CN104451490A - Method for preparing ultrafine grain titanium alloy by using alpha'' orthorhombic martensite microstructure - Google Patents

Method for preparing ultrafine grain titanium alloy by using alpha'' orthorhombic martensite microstructure Download PDF

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Publication number
CN104451490A
CN104451490A CN201410662915.9A CN201410662915A CN104451490A CN 104451490 A CN104451490 A CN 104451490A CN 201410662915 A CN201410662915 A CN 201410662915A CN 104451490 A CN104451490 A CN 104451490A
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titanium alloy
oblique
ultra
deformation
fine grain
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CN201410662915.9A
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刘彬
刘咏
相春杰
曹远奎
吴宏
谭艳妮
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Central South University
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Central South University
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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

Abstract

The invention discloses a method for preparing an ultrafine grain titanium alloy by using an alpha'' orthorhombic martensite microstructure. According to the method disclosed by the invention, based on the characteristic that a full alpha'' orthorhombic martensite structure can be obtained by using a double-phase titanium alloy consisting of specific components and having Mo equivalent of 4-8%, and by using a unique texture characteristic of alpha'' orthorhombic martensite, an ultrafine grain double-phase titanium alloy can be prepared by virtue of thermal deformation. The method specifically comprises the following steps: firstly, performing heat treatment on a deformed titanium alloy forging stock or sheared billet at Tbeta-Tbeta+80 DEG C (Tbeta is a beta phase transformation point), and quenching to room temperature to obtain the full alpha'' orthorhombic martensite structure; secondly, forging at Tbeta-(150-300) DEG C, and performing compressional deformation and block cold treatment; and finally, performing relief annealing treatment at 400-500 DEG C to obtain an ultrafine grain double-phase titanium alloy. By adopting the method disclosed by the invention, an ultrafine grain structure of which the average grain size is less than 0.5 micron can be obtained under the condition of small deformation, so that the method is suitable for various plastic deformation manners such as forging and extruding and is simple to operate; requirements can be met by virtue of conventional equipment; and therefore the method has a good application prospect.

Description

One utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy
Technical field
The present invention relates to the preparation method of the ultra-fine grain titanium alloy in materials science field, be specifically related to one and utilize α " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy.
Background technology
Titanium alloy has the little (4.51g/cm of density 3be about 40% of steel), intensity high (can more than 1000MPa be reached), antifatigue good (safe range of stress is the twice of steel), excellent corrosion resistance, good biocompatibility, the advantage such as nonmagnetic, enjoy the good reputation such as " space metal ", " marine metal " always, be obtained for widespread use in fields such as medical use, automobile making, aerospace and shipbuilding industries.Refinement titanium alloy tissue and obtain the performance such as intensity, fracture toughness property, antifatigue that the even nano level ultra-fine grain titanium alloy of submicron order can significantly improve titanium alloy, can increase substantially the ability of superplastic forming simultaneously, reduces superplastic forming temperature.For TC4 alloy, average grain size is less than the room temperature strength of the Ultra-fine Grained TC4 alloy of 1 μm can up to 1300MPa, superplasticity can be realized between 700 ~ 800 DEG C, more conventional grain-size is that the intensity of the TC4 alloy of about 10 μm improves about 30%, superplastic temperature reduces by more than 100 DEG C, therefore has important practical significance for the preparation of ultra-fine grain titanium alloy and organizational controls research.
At present, report/the published method preparing block body ultrafine grain titanium alloy has large plastic deformation method (Severe Plastic Deformation, and powder metallurgic method etc. SPD), wherein: Xi'an building university Zhao Xi one-tenth and Yang Xirong etc. disclose a kind of Equal Channel Angular Pressing preparation method (Chinese invention patent of high-strength superfine crystalline industrially pure titanium material, notification number CN101219444A and CN101624690A), concrete grammar is for be undertaken polishing by titanium alloy rod bar, smear lubricant process, then sample carried out the extruding of multi-pass equal-diameter bending passage and anneal, thus obtain Ultra-fine Grained titanium material.Through miter angle extruding deforming, grain-size is refined to 0.25 ~ 0.4 μm by original 23 ~ 28 μm, and room-temperature yield strength improves 50 ~ 90%.Shanghai Communications University Lv Wei is clean adopts the method for miter angle extruding deforming to prepare the titanium matrix composite (Chinese invention patent, notification number CN103572186A and CN103820744A) of Ultra-fine Grained with Wang Liqiang etc.The Li Hongyang of Beijing Institute of Technology etc. propose the method reversed with shearing compound and prepare titanium alloy micro-/ nano block (Chinese invention patent, notification number CN102234752A), specifically torsion extruding is combined with shear extrusion, realized the grain refining of titanium alloy material by the accumulative large sstrain amount of multi-pass processing.The Li Yuanyuan of South China Science & Engineering University etc. propose a kind of method for preparing powder metallurgy (Chinese invention patent, notification number CN102534301A) of high-strength low-modulus medical ultra-fine grain titanium matrix composite.In the method, obtain amorphous alloy powder by ball mill, then carry out plasma agglomeration obtain with β-Ti be matrix phase, the matrix material of the FeTi Ultra-fine Grained that is wild phase.Zhou Kechao etc. propose a kind of solution treatment in conjunction with viscous deformation and repeatedly timeliness to prepare the method (Chinese invention patent of Ultra-fine Grained near β titanium alloy (TC18), notification number CN103014574A), the β phase grain-size of the TC18 alloy obtained is 0.4 ~ 0.8 μm, and α phase grain-size is 0.1 ~ 0.3 μm.In above method, the method complex process such as Equal Channel Angular Pressing and torsion/shearing compound, working (machining) efficiency is low, resulting materials uneven microstructure, is difficult to realize maximizing and practical industrial production.Powder metallurgic method, owing to having the inherent defect such as impurity and hole, is difficult to realize significantly improving of performance.
Summary of the invention
Technical problem solved by the invention is to provide one to utilize α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy; this preparation method's technique is simple; easy to operate; can realize on the equipments such as the forging of routine, extruding; can be used for solving existing ultra-fine grain titanium alloy preparation method (as Equal Channel Angular Pressing etc.) complex process; cost is high, be difficult to the difficult problems such as practical.
Technical problem solved by the invention realizes by the following technical solutions:
One utilizes α " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy, comprises the following steps:
Step 1, be that the biphase titanium alloy material blank of alpha+beta is heated to T by type β~ T β+ 80 DEG C of (T βfor beta transformation point) carry out high-temperature heat treatment, carry out vacuum hardening process after thermal treatment completes, obtain " the biphase titanium alloy material of oblique side's martensitic structure that possesses α.
" the biphase titanium alloy material of oblique side's martensitic structure quickly heats up to T for step 2, the α that has by step 1 gained β-(150 ~ 300) DEG C temperature, this temperature isothermal treatment for short time 3 ~ 5 minutes, adopts high deformation speed to carry out pyroplastic deformability's process subsequently, finally the sample after deformation process is chilled to room temperature soon.
Step 3, the thermal deformation sample of step 2 gained is carried out Low-temperature stress-relief annealing process, after annealing, the cold or air cooling of stove is to room temperature, namely obtains the biphase titanium alloy with ultra-fine grained structure.
In the present invention, the alloy element in step 1 in titanium alloy material blank is one or several in Mo and Al, V, Nb, Cr, Zr, Sn, Zr, Si, and the Mo equivalent of alloy is 4 ~ 8%.
In the present invention, titanium alloy material selected in step 1 is heat-altered morphology blank, is preferably the forging stock of heat-altered morphology or excellent base.
In the present invention, in step 1, thermal treatment is carried out under vacuo, and in heat treatment process, vacuum tightness need higher than 1 × 10 -3pa, thermal treatment temp is T β~ T β+ 80 DEG C, soaking time is 1 ~ 4 hour.
In the present invention, in step 1, vacuum hardening processing mode is shrend, high-pressure helium or helium+nitrogen mixed gas quenching.
In the present invention, the biphase titanium alloy materials microstructure obtained in step 1 is mainly tiny acicular α " oblique side's martensite.
In the present invention, in step 2, the processing mode of pyroplastic deformability's process includes but not limited to forge hot and hot extrude, and it adopts treatment temp when forge hot and hot extrude process to be T β-(150 ~ 300) DEG C.For reducing the decomposition before being deformed of oblique side's martensite, plastic history adopts induction type rapid heating, isothermal treatment for short time and high-speed deformation method to carry out.Soaking time is 3 ~ 5 minutes, and the deformation strain speed of deformation process is 1 ~ 30s -1, under forging deformation condition, total deformation is 50% ~ 70%, and under extruding condition, extrusion ratio is 5 ~ 8, is chilled to room temperature soon after distortion.
In the present invention, the annealing temperature of the Low-temperature stress-relief annealing process in step 3 is 400 ~ 500 DEG C, and the anneal time is 2 ~ 5 hours.
Technical scheme provided by the present invention has following advantage and beneficial effect compared with the ultra-fine grain titanium alloy technology of preparing of prior art:
(1) the present invention utilize special component (Mo equivalent is 4 ~ 8%) biphase titanium alloy quenching gained α " oblique side's martensite has the feature of the defects such as highdensity dislocation, fault and tiny twin, in thermal deformation process, prepare ultra-fine grain titanium alloy material by the structure-reinforced dynamic recrystallization behavior of these superfines.
(2) technical scheme provided by the present invention is applicable to the multiple viscous deformation modes such as forging and extruding, and can carry out on the equipment such as the forging of routine, extruding, do not need other mould and frock, compared with conventional large plastometric set method (as Equal Channel Angular Pressing, high pressure torsion, multiway forging/compression etc.), more easily realize industrialization.
(3) prepare compared with ultra-fine grain titanium alloy method with existing distortion, the present invention can realize the super-refinement of microtexture under less deflection condition, is conducive to cutting down finished cost.
Accompanying drawing explanation
Fig. 1 is the EBSD figure of Ultra-fine Grained TC21 alloy prepared by embodiment 1.
Fig. 2 is the EBSD figure of Ultra-fine Grained TC16 alloy prepared by embodiment 2.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
Embodiment one:
Employing is of a size of Ti-6Al-2Sn-2Zr-3Mo-1Cr-2Nb-0.1Si (TC21, Mo equivalent is 5.27) the alloy forge hot state sample of Ф 40 × 60mm.By measuring its transformation temperature T βbe about 965 DEG C.Be 1 × 10 by sample in vacuum tightness -3be heated to 1000 DEG C under the vacuum state of Pa, be incubated and be cooled to room temperature with shrend after 1 hour, XRD analysis is carried out to its resultant and shows that quenching state alloy is for " oblique side's martensite is formed primarily of α.Subsequently sample is heated to texturing temperature 750 DEG C by induction heating mode, be incubated 3 minutes, warm forming machine forges, and deformation strain speed is about 20s -1, total deformation is 68%, jet cooling after forging completes.Finally the titanium alloy after forging is carried out stress relief annealing process in vacuum heat treatment furnace, treatment temp is 450 DEG C, and the time is 4 hours, and air cooling is to room temperature.As shown in Figure 1, average grain size is 0.35 μm to TC21 titanium alloy microtexture after distortion.
Embodiment two:
Employing is of a size of Ti-3Al-4Mo-4.5V (Mo equivalent is 7.2) the alloy forge hot state bar of Ф 35 × 50mm.By measuring its transformation temperature T βbe about 870 DEG C.Be 1 × 10 by bar in vacuum tightness -3be heated to 900 DEG C under the vacuum state of Pa, be incubated 1.5 hours, then use helium+nitrogen mixed gas quench cooled to room temperature.XRD analysis is carried out to its resultant and shows that quenching state alloy is for " oblique side's martensite is formed primarily of α.Subsequently the bar after quenching is heated to texturing temperature 680 DEG C by induction heating mode, be incubated 5 minutes, be incubated and terminate directly on heat extruder, to carry out crimp afterwards, extrusion ratio is 5, jet cooling after extruding completes.Finally the titanium alloy after extruding is carried out stress relief annealing process in vacuum heat treatment furnace, treatment temp is 400 DEG C, and 3 hours time, air cooling is to room temperature.As shown in Figure 2, average grain size is 0.43 μm to Ti-3Al-4Mo-4.5V alloy microtexture after distortion.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.

Claims (9)

1. utilizing α " oblique side's martensite microstructure prepares a method for ultra-fine grain titanium alloy, it is characterized in that, comprises the following steps:
Step 1, be that the biphase titanium alloy material blank of alpha+beta is heated to T by type β~ T β+ 80 DEG C are carried out high-temperature heat treatment, carry out vacuum hardening process after thermal treatment completes, and obtain and possess α " the biphase titanium alloy material of oblique side's martensitic structure, wherein, described T βfor beta transformation point;
" the biphase titanium alloy material of oblique side's martensitic structure quickly heats up to T for step 2, the α that has by step 1 gained β-(200 ~ 300) DEG C temperature, this temperature isothermal treatment for short time 3 ~ 5 minutes, adopts high deformation speed to carry out pyroplastic deformability's process subsequently, finally the sample after deformation process is chilled to room temperature soon, wherein, and described T βfor beta transformation point;
Step 3, the thermal deformation sample of step 2 gained is carried out Low-temperature stress-relief annealing process, after annealing, the cold or air cooling of stove is to room temperature, namely obtains the biphase titanium alloy with ultra-fine grained structure.
2. one according to claim 1 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy; it is characterized in that, the alloy element in step 1 in titanium alloy material blank is one or several in Mo and Al, V, Nb, Cr, Zr, Sn, Zr, Si.
3. one according to claim 2 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy, it is characterized in that, in described titanium alloy material blank, Mo equivalent is 4 ~ 8%.
4. " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy, it is characterized in that, described biphase titanium alloy material blank is the forging stock of heat-altered morphology or excellent base to utilize α according to any described in claims 1 to 3.
5. one according to claim 1 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy, it is characterized in that, in step 1, thermal treatment is carried out under vacuo, and in heat treatment process, vacuum tightness need higher than 1 × 10 -3pa, thermal treatment temp is T β~ T β+ 80 DEG C, soaking time is 1 ~ 4 hour.
6. one according to claim 1 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy, it is characterized in that, in step 1, vacuum hardening processing mode is shrend, high-pressure helium or helium+nitrogen mixed gas quenching.
7. one according to claim 1 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy; it is characterized in that; the biphase titanium alloy materials microstructure obtained in step 1 is mainly tiny acicular α " oblique side's martensite, " tiltedly the martensitic criterion of acceptability in side is hull beam is 0.02 ~ 0.4 μm to this acicular α, and length is 1 ~ 8 μm.
8. one according to claim 1 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy; it is characterized in that; in step 2, the processing mode of pyroplastic deformability's process is forge hot or hot extrude, and it adopts treatment temp when forge hot and hot extrude process to be T β-(150 ~ 300) DEG C, for reducing the decomposition before being deformed of oblique side's martensite, plastic history adopts induction type rapid heating, isothermal treatment for short time and high-speed deformation method to carry out, and soaking time is 3 ~ 5 minutes, and the deformation strain speed of deformation process is 1 ~ 30s -1, under forging deformation condition, total deformation is 50% ~ 70%, and under extruding condition, extrusion ratio is 5 ~ 8, is chilled to room temperature soon after distortion.
9. one according to claim 1 utilizes α, and " oblique side's martensite microstructure prepares the method for ultra-fine grain titanium alloy, it is characterized in that, the annealing temperature of the Low-temperature stress-relief annealing process in step 3 is 400 ~ 500 DEG C, and the anneal time is 2 ~ 5 hours.
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107604286A (en) * 2017-10-31 2018-01-19 成都先进金属材料产业技术研究院有限公司 A kind of beta-titanium alloy slab preparation method
CN107604285A (en) * 2017-10-31 2018-01-19 成都先进金属材料产业技术研究院有限公司 A kind of beta titanium alloy product forging method
CN108559935A (en) * 2018-07-05 2018-09-21 长沙理工大学 A kind of quick composite heat treating process improving titanium alloy mechanical property
CN109023190A (en) * 2018-10-08 2018-12-18 安徽工业大学 A kind of heat treatment method improving TC21 diphasic titanium alloy hardness
CN109182938A (en) * 2018-11-15 2019-01-11 西安交通大学 A kind of preparation method of the pure zirconium of Centimeter Level big crystal grain
CN109402542A (en) * 2018-12-05 2019-03-01 贵州大学 A method of gradient micro/nano-scale twin is obtained on TC21 titanium alloy surface layer
CN109554639A (en) * 2018-12-14 2019-04-02 陕西科技大学 A kind of method of high niobium Ti Al alloy lamellar structure refinement
CN110586824A (en) * 2019-08-26 2019-12-20 太原理工大学 Multidirectional isothermal forging method for refining titanium alloy grains by utilizing alpha' hexagonal martensite phase transformation
CN111979436A (en) * 2020-09-22 2020-11-24 西安稀有金属材料研究院有限公司 Preparation method for improving strength and toughness level of TC4 titanium alloy material
CN112662912A (en) * 2020-10-28 2021-04-16 西安交通大学 Ti-V-Mo-Zr-Cr-Al series high-strength metastable beta titanium alloy and preparation method thereof

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CN103014574A (en) * 2012-12-14 2013-04-03 中南大学 Preparation method of TC18 ultra-fine grain titanium alloy
CN103628010A (en) * 2013-12-17 2014-03-12 江苏大学 Photo-magnetic coupling method for improving plastic deformation capacity of aluminum matrix composite material
CN103732770A (en) * 2011-06-17 2014-04-16 钛金属公司 Method for the manufacture of alpha-beta TI-AL-V-MO-FE alloy sheets

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CN103732770A (en) * 2011-06-17 2014-04-16 钛金属公司 Method for the manufacture of alpha-beta TI-AL-V-MO-FE alloy sheets
CN103014574A (en) * 2012-12-14 2013-04-03 中南大学 Preparation method of TC18 ultra-fine grain titanium alloy
CN103628010A (en) * 2013-12-17 2014-03-12 江苏大学 Photo-magnetic coupling method for improving plastic deformation capacity of aluminum matrix composite material

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107604286B (en) * 2017-10-31 2019-10-01 成都先进金属材料产业技术研究院有限公司 A kind of beta-titanium alloy slab preparation method
CN107604285A (en) * 2017-10-31 2018-01-19 成都先进金属材料产业技术研究院有限公司 A kind of beta titanium alloy product forging method
CN107604286A (en) * 2017-10-31 2018-01-19 成都先进金属材料产业技术研究院有限公司 A kind of beta-titanium alloy slab preparation method
CN107604285B (en) * 2017-10-31 2019-10-01 成都先进金属材料产业技术研究院有限公司 A kind of beta titanium alloy product forging method
CN108559935A (en) * 2018-07-05 2018-09-21 长沙理工大学 A kind of quick composite heat treating process improving titanium alloy mechanical property
CN108559935B (en) * 2018-07-05 2019-12-06 长沙理工大学 Rapid composite heat treatment process for improving mechanical property of titanium alloy
CN109023190A (en) * 2018-10-08 2018-12-18 安徽工业大学 A kind of heat treatment method improving TC21 diphasic titanium alloy hardness
CN109182938A (en) * 2018-11-15 2019-01-11 西安交通大学 A kind of preparation method of the pure zirconium of Centimeter Level big crystal grain
CN109182938B (en) * 2018-11-15 2020-06-19 西安交通大学 Preparation method of centimeter-level large-grain pure zirconium
CN109402542B (en) * 2018-12-05 2020-09-15 贵州大学 Method for obtaining gradient micro-nano scale twin crystals on TC21 titanium alloy surface layer
CN109402542A (en) * 2018-12-05 2019-03-01 贵州大学 A method of gradient micro/nano-scale twin is obtained on TC21 titanium alloy surface layer
CN109554639B (en) * 2018-12-14 2021-07-30 陕西科技大学 Method for refining high-niobium TiAl alloy lamellar structure
CN109554639A (en) * 2018-12-14 2019-04-02 陕西科技大学 A kind of method of high niobium Ti Al alloy lamellar structure refinement
CN110586824B (en) * 2019-08-26 2021-06-08 太原理工大学 Multidirectional isothermal forging method for refining titanium alloy grains by utilizing alpha' hexagonal martensite phase transformation
CN110586824A (en) * 2019-08-26 2019-12-20 太原理工大学 Multidirectional isothermal forging method for refining titanium alloy grains by utilizing alpha' hexagonal martensite phase transformation
CN111979436A (en) * 2020-09-22 2020-11-24 西安稀有金属材料研究院有限公司 Preparation method for improving strength and toughness level of TC4 titanium alloy material
CN111979436B (en) * 2020-09-22 2021-11-16 西安稀有金属材料研究院有限公司 Preparation method for improving strength and toughness level of TC4 titanium alloy material
CN112662912A (en) * 2020-10-28 2021-04-16 西安交通大学 Ti-V-Mo-Zr-Cr-Al series high-strength metastable beta titanium alloy and preparation method thereof

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