CN106086739A - A kind of method preparing nano-structured titanium alloy material - Google Patents
A kind of method preparing nano-structured titanium alloy material Download PDFInfo
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- CN106086739A CN106086739A CN201610644359.1A CN201610644359A CN106086739A CN 106086739 A CN106086739 A CN 106086739A CN 201610644359 A CN201610644359 A CN 201610644359A CN 106086739 A CN106086739 A CN 106086739A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing 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
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The present invention discloses a kind of method preparing nano-structured titanium alloy material, including first applying Equal Channel Angular Pressing to process, makes the large plastometric set of the titanium alloy base material experience degree of depth；Again through rolling repeatedly, pulling eye, stretch, extrude and cross-forge step, to obtain the crystal structure of nanoscale, remake continuous high temperature, HIGH PRESSURE TREATMENT.The method obtains and makes its Nano-mter Ti-alloy material resisting fatigue, Resisting fractre and resistance to corrosion obtained and mechanical performance of excellence.
Description
Technical field
The invention belongs to metal material processing field, be specifically related to a kind of side preparing nano-structured titanium alloy material
Method.
Background technology
Titanium is a kind of argenteous transition metal, it is characterized by lightweight, intensity is high, tool metallic luster, also have good
Resistance to corrosion.Due to the chemical property that it is stable, good strong acid high temperature resistant, low temperature resistant, anti-, anti-highly basic, and high intensity,
Low-density, is " space metal " by good reputation.In metallic element, the specific strength of titanium is the highest.It is a kind of high intensity but low quality
Metal, and there is goodish ductility (especially in the environment of anaerobic).The surface of titanium is silvery white in color metallic luster.
Its fusing point at a relatively high (more than 1,649 degrees Celsius), so being good piece of refractory metal material.At present, titanium alloy is mainly applied
In aerospace field, meanwhile, titanium alloy demand in terms of field of medical materials is the most increasing, along with science and technology
Development, industrial quarters is more and more higher to the mechanical property requirements of titanium alloy material.
The method of conventionally manufactured titanium alloy material mainly has pendulum to be ground into shape, forging, drawing, rolling, swaging, torsion change
The working hardening such as shape, hydrostatic extrusion, to improve titanium alloy material intensity and to ensure certain toughness, but also can effectively refine crystalline substance
Grain.But the texture of the material obtained by said method has streamlined, and the crystal grain after refinement has directivity, and is little angle
Degree crystal boundary.Owing to titanium alloy is difficult-to-deformation material, the plasticity therefore obtaining material is poor, therefore, it is necessary to seek new technology and
Process, improves further titanium alloy material mechanical property, it is ensured that have high intensity and good on the premise of high density concurrently
Toughness.
Summary of the invention
It is an object of the invention to put forward a kind of method preparing nano-structured titanium alloy material.Mainly solve current titanium to close
The problem that gold copper-base alloy deformation is difficult, plasticity is poor, improves titanium alloy material resisting fatigue, Resisting fractre and resistance to corrosion simultaneously,
Obtain more optimal mechanical performance.
A kind of method preparing nano-structured titanium alloy material of the present invention, including by passages such as titanium alloy material processes
Corner extrusion, rolling so that it is the large plastometric set of the degree of depth, then through repeatedly stretching, extrude and cross-forge. obtain nanocrystalline structures
Titanium alloy material, it is characterised in that: Equal-channel Angular Pressing and rolling are the extruding of continuous non-isothermal and rolling.
The method of the invention described above, described Equal-channel Angular Pressing, rolling, its process sequence can be by extruding, rolling
Sequencing carry out, it is also possible to first rolling, the order of rear extruding are carried out, and they can also alternately, but technique should be
Continuous print, the temperature extruding and rolling each process section is not equal to.Be enough to make the large plastometric set of its degree of depth.
Described continuous non-isothermal, refers to that the Temperature Treatment that in whole technical process, each operation stage uses is different, but whole
Individual flow process is successional.
The method of the invention described above, farther includes nano-structured titanium alloy is carried out continuous high temperature, HIGH PRESSURE TREATMENT.Institute
State high temperature such as 700-850 DEG C in the ECAP in Fig. 6；Temperature 200-300 DEG C of hot-die, described high pressure is that high neat presses 500-
1200MPa, preferential 500-700MPa.
The method of the invention described above, farther includes pulling eye step.
The method of the invention described above, further, farther includes the annealing of titanium alloy.
The method of the invention described above, the temperature of its hot-die controls between 200-300 DEG C, and the temperature of roller controls at 20-
Between 50 DEG C.
The method of the invention described above, described nanometer, the average grain size of its nanometer is 40-70nm scope, preferably 40-
60nm scope.
The method of the invention described above, described equal channel angular is 90 degree of right angles, and Equal-channel Angular Pressing is various dimensions extruding,
Repeat 2-4 time.Equal-channel Angular Pressing is preferably the extruding of 3-dimensional degree, is preferably repeated 3 times.Described various dimensions extrude before and after referring to, a left side
Right, up and down and all directions omnibearing degree of depth shear extrusion such as torsion.
Described nano-structured titanium alloy material is pole stock.
The method of the present invention, its basic process is, first applies Equal-channel Angular Pressing (Equal-channel
Angular processing, ECAP) and rolling technology process, the preferred right angle of corner, ECAP extruding and rolling technology are regardless of elder generation
After, it is possible to alternately, make the large plastometric set of the titanium alloy base material experience degree of depth；Again through pulling eye repeatedly, stretch, extrude and cross-forge
Step, to obtain the crystal structure of nanoscale；Further, including the titanium alloy material work height continuously to nanostructured crystal phase
The temperature such as temperature in ECAP is 700-850 DEG C, and high pressure such as 500-1200MPa, preferential 500-700MPa process so that it is obtain anti-
Fatigue, Resisting fractre and resistance to corrosion, use continuous non-isothermal ECAP-to roll (Continuous Non-isothermal
ECAP-rolling) technology, makes titanium alloy reach superpower deformation.Each hot-die inlet diameter reduces step by step with minute yardstick, as often
Secondary by time reduce 0.002 inch (50.8 μm), the temperature of hot-die controls between 200-300 DEG C, and the temperature of roller then controls
Between 20-50 DEG C.Wherein, Equal-channel Angular Pressing ECAP is various dimensions extruding, repeats 2-4 time.Equal-channel Angular Pressing is excellent
Elect 3-dimensional degree (can be also simply referred to as 3D) extruding as, be preferably repeated 3 times.
Above-mentioned ECAP-rolls, and can set multiple ECAP and forge mould, and by corresponding roller institute " feedback connection ", these rollers are by cold
But the supply of agent maintains the temperature more much lower than the workpiece processed by ECAP.The body of rod outside ECAP forging mould
, then there is relative thermal expansion in sections, this thermal expansion can cause " back pressure " at ECAP die exit.This restraint is favourable
Formation in material internal fine structure.
The method of the invention described above, described extruding is at high static pressure such as 500-700MPa, can reach 1200MPa
Under, make processed titanium alloy material by a large amount of detrusions of controlled quantity, make material obtain the refinement of significant crystal grain.
Preferably, the method for the present invention, use the processing scheme of thermomechanical technique, in Fig. 6, whole process is directed to
High temperature, result shows, this thermomechanical processing scheme can make machined material internal structure realize more excellent homogeneity.
Such as, the characteristic evolution in the nanocrystalization processing of cp2 level titanium is investigated.Cp2 level titanium is annealed
During process, the load intensity when yield strain rate of 0.2% and limit surrender is up to 500-600MPa and 600-respectively
700MPa, and often with the forfeiture of quite significantly (the most unacceptable) ductility.But, when this titanium is made
After annealing, above-mentioned yield strain can just reach when 276Mpa is in 345MPa respectively.
On the other hand, under extremely low temperature, cp titanium being applied tension force stretching, typically less than 10% i.e. ruptures, and this works as
It is so unacceptable.But, when through scrupulous heat treatment, then the ductility of this kind of titanium can be made to reach acceptable water
Flat；But, this result is not easy to repeat.Therefore, the method for the present invention is taked to be combined ECAP processing with thermomechanical processing
The technique come can make processed titanium alloy material realize more optimal mechanical performance, as processed nano-structured cp 2 grades
With 4 grades of titaniums, the rod-shaped material of Ti-6Al-4V titanium alloy.Result shows, the controlled forging under technique of the present invention
Process, material (diameter 8.6mm, the bar of a length of 400mm) can be made to obtain along its length and on cross section and be more uniformly distributed
Internal structure, its characteristic variations is within ± 5%.And, to the cp2 level titanium after controlled conducting forging processing, as long as simply
Annealing, it is possible to promote the extension degree of more than 15%, and its intensity is not remarkably decreased.Therefore, it is possible to realizing routine
During the ductility of cp titanium so that it is intensity is greatly improved.Cp2 level and the performance improvement of 4 grades of titaniums, often exceeded
Advise medical Ti-6Al-4V titanium alloy.The yield strength of cp2 level titanium and extreme hot strength respectively reach 1000MPa
With the yield strength of more than 1100MPa, cp4 level titanium and extreme hot strength respectively reach 1050MPa Yu 1200MPa with
On.The improvement of these unprecedented performances, is possible not only to strengthen the performance of cp titanium device, and in some application-specific
The Ti-6Al-4V titanium alloy of routine replaced by middle cp class titanium.
The method of the invention described above, in some embodiments, also includes more heat treatment-machinery forging (rolling, broaching tool
Cutting and extrusion etc.) step, with the nano-structured processing of applicable Ti-6Al-4V Yu Ti-6Al-7Nb titanium alloy material, meanwhile,
For Ti-6Al-4V titanium alloy, after the thermomechanical technique of final step completes with machinery forging Combined Processing, as long as remaking one
Secondary process annealing, so that it may so that its extension power and fatigue resistance increase 50% and 10% respectively.
The method of the invention described above, the titanium alloy crystallite dimension of gained is about 30-70nm, preferably 40-60nm scope.
In preferred embodiments, the method preparing nano-structured titanium alloy material of the present invention, walk by the technique of Fig. 6
Rapid and technological parameter, in corner extrusion (ECAP) step I, temperature controls between 700-850 DEG C, and rolling and/or broaching tool are cut
Cutting and walk the temperature of poly-II and control between 200-400 DEG C, the temperature of stretching extrusion step III controls between 200-300 DEG C, titanium
Alloy grain size is reduced to 40-60nm scope.Use the ECAP mould at 90 ° of angles.In the poly-II of step and step III two benches many
The process of step, each processes the strain that all can derive heterogencity, the combination of these steps reasonably combined, Combinatorial Optimization
Accumulate SPD deflection, crystal grain refinement structure can be brought up continuously and formed, make the titanium alloy material being processed can realize optimizing
Homogeneous deformation and structure refinement.
Conventional titanium material is to be difficult to one of metal carrying out machining, although recent industrial practice has been proposed for many
Processing scheme, and achieve good surface finish ability.In part because of the low elastic modulus of titanium alloy, so needing
Will the equipment of bigger rigidity.The thermal conductance that titanium is relatively low with titanium alloy, then cause the increase of temperature in machining.Overcome
The measure to be taken of these problems will cause the rising of machining cost.This has resulted in the biggest problem.The side of the present invention
Method solves the problems referred to above, can be obviously improved and optimize the machining property of titanium alloy, solves titanium alloy material deformation
Problem difficult, that plasticity is poor, meanwhile, improves titanium alloy material resisting fatigue, Resisting fractre and resistance to corrosion.Obtaining more
Processing cost is not increased while the mechanical performance optimized.
Accompanying drawing explanation
The large plastometric set processing technological flow figure of Fig. 1 continuous Equal-channel Angular Pressing method (ECAP).
The evolution of titanium mechanical property when Fig. 2 gives lower 20 DEG C of the thermomechanical processing of controlled step.
Uniaxial tension stress-strain response curve after Fig. 3 SPD PROCESS FOR TREATMENT cp2 level titanium is nano-structured.
The TEM image within cp2 level titanium metal material after Fig. 4 SPD PROCESS FOR TREATMENT.
Tensile stress after Fig. 5 Ti-6Al-4V titanium alloy nano structuring processing should with strain stress relation and isometry stretching thereof
Become the TEM image of micro structure.
The process chart that Fig. 6 processes for Ti-6Al-4V titanium alloy nano structure, in figure, Np represents number of repetition, %
Represent the number of repetition being stretched to failure.
Detailed description of the invention
Following example are in order to further illustrate and to understand the essence of the present invention, but limit the present invention's never in any form
Scope.
The preparation of embodiment 1 continuous non-isothermal CEPT extruding cp2 Nano-mter Ti-alloy material
According to the flow chart of Fig. 1, can forge mould (preferably 3) by multiple ECAP, pressure is 500-700MPa, by rolling accordingly
Sub-institute " feedback connection ", these rollers maintain the temperature more much lower than the workpiece processed by ECAP by the supply of coolant
Degree.Hot-die temperature controls at 200-300 DEG C, and the temperature of roller controls at 20-50 DEG C, the rod segment outside ECAP forging mould
, then there is relative thermal expansion in section, this thermal expansion can cause " back pressure " at ECAP die exit.This restraint is conducive to
The formation of material internal fine structure.Titanium alloy material is inserted the passages such as hot-die, through the comprehensive corner extrusion of various dimensions, weight
Multiple three times, again non-isothermal roller repeatedly roll, stretch, extrude and cross-forge.According to inspection grain size detection case, can or repeat
Previous process flow process 2-4 time, it is thus achieved that nanocrystalline structures titanium alloy material, and make annealing treatment.
The nanocrystalline structures titanium alloy material obtained has the mechanical property of excellence, sees Fig. 2, adds with only with ECAP
Man-hour is compared, and the yield strength of Compound Machining and extreme hot strength add more than 80%.Fig. 2 marks " RA " curve represent
Area declines, and marks " % " and then refers to be stretched to lose efficacy.It should be noted that, the procedure of processing of indication is not to enter under room temperature environment
Row, but 200 DEG C-850 DEG C this in the range of realize.Additionally, annealing is performed a plurality of times between several steps.Thing
In reality, the strict control of temperature, is quite crucial for realizing the improvement of internal nanostructure and then material behavior；These add
Work step is suddenly own, will not bring too much cost.
The cp2 nanocrystalline structures titanium alloy material obtained presents high yield strength (reaching 1000MPa), in the limit
Presenting a platform under intensity (about 1200MPa), show that its extension performance also gets a promotion, its material hardness exceedes
3.6GPa, is shown in Fig. 3, expression be cp2 level titanium nano-structured after uniaxial tension stress-strain response curve.
The cp2 nanocrystalline structures titanium alloy material obtained, the size of its nanocrystal is at 30nm≤d≤70nm model
Enclose, see Fig. 4.As can be seen from Fig. 4, this material has this kind of crystal grain, and these crystal grain are generally almost without dislocation, this and tradition
The internal structure behavior of the metal or alloy after SPD PROCESS FOR TREATMENT is entirely different, and this nanostructured metal and conjunction exactly
The typical behaviour of gold copper-base alloy.Grainiess does not has dislocation, is the material list major reason that reveals high mechanical strength.Further,
These crystal grain are isometry behavior, and this gives the isotropism of its nanocrystal.
Embodiment 2Ti-6Al-4V titanium alloy nano structure is processed
By the method with reference to embodiment 1, process Ti-6Al-4V titanium alloy, it is thus achieved that nanocrystalline structures titanium alloy pole stock,
And make annealing treatment.The wherein comprehensive corner extrusion of various dimensions, repeats 2-4 time.
The nanometer Ti-6Al-4V titanium alloy material obtained, compared with conventional Ti-6Al-4V titanium alloy material, after processing
Material behavior is strengthened (see Fig. 5) really.From figure 5 it can be seen that present smoothing process at peak load, this is that a kind of material is gathered around
Having the typical characteristics of relatively high strain rate sensitivity, high strain rate sensitivity is then owing to the height extension of this material
Property.It can easily be seen that the yield strength of this material surpasses 1000MPa, and its ultimate tensile strength is close to 1200MPa.Wherein illustration
It is a typical cross-section of this nano structural material, average grain size therein about 70nm.The most annealing treatment
Reason just can promote the extension ability of up to 5～6%, and does not damage its hot strength, it is achieved its hot strength and extension performance
Promote simultaneously.
Embodiment 3Ti-6Al-4V titanium alloy nano structure is processed
According to process chart and the parameter of Fig. 6, Ti-6Al-4V titanium alloy is inserted the hot-die entrance of stage i, enter
In passage, through the comprehensive corner extrusion of 3-dimensional degree, temperature controls 700-850 DEG C on circulation (repetition) 2-4 time, entrance ii rank
The roller rolling of section and pulling eye, temperature controls 200-400 DEG C, enters the stretching extrusion of ii I-stage, and temperature controls 200-300
DEG C, last cross-forge arranges, it is thus achieved that nanocrystalline structures titanium alloy pole stock, and makes annealing treatment.
In above-mentioned technique, the Combinatorial Optimization to ii and ii I two stage process step can be taked to accumulate SPD
Deflection, enables and brings up crystal grain refinement structure formation continuously.
The nanometer Ti-6Al-4V titanium alloy material obtained, compared with the Ti-6Al-4V titanium alloy material of embodiment 2,
After the thermomechanical technique of a rear step completes with machinery forging Combined Processing, as long as remaking a process annealing, so that it may so that its exhibition
Prolong power and increase 50% and 10% respectively with fatigue resistance.Ti-6Al-4V titanium alloy nano crystallite dimension is reduced to 40-60nm model
Enclose.It is obviously improved material anti-fatigue performance.
Claims (10)
1. the method preparing nano-structured titanium alloy material, including by titanium alloy material through Equal-channel Angular Pressing,
Rolling so that it is the large plastometric set of the degree of depth, then through repeatedly stretching, extrude and cross-forge, it is thus achieved that nanocrystalline structures titanium alloy material
Material, it is characterised in that: Equal-channel Angular Pressing and rolling are the extruding of continuous non-isothermal degree and rolling.
2. the method for claim 1, farther includes nano-structured titanium alloy material is carried out continuous high temperature, high pressure
Process.
3. the method for claim 1, farther includes pulling eye and processes step.
4. the method as described in claim 1 or 3, farther includes annealing.
5. method as claimed in claim 4, the temperature of its hot-die controls between 200-300 DEG C, and the temperature of roller controls
Between 20-50 DEG C.
6. the method for claim 1, described nanometer, the average grain size of its nanometer is 30-70nm scope.
7. method as claimed in claim 6, the average grain size of described nanometer is 40-60nm scope.
8. the method for claim 1, it is characterised in that: described equal channel angular is 90 degree of right angles, and equal channel angular squeezes
Press and extrude for various dimensions, repeat 2-4 time.
9. method as claimed in claim 8, described various dimensions are 3-dimensional degree, are repeated 3 times.
10. the method for claim 1, described nano-structured titanium alloy material is pole stock.
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Cited By (2)
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| CN112063890A (en) * | 2020-09-29 | 2020-12-11 | 中国科学院金属研究所 | High-thermal-stability equiaxial nanocrystalline Ti-Ag alloy and preparation method thereof |
| US10960448B1 (en) | 2020-01-09 | 2021-03-30 | Prince Mohammad Bin Fahd University | Process for equal channel angular pressing fine grain titanium round tube |
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| US6399215B1 (en) * | 2000-03-28 | 2002-06-04 | The Regents Of The University Of California | Ultrafine-grained titanium for medical implants |
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| US6399215B1 (en) * | 2000-03-28 | 2002-06-04 | The Regents Of The University Of California | Ultrafine-grained titanium for medical implants |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10960448B1 (en) | 2020-01-09 | 2021-03-30 | Prince Mohammad Bin Fahd University | Process for equal channel angular pressing fine grain titanium round tube |
| US11344937B2 (en) | 2020-01-09 | 2022-05-31 | Prince Mohammad Bin Fahd University | Method for producing high strength titanium pipe |
| CN112063890A (en) * | 2020-09-29 | 2020-12-11 | 中国科学院金属研究所 | High-thermal-stability equiaxial nanocrystalline Ti-Ag alloy and preparation method thereof |
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