EP1066415B1 - Two phase titanium aluminide alloy - Google Patents

Two phase titanium aluminide alloy Download PDF

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Publication number
EP1066415B1
EP1066415B1 EP99935269A EP99935269A EP1066415B1 EP 1066415 B1 EP1066415 B1 EP 1066415B1 EP 99935269 A EP99935269 A EP 99935269A EP 99935269 A EP99935269 A EP 99935269A EP 1066415 B1 EP1066415 B1 EP 1066415B1
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Prior art keywords
alloy
titanium aluminide
aluminide alloy
content
pmta
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Expired - Lifetime
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EP99935269A
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German (de)
English (en)
French (fr)
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EP1066415A1 (en
EP1066415A4 (en
Inventor
Seetharama C. Deevi
C. T. Liu
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Chrysalis Technologies Inc
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Chrysalis Technologies Inc
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Priority claimed from US09/174,103 external-priority patent/US6214133B1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • 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
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the invention relates generally to two-phase titanium aluminide alloy compositions useful for resistive heating and other applications such as structural applications.
  • Titanium aluminide alloys are the subject of numerous patents and publications including U.S. Patent Nos. 4,842,819; 4,917,858; 5,232,661; 5,348,702; 5,350,466; 5,370,839; 5,429,796; 5,503,794; 5,634,992; and 5,746,846, Japanese Patent Publication Nos. 63-171862; 1-259139; and 1-42539; European Patent Publication No. 365174 and articles by V.R. Ryabov et al entitled "Properties of the Intermetallic Compounds of the System Iron-Aluminum" published in Metal Metalloved, 27, No.4, 668-673, 1969; S.M.
  • U.S. Patent No. 5,489,411 discloses a powder metallurgical technique for preparing titanium aluminide foil by plasma spraying a coilable strip, heat treating the strip to relieve residual stresses, placing the rough sides of two such strips together and squeezing the strips together between pressure bonding rolls, followed by solution annealing, cold rolling and intermediate anneals.
  • U.S. Patent No. 4,917,858 discloses a powder metallurgical technique for making titanium aluminide foil using elemental titanium, aluminum and other alloying elements.
  • 5,634,992 discloses a method of processing a gamma titanium aluminide by consolidating a casting and heat treating the consolidated casting above the eutectoid to form gamma grains plus lamellar colonies of alpha and gamma phase, heat treating below the eutectoid to grow gamma grains within the colony structure and heat treating below the alpha transus to reform any remaining colony structure a structure having ⁇ 2 laths within gamma grains.
  • US-A- 5 417 781 discloses titanium aluminide articles which contain elements such as chromium and/or manganese as well as relatively low levels of tungsten.
  • the invention defined by the alloy composition of claim 1 provides a two-phase titanium aluminum alloy having a lamellar microstructure controlled by colony size.
  • the alloy can be provided in various forms such as in the as-cast, hot extruded, cold and hot worked, or heat treated condition.
  • the alloy can be fabricated into an electrical resistance heating element having a resistivity of 60 to 200 ⁇ cm.
  • the alloy can include additional elements which provide fine particles such as second-phase or boride particles at colony boundaries.
  • the alloy can include grain-boundary equiaxed structures.
  • the alloying elements expressed within the definition of claim 1 can include but expressed in atomic percent, for example, up to 10 at% W, Nb and/or Mo.
  • the alloy can be processed into a thin sheet having a yield strength of more than 80 ksi (560 MPa), an ultimate tensile strength of more than 90 ksi (630 MPa), and/or tensile elongation of at least 1.5%.
  • the aluminum can be present in an amount of 40 to 50 at%, preferably about 46 at%.
  • the titanium can be present in the amount of at least 45 at%, preferably at least 50 at%.
  • the alloy can include 45 to 55 at% Ti, 40 to 50 at% Al, 1 to 5 at% Nb, 0.5 to 2 at% W, and 0.1 to 0.3 at% B.
  • the alloy is free of Cr, V, Mn and/or Ni.
  • the invention provides two-phase TiAl alloys with thermo-physical and mechanical properties useful for various applications such as resistance heater elements.
  • the alloys exhibit useful mechanical properties and corrosion resistance at elevated temperatures up to 1000°C and above.
  • the TiAl alloys have extremely low material density (about 4.0 g/cm 3 ), a desirable combination of tensile ductility and strength at room and elevated temperatures, high electrical resistance, and/or can be fabricated into sheet material with thickness ⁇ 10 mil.
  • One use of such sheet material is for resistive heating elements of devices such as cigarette lighters.
  • the sheet can be formed into a tubular heating element having a series of heating strips which are individually powered for lighting portions of a cigarette in an electrical smoking device of the type disclosed in U.S. Patent Nos. 5,591,368 and 5,530,225, the disclosures of which are hereby incorporated by reference.
  • the alloys can be free of elements such as Cr, V, Mn and/or Ni.
  • tensile ductility of dual-phase TiAl alloys with lamellar structures can be mainly controlled by colony size, rather than such alloying elements.
  • the invention thus provides high strength TiAl alloys which can be free of Cr, V, Mn and/or Ni.
  • Table 1 lists nominal compositions of alloys investigated wherein the base alloy contains 46.5 at% Al, balance Ti. Small amounts of alloying additions were added for investigating effects on mechanical and metallurgical properties of the two-phase TiAl alloys. Nb in amounts up to 4% was examined for possible effects on oxidation resistance, W in amounts of up to 1.0% was examined for effects on microstructural stability and creep resistance, and Mo in amounts of up to 0.5% was examined for effects on hot fabrication. Boron in amounts up to 0.18% was added for refinement of lamellar structures in the dual-phase TiAl alloys.
  • the alloy rods extruded at 1365 to 1400°C showed an irregular shape whereas PMTA-8 hot-extruded at 1335°C exhibited much smoother surfaces without surface irregularities. However, no cracks were observed in any of the hot-extruded alloy rods.
  • microstructures of the alloys were examined in the as-cast and heat treated conditions (listed in Table 2) by optical metallography and electron superprobe analyses.
  • the as-cast condition all the alloys showed lamellar structure with some degree of segregation and coring.
  • Figures 1 and 2 show the optical micrographs, with a magnification of 200X and 500X, respectively, for hot extruded alloys PMTA-1 to 4 stress-relieved for 2 hours at 1000°C. All the alloys showed fully lamellar structures, with a small amount of equiaxed grain structures at colony boundaries. Some fine particles were observed at colony boundaries, which are identified as borides by electron microprobe analyses. Also, there is no apparent difference in microstructural features among these four PMTA alloys.
  • FIG. 3 is a back-scattered image of PMTA-2, showing the formation of second-phase particles (borides) in a bright contrast at colony boundaries.
  • the composition of the borides was determined and listed in Table 3 together with that of the lamellar matrix.
  • the second-phase particles are essentially (Ti,W,Nb) borides, which are decorated and pinned lamellar colony boundaries.
  • Figures 5 and 6 show the optical microstructures of hot extruded PMTA-3 and 2 annealed for 1 day and 3 days at 1000°C, respectively. Grain-boundary equiaxed structures are clearly observed in these long-term annealed specimens, and the amount increases with the annealing time at 1000°C. A significant amount of equiaxed grain structures exists in the specimen annealed for 3 days at 1000°C.
  • FIG. 7 shows the optical microstructures of the TiAlCr sheet in both as-received and annealed (3 days at 1000°C) conditions.
  • the TiAlCr sheet has a duplex structure, and its grain structure shows no significant coarsening at 1000°C.
  • Tensile sheet specimens with a thickness of 9-20 mils and a gage length of 0.5 in were sectioned from the hot extruded alloys rods after annealing for 2 hours at 1000°C, using a EDM machine. Some of the specimens were re-annealed up to 3 days at 1000°C prior to tensile testing. Tensile tests were performed on an Instron testing machine at a strain rate of 0.1 inch/second at room temperature. Table 4 summarizes the tensile test results.
  • alloys stress-relieved for 2 hours at 1000°C exhibited 1 % or more tensile elongation at room temperature in air.
  • the tensile elongation was not affected when the specimen thickness varied from 9 to 20 mils.
  • alloy PMTA-4 appears to have the best tensile ductility. It should be noted that a tensile elongation of 1.6% obtained from a 20-mil thick sheet specimen is equivalent to 4% elongation obtained from rod specimens with a gage diameter of 0.12 in.
  • the tensile elongation appears to increase somewhat with annealing time at 1000°C, and the maximum ductility is obtained in the specimen annealed for 1 day at 1000°C.
  • All the alloys are exceptionally strong, with a yield strength of more than 100 ksi (700 MPa) and ultimate tensile strength more than 115 ksi (800 MPa) at room temperature.
  • the high strength is due to the refined fully lamellar structures produced in these TiAl alloys.
  • the TiAlCr sheet material has a yield strength of only 61 ksi (420 MPa) at room temperature.
  • the PMTA alloys are stronger that the TiAlCr sheet by as much as 67%.
  • the PMTA alloys including 0.5 % Mo exhibited significantly increased strengths, but slightly lower tensile elongation at room temperature.
  • Figures 8a-b and 9a-b show the optical micrographs of PMTA-6 and 7 hot extruded at 1380°C and 1365°C, respectively. Both alloys showed lamellar grain structures with little intercolony structures. Large colony grains (see Figure 10) were observed in both alloys hot extruded at 1380°C and 1365°C, which probably resulted from abnormal grain growth in the alloys containing low levels of boron after hot extrusion. There is no significant difference in microstructural features in these two PMTA alloys.
  • Figures 11a-d show the effect of heat treatment on microstructures of PMTA-8 hot extruded at 1335°C.
  • the alloy extruded at 1335°C showed much finer colony size and much more intercolony structures, as compared with those hot extruded at 1380°C and 1365°C.
  • Heat treatment for 2 h at 1000°C did not produce any significant change in the as-extruded structure ( Figure 11a).
  • heat treatment for 30 mins at 1340°C resulted in a substantially larger colony structure (Figure 11b).
  • Lowering the heat-treatment temperature from 1340°C to 1320-1315°C (a difference by 20-25°C) produced a sharp decrease in colony size, as indicated by Figures 11c and 11d.
  • the annealing at 1320-1315°C also appears to produce more intercolony structures in PMTA-8.
  • the abnormal grain growth is almost completely eliminated by hot extrusion at 1335°C.
  • Tables 7 and 8 also show the tensile properties of PMTA- 6 and 7 heat treated for 20 min. at 1320°C and 1315°C, respectively.
  • the heat treatment at 1320-1315°C resulted in higher tensile elongation, but lower strength at the test temperatures.
  • PMTA-8 hot extruded at 1335°C and annealed for 20 min at 1315°C exhibited the best tensile ductility at room and elevated temperatures. This alloy showed a tensile ductility of 3.3% and 11.7% at room temperature and 800°C, respectively.
  • PMTA-8 heat treated at 1315°C appears to be substantially stronger than known TiAl alloys.
  • the oxidation behavior of PMTA-2, -5 and-7 was studied by exposing sheet samples (9-20 mils thick) at 800°C in air. The samples were periodically removed from furnaces for weight measurement and surface examination. The samples showed a very low weight gain without any indication of spalling. It appears that the alloying additions of W and Nb affect the oxidation rate of the alloys at 800°C, and W is more effective in improving the oxidation resistance of TiAl alloys. Among the alloys, PMTA-7 exhibits the lowest weight gain and the best oxidation resistance at 800°C. Oxidation of PMTA-7 indicated that oxide scales are fully adherent with no indication of microcracking and spalling. This observation clearly suggests that the oxide scales formed at 800°C are well adherent to the base material and are very protective.
  • Figure 12 is a graph of resistivity in microhms versus temperature for samples 1 and 2 which were cut from an ingot having a nominal composition of PMTA-4, i.e. 30.8 wt% Al, 7.1 wt% Nb, 2.4 wt% W, and 0.045 wt% B.;
  • Figure 13 is a graph of hemispherical total emissivity versus temperature for samples 1 and 2;
  • Figure 14 is a graph of diffusivity versus temperature for samples 80259-1, 80259-2 and 80259-3 cut from the same ingot as samples 1 and 2;
  • Figure 15 is a graph of specific heat versus temperature for titanium aluminide in accordance with the invention; and
  • Figure 16 is a graph of thermal expansion versus temperature for samples 80259-1H, 80259-1C, 80259-2H, 80259-3H, and 80259-3C cut from the same ingot as samples 1 and 2.
  • the hot PMTA alloys extruded at 1365 to 1400°C exhibited mainly lamellar structures with little intercolony structures while PMTA-8 extruded at 1335°C showed much finer colony structures and more intercolony structures.
  • the heat treatment of PMTA-8 at 1315-1320°C for 20 min. resulted in fine lamellar structures.
  • the alloys may include (Ti,W,Nb) borides formed at colony boundaries.
  • tungsten in the hot-extruded alloys is not uniformly distributed, suggesting the possibility of high electrical resistance of TiAl alloys containing W additions. The inclusion of 0.5 at.
  • % Mo significantly increases the yield and ultimate tensile strengths of the TiAl alloys, but lowers the tensile elongation to a certain extent at room temperature.
  • PMTA 1-4 PMTA-4 with the alloy composition Ti-46.5 Al-3 Nb-0.5 W-0.2 B (at%) has the best combination of tensile ductility and strength at room temperature.
  • PMTA-4 is stronger than the TiAlCr sheet by 67%.
  • the TiAlCr sheet showed no bend ductility at room temperature while PMTA-4 has an elongation of 1.4%.
  • the tensile elongation of TiAl alloys is independent of sheet thickness in the range of 9 to 20 mils.
  • the alloys PMTA 4, 6 and 7 heat treated at 1000°C for 2h showed excellent strength at all temperatures up to 800°C, independent of hot extrusion temperature.
  • Hot extrusion temperatures of 1400-1365°C however, provides lower tensile ductilities ( ⁇ 4%) at room and elevated temperatures.
  • a significant increase in tensile ductility is obtained at all temperatures when the extrusion temperature is 1335°C.
  • PMTA-8 Ti-46.5 Al-3 Nb-1W-0.5B hot extruded at 1335°C and annealed at 1315°C for 20 min.
  • titanium aluminide can be manufactured into various shapes or products such as electrical resistance heating elements.
  • the compositions disclosed herein can be used for other purposes such as in thermal spray applications wherein the compositions could be used as coatings having oxidation and corrosion resistance.
  • the compositions could be used as oxidation and corrosion resistant electrodes, furnace components, chemical reactors, sulfidization resistant materials, corrosion resistant materials for use in the chemical industry, pipe for conveying coal slurry or coal tar, substrate materials for catalytic converters, exhaust walls and turbocharger rotors for automotive and diesel engines, porous filters, etc.
  • the resistivity of the heater material can be varied by changes in composition such as adjusting the aluminum content of the heater material, processing or by incorporation of alloying additions. For instance, the resistivity can be significantly increased by incorporating particles of alumina in the heater material.
  • the heater material can optionally include ceramic particles to enhance creep resistance and/or thermal conductivity.
  • the heater material can include particles or fibers of electrically conductive material such as nitrides of transition metals (Zr, Ti, Hf), carbides of transition metals, borides of transition metals and MoSi 2 for purposes of providing good high temperature creep resistance up to 1200°C and also excellent oxidation resistance.
  • the heater material may also incorporate particles of electrically insulating material such as Al 2 O 3 , Y 2 O 3 , Si 3 N 4 , ZrO 2 for purposes of making the heater material creep resistant at high temperature and also improving thermal conductivity and/or reducing the thermal coefficient of expansion of the heater material.
  • the electrically insulating/conductive particles/fibers can be added to a powder mixture of Fe, Al, Ti or iron aluminide or such particles/fibers can be formed by reaction synthesis of elemental powders which react exothermically during manufacture of the heater element.

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  • Crystallography & Structural Chemistry (AREA)
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EP99935269A 1998-02-02 1999-02-02 Two phase titanium aluminide alloy Expired - Lifetime EP1066415B1 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US174103 1993-12-28
US1748398A 1998-02-02 1998-02-02
US17483 1998-02-02
US09/174,103 US6214133B1 (en) 1998-10-16 1998-10-16 Two phase titanium aluminide alloy
PCT/US1999/002212 WO1999051787A1 (en) 1998-02-02 1999-02-02 Two phase titanium aluminide alloy

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EP1066415A1 EP1066415A1 (en) 2001-01-10
EP1066415A4 EP1066415A4 (en) 2001-05-09
EP1066415B1 true EP1066415B1 (en) 2002-07-24

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EP (1) EP1066415B1 (enExample)
JP (1) JP4664500B2 (enExample)
KR (1) KR100641905B1 (enExample)
CN (1) CN1100153C (enExample)
AT (1) ATE221137T1 (enExample)
AU (1) AU751819B2 (enExample)
BR (1) BR9908529A (enExample)
CA (1) CA2319505C (enExample)
DE (1) DE69902245T2 (enExample)
ID (1) ID26231A (enExample)
NO (1) NO333617B1 (enExample)
WO (1) WO1999051787A1 (enExample)

Cited By (1)

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RU2523049C1 (ru) * 2013-06-28 2014-07-20 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Способ получения отливок сплавов на основе гамма алюминида титана

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US6425964B1 (en) * 1998-02-02 2002-07-30 Chrysalis Technologies Incorporated Creep resistant titanium aluminide alloys
GB9915394D0 (en) * 1999-07-02 1999-09-01 Rolls Royce Plc A method of adding boron to a heavy metal containung titanium aluminide alloy and a heavy containing titanium aluminide alloy
WO2010042969A1 (en) * 2008-10-17 2010-04-22 Silverbrook Research Pty Ltd Inkjet printhead with titanium aluminium alloy heater
JP5605546B2 (ja) * 2009-04-27 2014-10-15 国立大学法人九州工業大学 α＋β型チタン合金とその製造方法並びにチタン合金材の製造方法
KR101158477B1 (ko) * 2009-12-24 2012-06-20 포항공과대학교 산학협력단 고강도 및 고연성 티타늄 합금의 제조방법
CN103820676B (zh) * 2014-03-12 2016-03-02 北京工业大学 一种Cr、V合金化β相凝固高Nb-TiAl合金及其制备方法
CN103820674B (zh) * 2014-03-12 2016-05-25 北京工业大学 一种W、Mn合金化β相凝固高Nb-TiAl合金及其制备方法
CN104404305A (zh) * 2014-12-22 2015-03-11 西北有色金属研究院 一种钇元素改性tb2钛合金
DE102016203017B3 (de) * 2016-02-25 2017-08-10 Continental Automotive Gmbh Verfahren zur Herstellung eines Katalysators
CN105821470B (zh) * 2016-04-14 2018-09-25 南京理工大学 一种双重结构TiAl合金及其制备方法
US20180230576A1 (en) * 2017-02-14 2018-08-16 General Electric Company Titanium aluminide alloys and turbine components
CN107937753B (zh) * 2017-11-27 2019-06-25 长春工业大学 一种具有双峰分布特征的TiAl混晶结构合金及制法
CN113245743B (zh) * 2021-07-01 2021-10-15 西安稀有金属材料研究院有限公司 增材制造钛铝金属间化合物用钛药芯焊丝及其制备方法
CN115612874B (zh) * 2022-09-30 2023-08-04 中国航发北京航空材料研究院 一种大尺寸细晶TiAl合金靶材的制备方法

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RU2523049C1 (ru) * 2013-06-28 2014-07-20 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Способ получения отливок сплавов на основе гамма алюминида титана

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AU751819B2 (en) 2002-08-29
NO333617B1 (no) 2013-07-22
ATE221137T1 (de) 2002-08-15
NO20003891D0 (no) 2000-07-28
JP4664500B2 (ja) 2011-04-06
WO1999051787A9 (en) 2000-06-22
EP1066415A1 (en) 2001-01-10
CA2319505A1 (en) 1999-10-14
AU5078399A (en) 1999-10-25
ID26231A (id) 2000-12-07
CN1292038A (zh) 2001-04-18
WO1999051787A1 (en) 1999-10-14
KR20010040579A (ko) 2001-05-15
KR100641905B1 (ko) 2006-11-06
NO20003891L (no) 2000-10-02
DE69902245T2 (de) 2003-03-27
EP1066415A4 (en) 2001-05-09
JP2002510750A (ja) 2002-04-09
BR9908529A (pt) 2000-12-05
DE69902245D1 (de) 2002-08-29
CA2319505C (en) 2009-10-06
CN1100153C (zh) 2003-01-29

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