US20100180991A1 - Titanium alloy heat treatment process, and part thus obtained - Google Patents

Titanium alloy heat treatment process, and part thus obtained Download PDF

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Publication number
US20100180991A1
US20100180991A1 US12/646,679 US64667909A US2010180991A1 US 20100180991 A1 US20100180991 A1 US 20100180991A1 US 64667909 A US64667909 A US 64667909A US 2010180991 A1 US2010180991 A1 US 2010180991A1
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stage
temperature
alloy
titanium alloy
heat treatment
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Philippe Heritier
Laurent Cluzel
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Aubert and Duval SA
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Aubert and Duval SA
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    • 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
    • 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

Definitions

  • the present invention relates to a Ti 5-5-5-3 titanium alloy (meaning 5% aluminum, 5% vanadium, 5% molybdenum, 3% chromium on a titanium base) and more particularly a heat treatment for said alloy, the object of which is to improve the standard and uniformity of its mechanical properties.
  • the Ti 5-5-5-3 alloy is a quasi-beta type titanium alloy which at ambient temperature, has two phases, an alpha phase (hereinafter “ ⁇ ”) and a beta phase (hereinafter “ ⁇ ”), and which has a ⁇ transition (hereinafter “ ⁇ -transus”) between a domain where the ⁇ and ⁇ phases coexist and the pure ⁇ phase domain.
  • ⁇ alpha phase
  • ⁇ beta phase
  • ⁇ -transus ⁇ transition
  • the temperature at which the ⁇ -transus is found varies between 840° C. and 860° C. depending on the composition of the Ti 5-5-5-3 alloy.
  • the Ti 5-5-5-3 alloy has both low density and high mechanical strength. This is why it is highly prized in applications in the aeronautical field, for example to produce landing gear parts and structural parts. However, this alloy is very sensitive to microstructural flaws. Parts made of Ti 5-5-5-3 are usually obtained after thermomechanical transformation steps followed by heat treatment steps.
  • thermomechanical transformation steps are carried out in the beta phase domain, in other words at temperatures which are higher than the ⁇ -transus temperature of the alloy and at which the beta phase grains form the matrix of the alloy, then in the alpha-beta phase domain, in other words at temperatures which are lower than the ⁇ -transus temperature of the alloy.
  • the half-finished products obtained after the thermomechanical transformation steps have, at ambient temperature, a microstructure comprising primary alpha phase in the form of globular particles and elongated particles, secondary alpha phase in the form of lamellar particles, and beta phase.
  • the primary alpha phase represents 10 to 30% of the structure.
  • this percentage is measured by optical micrograph image analysis: the extent of the area occupied by said phase on the micrograph is measured by comparison with a reference grid.
  • the parts made of Ti 5-5-5-3 alloy are subjected to conventional heat treatments to obtain the desired mechanical properties.
  • a common heat treatment of the Ti 5-5-5-3 alloy consists of carrying out in succession:
  • the dispersion of the mechanical properties of parts made of Ti 5-5-5-3 alloy obtained after conventional heat treatments is due to heterogeneity of the microstructure of the alloy, which itself is the result of the initial texture of the alloy following the thermomechanical transformation steps.
  • the Ti 5-5-5-3 alloy has a heterogeneous alpha phase distribution within the microstructure.
  • the alpha phase appears in the form of particles elongated in a dominant orientation resulting from the forging or rolling direction during the last thermomechanical transformations. This dominant orientation of the alpha phase particles leads to mechanical properties which, measured in a direction parallel to that of the alpha particles, are acceptable, but which are very inadequate in a direction transverse to that of the alpha particles.
  • the object of the invention is to improve the standard and uniformity of the mechanical properties of a part made of Ti 5-5-5-3 alloy while avoiding the above-mentioned drawbacks of the prior art.
  • the invention relates to a heat treatment process for the Ti 5-5-5-3 titanium alloy, which has the following composition, in weight percent:
  • the heat treatment process according to the invention comprises the following successive steps:
  • the above-mentioned heat treatment stages are carried out at temperatures below the ⁇ -transus temperature of the Ti 5-5-5-3 alloy.
  • the microstructure of the alloy after the thermomechanical transformations is heterogeneous.
  • the first stage according to the invention allows the microstructure of the alloy which has been affected by the preceding thermomechanical transformations to be homogenised.
  • the first stage temperature is slightly lower than the ⁇ -transus temperature of the Ti 5-5-5-3 alloy, so as to solution treat as much alpha phase as possible without however eliminating this phase which remains necessary to avoid an excessive increase in the size of the grain.
  • the beta phase grains would grow uncontrollably leading to a significant reduction in the mechanical properties, particularly tensile strength.
  • the temperature and duration of the first stage are determined so as to obtain a quantity of alpha phase of between 2 and 5% at the end of the first stage.
  • the second stage according to the invention is defined so as to precipitate an equiaxial globular primary alpha phase. Because of the first stage in which the microstructure of the alloy was homogenised, the new alpha phase nuclei appear in a homogeneous distribution in the microstructure of the alloy and their growth occurs equiaxially during the second stage to form globular primary alpha phase particles.
  • the microstructure of the alloy is homogeneous and the first two heat stages carried out according to the invention have allowed a homogeneous globularisation of the primary alpha phase within the microstructure and an adequate proportion of said primary alpha phase to be obtained.
  • the Ti 5-5-5-3 alloy has homogeneous and improved mechanical properties (ductility, toughness, tensile strength and resistance to fatigue). More specifically, the presence of homogeneously distributed globular primary alpha phase markedly improves the ductility of the alloy.
  • the inventors have been able to demonstrate that the compromise between the tensile strength and ductility of the alloy was optimal when the quantity of globular primary alpha phase at the end of the second stage was between 10 and 15%.
  • the temperature and duration of the second stage of the heat treatment according to the invention are therefore preferably determined to obtain a quantity of globular primary alpha phase at the end of the second stage of between 10 and 15% in a beta phase matrix.
  • the temperature of the second stage is between 770° C. and 790° C.
  • the first stage is preferably carried out at a temperature between the ⁇ -transus temperature less 20° C. and the ⁇ -transus temperature less 30° C. and the second stage is carried out at a temperature of between 770 and 790° C.
  • the first and second stages are preferably performed successively.
  • the cooling speed between the first stage and the second stage is preferably between 1.5° C. and 5° C. per minute, and cooling at the end of the second stage is carried out to ambient temperature at a speed of between 5° C. and 150° C. per minute.
  • the third stage is known as ageing as is standard practice for this type of alloy.
  • the titanium alloy is maintained at the temperature of the third stage for six to ten hours, preferably about eight hours.
  • the invention also relates to a part made of Ti 5-5-5-3 alloy, characterised in that it has been obtained from a half-finished product obtained by the above heat treatment process.
  • FIG. 1 is a micrograph of the Ti 5-5-5-3 alloy that has undergone conventional heat treatment before ageing
  • FIG. 2 shows diagrammatically an example of the three heat treatment stages according to the invention
  • FIG. 3 shows a micrograph of the Ti 5-5-5-3 alloy that has undergone the first and second heat treatment stages according to the invention
  • FIG. 4 shows a micrograph of the above alloy after it has undergone the third heat treatment stage according to the invention.
  • the Ti 5-5-5-3 alloy heat treatment process according to the invention applies to parts that have, as is standard, been shaped following one or more thermomechanical transformation steps performed in the beta phase domain, followed by steps performed in the alpha-beta phase domain. These may be thermomechanical transformation steps through rolling, forging or extrusion.
  • the parts obtained after such thermomechanical transformation steps have, at ambient temperature, a microstructure comprising primary alpha phase in the form of globular particles and elongated particles, secondary alpha phase in the form of lamellar particles, and beta phase.
  • the texture of the alloy is affected (orientation of the different alpha phase morphologies), and the microstructure of the alloy is very heterogeneous.
  • the alpha phase particles are in the form of needles which are distributed in particular in the region of the beta phase grain boundaries.
  • the alpha phase particles may be contiguous and form ribbons which have a detrimental effect on the toughness and resistance to fatigue and ductility of the alloy.
  • the alpha phase particles 1 have heterogeneous sizes and distributions within the microstructure 2 of the alloy.
  • the alpha phase 1 moreover is in the form of elongated particles, oriented in a dominant orientation resulting from the forging or rolling direction during the final thermomechanical transformation steps. This dominant orientation of the alpha phase particles does not allow isotropic mechanical properties to be obtained within the alloy.
  • One of the objects of the heat treatment according to the invention is therefore to homogenise the microstructure of the Ti 5-5-5-3 alloy.
  • the inventors have developed an optimised Ti 5-5-5-3 alloy heat treatment as shown diagrammatically in FIG. 2 , comprising the following steps and stages:
  • the first stage 4 situated between 810° C. and 840° C. and a little lower than the ⁇ -transus temperature of the alloy, according to the invention, allows the microstructure of the alloy affected by the previous thermomechanical transformation steps to be homogenised, and as much alpha phase as possible to be solution treated, without however completely eliminating said alpha phase.
  • the temperature and duration of the first stage 4 are determined to obtain a quantity of alpha phase of between 2 and 5% at the end of the first stage 4 .
  • a minimum content of 2% ensures that the beta phase grains do not grow uncontrollably, which would have the consequence of considerably reducing the mechanical characteristics of the alloy particularly the tensile mechanical properties.
  • an alpha phase content of less than 5% is preferable to allow good homogenisation of the microstructure of the alloy, and in particular to break the alpha phase ribbons which formed following the thermomechanical treatments.
  • the ⁇ -transus temperature varies depending on the exact composition of the Ti 5-5-5-3 alloy.
  • the temperature of the first stage 4 is determined depending on the exact composition of the Ti 5-5-5-3 alloy and its ⁇ -transus temperature.
  • the first stage 4 is carried out at a temperature between the ⁇ -transus temperature less 20° C. and the ⁇ -transus temperature less 30° C., regardless of the Ti 5-5-5-3 composition.
  • the duration of the first stage 4 is between one and three hours and is a function in particular of the geometry and bulk (diameter, thickness) of the part. The bulkier the part, the longer the stage lasts.
  • the second stage 6 is defined to allow the precipitation of globular primary alpha phase. Because of the first stage which allowed a homogeneous structure of the alloy to be obtained, the new alpha phase nuclei appear in the course of the second stage 6 , in a homogeneous distribution in the beta matrix of the alloy, and the growth of the alpha nuclei occurs equiaxially during the second stage 6 to form globular primary alpha phase particles 11 , as shown in FIG. 3 .
  • the microstructure of the alloy is homogeneous and the heat treatment according to the invention allows, moreover, a homogeneous globularisation of the primary alpha phase 11 to be obtained within the microstructure (see the micrograph in FIG. 3 ).
  • the presence of globular primary alpha phase 11 distributed homogeneously in the microstructure 12 of the alloy improves the ductility of the alloy.
  • the double solution treatment by the first two stages of the invention homogenises the microstructure of the alloy and prepares it so that it responds more isotropically to the ageing treatment of the third stage.
  • the mechanical properties within the alloy are perfectly isotropic and improved compared with those conferred by a conventional heat treatment.
  • the inventors have been able to demonstrate that the compromise between the tensile strength and ductility of the alloy was optimal when the quantity of globular primary alpha phase 11 at the end of the second stage 6 was between 10 and 15%.
  • the second stage temperature is between 770° C. and 790° C. to obtain a quantity of globular primary alpha phase of between 10 and 15% at the end of the second stage 6 .
  • the duration of the second stage 6 is between two and five hours and is also a function of the geometry and bulk (diameter, thickness) of the part. The bulkier the part, the longer the stage lasts.
  • the cooling speed 5 between the first stage and the second stage is preferably between 1.5° C. and 5° C. per minute and is, for example, carried out without removing the part from the treatment furnace.
  • the part therefore cools progressively in a controlled manner inside the furnace, the set temperature of which has been lowered progressively or immediately until it reaches the temperature of the second stage 6 .
  • a cooling speed of over 1.5° C./min is preferred to avoid a change occurring in the distribution of primary alpha phase during cooling speeds that are too low which could be detrimental to obtaining good mechanical properties.
  • a cooling speed of more than 5° C./min could lead to the precipitation of needle-type alpha phase which is detrimental to obtaining good mechanical properties such as elongation at rupture.
  • an excess of needle-type alpha phase in the structure of the material increases the risk of brittle fracture.
  • Cooling performed in the open air is not usually advisable, as its speed is difficult to control and, in many cases, the temperature of the part drop too low, requiring reheating to the second stage temperature. Such reheating must be avoided, for the reasons already stated, and cooling inside the furnace is an advantageous solution for implementing the invention. Moreover, carrying out air cooling by removing the part from the furnace requires handling the part at high temperature, which is difficult to perform.
  • the first 4 and second 6 stages are, preferably, carried out successively.
  • This successive performance of the two stages is preferred, thus separating them by a progressive cooling to avoid any change occurring in the primary alpha phase distribution during an intermediate stage, which could be detrimental to obtaining good mechanical properties.
  • the cooling 7 following the second stage 6 is carried out to ambient temperature at a speed preferably of between 5° C. and 150° C. per minute. This is for example air cooling carried out after having removed the part from the treatment furnace.
  • the cooling speed following the second stage should be less than 150° C. per minute to avoid too heterogeneous a hardening between the surface and the core of the part and avoid the risk of contraction cracking (superficial cracking) during cooling.
  • a speed of at least 5° C. per minute is preferable to anticipate a homogeneous response to the subsequent tempering treatment during which hardening precipitation occurs.
  • the third stage 9 is known as the ageing stage as is standard practice for this type of alloy, the object of which is to harden the alloy by alpha phase precipitation.
  • the titanium alloy is maintained at the temperature of the third stage 9 for six to ten hours, preferably about eight hours.
  • the microstructure obtained after this third stage 9 is illustrated in FIG. 4 .
  • the mechanical properties of the Ti 5-5-5-3 alloy are isotropic, and have been improved compared with those of parts made of Ti 5-5-5-3 alloy obtained by conventional heat treatments. Because of the heat treatment according to the invention, it has been possible in particular to improve the tensile strength and ductility of parts made of Ti 5-5-5-3. On the parts tested, Rm values of more than 1290 MPa, elongation values “A” of more than 5% and reduction in area values “Z” of more than 15% have in fact been obtained.
  • the effects of the invention are particularly remarkable on bulky parts, in other words parts with a thickness or diameter of more than 100 mm.

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
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  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Heat Treatment Of Steel (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
US12/646,679 2008-12-24 2009-12-23 Titanium alloy heat treatment process, and part thus obtained Abandoned US20100180991A1 (en)

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US14074808P 2008-12-24 2008-12-24
FR0859071A FR2940319B1 (fr) 2008-12-24 2008-12-24 Procede de traitement thermique d'un alliage de titane, et piece ainsi obtenue
FR0859071 2008-12-24
US12/646,679 US20100180991A1 (en) 2008-12-24 2009-12-23 Titanium alloy heat treatment process, and part thus obtained

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CN (1) CN102317484A (zh)
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FR (1) FR2940319B1 (zh)
RU (1) RU2011130876A (zh)
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Cited By (8)

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US20080078482A1 (en) * 2006-09-28 2008-04-03 Cotton James D Thermal processing method for improved machinability of titanium alloys
EP2546370A1 (en) * 2011-07-13 2013-01-16 FMW Composite Systems, Inc. Method of making high strength-high stiffness beta titanium alloy
CN103237915A (zh) * 2010-09-27 2013-08-07 威森波-阿维斯玛股份公司 近β钛合金的锻造制品的制备方法
US20150080150A1 (en) * 2013-09-16 2015-03-19 O-Ta Precision Industry Co., Ltd. Golf club head and low density alloy thereof
US9972840B2 (en) * 2013-03-29 2018-05-15 Kubota Corporation Titanium oxide compound, and electrode and lithium ion secondary battery each manufactured using same
US10119178B2 (en) 2012-01-12 2018-11-06 Titanium Metals Corporation Titanium alloy with improved properties
KR20180122026A (ko) * 2016-04-25 2018-11-09 아르코닉 인코포레이티드 티타늄, 알루미늄, 니오븀, 바나듐 및 몰리브덴의 bcc 재료, 및 그로부터 제조된 제품
US20230063778A1 (en) * 2021-08-24 2023-03-02 Titanium Metals Corporation Alpha-beta ti alloy with improved high temperature properties

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CN103820743A (zh) * 2012-11-16 2014-05-28 李彬 一种钛基材料的热处理方法
CN105177480B (zh) * 2015-08-28 2017-05-17 西北有色金属研究院 一种热处理制备具有混合组织的bt25y钛合金的方法
CN106521239B (zh) * 2016-11-21 2018-07-20 西北有色金属研究院 一种核反应堆用高冲击韧性低活化钛合金
CN106967938A (zh) * 2017-05-05 2017-07-21 东南大学 一种高强度高塑性钛合金的制备方法
CN107217173A (zh) * 2017-05-27 2017-09-29 中国科学院金属研究所 具有高强高塑和良好断裂韧性的钛合金及其制备工艺
EP3692179A4 (en) * 2017-10-06 2021-09-15 Monash University ENHANCED HEAT-TREATED TITANIUM ALLOY
FR3100821B1 (fr) * 2019-09-16 2021-09-24 Lisi Aerospace Elément de fixation en alliage de titane et procédé de fabrication
CN111826538B (zh) * 2020-07-28 2023-01-24 成都露思特新材料科技有限公司 双态组织的钛合金的制备方法及双态组织的钛合金

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US20070102073A1 (en) * 2004-06-10 2007-05-10 Howmet Corporation Near-beta titanium alloy heat treated casting

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WO2001092589A1 (fr) * 2000-05-29 2001-12-06 Sumitomo Metal Industries, Ltd. Alliage de titane presentant une excellente ductilite, resistance a la fatigue et rigidite et son procede de production
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US20070102073A1 (en) * 2004-06-10 2007-05-10 Howmet Corporation Near-beta titanium alloy heat treated casting

Cited By (15)

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Publication number Priority date Publication date Assignee Title
US8500929B2 (en) * 2006-09-28 2013-08-06 The Boeing Company Thermal processing method for improved machinability of titanium alloys
US20080078482A1 (en) * 2006-09-28 2008-04-03 Cotton James D Thermal processing method for improved machinability of titanium alloys
EP2623628A4 (en) * 2010-09-27 2016-06-29 Public Stock Company Vsmpo Avisma Corp PROCESS FOR MANUFACTURING CONTRAINTS PRODUCED FROM TITANIUM PSEUDO-BETA ALLOYS
CN103237915A (zh) * 2010-09-27 2013-08-07 威森波-阿维斯玛股份公司 近β钛合金的锻造制品的制备方法
US9297059B2 (en) 2010-09-27 2016-03-29 Public Stock Company, “VSMPO-AVISMA Corporation” Method for the manufacture of wrought articles of near-beta titanium alloys
EP2546370A1 (en) * 2011-07-13 2013-01-16 FMW Composite Systems, Inc. Method of making high strength-high stiffness beta titanium alloy
US10119178B2 (en) 2012-01-12 2018-11-06 Titanium Metals Corporation Titanium alloy with improved properties
US9972840B2 (en) * 2013-03-29 2018-05-15 Kubota Corporation Titanium oxide compound, and electrode and lithium ion secondary battery each manufactured using same
US20150080150A1 (en) * 2013-09-16 2015-03-19 O-Ta Precision Industry Co., Ltd. Golf club head and low density alloy thereof
US9750990B2 (en) * 2013-09-16 2017-09-05 O-Ta Precision Industry Co., Ltd. Golf club head and low density alloy thereof
KR20180122026A (ko) * 2016-04-25 2018-11-09 아르코닉 인코포레이티드 티타늄, 알루미늄, 니오븀, 바나듐 및 몰리브덴의 bcc 재료, 및 그로부터 제조된 제품
CN109257932A (zh) * 2016-04-25 2019-01-22 奥科宁克有限公司 钛、铝、铌、钒和钼的bcc材料以及由其制成的产品
EP3449024A4 (en) * 2016-04-25 2019-12-04 Arconic Inc. BCC MATERIALS OF TITANIUM, ALUMINUM, NIOB, VANADIUM AND MOLYBDEN AND PRODUCTS MANUFACTURED THEREFROM
KR102251066B1 (ko) * 2016-04-25 2021-05-11 아르코닉 인코포레이티드 티타늄, 알루미늄, 니오븀, 바나듐 및 몰리브덴의 bcc 재료, 및 그로부터 제조된 제품
US20230063778A1 (en) * 2021-08-24 2023-03-02 Titanium Metals Corporation Alpha-beta ti alloy with improved high temperature properties

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JP2012514129A (ja) 2012-06-21
EP2379760A1 (fr) 2011-10-26
RU2011130876A (ru) 2013-01-27
WO2010072972A1 (fr) 2010-07-01
FR2940319A1 (fr) 2010-06-25
FR2940319B1 (fr) 2011-11-25
CA2748380A1 (fr) 2010-07-01
CN102317484A (zh) 2012-01-11

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