CN107904530B - A kind of heat treatment method of thinning TiAl alloy full sheet layer group size - Google Patents

A kind of heat treatment method of thinning TiAl alloy full sheet layer group size Download PDF

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CN107904530B
CN107904530B CN201711269883.6A CN201711269883A CN107904530B CN 107904530 B CN107904530 B CN 107904530B CN 201711269883 A CN201711269883 A CN 201711269883A CN 107904530 B CN107904530 B CN 107904530B
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tial alloy
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CN107904530A (en
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梁永锋
陈林
林均品
张来启
郝国建
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University of Science and Technology Beijing USTB
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

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Abstract

The invention proposes a kind of heat treatment methods of thinning TiAl alloy full sheet layer group size, belong to technical field of metal material preparation.Compared with other tissues of TiAl alloy, full sheet layer TiAl alloy tissue elevated temperature strength, creep-resistant property and fracture toughness with higher.But alloy need to be heated to single-phase alpha phase zone and is heat-treated by complete lamellar structure, and crystal grain is grown up seriously under the conditions of this high temperature is single-phase, cause full sheet layer group size coarse, and room temperature toughness plasticity degradation influences room temperature processing and assembly.Tiny complete lamellar structure is the desired tissue of TiAl alloy.The present invention can finally obtain tiny complete lamellar structure, average platelet rolls into a ball size Control at 20~100 μm by quenching and being tempered two-step thermal treatment process.Due to having both applied at elevated temperature performance and low temperature toughness plasticity, this tiny complete lamellar structure is with a wide range of applications.

Description

A kind of heat treatment method of thinning TiAl alloy full sheet layer group size
Technical field
It is the invention belongs to technical field of metal material preparation, in particular to a kind of that tiny martensite group is obtained by quenching It knits, then be suitably tempered and obtain the heat treatment mode of tiny complete lamellar structure.
Background technique
TiAl alloy becomes close due to having the characteristics that high light specific gravity, intensity, mechanical behavior under high temperature and excellent in oxidation resistance The hot spot that people research and develop over year.The density of TiAl alloy is only the half of nickel base superalloy, in 600~900 DEG C of temperature Section is possible to that high temperature alloy is replaced to make certain aerospace structure parts and the rotation of Surface power drive system or move back and forth knot Component is, it can be achieved that thrust-weight ratio and fuel efficiency increase substantially.
There are four types of typical microstructures for TiAl alloy: nearly γ organizes (NG), bifurcation tissue (Duplex), nearly lamellar structure (NL) and complete lamellar structure (FL).Since complete lamellar structure has higher elevated temperature strength, creep resistant compared to other tissues Performance and fracture toughness are the desired tissues of TiAl alloy application.And tiny crystal grain (lamella group) helps to improve TiAl conjunction The intensity and plasticity of gold, therefore the full sheet layer Youth League organization of fine uniform is direction and the hot spot of research.
The method and approach of the lamella of TiAl alloy refinement at present group mainly has: hot-working method, addition fining agent method, alloying And heat treating process etc..
Wherein, mainly have by the report that hot-working is rolled into a ball come thinning TiAl alloy sheet interlayer: L.Cheng et al. is in Journal " the Deformation and dynamic recrystallization that of Alloys and Compounds magazine is delivered Behavior of a high Nb containing TiAl alloy " and G.Wang et al. in Materials Science " the Flow behavior and microstructure evolution of a P/M that and Engineering A is delivered TiAl alloy during high temperature deformation " etc..The hot-working of these document reports is to TiAl The influence of alloy sheet interlayer group's size mainly causes dynamic recrystallization by carrying out deformation appropriate at high temperature, closes TiAl Gold plaque layer group is broken to occur nodularization again to refine crystal grain.TiAl alloy after general hot-working is bifurcation tissue, to obtain Complete lamellar structure also needs reheating to keep the temperature to the monophase field α and carries out the processing of full sheet layer.It is abnormal due to being easy in the monophase field α crystal grain Grow up, cause lamella Youth League organization coarse (generally at 200~1000 μm), so as to cause obtained complete lamellar structure plasticity compared with Difference.In order to avoid crystal grain is in the monophase field α abnormal growth, reheating temperature can be reduced, obtain the relatively fine nearly lamella of tissue Tissue, but its mechanical behavior under high temperature will be affected again.
Mainly have by the report that addition fining agent refines lamella group: what D.Hu was delivered on Intermetallics magazine " Effect of composition on grain refinement in TiAl-based alloys " and T.T.Cheng exist " the The mechanism of grain refinement in TiAl alloys delivered on Intermetallics magazine By boron addition an alternative hypothesis " etc., these reports are mainly taught through addition B member Element forms TiB or TiB as fining agent2Promote grain nucleation so as to cause crystal grain refinement as heterogeneous forming core core, and visits The refinement mechanism that B element rolls into a ball lamella and the influence to phase transformation and performance are begged for.But the thinning effect of B element is a certain amount of After tend to be saturated, excessive fining agent will have an adverse effect to mechanical property.
Mainly have by the report that alloyage refines lamella group: P.J.Maziasz et al. is in Intermetallics magazine " the Effects of B and W alloying additions on the formation and stability delivered Of lamellar structures in two-phase γ-TiAl ", Z.C.Liu et al. is sent out in Intermetallics magazine " the Effects of Nb and Al on the microstructures and mechanical properties of of table High Nb containing TiAl base alloys " and D.J.Larson et al. delivered in Intermetallics 《Tungsten segregation inα2+ γ titanium aluminides " etc..By adding Nb, W in TiAl alloy Equal beta stable elements carry out alloy and in phase transition process in a manner of β solidification by the inhibition to crystal boundary and phase boundary To refine lamella group and piece interlamellar spacing.But the beta stable element of high-content easily causes β segregation, and then generates at room temperature Brittle B2 phase causes Alloy At Room Temperature plasticity to decline.Excessive high temperature β phase will also cause elevated temperature strength reduction.
Mainly have by the report of heat treatment refinement lamella group: J.N.Wang et al. is delivered in Intermetallis magazine Article " Refining of coarse lamellar microstructure of TiAl alloys by rapid heat Treatment " elaborate the rapid cooling that different numbers are carried out near α transformation temperature;J.Yang et al. exists Intermetallics magazine is published an article " Control of the homogeneity of the lamellar Structure of a TiAl alloy refined by heat treatment " it elaborates to carry out heat near α transformation temperature Patent " the Heat treatment of gamma titanium aluminide that circulation and T.J.Kelly et al. are delivered Alloys " elaborate long term annealing etc. near α transformation temperature, to obtain relatively fine complete lamellar structure.But these Method and process is complicated, and process cycle is longer.
The present invention finally obtains full sheet of the average-size in 20~100 μ ms by quenching+tempering two-step thermal processing Layer tissue, this is refined crystal grain for TiAl alloy, improves its service performance and be of great significance using temperature.
Summary of the invention
The object of the present invention is to provide a kind of heat treatment methods of thinning TiAl alloy full sheet layer group size, pass through brine ice Quenching obtains tiny martensitic structure, then carries out suitably being tempered to obtain tiny complete lamellar structure.The method can be big Width reduces TiAl alloy full sheet layer and rolls into a ball size, to improve its mechanical property.Simultaneously this method compared with existing heat treatment method, Process cycle is shortened, efficiency is greatly improved.
The heat treatment method of a kind of thinning TiAl alloy full sheet layer group size, which is characterized in that after soak, using quenching The method of fire obtains tiny martensitic structure, then the sample with martensitic structure is carried out at a certain temperature appropriate Tempering can get the full sheet layer TiAl alloy tissue of fine uniform;
Specific steps process is:
Step 1, the preparation of raw material: TiAl alloy sample is polished, is cleaned by ultrasonic, dry up after be put into vacuumize and fill Processing is sealed in the quartz ampoule of argon gas.
Step 2, soak and quenching heat treatment: the sample after tube sealing is put into high temperature Muffle furnace and is heated, in TβTurn The more than temperature single-phase humidity province 10~30 DEG C of β keeps the temperature 0.5~3h;Brine ice quenching treatment is carried out later.
Step 3, the stone for vacuumizing applying argon gas secondary seal: will be put into after the polishing of quenched sample, ultrasonic cleaning, drying Ying Guanzhong is sealed processing.
Step 4, tempering heat treatment;Sample after tube sealing is put into high temperature Muffle furnace and is heated, in TαTransition temperature The above single-phase humidity province 10~30 DEG C of α keeps the temperature 0.5~3h, and furnace cooling to room temperature, obtaining average-size is 20~100 μm Complete lamellar structure.
Further, it is in vacuum sealing applying argon gas guard mode when TiAl alloy sample is heat-treated, and in vacuum tube Placing titanium ingot prevents from aoxidizing.
Further, hardening media is brine ice, and brine strength is 5~15%, and temperature is less than 0 DEG C.
Further, TiAl alloy quenching heat treatment cooling velocity is greater than 500 DEG C of s-1
Due to taking above-mentioned technical proposal, make the invention has the following advantages that
(1) present invention uses cryosel water quenching, and salt is precipitated while forming steam blanket in cooling down workpiece using salt water Crystal explosion destroys steam blanket, improves cooling velocity, is conducive to the formation of martensite.
(2) present invention makes it in second step using the method for the martensite α for obtaining tiny (2~5 μm) after high temperature quenching It (is tempered in the monophase field α) in drawing process, crystal grain, which is grown up, in the short time is controlled.And previous full sheet layer processing, need by Alloy directly heats single-phase alpha phase zone and is heat-treated, and crystal grain is grown up seriously under the conditions of this high temperature is single-phase, leads to full sheet layer group Size is coarse, performance decline.The present invention due to the refinement of initial alpha crystal grain makes that tiny (α can be formed during furnace is cold2+γ) Lamella group.
(3) present invention is by TβThe single-phase humidity province quenching of more than transition temperature 10~30 DEG C of β and TαTransition temperature with The upper single-phase humidity province tempering of 10~30 DEG C of α, this method universality is higher, can be used at the structure refinement of a variety of TiAl alloys Reason.
(4) device therefor of the present invention is simple, the simple process and period is short, therefore processing cost is lower.
Detailed description of the invention
The micro-organization chart of Fig. 1 Ti-43Al-9V-Y alloy sample: it (a) is obtained to be quenched after 1350 DEG C of heat preservation 3h Tiny martensitic structure, (b) for qtenched sample pass through 1250 DEG C of cold obtained tiny complete lamellar structures of heat preservation 1h furnace.
The micro-organization chart of Fig. 2 Ti-43Al-9V-Y alloy sample: it (a) is obtained to be quenched after 1360 DEG C of heat preservation 1h Tiny martensitic structure, (b) for qtenched sample pass through 1250 DEG C of cold obtained tiny complete lamellar structures of heat preservation 3h furnace.
The micro-organization chart of Fig. 3 Ti-42.5Al-6Nb-1Cr alloy sample: (a) for after 1400 DEG C of heat preservation 3h at quenching Obtained tiny martensitic structure is managed, (b) passes through 1250 DEG C of cold obtained tiny full sheet layer groups of heat preservation 1h furnace for qtenched sample It knits.
The micro-organization chart of Fig. 4 Ti-42.5Al-6Nb-3V alloy sample: (a) being to be quenched after 1380 DEG C of heat preservation 3h Obtained tiny martensitic structure (b) passes through 1250 DEG C of cold obtained tiny complete lamellar structures of heat preservation 1h furnace for qtenched sample, (c) pass through 1260 DEG C of cold obtained tiny complete lamellar structures of heat preservation 1h furnace for qtenched sample.
The tiny full sheet layer of Fig. 5 TiAl alloy rolls into a ball heat treatment process route.
Specific embodiment
Technical solution of the present invention is further illustrated below with reference to embodiment
Embodiment 1
The present embodiment is by taking Ti-43Al-9V-Y wrought alloy as an example, by TβMore than transition temperature 10 DEG C of humidity province quenchings And TαIt is more than transition temperature that 10 DEG C of humidity province tempering, finally obtain tiny full sheet tissue.Detailed process is as follows:
Step 1: the preparation of raw material.It takes from forging ingot having a size of 15mm × 10mm × 10mm square, sample is carried out It after polishing, ultrasonic cleaning and drying, is put into the quartz ampoule for vacuumize applying argon gas and is sealed processing, when sealing is put into titanium ingot With spacing samples, protection against oxidation is carried out.
Step 2: soak and quenching heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, is heated to 1350 DEG C (single-phase TβMore than transition temperature 10 DEG C) heat preservation 3h, then carry out cryosel water quenching.Cryosel water concentration is 5%.It is obtained after quenching Tissue be tiny martensite lath tissue, see Fig. 1 (a).
Step 3: secondary seal.The stone for vacuumizing applying argon gas will be put into after the polishing of quenched sample, ultrasonic cleaning, drying Ying Guanzhong is sealed processing.It is put into titanium ingot and spacing samples when sealing, carries out protection against oxidation.
Step 4: tempering heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, 1250 DEG C of (T are heated toαTransformation temperature Du or more 10 DEG C) heat preservation 1h, furnace cooling.Tempered structure is complete lamellar structure, and average platelet group size is refined to 30 μm, such as schemes Shown in 1 (b).
Embodiment 2
The present embodiment is by taking Ti-43Al-9V-Y alloy as an example, by TβThe quenching of more than transition temperature 20 DEG C of humidity provinces and TαIt is more than transition temperature that 10 DEG C of humidity province tempering, finally obtain tiny full sheet tissue.Detailed process is as follows:
Step 1: the preparation of raw material.It takes from forging ingot having a size of 15mm × 10mm × 10mm square, sample is carried out It after polishing, ultrasonic cleaning and drying, is put into the quartz ampoule for vacuumize applying argon gas and is sealed processing, when sealing is put into titanium ingot With spacing samples, protection against oxidation is carried out.
Step 2: soak and quenching heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, is heated to 1360 DEG C (single-phase TβMore than transition temperature 20 DEG C) heat preservation 1h, then carry out cryosel water quenching.Cryosel water concentration is 10%.It is obtained after quenching Tissue be tiny martensite lath tissue, see Fig. 2 (a).
Step 3: secondary seal.The stone for vacuumizing applying argon gas will be put into after the polishing of quenched sample, ultrasonic cleaning, drying Ying Guanzhong is sealed processing.It is put into titanium ingot and spacing samples when sealing, carries out protection against oxidation.
Step 4: tempering heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, 1250 DEG C of (T are heated toαTransformation temperature Du or more 10 DEG C) heat preservation 3h, furnace cooling.Tempered structure is complete lamellar structure, and average platelet group size is refined to 50 μm, such as schemes Shown in 2 (b).
Embodiment 3
The present embodiment is by taking Ti-42.5Al-6Nb-1Cr casting alloy as an example, by TβMore than transition temperature 20 DEG C of temperature Area's quenching and TαIt is more than transition temperature that 10 DEG C of humidity province tempering, finally obtain tiny full sheet tissue.Detailed process is as follows:
Step 1: the preparation of raw material.It is taken from ingot casting having a size of 7mm × 7mm × 3mm square, sample is beaten After mill, ultrasonic cleaning and drying, be put into the quartz ampoule for vacuumize applying argon gas and be sealed processing, when sealing be put into titanium ingot and Spacing samples carry out protection against oxidation.
Step 2: soak and quenching heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, is heated to 1400 DEG C (single-phase TβMore than transition temperature 20 DEG C) heat preservation 2h, then carry out cryosel water quenching.Cryosel water concentration is 5%.It is obtained after quenching Tissue be tiny martensite lath tissue, see Fig. 3 (a).
Step 3: secondary seal.The stone for vacuumizing applying argon gas will be put into after the polishing of quenched sample, ultrasonic cleaning, drying Ying Guanzhong is sealed processing.It is put into titanium ingot and spacing samples when sealing, carries out protection against oxidation.
Step 4: tempering heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, 1250 DEG C of (T are heated toαTransformation temperature Du or more 10 DEG C) heat preservation 1h, furnace cooling.Tempered structure is complete lamellar structure, and average platelet group size is refined to 70 μm, such as schemes Shown in 3 (b).
Embodiment 4
The present embodiment is by taking Ti-42.5Al-6Nb-3V casting alloy as an example, by TβMore than transition temperature 20 DEG C of humidity provinces Quenching and TαIt is more than transition temperature that 10 DEG C of humidity province tempering, finally obtain tiny full sheet tissue.Detailed process is as follows:
Step 1: the preparation of raw material.It is taken from ingot casting having a size of 7mm × 7mm × 3mm square, sample is beaten After mill, ultrasonic cleaning and drying, be put into the quartz ampoule for vacuumize applying argon gas and be sealed processing, when sealing be put into titanium ingot and Spacing samples carry out protection against oxidation.
Step 2: soak and quenching heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, is heated to 1380 DEG C (single-phase TβMore than transition temperature 20 DEG C) heat preservation 3h, then carry out cryosel water quenching.Cryosel water concentration is 5%.It is obtained after quenching Tissue be tiny martensite lath tissue, see Fig. 4 (a).
Step 3: secondary seal.The stone for vacuumizing applying argon gas will be put into after the polishing of quenched sample, ultrasonic cleaning, drying Ying Guanzhong is sealed processing.It is put into titanium ingot and spacing samples when sealing, carries out protection against oxidation.
Step 4: tempering heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, 1250 DEG C of (T are heated toαTransformation temperature Du or more 10 DEG C) heat preservation 1h, furnace cooling.Tempered structure is complete lamellar structure, and average platelet group size is refined to 40 μm, such as schemes Shown in 4 (b).
Embodiment 5
The present embodiment is by taking Ti-42.5Al-6Nb-3V casting alloy as an example, by TβMore than transition temperature 20 DEG C of humidity provinces Quenching and TαIt is more than transition temperature that 20 DEG C of humidity province tempering, finally obtain tiny full sheet tissue.Detailed process is as follows:
Step 1: the preparation of raw material.It is taken from ingot casting having a size of 7mm × 7mm × 3mm square, sample is beaten After mill, ultrasonic cleaning and drying, be put into the quartz ampoule for vacuumize applying argon gas and be sealed processing, when sealing be put into titanium ingot and Spacing samples carry out protection against oxidation.
Step 2: soak and quenching heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, is heated to 1380 DEG C (single-phase TβMore than transition temperature 20 DEG C) heat preservation 3h, then carry out cryosel water quenching.Cryosel water concentration is 5%.It is obtained after quenching Tissue be tiny martensite lath tissue, see Fig. 4 (a).
Step 3: secondary seal.The stone for vacuumizing applying argon gas will be put into after the polishing of quenched sample, ultrasonic cleaning, drying Ying Guanzhong is sealed processing.It is put into titanium ingot and spacing samples when sealing, carries out protection against oxidation.
Step 4: tempering heat treatment.Sample after tube sealing is put into high temperature Muffle furnace, 1260 DEG C of (T are heated toαTransformation temperature Du or more 20 DEG C) heat preservation 1h, furnace cooling.Tempered structure is complete lamellar structure, and average platelet group size is refined to 60 μm, such as schemes Shown in 4 (c).

Claims (4)

1. a kind of heat treatment method of thinning TiAl alloy full sheet layer group size, which is characterized in that after soak, using quenching Method obtain tiny martensitic structure, then the sample with martensitic structure is carried out appropriate time at a certain temperature Fire processing, can get the full sheet layer TiAl alloy tissue of fine uniform;
Specific steps process is:
Step 1, the preparation of raw material: TiAl alloy sample is polished, is cleaned by ultrasonic, dry up after be put into and vacuumize applying argon gas Quartz ampoule in be sealed processing;
Step 2, soak and quenching heat treatment: the sample after tube sealing is put into high temperature Muffle furnace and is heated, in TβTransition temperature The above single-phase humidity province 10~30 DEG C of β keeps the temperature 0.5~3h, carries out brine ice quenching treatment later, and obtained tissue is 2~5 μm tiny martensite lath structure;
Step 3, the quartz ampoule for vacuumizing applying argon gas secondary seal: will be put into after the polishing of quenched sample, ultrasonic cleaning, drying In be sealed processing;
Step 4, tempering heat treatment;Sample after tube sealing is put into high temperature Muffle furnace and is heated, in TαMore than transition temperature 10 The single-phase humidity province~30 DEG C of α, keeps the temperature 0.5~3h, and furnace cooling to room temperature obtains the full sheet that average-size is 20~100 μm Layer tissue.
2. the heat treatment method of a kind of thinning TiAl alloy full sheet layer group size according to claim 1, which is characterized in that TiAl alloy sample is in vacuum sealing applying argon gas guard mode when being heat-treated, and the anti-block of titanium ingot is placed in vacuum tube Change.
3. the heat treatment method of a kind of thinning TiAl alloy full sheet layer group size according to claim 1, which is characterized in that quench Fiery medium is brine ice, and brine strength is 5~15%, and temperature is less than 0 DEG C.
4. the heat treatment method of a kind of thinning TiAl alloy full sheet layer group size according to claim 1, which is characterized in that TiAl alloy quenching heat treatment cooling velocity is greater than 500 DEG C of s-1
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CN108385046B (en) * 2018-04-23 2021-01-19 江苏理工学院 Heat treatment method of TiAl-V alloy
CN109136806B (en) * 2018-11-09 2020-12-25 中国石油大学(华东) Preparation method of NiTi monocrystal in solid state by cyclic heat treatment
CN109797314B (en) * 2019-03-28 2020-10-30 陕西科技大学 High-niobium TiAl alloy with nano-scale grains and preparation method thereof
CN110079700A (en) * 2019-04-24 2019-08-02 江苏理工学院 A kind of TiAl alloy and preparation method thereof
CN110079753A (en) * 2019-04-24 2019-08-02 江苏理工学院 A kind of forging method for eliminating TiAl alloy remnants lamella
CN110144536B (en) * 2019-06-06 2021-07-16 南昌航空大学 Processing method of TiAl-based alloy with fine lamellar structure
CN112063944B (en) * 2020-07-30 2021-06-11 西北工业大学 Heat treatment method for controlling beta solidification casting TiAl alloy fine grain structure

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CN102011077B (en) * 2010-12-17 2012-09-05 北京航空航天大学 Method for controlling structure refinement of cast TiAl-based alloy and form of boride
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