CN107354331B - The method for controlling TiAl-base alloy oriented freezing organization lamellar orientation as substrate seed crystal using refractory metal - Google Patents

The method for controlling TiAl-base alloy oriented freezing organization lamellar orientation as substrate seed crystal using refractory metal Download PDF

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CN107354331B
CN107354331B CN201710575889.XA CN201710575889A CN107354331B CN 107354331 B CN107354331 B CN 107354331B CN 201710575889 A CN201710575889 A CN 201710575889A CN 107354331 B CN107354331 B CN 107354331B
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tial
refractory metal
directional solidification
seed crystal
base alloy
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CN107354331A (en
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苏彦庆
刘桐
骆良顺
王亮
李新中
陈瑞润
郭景杰
傅恒志
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Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/04Influencing the temperature of the metal, e.g. by heating or cooling the mould
    • B22D27/045Directionally solidified castings
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium

Abstract

The method for controlling TiAl-base alloy oriented freezing organization lamellar orientation as substrate seed crystal using refractory metal, it is related to a kind of TiAl-base alloy directional freeze method, and in particular to a kind of method for being oriented solidification control TiAl-base alloy oriented freezing organization lamellar orientation as substrate seed crystal material using refractory metal.The present invention is to solve the problems, such as that Composition Transient is longer in conventional seed-grain method directional solidification process.This method: one, foundry alloy melting;Two, refractory metal and directional solidification bar connect;Three, start directional solidification.The present invention is compared with traditional seed-grain method, and when doing substrate seed crystal material directional solidification using refractory metal, this method has many advantages, such as shorter Composition Transient, the technique of simplification and higher growth stability.The invention belongs to TiAl-base alloy directional solidification fields.

Description

TiAl-base alloy oriented freezing organization lamella is controlled by substrate seed crystal of refractory metal The method of orientation
Technical field
It is related to that the present invention relates to a kind of TiAl-base alloy directional freeze methods, and in particular to make using a kind of refractory metal The method for being oriented solidification control TiAl-base alloy oriented freezing organization lamellar orientation for substrate seed crystal material.
Background technique
TiAl-base alloy is a kind of high temperature structural material in the great application prospect of aerospace field, uses temperature Range is between 650 DEG C~1000 DEG C.The room temperature texture of TiAl-base alloy is usually by γ phase (TiAl) and α2Phase (Ti3Al it) constitutes, Studies have shown that complete lamellar structure (α2+ γ) there is optimal comprehensive mechanical property.But the lamella of full sheet layer TiAl-base alloy Orientation has apparent anisotropy, and when lamellar orientation is consistent with alloy Impact direction, full sheet layer TiAl alloy can express Optimal strong plasticity.
Research heat both at home and abroad is had become using the lamellar orientation in directional solidification technique control TiAl alloy based alloy at present Point, still, since TiAl alloy itself is used as a kind of intermetallic compound, the complexity of process of setting results in directional solidification Its lamellar structure is controlled with very big difficulty.Its meeting after undergoing the solid-solid phase change process after a series of complex liquid-solid-phase changeable Form γ/α2Lamellar structure, in liquid/solid phase transition process, different primary phases leads to subsequent solidification path and final lamellar orientation Difference, people will use directional solidification technique control using solidification path different corresponding to two different primary phases as boundary's point Lamellar orientation processed is divided into two methods, i.e. control solidification path method and seed-grain method.
It is leading phase that seed-grain method directional solidification TiAl alloy, which is to control α phase, and satisfactory seed crystal is placed on fusing The bottom of alloy grows directional solidificating alloy on the basis of seed crystal, so that α phase is formed under the adductive crystallization of bottom seed crystal The lamellar structure parallel with the direction of growth.But in seed-grain method directional solidification process, seed crystal alloy and directional solidificating alloy Ingredient is often different, most common seed crystal alloy Ti-43Al-3Si alloy, the seed crystal alloy and current excellent combination property And the TiAl-base alloy component difference with prospect of the application is larger, such as Ti-48Al-2Cr-2Nb, Ti-48Al-5Nb.Therefore, In seed-grain method directional solidification process, often there is longer Composition Transient between seed crystal alloy and directional solidificating alloy.? In directional solidification process, Composition Transient is often also the critical stage of microstructure transformation, and longer Composition Transient may The fringe time of microstructure heredity can be made to elongate, reduce the stability of lamellar orientation.
Summary of the invention
The purpose of the present invention is to solve the longer problem in Composition Transient in conventional seed-grain method directional solidification process, Provide a kind of method that TiAl-base alloy oriented freezing organization lamellar orientation is controlled as substrate seed crystal using refractory metal.
Using refractory metal as substrate seed crystal control TiAl-base alloy oriented freezing organization lamellar orientation method according to Lower step carries out:
One, foundry alloy melting: melting is carried out to TiAl-base alloy using vacuum induction water jacketed copper crucible, and pours and casts out female conjunction Ingot;
Two, refractory metal and directional solidification bar connect: being cut from mother alloy ingot using spark cutting method The refractory metal of same diameter and cylindrical rod material reason are bonded to together, are put into ceramic tube by cylinder bar, then will pottery Porcelain tube is incorporated in the Bridgman directional solidification furnace of high-purity argon gas protection, and the linkage interface of refractory metal and cylinder bar Lower than the freezing interface of directional solidification starting;
Three, start directional solidification: starting Bridgman directional solidification furnace is heated to 1500 DEG C~1800 DEG C and carries out hot steady Fixedization handle 15 minutes~30 minutes, start directional solidification drawing device, directional solidification growth rate be 10 μm/s~50 μm/ S, it is oriented solidification under 10 DEG C/mm~30 DEG C/mm temperature gradient, until rapid quenching is carried out when directional solidification 40mm, when fixed When being reduced to 200 DEG C or less to solidification room temperature, directional solidification room is opened, directional solidificating alloy ingot casting is obtained.
TiAl-base alloy described in step 1 is by atomic percentage content by 47% Al, 1.0% W, 0.5% Si and remaining The Ti of amount is formed;Or the TiAl-base alloy is made of by atomic percentage content 47% Al and the Ti of surplus.
Refractory metal described in step 2 is Ti or Nb.
The diameter of cylinder bar described in step 2 is 6mm.
" Bridgman device for directionally solidifying " of the present invention comes from Liu Tong, Luo Liangshun, Su Yanqing et al. in 2016,31 (5): 618-626 is published in entitled " the Effect of growth rate of Journal of Material Research on microstructures and microhardness in directionally solidified Ti–47Al– 1.0W–0.5Si alloy》。
The present invention is substituted using high-melting-point pure metal Ti, Nb as substrate seed crystal in seed-grain method directional solidification process Conventional seed crystal alloy, since the temperature of directional solidification heating is 1600 DEG C, and the fusing point of pure Ti is 1680 DEG C, and the fusing point of Nb is 2468 DEG C, therefore the heating temperature of directional solidification can not be by high-melting-point pure metal seed crystal alloy melting, and directional solidificating alloy Start to orient in high-melting-point pure metal seed crystal alloy interface forward position after starting directional solidification pull system for molten condition Growth, so that Composition Transient be not present between seed crystal alloy and directional solidificating alloy, and Ti, Nb be as strong β phase stable element, Alloy can be made to come into being leading phase β phase in directional solidification simultaneously, to achieve the purpose that controlling alloy sheet interlayer is orientated.
The present invention uses high-melting-point pure metal Ti and Nb as seed crystal base material, using common Bridgman directional solidification System controls TiAl-base alloy oriented freezing organization lamellar orientation, eliminates original as substrate seed crystal by using refractory metal Beginning as cast condition area's microstructure to starting interface microstructure adverse effect, while ensure alloy leading phase be β phase, to reach Control the purpose of alloy sheet interlayer orientation.
It is binary Ti-47Al (at.%) by directional solidification TiAl alloy ingredient prepared by refractory metal seed crystal material With polynary Ti-47Al-1.0W-0.5Si (at.%) alloy.The present invention is done compared with traditional seed-grain method using refractory metal When substrate seed crystal material directional solidification, this method has shorter Composition Transient, the technique of simplification and higher growth steady The advantages that qualitative.
Detailed description of the invention
Fig. 1 is using high-melting-point pure metal Ti in embodiment 1 as substrate seed crystal material directional solidification Ti-47Al-1.0W- 0.5Si alloy seeding interface micro-organization chart;
Fig. 2 is using high-melting-point pure metal Ti in embodiment 1 as substrate seed crystal material directional solidification Ti-47Al-1.0W- 0.5Si alloy seeding interface seeding Interface composition line scanning figure, a indicates that Al, b indicate that Si, c indicate that W, d indicate Ti in figure;
Fig. 3 is using high-melting-point pure metal Ti in embodiment 1 as substrate seed crystal material directional solidification Ti-47Al-1.0W- Micro-organization chart of 0.5Si alloy steady-state growth area;
Fig. 4 is using high-melting-point pure metal Nb in embodiment 2 as substrate seed crystal material directional solidification Ti-47Al-1.0W- 0.5Si alloy seeding interface micro-organization chart;
Fig. 5 is using high-melting-point pure metal Nb in embodiment 2 as substrate seed crystal material directional solidification Ti-47Al-1.0W- 0.5Si alloy seeding interface seeding Interface composition line scanning figure, a indicates that Ti, b indicate that Al, c indicate that W, d indicate Si, e in figure Indicate Nb;
Fig. 6 is using high-melting-point pure metal Nb in embodiment 2 as substrate seed crystal material directional solidification Ti-47Al-1.0W- Micro-organization chart of 0.5Si alloy steady-state growth area;
Fig. 7 is drawn using high-melting-point pure metal Ti as substrate seed crystal material directional solidification Ti-47Al alloy in embodiment 3 Brilliant interface micro-organization chart;
Fig. 8 is drawn using high-melting-point pure metal Ti as substrate seed crystal material directional solidification Ti-47Al alloy in embodiment 3 Brilliant interface seeding Interface composition line scanning figure;
Fig. 9 is steady as substrate seed crystal material directional solidification Ti-47Al alloy using high-melting-point pure metal Ti in embodiment 3 State vitellarium micro-organization chart;
Figure 10 is using high-melting-point pure metal Nb in embodiment 4 as substrate seed crystal material directional solidification Ti-47Al alloy Seeding interface micro-organization chart;
Figure 11 is using high-melting-point pure metal Nb in embodiment 4 as substrate seed crystal material directional solidification Ti-47Al alloy Seeding interface seeding Interface composition line scanning figure;
Figure 12 is using high-melting-point pure metal Nb in embodiment 4 as substrate seed crystal material directional solidification Ti-47Al alloy Micro-organization chart of steady-state growth area.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment Any combination.
Specific embodiment 1: present embodiment controls TiAl-base alloy directional solidification by substrate seed crystal of refractory metal The method of tissue lamellar orientation follows the steps below:
One, foundry alloy melting: melting is carried out to TiAl-base alloy using vacuum induction water jacketed copper crucible, and pours and casts out female conjunction Ingot;
Two, refractory metal and directional solidification bar connect: being cut from mother alloy ingot using spark cutting method The refractory metal of same diameter and cylindrical rod material reason are bonded to together, are put into ceramic tube by cylinder bar, then will pottery Porcelain tube is incorporated in the Bridgman directional solidification furnace of high-purity argon gas protection, and the linkage interface of refractory metal and cylinder bar Lower than the freezing interface of directional solidification starting;
Three, start directional solidification: starting Bridgman directional solidification furnace is heated to 1500 DEG C~1800 DEG C and carries out hot steady Fixedization handle 15 minutes~30 minutes, start directional solidification drawing device, directional solidification growth rate be 10 μm/s~50 μm/ S, it is oriented solidification under 10 DEG C/mm~30 DEG C/mm temperature gradient, until rapid quenching is carried out when directional solidification 40mm, when fixed When being reduced to 200 DEG C or less to solidification room temperature, directional solidification room is opened, directional solidificating alloy ingot casting is obtained.
Specific embodiment 2: the present embodiment is different from the first embodiment in that TiAl base described in step 1 is closed Gold by atomic percentage content by 47% Al, 1.0%~W, 0.5% Si and the Ti of surplus form;Or the TiAl base Alloy is made of by atomic percentage content 47% Al and the Ti of surplus.It is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two described in step 2 Refractory metal be Ti or Nb.It is other identical as one of specific embodiment one or two.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three described in step 2 The diameter of cylinder bar is 6mm.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: being heated in step 3 unlike one of present embodiment and specific embodiment one to four To 1700 DEG C and carry out thermostabilization processing 18 minutes~25 minutes.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: being heated in step 3 unlike one of present embodiment and specific embodiment one to five To 1600 DEG C and carry out thermostabilization processing 20 minutes.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: pull in step 3 unlike one of present embodiment and specific embodiment one to six Rate is 40 μm/s.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: pull in step 3 unlike one of present embodiment and specific embodiment one to seven Rate is 30um/s.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight 15 in step 3 DEG C/mm~25 DEG C/mm temperature gradient under be oriented solidification.It is other identical as one of specific embodiment one to eight.1
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine 20 in step 3 DEG C/temperature gradient of mm under be oriented solidification.It is other identical as one of specific embodiment one to nine.
Using following experimental verifications effect of the present invention:
Embodiment 1:
The present embodiment is using high-melting-point pure metal Ti as seed crystal base material directional solidification Ti-47Al-1.0W-0.5Si Alloy is realized by following step:
One, by the Ti-47Al-1.0W-0.5Si alloy cast ingot of the Φ 6mm × 100mm cut from master alloy and Φ 6mm × The pure Ti bar physical adhesion of 20mm has then been put into Y to together2O3The Al of coating2O3In ceramic tube, it is connected to directional solidification System pumping rod;
Two, start directional solidification vacuum system, vacuumize, and be passed through high-purity argon gas, then start heating device, be heated to Temperature at directional solidification startup interface is 1600 DEG C, then carries out the thermostabilization processing of 30min, guarantees directional solidificating alloy The stability of melt;
Three, start directional solidification drawing device, directional solidification growth rate control is 10 μm/s;
Four, when pull is to 40mm, rapid quenching, solid/liquid interfaces when can retain alloy oriented growth are carried out;
Five, directional solidification heating system is closed, when directional solidification room temperature is reduced to 200 DEG C or less, opens orientation Room is solidified, directional solidificating alloy ingot casting is obtained;
It is longitudinally slit along directional solidification ingot casting using Electric Discharge Wire-cutting Technology, it is obtained by standard metallographic preparation method of sample Take the macro microstructure in directional solidification ingot casting seed crystal seeding interface, it can be seen that obtain and grow in front of seed crystal seeding interface The parallel lamellar structure in direction is shown in Fig. 1, and show that alloying component transition region is only 1.2mm by component lines scanning, sees Fig. 2, and And the lamellar structure parallel with the direction of growth grows to always the steady-state growth stage of directional solidificating alloy, sees Fig. 3.
Embodiment 2:
The present embodiment is using high-melting-point pure metal Nb as seed crystal base material directional solidification Ti-47Al-1.0W-0.5Si Alloy is realized by following step:
One, by the Ti-47Al-1.0W-0.5Si alloy cast ingot of the Φ 6mm × 100mm cut from master alloy and Φ 6mm × The pure Ti bar physical adhesion of 20mm has then been put into Y to together2O3The Al of coating2O3In ceramic tube, it is connected to directional solidification System pumping rod;
Two, start directional solidification vacuum system, vacuumize, and be passed through high-purity argon gas, then start heating device, be heated to Temperature at directional solidification startup interface is 1600 DEG C, then carries out the thermostabilization processing of 15min, guarantees directional solidificating alloy The stability of melt;
Three, start directional solidification drawing device, directional solidification growth rate control is 30 μm/s;
Four, when pull is to 40mm, rapid quenching is carried out, solid/liquid interfaces when retaining alloy oriented growth;
Five, directional solidification heating system is closed, when directional solidification room temperature is reduced to 200 DEG C or less, opens orientation Room is solidified, directional solidificating alloy ingot casting is obtained;
It is longitudinally slit along directional solidification ingot casting using Electric Discharge Wire-cutting Technology, it is obtained by standard metallographic preparation method of sample Directional solidification ingot casting seed crystal seeding interface macrostructure is taken, it can be seen that about five columns are obtained in front of seed crystal interface Crystalline substance, lamellar structure and the direction of growth are shown in Fig. 4 close to parallel in each column crystal.And by component lines scanning obtain alloy at Point transition region is only 0.6mm, sees Fig. 5.And lamellar structure of the directional solidificating alloy in the steady-state growth stage also inherits seeding circle Microstructure at face, is shown in Fig. 6.
Embodiment 3:
The present embodiment is passed through using high-melting-point pure metal Ti as seed crystal base material directional solidification Ti-47Al alloy following Step is realized:
One, by the Ti-47Al-1.0W-0.5Si alloy cast ingot of the Φ 6mm × 100mm cut from master alloy and Φ 6mm × The pure Ti bar of 20mm docks, and has then been put into Y2O3The Al of coating2O3In ceramic tube, it is connected to directional solidification system pumping rod;
Two, start directional solidification vacuum system, vacuumize, and be passed through high-purity argon gas, then start heating device, be heated to Temperature at directional solidification startup interface is 1600 DEG C, then carries out the thermostabilization processing of 15min, guarantees directional solidificating alloy The stability of melt;
Three, start directional solidification drawing device, directional solidification growth rate control is 30 μm/s;
Four, when pull is to 40mm, rapid quenching is carried out, solid/liquid interfaces when retaining alloy oriented growth;
Five, directional solidification heating system is closed, when directional solidification room temperature is reduced to 200 DEG C or less, opens orientation Room is solidified, directional solidificating alloy ingot casting is obtained;
It is longitudinally slit along directional solidification ingot casting using Electric Discharge Wire-cutting Technology, it is obtained by standard metallographic preparation method of sample Directional solidification ingot casting seed crystal seeding interface macrostructure has been taken, has been obtained in front of seed crystal seeding interface close with the direction of growth Parallel lamellar structure, is shown in Fig. 7, and show that alloying component transition region is only 1.0mm by component lines scanning, sees Fig. 8, and with The parallel lamellar orientation of the direction of growth grows to always the steady-state growth stage, sees Fig. 9.
Embodiment 4:
The present embodiment is passed through using high-melting-point pure metal Nb as seed crystal base material directional solidification Ti-47Al alloy following Step is realized:
One, by the Ti-47Al-1.0W-0.5Si alloy cast ingot of the Φ 6mm × 100mm cut from master alloy and Φ 6mm × The pure Ti bar of 20mm docks, and has then been put into Y2O3The Al of coating2O3In ceramic tube, it is connected to directional solidification system pumping rod;
Two, start directional solidification vacuum system, vacuumize, and be passed through high-purity argon gas, then start heating device, be heated to Temperature at directional solidification startup interface is 1600 DEG C, then carries out the thermostabilization processing of 15min, guarantees directional solidificating alloy The stability of melt;
Three, start directional solidification drawing device, directional solidification growth rate control is 50 μm/s;
Four, when pull is to 40mm, rapid quenching is carried out, solid/liquid interfaces when retaining alloy oriented growth;
Five, directional solidification heating system is closed, when directional solidification room temperature is reduced to 200 DEG C or less, opens orientation Room is solidified, directional solidificating alloy ingot casting is obtained;
It is longitudinally slit along directional solidification ingot casting using Electric Discharge Wire-cutting Technology, it is obtained by standard metallographic preparation method of sample The macro microstructure in directional solidification ingot casting seed crystal seeding interface has been taken, has obtained in front of seed crystal seeding interface and is connect with the direction of growth Subparallel lamellar structure, is shown in Figure 10.And show that alloying component transition region is only 0.6mm by component lines scanning, see Figure 11.And And the lamellar orientation parallel with the direction of growth grows to always the steady-state growth stage, sees Figure 12.

Claims (8)

1. in the method that refractory metal controls TiAl-base alloy oriented freezing organization lamellar orientation as substrate seed crystal, feature exists In using refractory metal as substrate seed crystal control TiAl-base alloy oriented freezing organization lamellar orientation method according to the following steps It carries out:
One, foundry alloy melting: melting is carried out to TiAl-base alloy using vacuum induction water jacketed copper crucible, and pours and casts out master alloy Ingot;
Two, refractory metal and directional solidification bar connect: cylinder is cut from mother alloy ingot using spark cutting method The refractory metal of same diameter and cylindrical rod material reason are bonded to together, are put into ceramic tube, then by ceramic tube by bar It is incorporated in the Bridgman directional solidification furnace of high-purity argon gas protection, and the linkage interface of refractory metal and cylinder bar is lower than The freezing interface of directional solidification starting;
Three, start directional solidification: starting Bridgman directional solidification furnace is heated to 1500 DEG C~1800 DEG C and carries out thermostabilization Processing 15 minutes~30 minutes starts directional solidification drawing device, is 10 μm/s~50 μm/s, 10 in directional solidification growth rate DEG C/mm~30 DEG C/mm temperature gradient under be oriented solidification, until when directional solidification 40mm, rapid quenching is carried out, when orientation is solidifying Gu room temperature is reduced to 200 DEG C or less, directional solidification room is opened, directional solidificating alloy ingot casting is obtained;
Refractory metal described in step 2 is Nb;TiAl-base alloy described in step 1 is by atomic percentage content by 47% The Ti composition of Al, 1.0% W, 0.5% Si and surplus;Or the TiAl-base alloy presses atomic percentage content by 47% The Al and Ti of surplus composition.
2. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that the diameter of cylinder bar described in step 2 be 6mm.
3. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that be heated in step 3 1700 DEG C and carry out thermostabilization handle 18 minutes~25 minutes.
4. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that be heated in step 3 1600 DEG C and carry out thermostabilization handle 20 minutes.
5. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that in step 3 withdrawing rate be 40 μm/s.
6. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that in step 3 withdrawing rate be 30um/s.
7. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that be oriented solidification under 15 DEG C/mm~25 DEG C/mm temperature gradient in step 3.
8. controlling TiAl-base alloy oriented freezing organization lamella as substrate seed crystal using refractory metal according to claim 1 to take To method, it is characterised in that solidification is oriented in step 3 under the temperature gradient of 20 DEG C/mm.
CN201710575889.XA 2017-07-14 2017-07-14 The method for controlling TiAl-base alloy oriented freezing organization lamellar orientation as substrate seed crystal using refractory metal Expired - Fee Related CN107354331B (en)

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