5906692A (en) * 1993-12-28 1999-05-25 Alliedsignal Inc. Process for producing forged α-2 based titanium aluminides having fine grained and orthorhombic transformed microstructure and articles made therefrom
US5954724A (en) * 1997-03-27 1999-09-21 Davidson; James A. Titanium molybdenum hafnium alloys for medical implants and devices
US6726787B2 (en) * 1999-01-07 2004-04-27 Jiin-Huey Chern Lin Process for making a work piece having a major phase of α from a titanium alloy
US20050161130A1 (en) * 2002-04-04 2005-07-28 Toyonobu Tanaka Super-elastic titanium alloy for medical uses

Family Cites Families (4)

* Cited by examiner, † Cited by third party
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US4799975A (en) * 1986-10-07 1989-01-24 Nippon Kokan Kabushiki Kaisha Method for producing beta type titanium alloy materials having excellent strength and elongation
US5169597A (en) * 1989-12-21 1992-12-08 Davidson James A Biocompatible low modulus titanium alloy for medical implants
US5698050A (en) * 1994-11-15 1997-12-16 Rockwell International Corporation Method for processing-microstructure-property optimization of α-β beta titanium alloys to obtain simultaneous improvements in mechanical properties and fracture resistance
US6409852B1 (en) * 1999-01-07 2002-06-25 Jiin-Huey Chern Biocompatible low modulus titanium alloy for medical implant

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5281285A (en) * 1992-06-29 1994-01-25 General Electric Company Tri-titanium aluminide alloys having improved combination of strength and ductility and processing method therefor
US5906692A (en) * 1993-12-28 1999-05-25 Alliedsignal Inc. Process for producing forged α-2 based titanium aluminides having fine grained and orthorhombic transformed microstructure and articles made therefrom
US5954724A (en) * 1997-03-27 1999-09-21 Davidson; James A. Titanium molybdenum hafnium alloys for medical implants and devices
US6726787B2 (en) * 1999-01-07 2004-04-27 Jiin-Huey Chern Lin Process for making a work piece having a major phase of α from a titanium alloy
US20050161130A1 (en) * 2002-04-04 2005-07-28 Toyonobu Tanaka Super-elastic titanium alloy for medical uses

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109371347A (zh) * 2018-12-11 2019-02-22 陕西宏远航空锻造有限责任公司 一种Ti-6242钛合金三态组织锻件的制备方法

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US20130139933A1 (en) 2013-06-06

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