CN104328501A - Lamellar orientation completely controllable TiAl single crystal alloy and preparation method thereof - Google Patents
Lamellar orientation completely controllable TiAl single crystal alloy and preparation method thereof Download PDFInfo
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- CN104328501A CN104328501A CN201410528019.3A CN201410528019A CN104328501A CN 104328501 A CN104328501 A CN 104328501A CN 201410528019 A CN201410528019 A CN 201410528019A CN 104328501 A CN104328501 A CN 104328501A
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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
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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Abstract
The invention discloses a lamellar orientation completely controllable TiAl intermetallic compound single crystal and a preparation method thereof. The material composition expression formula of the TiAl alloy provided by the invention is TiaAlbNbc (atomic percent), wherein a is greater than or equal to 42 and smaller than or equal to 55, b is greater than or equal to 43 and is smaller than or equal to 49, c is greater than or equal to 2 and is smaller than or equal to 9, and a+b+c=100. The preparation method of the controllable lamellar orientation TiAl single crystal alloy provided by the invention includes: conducting electromagnetic induction levitation melting of a TiAl alloy master ingot in a water-cooled copper crucible, and carrying out suction casting to obtain a directionally solidified bar; putting the bar into a high purity corundum crucible with an inner wall sintered with a high-purity yttrium oxide coating to perform Bridgman directional solidification; and changing solidification parameters to control the solid-state phase transformation process so as to make the single crystal lamellar orientation completely controllable and acquire the TiAl intermetallic compound single crystal with the lamellar orientation parallel to the growth direction.
Description
Technical field
The invention belongs to inter-metallic compound material technical field, be specifically related to completely controlled TiAl single crystal alloy of a kind of lamellar orientation and preparation method thereof.
Background technology
TiAl intermetallic compound is a kind of novel light high-temperature structural material, its proportion is less than 50% of nickel base superalloy, having the advantages such as high ratio is strong, Gao Bigang, anti-corrosion, wear-resisting, high temperature resistant and excellent oxidation-resistance and creep resistance, is the ideal material of alternative Ni based high-temperature alloy.
Mechanical property and its lamellar orientation of complete lamellar structure TiAl alloy have close relationship.By to the research with single-orientated full sheet layer many twin crystal PST (Polysynthetic twinned crystal), find that its intensity and plasticity present obvious anisotropy.Due to this anisotropy of complete lamellar structure, when lamellar orientation is suitable, it is made to be more suitable for the such ask for something of blade of aviation engine high temperature resistant, and only by the service condition of one-dimensional square to load.If TiAl alloy can be adopted the method for directional freeze produce the engine blade of complete lamellar structure, and its lamellar structure orientation is made to be parallel to the axis direction of growth of crystal (in the directional freeze) of blade, extremely beneficial beyond doubt.The robot systems such as Yamaguchi have studied the impact of TiAl alloy lamellar orientation on mechanical property, and find when loading direction is parallel with lamellar orientation, yield strength and unit elongation reach best of breed.Therefore, the use properties of TiAl alloy to be improved further, just must control, to obtain the orientation TiAl intermetallic compound monocrystalline complete lamellar structure consistent with loading direction the lamellar orientation of final tissue.
At present, the control method of domestic and international TiAl alloy lamellar orientation mainly comprises seed-grain method and changes the non-seed-grain method of solidification path.The people such as Yamaguchi, Johnson solidify seed-grain method by α phase, select Ti-Al-Si system alloy as seed crystal, obtain by necking down crystal separation method the monocrystalline PST that lamellar orientation is parallel to the direction of growth completely.Seed crystal composition usually and mother alloy composition there are differences cause the composition of directional solidificating alloy and performance uneven, and the complicated process of preparation of seed crystal.Therefore, seed-grain method has obvious deficiency.
In non-seed-grain method, do not study both at home and abroad at present and obtain the full sheet layer TiAl single crystal organization parallel with the direction of growth.Lin Junpin etc., under lower G/V condition, adopt the method for " from seed-grain method " (double directional solidification) to obtain the full sheet layer single crystal organization parallel with the direction of growth to Ti-46Al-5Nb alloy.They think, lower G/V technique makes β phase dendrite interval under suitable conditions, the single-orientated α phase parallel with the direction of growth can be obtained by full Peritectic Reaction, and the α variant that solid-state phase changes β → α generates not coordination phase can not occur, thus complete the control to lamellar orientation.This method needs the directional freeze of carrying out twice same process, and the many process of setting of more common non-seed-grain method, have increased the weight of the pollution of crucible material alloy, unfavorable to the industrialization of directional freeze TiAl alloy.
The domestic and international research all for a change solidification path controlling lamellar orientation about non-seed-grain method, can not control monocrystalline lamellar orientation, and not obtain the completely parallel single-chip layer tissue with the direction of growth before.For solving this technical barrier, the solid-state directed phase transition process of TiAl alloy becomes the key controlling lamellar orientation.From phasor, complete lamellar structure TiAl alloy also must experience β → α and α → α after solidifying
2the solid-state phase changes of+γ.When primary phase is β phase time, selecting excellence evaluation is <001>, and its phase relation is: { 110}
β// { 0001}
α// { 111}
γ [25], and { 110}
β12 variablees in 4 be parallel to the direction of growth, 8 with the direction of growth tilt at 45 °
[16,26], in the lamellar structure formed after experience solid-state phase changes, only have the orientation of 1/3 habit plane to be parallel to the direction of growth.Obviously, the orientation of TiAl alloy final piece layer tissue, not only depends on the direction of growth of nascent β phase, the solid-state phase changes process after also depending on.So β → α solid-state phase changes process is also the key controlling lamellar orientation.And up to now about the research that TiAl lamellar orientation controls, all concentrate on process of setting, and ignore the solid-state phase changes process after solidifying.
Therefore, not only want control solidi fication process, directional freeze primary phase is made to be β phase, and the forming core that will control cenotype in the directed solid-state phase changes process of TiAl alloy is grown up, phase boundary directional migration process, make it only remain in directed solid-state phase changes with the direction of growth to be the lamellar orientation of 0 °, complete the control to TiAl alloy lamellar orientation under continuously-directional liquid-solid-phase changeable-solid-state phase changes condition.
Summary of the invention
The object of the invention is by controlling continuously-directional liquid-solid-phase changeable-solid-state phase changes process, TiAl intermetallic compound monocrystalline providing a kind of lamellar orientation completely controlled and preparation method thereof.
The TiAl intermetallic compound monocrystalline that lamellar orientation is completely controlled, with atomic percentage, its alloying constituent expression formula is Ti
aal
bnb
c, wherein, 42≤a≤55,43≤b≤49,2≤c≤9, a+b+c=100.
The preparation of the TiAl intermetallic compound monocrystalline that above-mentioned lamellar orientation is completely controlled, comprises following concrete steps:
The first step: choose Ti, Al, Nb pure metal starting material that purity is 99.999%, carry out proportioning according to alloying constituent, be less than 10 in vacuum tightness
-3master alloy melting in the cold crucible levitation melting stove of Pa, makes alloying constituent homogenizing through 3 ~ 4 meltings, and directional freeze bar is cast in suction;
Second step: the corundum crucible that high-purity yttrium oxide coating put into by TiAl alloy coupon is carried out directional freeze, is evacuated to 5 × 10
-3pa, then in system, be filled with high-purity argon protection gas;
3rd step: regulate inductive source power to heat sample, holding temperature is 1450 ~ 1650K, and soaking time is 15 ~ 30min, starts directional freeze, and controlling directional freeze withdrawing rate is 5 ~ 20 μm/s; Continued propagation, to specimen length 50mm place, starts fast quenching and carries out rapid quenching to directional freeze sample, retain solid-liquid interface.
In the first step, directional freeze diameter of rod is Φ (4 ~ 6mm) × 100mm.
In second step, the corundum crucible of high-purity yttrium oxide coating is of a size of Φ (7 ~ 9mm) × 100mm; High-purity argon protection gas charge is 0.04 ~ 0.06MPa.
Principle of the present invention: adopt Bridgman directional solidification process to control TiAl alloy lamellar orientation, parameter thermograde and growth velocity is solidified by changing, first ensure that primary phase is full β phase, secondly eliminated by crystal grain competition in process of setting and obtain monocrystalline, and in process of setting, there is the corresponding specific withdrawing rate of a critical temperature, under this withdrawing rate, final lamellar orientation and the direction of growth are that the α phase of 45 ° is moved by phase boundary and eliminated, make only to retain the final lamellar orientation α phase parallel with the direction of growth in 12 the α variablees obtained in β → α phase transformation, thus the control completed lamellar orientation.
The present invention compared with prior art, tool has the following advantages: 1. adopt common Bridgman directional solidification process, parameter is solidified by regulating, control continuously-directional liquid-solid-phase changeable-directed solid-state phase changes, ensure full beta-phase growth and by controlling final lamellar orientation in solid-state phase changes, and obtain the TiAl alloy single crystal organization that lamellar orientation is parallel to the direction of growth completely.
2. present invention effectively prevents the shortcoming that seed-grain method composition performance is uneven, in single directional freeze process, just obtain the single crystal organization of desirable lamellar orientation simultaneously, simplify technique.
3. the present invention is in preparation TiAl alloy monocrystalline process, can control its monocrystalline lamellar orientation completely under certain limit solidifies parameter.The present invention is that the industrial applications of directional freeze TiAl alloy provides theoretical basis.
Accompanying drawing explanation
Fig. 1 is prior art part Ti-Al binary alloy phase diagram.
Fig. 2 is the micro-organization chart of the maximum vertical section (a) of directional freeze sample of the present invention and lamellar orientation (b).
Fig. 3 is directional freeze sample of the present invention competition section vertical section micro-organization chart.
Fig. 4 is the micro-organization chart of the maximum vertical section (a) of directional freeze sample of the present invention and lamellar orientation (b).
Fig. 5 is directional freeze sample of the present invention competition section vertical section micro-organization chart.
Fig. 6 is the micro-organization chart of the maximum vertical section (a) of directional freeze sample of the present invention and lamellar orientation (b).
Fig. 7 is directional freeze sample of the present invention quenching solid-liquid interface.
Note: in accompanying drawing 2-7, the microstructure direction of growth is from right to left.
Embodiment
TiAl intermetallic compound monocrystalline that a kind of lamellar orientation of the present invention is completely controlled and preparation method thereof, its embodiment is as follows:
(1) selection primary phase is the Ti-Al-Nb ternary alloy of full β phase.According to multicomponent alloy phasor and phase choosing principles, as Fig. 1, by the proportion relation between adjustment atomic component, its first precipitated phase is made to be all β phase.Specifically, improve the content of Nb, reduce the relative proportion of Al, form wider β phase region.
(2) according to 1) alloying constituent that obtains, adopt the configuration of high pure metal constituent element, and under high-purity Ar gas shielded, adopt cold crucible electromagnetic levitation-melt equipment to found mother alloy.Mother alloy repeatedly melting obtains uniform master alloy ingot, and mother alloy bar is cast in suction.
(3) TiAl alloy bar is inserted the corundum crucible of inwall sintering high-purity yttrium oxide coating; corundum crucible is of a size of Φ (5 ~ 8mm) × 100mm; put into Bridgman directional solidification furnace, when suction puts 5 × 10-3Pa, be filled with 0.04 ~ 0.06MPa high-purity argon protection gas.
(4) regulate inductive source power to heat sample, holding temperature is 1450 ~ 1650K, and soaking time is 15 ~ 30min, starts directional freeze, and controlling directional solidification growth speed is 5 ~ 20 μm/s;
(5) at given pace continued propagation to specimen length 50mm place, start fast quenching rapid quenching is carried out to directional freeze sample, retain solid-liquid interface.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Testing alloying constituent used is Ti
47al
45nb
8(atomic percent at%), its metal constituent element purity is 99.999%, under high-purity Ar gas shielded, adopts cold crucible electromagnetic levitation-melt equipment to found mother alloy under vacuum tightness is 5 × 10-3Pa.Obtain uniform master alloy ingot through 4 meltings, and Φ 4 × 100mm mother alloy bar is cast in suction.TiAl alloy coupon is put into the corundum crucible that inwall scribbles high-purity yttrium oxide and carry out directional freeze experiment, be evacuated to 5 × 10-3Pa, then in system, be filled with 0.05MPa high-purity argon protection gas., regulate inductive source power to heat sample, holding temperature is 1550K, and soaking time is 25min, starts directional freeze, and controlling directional solidification growth speed is 5 μm/s; When pull length is to specimen length 50mm place, start fast quenching and rapid quenching is carried out to sample, retain solid-liquid interface.Microstructural characterisation is carried out to the maximum vertical section of this cylinder sample, observe solidifying first precipitated phase, grain size and lamellar orientation and analyzing under this withdrawing rate, as shown in Fig. 2 (a) He Fig. 2 (b), discovery obtains the TiAl alloy monocrystalline that lamellar orientation is parallel to the direction of growth.Growth velocity is less when being 5 μm/s, and the enrichment of solute can fully be spread, and growth can be stablized and be carried out, and crystal grain has the sufficient time to grow up, so gained crystal grain is comparatively thick until obtain single crystal growing.
Directional freeze competition section microstructure when Fig. 3 is 5 μm/s.Due in β → α solid-state phase changes, different with the mismatch at 45 ° of lamellas, two kinds of interfaces owing to forming 0 °, cause the difference of different phase boundary mobilities, so one exists critical withdrawing rate 5 μm/s, below this withdrawing rate, formed 0 ° with the α grain nucleation of 45 ° of lamellar orientations after 0 ° of grain growing motivating force comparatively large, finally eliminate 45 ° of crystal grain, obtain the monocrystalline that lamellar orientation is parallel to the direction of growth.
Embodiment 2
Adopt alloying constituent in the same manner as in Example 1 and method, holding temperature is 1550K, and soaking time is 25min, starts directional freeze, and controlling directional solidification growth speed is 15 μm/s; As shown in Fig. 4 (a) He Fig. 4 (b), the α phase of what β → α solid-state phase changes retained under this withdrawing rate is 45 ° of lamellar orientations, so be finally organized as the monocrystalline that lamellar orientation is 45 °.
Directional freeze competition section microstructure when Fig. 5 is 15 μm/s.When this withdrawing rate, 45 ° of crystal grain solid-state phase changes nuclear driving forces are greater than 0 ° of crystal grain, so that 0 ° of crystal grain can not grow, and obtain the TiAl alloy monocrystalline that lamellar orientation and the direction of growth are 45 °.
Embodiment 3
Adopt alloying constituent in the same manner as in Example 1 and method, holding temperature is 1550K, and soaking time is 25min, starts directional freeze, and controlling directional solidification growth speed is 20 μm/s; As shown in Fig. 6 (a) He Fig. 6 (b), acquisition lamellar orientation and the direction of growth are the monocrystalline of 45 °.
Fig. 7 is the solid-liquid interface that rapid quenching retains, and its dendritic growth pattern is 4 heavy symmetries, and have obvious secondary dendrite and do in 90 ° of vertical relations with a dendrite, can infer in directional freeze process, the β phase of isometric system is primary phase.
Embodiment 4
Adopt the method identical with embodiment 1, alloying constituent used is Ti
55al
43nb
2, holding temperature is 1650K, and soaking time is 30min, and directional solidification growth speed is 5 μm/s, obtains the TiAl alloy monocrystalline being parallel to the direction of growth with lamellar orientation.
Embodiment 5
Adopt the method identical with embodiment 1, alloying constituent used is Ti
48al
43nb
9, holding temperature is 1450K, and soaking time is 30min, and directional solidification growth speed is 10 μm/s, and acquisition lamellar orientation and the direction of growth are the TiAl alloy monocrystalline of 45 °.
Embodiment 6
Adopt the method identical with embodiment 1, alloying constituent used is Ti
51al
45nb
6, holding temperature is 1650K, and soaking time is 15min, and directional solidification growth speed is 5 μm/s, obtains the TiAl alloy monocrystalline being parallel to the direction of growth with lamellar orientation.
Embodiment 7
Adopt the method identical with embodiment 1, alloying constituent used is Ti
42al
49nb
9, holding temperature is 1550K, and soaking time is 25min, and directional solidification growth speed is 5 μm/s, obtains the TiAl alloy monocrystalline being parallel to the direction of growth with lamellar orientation.
Claims (7)
1. the TiAl intermetallic compound monocrystalline that lamellar orientation is completely controlled, is characterized in that, with atomic percentage, its alloying constituent expression formula is Ti
aal
bnb
c, wherein, 42≤a≤55,43≤b≤49,2≤c≤9, a+b+c=100.
2. the TiAl intermetallic compound monocrystalline that lamellar orientation as claimed in claim 1 is completely controlled, is characterized in that, prepared by following steps:
The first step: choose Ti, Al, Nb pure metal starting material that purity is 99.999%, carry out proportioning according to alloying constituent, be less than 10 in vacuum tightness
-3master alloy melting in the cold crucible levitation melting stove of Pa, makes alloying constituent homogenizing through 3 ~ 4 meltings, and directional freeze bar is cast in suction;
Second step: the corundum crucible that high-purity yttrium oxide coating put into by TiAl alloy coupon is carried out directional freeze, is evacuated to 5 × 10
-3pa, then in system, be filled with high-purity argon protection gas;
3rd step: regulate inductive source power to heat sample, holding temperature is 1450 ~ 1650K, and soaking time is 15 ~ 30min, starts directional freeze, and controlling directional freeze withdrawing rate is 5 ~ 20 μm/s; Continued propagation, to specimen length 50mm place, starts fast quenching and carries out rapid quenching to directional freeze sample, retain solid-liquid interface.
3. the TiAl intermetallic compound monocrystalline that lamellar orientation as claimed in claim 2 is completely controlled, it is characterized in that, in the first step, directional freeze diameter of rod is Φ (4 ~ 6mm) × 100mm.
4. the TiAl intermetallic compound monocrystalline that lamellar orientation as claimed in claim 2 is completely controlled, it is characterized in that, in second step, the corundum crucible of high-purity yttrium oxide coating is of a size of Φ (7 ~ 9mm) × 100mm; High-purity argon protection gas charge is 0.04 ~ 0.06MPa.
5. a preparation for the TiAl intermetallic compound monocrystalline that lamellar orientation as claimed in claim 1 is completely controlled, is characterized in that, comprises following concrete steps:
The first step: choose Ti, Al, Nb pure metal starting material that purity is 99.999%, carry out proportioning according to alloying constituent, be less than 10 in vacuum tightness
-3master alloy melting in the cold crucible levitation melting stove of Pa, makes alloying constituent homogenizing through 3 ~ 4 meltings, and directional freeze bar is cast in suction;
Second step: the corundum crucible that high-purity yttrium oxide coating put into by TiAl alloy coupon is carried out directional freeze, is evacuated to 5 × 10
-3pa, then in system, be filled with high-purity argon protection gas;
3rd step: regulate inductive source power to heat sample, holding temperature is 1450 ~ 1650K, and soaking time is 15 ~ 30min, starts directional freeze, and controlling directional freeze withdrawing rate is 5 ~ 20 μm/s; Continued propagation, to specimen length 50mm place, starts fast quenching and carries out rapid quenching to directional freeze sample, retain solid-liquid interface.
6. the preparation of the TiAl intermetallic compound monocrystalline that lamellar orientation as claimed in claim 5 is completely controlled, it is characterized in that, in the first step, directional freeze diameter of rod is Φ (4 ~ 6mm) × 100mm.
7. the preparation of the TiAl intermetallic compound monocrystalline that lamellar orientation as claimed in claim 5 is completely controlled, it is characterized in that, in second step, the corundum crucible of high-purity yttrium oxide coating is of a size of Φ (7 ~ 9mm) × 100mm; High-purity argon protection gas charge is 0.04 ~ 0.06MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410528019.3A CN104328501B (en) | 2014-10-09 | 2014-10-09 | TiAl single crystal alloy with fully controllable lamellar orientation and preparation method thereof |
| RU2017115945A RU2701438C2 (en) | 2014-10-09 | 2015-10-09 | Monocrystalline material of intermetallic compound of titanium and aluminium and methods for production thereof |
| EP15849516.8A EP3205753B1 (en) | 2014-10-09 | 2015-10-09 | Preparation method for a tial intermetallic compound single crystal material |
| US15/517,165 US10570531B2 (en) | 2014-10-09 | 2015-10-09 | TiAl intermetallic compound single crystal material and preparation method therefor |
| PCT/CN2015/091508 WO2016055013A1 (en) | 2014-10-09 | 2015-10-09 | Tial intermetallic compound single crystal material and preparation method therefor |
| JP2017538285A JP6944874B2 (en) | 2014-10-09 | 2015-10-09 | Single crystal material of TiAl intermetallic compound and its manufacturing method |
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| CN104878444A (en) * | 2015-05-13 | 2015-09-02 | 南京理工大学 | Preparation method of TiAl-base alloy monocrystal |
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| CN101875106B (en) * | 2009-11-20 | 2011-12-28 | 北京科技大学 | Preparation method of directional solidification high-niobium TiAl-base alloy |
| CN102011195B (en) * | 2010-11-23 | 2012-06-06 | 北京科技大学 | Preparation method of directional solidification high-Nb TiAl alloy single crystal |
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| CN113122756A (en) * | 2021-04-20 | 2021-07-16 | 西北工业大学 | Titanium-aluminum alloy with multistage twin crystal staggered structure and preparation method thereof |
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