EP1772528B1 - Titanium alloy and method of manufacturing titanium alloy material - Google Patents

Titanium alloy and method of manufacturing titanium alloy material Download PDF

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Publication number
EP1772528B1
EP1772528B1 EP04745513A EP04745513A EP1772528B1 EP 1772528 B1 EP1772528 B1 EP 1772528B1 EP 04745513 A EP04745513 A EP 04745513A EP 04745513 A EP04745513 A EP 04745513A EP 1772528 B1 EP1772528 B1 EP 1772528B1
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EP
European Patent Office
Prior art keywords
titanium alloy
cold
present
cross
reduction rate
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.)
Expired - Lifetime
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EP04745513A
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German (de)
English (en)
French (fr)
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EP1772528A4 (en
EP1772528A1 (en
Inventor
Atsuhiko c/o Sumitomo Metals KURODA
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Nippon Steel Corp
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Nippon Steel and Sumitomo Metal Corp
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Publication of EP1772528A1 publication Critical patent/EP1772528A1/en
Publication of EP1772528A4 publication Critical patent/EP1772528A4/en
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Publication of EP1772528B1 publication Critical patent/EP1772528B1/en
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Classifications

    • 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 relates to titanium alloys in use in chemical industry members such as machine structure members and heat exchanger members and consumer goods members such as golf clubs, and a method for manufacturing titanium alloy materials.
  • the present invention particularly relates to titanium alloys with an excellent cold workability and superplasticity characteristics, and a method for manufacturing the titanium alloy materials.
  • Heat exchangers are instruments capable of transmitting thermal energy between different fluids.
  • the heat exchangers are used in, for example, air conditioners, refrigerators, air preheating equipment of burners, radiators in automobiles, parts for the chemical industry, parts for seawater and the like.
  • heat exchangers made of titanium are used in fields requiring excellent corrosion resistance such as in the chemical industry or in salt water.
  • titanium alloy which are light and strong are used as a material for such heat exchangers.
  • a Ti-6Al-4V alloy has been widely used as the heat exchanger material due to its excellent superplasticity characteristics as described in, for example, Non-patent document 1.
  • this alloy has poor cold workability. For example, when thin plates are manufactured by cold rolling the Ti-6A1-4V alloy plate which is wrapped around a coil, there is a drawback that the number of intermediate annealing needs to be increased.
  • Non-patent document 2 shows that a Ti-9V-2Mo-3Al alloy is a titanium alloy which has an excellent cold workability and also an excellent superplasticity workability.
  • this alloy contains Mo as an essential element, which results in a high cost of raw materials. Also, because of a high melting point of Mo, there is a higher incidence of unmelted portions or solidification segregation in melting.
  • Patent document 1 describes a titanium alloy with excellent superplasticity workability containing, by mass %, A1 of 5.5 to 6.5%, V of 3.5 to 4.5%, O of 0.2% or less, Fe of 0.15 to 3.0%, Cr of 0.15 to 3.0% and Mo of 0.85 to 3.15%, in which Fe, Cr and Mo are within a range represented by a specific equation and an average grain diameter of an ⁇ crystal is 6 ⁇ m or less.
  • This alloy can be said to be superior to the Ti-6AI-4V alloy in the superplasticity workability, but the cold workability is not considered.
  • this alloy has a high content of A1 which is 5.5% or more, which results in high deformation resistance in the cold rolling and a high possibility of cracks occurring in the edges of a plate if this alloy is subjected to cold rolling process at a cross-section reduction rate of 50%.
  • Patent document 2 describes a titanium alloy with excellent workability which contains, by mass %, A1 of 3.0 to 5.0%, V of 2.1 to 3.7%, Mo of 0.85 to 3.15%, O of 0.15% or less, and further one or more elements of Fe, Cr, Ni and Co, in which the content of these elements is in a range represented by a specific equation. There is also described a manufacturing method of a titanium alloy material in a specific hot rolling condition, and a superplastic processing method of the titanium alloy material in the specific heat treatment condition. However, since this alloy contains Mo, there will be the same problem with the alloy described in Non-patent document 2.
  • An object of the present invention is to provide titanium alloys with the excellent cold workability and the superplasticity characteristics and a method for manufacturing the titanium alloy materials. Means adapted to solve the problem
  • the present invention was accomplished as a result of repeated research made by the present inventors based on a Ti-3A1-2.5V alloy which is said to have the excellent cold workability.
  • the present invention is characterized by titanium alloys as shown in (1) below, and a method for manufacturing a titanium alloy material as shown in (2) below.
  • a method for manufacturing cold rolled titanium alloy plate is characterized in that the titanium alloy described in the above (1) is subjected to cold working at a cross-section reduction rate of 40% or more.
  • a titanium alloy of the present invention has a sufficient cold workability as well as the excellent superplasticity characteristics. Therefore, it is possible to easily produce a coil by the cold rolling, and a material for a super-plastic application, having a uniform distribution in a plate thickness, can be manufactured. Therefore, it is possible to easily produce thin plates made of titanium alloy at a low cost, allowing for the expansion of an application field for the titanium alloy thin plates. Best mode for carrying out the invention
  • Al is an element that plays a very important role in increasing the strength of the titanium alloy. Al is also an effective element for stabilizing the ⁇ phase of the titanium alloy.
  • the superplasticity characteristics are exhibited in a temperature range in which the ratio of the a phase and the ⁇ phase is approximately 50/50. If the content of A1 is low, this temperature range is narrowed, which results in difficulties obtaining stable superplasticity characteristics.
  • the content ofAl needs to be 2.0% or more so as to obtain the superplasticity characteristics in a wider temperature range. However, the cold workability reduces as the content ofAl increases.
  • the content of A1 is limited to 2.0 to 4.0%.
  • V is an effective element for stabilizing the ⁇ phase of titanium alloys, and has an effect of increasing the ratio of the ⁇ phase in a temperature range of about 800 to 850 °C.
  • the content of V is 4.0% or more, the temperature range in which the ratio of the ⁇ phase and the B phase is approximately 50/50 can be increased.
  • the content of V exceeds 9.0%, oxidation resistance characteristics of the titanium alloy material are deteriorated. This is because an oxide of V has a sublimation property, so that a scale generated on the surface of the alloy is not dense but has a high permeability of oxygen if the titanium alloy in which the content of V exceeds 9.0% is exposed to a high temperature. Therefore, cracks occur more easily on the surface of the alloy, and a high temperature ductility is decreased. Accordingly, the content of V is limited to 4.0 to 9.0%.
  • Zr is an element that may not be optionally added. If Zr is added, it contributes to strengthen the titanium alloy due to a solid solution strengthening effect thereof. If a titanium alloy containing Zr is exposed to the high temperature, a strong Zr oxide is formed on the surface thereof to suppress oxidation inside the alloy, so that a generation of the cracks can be prevented in a deformation of the titanium alloy at the high temperature. Therefore, elongation of the titanium alloy is increased at the high temperature, and the superplasticity characteristics are improved. These effects are largely exhibited in 0.5% or more. However, Zr is an expensive element, and the oxidation suppression effect described above is saturated if the content of Zr exceeds 2.0%, leading to a cost increase. Therefore, if Zr is contained, the content is preferably limited to 2.0% or less.
  • Sn is also an element that may not be necessarily added. Although Sn does not contributes to stabilize the ⁇ phase or the ⁇ phase, it is an element that contributes to strengthen the titanium alloy To obtain such effect of Sn, the content is preferably 0.2% or more. However, if the content of Sn exceeds 3.0%, a low melting point region is formed in solidification process, and the cracks occur from this region as a starting point. Therefore, if Sn is contained, the content is preferably 3.0% or less.
  • Certain titanium alloys of the present invention have the chemical compositions described above, the balance being Ti and impurities.
  • Other alloys of the invention contain one or more elements selected from Fe of 0.20 to 1.0%, Cr of 0.01 to 1.0%, Cu of 0.01 to 1.0% and Ni of 0.01 to 1.0% as substitute for a part of Ti. This is based on the following reasons.
  • Fe and Cr are elements contained, as impurities, in a titanium sponge which is a titanium raw material, or in an aluminum-vanadium alloy which is an additional material. Therefore, Fe of less than 0.20% and Cr of less than 0.01% are contained in the titanium alloy even if these elements are not positively added. These elements are ⁇ -phase stabilizing elements having the same effect as V, but they are cheaper than V. Accordingly, cost reduction can be realized by positively adding these elements, so that it is desirable to contain Fe of 0.20% or more and Cr of 0.01% or more. However, Fe and Cr are eutectoid type elements forming an intermetallic compound in the titanium alloy. If the Fe and Cr contents exceed 1.0% each, there will be embrittlement caused by excessive precipitation of the intermetallic compound.
  • Cu and Ni are ⁇ stabilizing elements in the same manner as V, and are effective to increase the ratio of the B phase in a temperature range of 800 to 850 °C. These elements are cheaper than V, and can be added as an alternative element to V It is desirable to use Cu at 0.01% or more and Ni at 0.01% or more in order to obtain this effect. However, an intermetallic compound is formed and cold workability is lowered if Cu or Ni exceed 1.0% each, because Cu and Ni are eutectoid type elements for titanium.
  • the ratio of the ⁇ phase is lowered in a temperature range of 800 to 850 °C, and the superplasticity characteristics are hardly exhibited in this temperature range.
  • the Veq exceeds 9.5, the ratio of the ⁇ phase is lowed, the superplasticity characteristics deteriorate in a temperature range of 800 to 850 °C and the specific gravity of the alloy itself increases. Accordingly, if Fe and/or Cr are contained to the titanium alloy of the present invention, it is necessary to limit Veq in a range of 4.0 to 9.5.
  • O (oxygen), C (carbon), N (nitrogen) and H (hydrogen) are major impurities contained in the titanium alloy of the present invention.
  • O is an impurity contained in the titanium sponge and a raw material of V, while C and N are impurities contained in the titanium sponge.
  • H is an impurity which is absorbed from an atmosphere in heating or absorbed in an acid pickling process. Impurities are preferably as low as possible in a range where O is 0.2% or less, C is 0.01% or less, N is 0.01% or less, and H is 0.01% or less.
  • An ingot is prepared by an ordinary melting method such as VAR and is subjected to hot bloom forging or hot rolling so as to form a slab, after which hot rolling is conducted to prepare a hot coil, followed by the cold rolling to a target plate thickness and annealing to provide the titanium alloy material.
  • the cold rolling is a step that largely influences product characteristics, and a titanium alloy material with the excellent superplasticity characteristics at the high temperature can be obtained particularly by the cold working (cold rolling) at the cross-section reduction rate of 40% or more. This is based on the following reasons.
  • a crystal grain diameter in the titanium alloy particularly a grain diameter of a pro-eutectoid ⁇ phase is decreased. Then, if the grain diameter in the titanium alloy is decreased, elongation is increased upon superplastic deformation at the high temperature, thereby the titanium alloy material with the excellent superplasticity characteristics at the high temperature is exhibited.
  • the cross-section reduction rate is increased in the cold rolling, the elongation upon superplastic deformation at the high temperature is sharply increased up to the cross-section reduction rate of about 40%, and less change is observed in a region of 40% or more.
  • the cold working is performed at the cross-section reduction rate of 40% or more.
  • the cross-section reduction rate there is no particular upper limit in the cross-section reduction rate, when the cold rolling is performed at a cross-section reduction rate of exceeding 80%, the edge cracks occur in the edges of the plate. Accordingly, it is desirable in the cold working to limit the cross-section reduction rate in 80% or less.
  • the cold working may be performed in a condition that the cross-section reduction rate exceeds 80%.
  • cross-section reduction rate is obtained by the following equation (a).
  • Cross - section reduction rate % cross - section area before working cross - section area after working / cross - section area before working ⁇ 100
  • a button ingot with a width of 50 mm, a thickness of 15 mm and a longitude of 80 mm was prepared.
  • the button ingot was heated at 850 °C, it was subjected to hot rolling to prepare a hot-rolled plate with a thickness of 5 mm.
  • this hot-rolled plate was annealed at 750 °C for ten minutes, an oxide scale was removed by shot blast and acid pickling, and the surface was further machined to a thickness of 4mm by machining so as to prepare a material for the cold rolling.
  • This material was subjected to the cold rolling to prepare a cold-rolled plate with a thickness of 2 mm.
  • an evaluation of cold-rolling property presence of cracks in the edges on the surface of the cold-rolled plate was performed by visual observation.
  • a plate with no cracks in the cold rolling was subjected to a heat treatment in an argon atmosphere at 700 °C for 30 minutes, followed by cold rolling to a thickness of 1.5 mm, and again subjected to the heat treatment in the argon atmosphere at 700 °C for 30 minutes to provide a test specimen. From this test specimen, a plate type test piece with a thickness of 1.5 mm and a width of 12.5 mm in a parallel part was obtained so that the longitudinal direction of the test piece was in parallel to the rolling direction.
  • the distance between gauge marks of this tensile test piece was set to be 20mm, and a tensile test was conducted at a test temperature of 800 °C and a tensile speed of 9 mm/min., so as to measure elongation at fracture.
  • Table 1 shows chemical compositions of the cold-rolled plate, evaluations of cold rolling property and elongation at fracture.
  • a plate with no cracks is indicated as [ ⁇ ] and a plate with cracks is indicated as [ ⁇ ] when a cold-rolled plate with a thickness of 2 mm was prepared.
  • a plate of exceeding 200% in elongation at fracture is indicated as [ ⁇ ]
  • a plate of 200% or less in elongation at fracture is indicated as [ ⁇ ] when a tensile test was conducted at 800 °C.
  • alloys satisfying the chemical compositions specified in the present invention are capable of being cold rolled to obtain an excellent superplastic elongation.
  • a material for cold rolling containing Al of 3.0%, V of 5.0% and the balance being Ti and impurities was prepared with a thickness of 4 mm in the same manner with Example 1.
  • the material for cold rolling was subjected to a cold rolling in different cross-section reduction rates to prepare cold-rolled plates with thicknesses of 3.5 mm, 3.0 mm, 2.5 mm, 2.0 mm and 1.5 mm. After these cold-rolled plates were subjected to the heat treatment in the argon atmosphere at 700 °C for 30 minutes, a plate type test piece with a thickness of 1.0 mm and a width of 12.5 mm in a parallel part was obtained so that the longitudinal direction of the test piece was in parallel with the rolling direction.
  • the distance between the gauge marks in this tensile test piece was set to 20 mm, and the tensile test was conducted at the test temperature of 800 °C and a tensile speed of 9 mm/min., so as to measure the elongation at fracture.
  • the cold-rolled plate with a thickness of 2.0 mm was subjected to the heat treatment in the argon atmosphere at 700 °C for 30 minutes, followed by the cold rolling to a thickness of 1.5 mm or 1.0 mm, and again subjected to the hot treatment in the argon atmosphere at 700 °C for 30 minutes so as to prepare a test specimen. From this test specimen, the plate type test piece with the thickness of 1.0 mm and the width of 12.5mm in the parallel part was obtained, and the same tensile test as described above was conducted to measure the elongation at fracture. Table 2 shows the cross-section reduction rate and the elongations at fracture.
  • the elongation at fracture is increased in accordance with the increase of the cross-section reduction rate, and there is almost no change in the elongation at fracture under a condition that the cross-section reduction rate is 40% or more. Also, from the results of No. 39 and No. 40, it is understood that an excellent elongation at fracture is observed if the cross-section reduction rate before the intermediate annealing is 40% or more, even though the cold rolling rate after the intermediate annealing is low.
  • the titanium alloy of the present invention has the sufficient cold workability as well as the excellent superplasticity characteristics. Accordingly, it is possible to easily prepare the coil by the cold rolling, and also to manufacture a material for a super-plastic application having a uniform distribution in a plate thickness. Therefore, the titanium alloy thin plates can be easily manufactured at a low cost, allowing the expansion of the application field for the titanium alloy thin plates.

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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)
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EP04745513A 2004-06-02 2004-06-02 Titanium alloy and method of manufacturing titanium alloy material Expired - Lifetime EP1772528B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2004/007614 WO2005118898A1 (ja) 2004-06-02 2004-06-02 チタン合金およびチタン合金材の製造方法

Publications (3)

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EP1772528A1 EP1772528A1 (en) 2007-04-11
EP1772528A4 EP1772528A4 (en) 2008-02-20
EP1772528B1 true EP1772528B1 (en) 2013-01-30

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US (1) US20070131314A1 (zh)
EP (1) EP1772528B1 (zh)
CN (1) CN1954087B (zh)
WO (1) WO2005118898A1 (zh)

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DE102007040132A1 (de) * 2007-08-24 2009-02-26 Gfe Fremat Gmbh Verfahren zur Herstellung von Bändern bzw. Folien aus TiAl6V4
KR101745999B1 (ko) * 2009-06-29 2017-06-12 보르그워너 인코퍼레이티드 내피로성 주조 티타늄 합금 물품
CN102230097B (zh) * 2011-03-31 2012-06-27 西北有色金属研究院 一种钛合金棒材的制备方法
CN104520456A (zh) * 2012-08-10 2015-04-15 新日铁住金株式会社 钛合金材料
CN105779818B (zh) * 2014-12-25 2017-10-10 北京有色金属研究总院 一种高强高韧β型钛合金及其制备方法
CN106319282B (zh) * 2015-06-17 2018-05-25 中国科学院金属研究所 一种低成本、高塑性、耐海水腐蚀钛合金
RU2606677C1 (ru) * 2015-09-24 2017-01-10 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") Сплав на основе титана (варианты) и изделие, выполненное из него
CN105668886B (zh) * 2016-04-16 2018-04-06 黄其江 轻质小型海水淡化装置
CN107779670B (zh) * 2017-11-23 2020-12-29 中国航发北京航空材料研究院 一种高精度钛合金板材及其制备方法
CN107779669B (zh) * 2017-11-23 2020-09-22 中国航发北京航空材料研究院 一种用于加工压力管材的钛合金及其制备方法
US10913991B2 (en) 2018-04-04 2021-02-09 Ati Properties Llc High temperature titanium alloys
US11001909B2 (en) * 2018-05-07 2021-05-11 Ati Properties Llc High strength titanium alloys
CN108893630B (zh) * 2018-08-03 2019-08-02 燕山大学 一种高强耐腐蚀钛合金及其制备方法
CN108950302B (zh) * 2018-08-03 2019-08-02 中鼎特金秦皇岛科技股份有限公司 一种高强耐腐蚀钛合金及其制备方法
US11268179B2 (en) 2018-08-28 2022-03-08 Ati Properties Llc Creep resistant titanium alloys
CN109082561A (zh) * 2018-09-27 2018-12-25 燕山大学 一种高塑性钛合金及其制备方法

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CN1954087B (zh) 2010-04-14
WO2005118898A1 (ja) 2005-12-15
CN1954087A (zh) 2007-04-25
US20070131314A1 (en) 2007-06-14
EP1772528A4 (en) 2008-02-20
EP1772528A1 (en) 2007-04-11

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