CN105821470A - Dual-structure titanium aluminum (TiAl) alloy and preparation method thereof - Google Patents

Dual-structure titanium aluminum (TiAl) alloy and preparation method thereof Download PDF

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CN105821470A
CN105821470A CN201610231315.6A CN201610231315A CN105821470A CN 105821470 A CN105821470 A CN 105821470A CN 201610231315 A CN201610231315 A CN 201610231315A CN 105821470 A CN105821470 A CN 105821470A
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rod
tial alloy
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CN105821470B (en
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陈�光
祁志祥
葛志军
李沛
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Nanjing University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B21/00—Unidirectional solidification of eutectic materials
    • C30B21/04—Unidirectional solidification of eutectic materials by zone-melting
    • 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
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/52—Alloys

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a dual-structure titanium aluminum (TiAl) alloy and a preparation method thereof. The atomic percentage of the TiAl alloy compositions is TiaAlb, wherein a is more than 49 and less than 50.6, b is more than 49.4 and less than 51, and a plus b is equal to 100, the main body of the dual-structure TiAl alloy is a columnar crystal, and gamma-phase equiaxed grains are generated at a grain boundary of the columnar crystal; the preparation of the TiAl alloy comprises the following steps: selecting suitable compositions according to the phase diagram of a TiAl binary alloy system; using a water cooled copper crucible and a vacuum non-consumable arc melting furnace to prepare a cylindrical rod master alloy; using an optical floating zone crystal growing apparatus to carry out directional solidification on the master alloy to obtain the dual-structure TiAl alloy. The dual-structure TiAl alloy disclosed by the invention comprises the columnar crystal and an equiaxed grain structure, wherein the equiaxed grain structure is at the grain boundary of the columnar crystal, so that performance characteristics of a columnar crystal structure can be kept, and then performances of the alloy can be simply and effectively improved.

Description

A kind of dual structure TiAl alloy and preparation method thereof
Technical field
The invention belongs to high-strength light technical field of structural materials, be specifically related to a kind of dual structure TiAl alloy and preparation method thereof.
Background technology
TiAl alloy has the advantages such as the antioxygenic property of low-density, Gao Biqiang, good high-temperature behavior and excellence, is with gram for the Aero-Space high temperature use of loss of weight unit, particularly electromotor optimal candidate material.GE company of the U.S. successfully utilizes Ti-48Al-2Cr-2Nb(4822) two-stage low-pressure turbine blade after alloy development Boeing, make single aircraft engine loss of weight about 200Kg.Airbus SAS utilizes forging TiAl alloy, has manufactured PW1100G engine blade, and has the most successfully taken a flight test.Additionally, the parts such as automobile charging turbine blade all have extensive application demand to TiAl alloy.
Although TiAl alloy has irreplaceable remarkable advantage, but its brittleness at room temperature result in TiAl alloy to be difficult to, and limits its further application on high-temperature component.Preparing TiAl based composites is numerous a kind of effective ways for improving TiAl alloy brittleness at room temperature problem, but it typically uses additional compound method, and its interface problem highlights, it is impossible to be effectively improved performance.Such as, Cui likes equality people and utilizes solid-liquid reaction method to prepare the TiAl matrix composite sheet (" Acta Metallurgica Sinica ", 2013) of reinforcement layered distribution, and in fact the method does not has the effectively room-temperature property improving TiAl alloy, and reason is exactly the most crisp TiB2Enriched layer causes in interface.In addition, Chen Guang seminar finds to utilize directional freeze method to prepare column crystal or monocrystalline TiAl alloy also can improve TiAl alloy temperature-room type plasticity (a kind of high-strength high-ductility TiAl alloy material and preparation method thereof, number of patent application: 201410529844.5), but success rate ratio that the method obtains TiAl monocrystalline is relatively low, it is difficult to be able to business application.
Summary of the invention
It is an object of the invention to provide a kind of dual structure TiAl alloy and preparation method thereof.
The technical solution realizing the object of the invention is: a kind of dual structure TiAl alloy, described alloy atom percentage expression formula is TiaAlb, wherein 49 ＜ a ＜ 50.6,49.4 ＜ b ＜ 51, a+b=100, described TiAl alloy main body is column crystal, and raw γ phase equiax crystal in the grain boundaries of column crystal.
A kind of method of TiAl alloy preparing above-mentioned dual structure, comprises the following steps:
The first step: choose raw material according to target TiAl alloy composition, determines that its alloy atom percentage expression formula is TiaAlb, wherein 49 ＜ a ＜ 50.6,49.4 ＜ b ＜ 51, a+b=100；
Second step: use water jacketed copper crucible at least 4 above-mentioned raw materials of suspension smelting furnace melt back, then use the TiAl alloy cylindrical rod that a diameter of 6-8mm prepared by vacuum non-consumable arc-melting furnace；
3rd step: under argon air-flow protection, uses optics float-zone crystal grower that cylindrical rod alloy is oriented solidification, obtains described dual structure TiAl alloy.
In the first step, the purity of raw material is not less than 99.999%.
In second step, the vacuum in water jacketed copper crucible suspension smelting furnace is less than 10-2Pa, the vacuum of vacuum non-consumable arc-melting furnace is less than 10-2Pa。
In 3rd step, during the growth of optics float-zone crystal, lower end is length at the seed crystal rod of 20-30mm, and upper end is that length is less than the TiAl alloy cylindrical rod of 190mm as feeding rod, and both compositions are identical；By coaxial with seed crystal rod for feeding rod and be perpendicular to the horizontal plane spacing setting with 1-3mm apart during directional solidification, and this spacing is positioned at four filament focusing center；It is passed through flow to protect at the noble gas (argon or nitrogen) of 3-5L/min; and regulate seed crystal rod and the feeding synchronized rotation of rod opposite direction; rotating speed is 30r/min; within 5min, power is all ramped up 65.5%, adjusts feeding rod and contact with each other with seed crystal rod, when stablizing to floating region after insulation 5-10min; growth regulation speed is 5-20mm/h; proceeding by directional solidification, solidification slowly reduces power after terminating, slowly separate with residue feeding rod sample simultaneously and by solidifying sample.
The present invention compared with prior art, has a significant advantage that
(1) the TiAl dual structure of the present invention can regard the one in composite as, but is surface crack, solves interface problem intrinsic in composite；(2) present invention is the heating feature utilizing optics float-zone crystal grower unique, and the dual structure TiAl alloy composite process that a step is prepared is simple, and the preparation to composite has important references value；(3) the TiAl alloy subject organization of the present invention is still column crystal, can keep the performance characteristics of columanar structure, therefore can also simply be effectively improved alloy property.
The present invention is described in detail below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is TiAl alloy Binary Phase Diagram.
Fig. 2 is the directional solidification TiAl alloy solid liquid interface microscopic structure (a is overall diagram, and b is the line scanning composition power spectrum figure of magnification region in a) of embodiment 1.
Fig. 3 is directional solidification TiAl alloy optical microstructure (a is overall diagram, and b is the organization charts of magnification region in a) of embodiment 1.
Fig. 4 is the non-dual structure columnar structure TiAl alloy microscopic structure of comparative example 1.
Fig. 5 is the non-dual structure monocrystalline TiAl alloy microscopic structure of comparative example 2.
Fig. 6 be the stable section of comparative example 3 of the present invention be non-dual structure monocrystalline TiAl alloy microscopic structure.
Detailed description of the invention
Embodiment 1
(1) according to the TiAl alloy Binary Phase Diagram shown in Fig. 1, high-purity Ti and the Al raw material selecting purity to be 99.999%, formulated component is Ti50Al50Alloy so that alloy can occur L+ α → γ phase transformation.It is 3 × 10 in vacuum-3Melt back 4 times in the suspension smelting furnace of Pa；Then, by melted alloy under identical vacuum, the cylindrical rod of the vacuum non-consumable a diameter of 6mm of arc-melting furnace melting is used；
(2) being oriented solidification in the optics float-zone crystal grower under argon air-flow protection, lower end is length at the seed crystal rod of 20-30mm, and upper end is that length is less than the TiAl alloy cylindrical rod of 190mm as feeding rod, and both compositions are identical；By coaxial with seed crystal rod for feeding rod and be perpendicular to horizontal plane and arrange during directional solidification, feeding rod apart 1-3mm excellent with seed crystal, and this spacing is positioned at four filament focusing center；It is passed through flow to protect at the inert nitrogen gas of 4L/min; and regulate seed crystal rod and the feeding synchronized rotation of rod opposite direction; rotating speed is 30r/min, and power is all ramped up within 5min 65.5%, adjusts feeding rod and contacts with each other with seed crystal rod; when stablizing to floating region after insulation 10min; growth regulation speed is 15mm/h, proceeds by directional solidification, after sample carries out a period of time; cut off rapidly electric current, to retain solid-liquid district pattern.Fig. 2 is solid-liquid district pattern, dendritic arm dry with dendrite become 60 °, illustrate that it is that α phase solidifies.
(3) constituency at solid-liquid pattern is entered line scan, find that dark structure is rich Al phase.Due to the heating feature that optics floating region is unique, the center temperature is low, understands in conjunction with TiAl alloy phasor, after Al is enriched to a certain degree, it may occur that L+ α → γ phase transformation.Therefore, center can retain γ phase.And both sides temperature is high, having little time L+ α → γ phase transformation, α phase can generate lamellar structure in cooling subsequently.Concrete tissue is as it is shown on figure 3, thus can get the TiAl alloy of dual structure.
Embodiment 2
Employing composition is Ti50.5Al49.5Alloy, use the cylindrical rod of a diameter of 8mm, under the growth rate of 20mm/h, be oriented solidification, other conditions, with embodiment 1, still can get dual structure TiAl alloy as described in Example 1.
Embodiment 3
Employing composition is Ti49Al51Alloy, use the cylindrical rod of a diameter of 6mm, under the growth rate of 15mm/h, be oriented solidification, other conditions, with embodiment 1, still can get dual structure TiAl alloy as described in Example 1.
Comparative example 1
Employing composition is Ti56Al44Alloy, in the case of growth rate is 15mm/h, be oriented solidification, other are with embodiment 1, and obtaining stable section as shown in Figure 4 is non-dual structure columnar structure TiAl alloy.
Comparative example 2
Employing composition is Ti57.2Al42.8Alloy, in the case of growth rate is 15mm/h, be oriented solidification, other are with embodiment 1, and obtaining stable section as shown in Figure 5 is non-dual structure monocrystalline TiAl alloy.
Comparative example 3
Employing composition is Ti50Al50Alloy, in the case of growth rate is 25mm/h, be oriented solidification, other conditions are with embodiment 1, and obtaining stable section as shown in Figure 6 is non-dual structure monocrystalline TiAl alloy.
Comparative example 4
Employing composition is Ti50Al50Alloy, in the case of growth rate is 20mm/h, the alloy of a diameter of 4mm is oriented solidification, other conditions with embodiment 1, obtain as described in comparative example 3 the monocrystalline TiAl alloy that stable section is non-dual structure.

Claims (9)

1. a dual structure TiAl alloy, it is characterised in that described alloy atom percentage expression formula is TiaAlb, wherein, 49 ＜ a ＜ 50.6,49.4 ＜ b ＜ 51, a+b=100, described TiAl alloy main body is column crystal, and raw γ phase equiax crystal in the grain boundaries of column crystal.
2. TiAl alloy as claimed in claim 1, it is characterised in that prepared by following steps:
The first step: choose raw material according to target TiAl alloy composition；
Second step: use water jacketed copper crucible at least 4 above-mentioned raw materials of suspension smelting furnace melt back, then use the TiAl alloy cylindrical rod that a diameter of 6-8mm prepared by vacuum non-consumable arc-melting furnace；
3rd step: under argon air-flow protection, uses optics float-zone crystal grower that cylindrical rod alloy is oriented solidification, obtains described dual structure TiAl alloy.
3. TiAl alloy as claimed in claim 2, it is characterised in that in the first step, the purity of raw material is not less than 99.999%.
4. TiAl alloy as claimed in claim 2, it is characterised in that in second step, the vacuum in water jacketed copper crucible suspension smelting furnace is less than 10-2Pa, the vacuum of vacuum non-consumable arc-melting furnace is less than 10-2Pa。
5. TiAl alloy as claimed in claim 2, it is characterised in that in the 3rd step, during the growth of optics float-zone crystal, lower end is the length seed crystal rod at 20-30mm, and upper end is that length is less than the TiAl alloy cylindrical rod of 190mm as feeding rod, and both compositions are identical；By coaxial with seed crystal rod for feeding rod and be perpendicular to the horizontal plane spacing setting with 1-3mm apart during directional solidification, and this spacing is positioned at four filament focusing center；It is passed through flow to protect at the noble gas of 3-5L/min; and regulate seed crystal rod and the feeding synchronized rotation of rod opposite direction; rotating speed is 30r/min; within 5min, power is all ramped up 65.5%, adjusts feeding rod and contact with each other with seed crystal rod, when stablizing to floating region after insulation 5-10min; growth regulation speed is 5-20mm/h; proceeding by directional solidification, solidification slowly reduces power after terminating, slowly separate with residue feeding rod sample simultaneously and by solidifying sample.
6. the preparation method of TiAl alloy as claimed in claim 1, it is characterised in that comprise the steps:
The first step: choose raw material according to target TiAl alloy composition；
Second step: use water jacketed copper crucible at least 4 above-mentioned raw materials of suspension smelting furnace melt back, then use the TiAl alloy cylindrical rod that a diameter of 6-8mm prepared by vacuum non-consumable arc-melting furnace；
3rd step: under argon air-flow protection, uses optics float-zone crystal grower that cylindrical rod alloy is oriented solidification, obtains described dual structure TiAl alloy.
7. preparation method as claimed in claim 6, it is characterised in that in the first step, the purity of raw material is not less than 99.999%.
8. preparation method as claimed in claim 6, it is characterised in that in second step, the vacuum in water jacketed copper crucible suspension smelting furnace is less than 10-2Pa, the vacuum of vacuum non-consumable arc-melting furnace is less than 10-2Pa。
9. preparation method as claimed in claim 6, it is characterised in that in the 3rd step, during the growth of optics float-zone crystal, lower end is the length seed crystal rod at 20-30mm, and upper end is that length is less than the TiAl alloy cylindrical rod of 190mm as feeding rod, and both compositions are identical；By coaxial with seed crystal rod for feeding rod and be perpendicular to the horizontal plane spacing setting with 1-3mm apart during directional solidification, and this spacing is positioned at four filament focusing center；It is passed through flow to protect at the noble gas of 3-5L/min; and regulate seed crystal rod and the feeding synchronized rotation of rod opposite direction; rotating speed is 30r/min; within 5min, power is all ramped up 65.5%, adjusts feeding rod and contact with each other with seed crystal rod, when stablizing to floating region after insulation 5-10min; growth regulation speed is 5-20mm/h; proceeding by directional solidification, solidification slowly reduces power after terminating, slowly separate with residue feeding rod sample simultaneously and by solidifying sample.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113528926A (en) * 2021-06-11 2021-10-22 南京理工大学 Oriented FeAl-based alloy and preparation method thereof

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JP2001328899A (en) * 2000-05-18 2001-11-27 Tokyo Inst Of Technol METHOD FOR CONTROLLING LAMELLA ORIENTATION OF TiAl SINGLE CRYSTAL ALLOY
US6436208B1 (en) * 2001-04-19 2002-08-20 The United States Of America As Represented By The Secretary Of The Navy Process for preparing aligned in-situ two phase single crystal composites of titanium-niobium alloys
CN1752265A (en) * 2005-10-26 2006-03-29 北京科技大学 Heating technology for refining TiAl alloy ingot microscopic texture
CN101176946A (en) * 2007-11-28 2008-05-14 哈尔滨工业大学 Method for vacuum scattering intermetallic compound for coupling TiAL
CN102011078A (en) * 2010-12-23 2011-04-13 哈尔滨工业大学 Method for refined and directional solidification of titanium aluminium alloy slab surface structure
CN103074536A (en) * 2013-01-31 2013-05-01 南京理工大学 Carbon-silicon-tungsten-yttrium lamellar structure high-niobium titanium-aluminum alloy and preparation method thereof
CN103409660A (en) * 2013-08-12 2013-11-27 南京理工大学 Novel Beta/Gamma-TiAl alloy with ultra-fine grain
CN103498065A (en) * 2013-09-05 2014-01-08 西北工业大学 TiAl alloy crystal grain refinement method
CN103757571A (en) * 2014-01-24 2014-04-30 中国科学院金属研究所 Preparation method for gamma-TiAl alloy fine fully lamellar microstructure with preferred oriented lamellar interface
CN103789598A (en) * 2014-02-28 2014-05-14 南京理工大学 Directional TiAl-based alloy and preparation method thereof
CN104152745A (en) * 2014-08-25 2014-11-19 钢铁研究总院 Cast highniobium titanium-aluminum alloy and preparation method thereof

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US5232661A (en) * 1991-01-31 1993-08-03 Nippon Steel Corporation γ and β dual phase TiAl based intermetallic compound alloy having superplasticity
CN1292038A (en) * 1998-02-02 2001-04-18 菲利普莫里斯生产公司 Two phase titanium aluminide alloy
JP2001328899A (en) * 2000-05-18 2001-11-27 Tokyo Inst Of Technol METHOD FOR CONTROLLING LAMELLA ORIENTATION OF TiAl SINGLE CRYSTAL ALLOY
US6436208B1 (en) * 2001-04-19 2002-08-20 The United States Of America As Represented By The Secretary Of The Navy Process for preparing aligned in-situ two phase single crystal composites of titanium-niobium alloys
CN1752265A (en) * 2005-10-26 2006-03-29 北京科技大学 Heating technology for refining TiAl alloy ingot microscopic texture
CN101176946A (en) * 2007-11-28 2008-05-14 哈尔滨工业大学 Method for vacuum scattering intermetallic compound for coupling TiAL
CN102011078A (en) * 2010-12-23 2011-04-13 哈尔滨工业大学 Method for refined and directional solidification of titanium aluminium alloy slab surface structure
CN103074536A (en) * 2013-01-31 2013-05-01 南京理工大学 Carbon-silicon-tungsten-yttrium lamellar structure high-niobium titanium-aluminum alloy and preparation method thereof
CN103409660A (en) * 2013-08-12 2013-11-27 南京理工大学 Novel Beta/Gamma-TiAl alloy with ultra-fine grain
CN103498065A (en) * 2013-09-05 2014-01-08 西北工业大学 TiAl alloy crystal grain refinement method
CN103757571A (en) * 2014-01-24 2014-04-30 中国科学院金属研究所 Preparation method for gamma-TiAl alloy fine fully lamellar microstructure with preferred oriented lamellar interface
CN103789598A (en) * 2014-02-28 2014-05-14 南京理工大学 Directional TiAl-based alloy and preparation method thereof
CN104152745A (en) * 2014-08-25 2014-11-19 钢铁研究总院 Cast highniobium titanium-aluminum alloy and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113528926A (en) * 2021-06-11 2021-10-22 南京理工大学 Oriented FeAl-based alloy and preparation method thereof

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