CN103614680B - A kind of preparation method of super-elasticity high strength beta-titanium alloy band - Google Patents
A kind of preparation method of super-elasticity high strength beta-titanium alloy band Download PDFInfo
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Abstract
The invention provides a kind of preparation method of super-elasticity high strength beta-titanium alloy band, the method is: it is cold rolling by thickness to be that the beta-titanium alloy sheet material of 2mm carries out many rolling processes, and anneal is carried out between adjacent rolling process, obtain the cold rolling state band that thickness is 0.2mm ~ 0.25mm, then cold rolling state band is carried out ageing treatment, obtain super-elasticity high strength beta-titanium alloy band.The maximum of beta-titanium alloy band prepared by the present invention can reach 2.3% by recovery strain, tensile strength is 900MPa ~ 1000MPa, Young's modulus is 50GPa ~ 60GPa, elongation is 8% ~ 10%, this beta-titanium alloy band has excellent elastic performance while having high strength and good plasticity, can be widely used in the numerous areas such as medicine equipment, electronic component, sensor.
Description
Technical field
The invention belongs to titanium alloy material processing technique field, be specifically related to a kind of preparation method of super-elasticity high strength beta-titanium alloy band.
Background technology
Superelastic alloy has been widely used in medical, the civilian and industrial circle such as electronic component, sensor.Traditional Ni-Ti alloy has unique shape memory effect and super-elasticity due to stress-induced martensite transformation and reverted austenite thereof, and this makes Ni-Ti alloy successfully be applied to Medical rack, medical guiding wire, spectacle frame, anti-pain in the back tights, especially orthodontic.But large quantifier elimination shows that nickel element has potential teratogenecity and carinogenicity; Although the titanium oxide that NiTi surface is formed has corrosion resistance, in fluoride ion environment, the stripping of nickel ion produces toxicity to cell.From bio-medical security consideration, development of new Ni-free super elastic alloy has become the important directions that investigation of materials person pays close attention to.
Research shows, much has super-elasticity in various degree without nickel beta-titanium alloy, comprises Ti-Nb system, Ti-Nb-Zr system, Ti-Nb-Sn system, Ti-Mo-Al system, Ti-Nb-Zr-Sn system, Ti-Zr-Nb-Fe system etc.These comprise without the hyperelastic exemplary of nickel beta-titanium alloy: Ti-Zr-Nb-Fe system Alloy At Room Temperature super-elasticity maximum can recovery strain can to reach 2.1 ~ 3.1%(see application number be the Chinese invention patent of 201210159967.5), Ti-24Nb-4Zr-7.9Sn Alloy At Room Temperature super-elasticity maximum can recovery strain to reach 3.3%(see application number be the Chinese invention patent of 200410092858.1).In recent years, Ti-Nb system superelastic alloy obtained studying the most widely, and a lot of investigator both at home and abroad forms polynary system alloy to improve super-elasticity by adding the elements such as Zr, Al, Ta.But the larger regime of elastic deformation that most of superelastic ss titanium alloy shows and lower plasticity make the processing of its meticulous titanium material (band, foil, silk material etc.) prepare and are subject to certain limitation.The processing preparation of current titanium or titanium alloy band, foil, silk material etc. all adopts the mode of room temperature cold deformation, to obtain good surface quality and qualified mechanical property.For the cold deformation of superelastic ss titanium alloy, wider elastic range makes material rebounds amount very large; And due to lower plasticity, be easy to during material generation viscous deformation plastic instability occurs.If do not have reasonably mechanism to eliminate the increase of energy in material, under larger plastix strain, material will destroy.Therefore, the processing preparation with the fine materials of superelastic ss titanium alloy is the difficult point in this field always.
In recent years, to the TLM titanium alloy of its independent development, (nominal chemical composition is Ti-25Nb-3Zr-2Sn-3Mo to Xibei Inst. of Non-Ferrous Metals, wt%, belong to beta-titanium alloy) recoverable deformation behavior and the research of elastic mechanism more ripe, this alloy sheets of research discovery, bar have the maximum flexibility recovery strain of 1.5% ~ 1.8% at ambient temperature, and its temperature-room type plasticity can reach 20% ~ 40%.Based on less elastic recovery and excellent plasticity, alloy is easy to the preparation realizing the meticulous titanium material such as band, foil under multi-pass cold deformation and intermediate annealing process combine condition.Controlled by follow-up system of ageing treatment, adjust super-elasticity, intensity and plasticity coupling further.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of super-elasticity high strength beta-titanium alloy band.The method, ensureing to have excellent elastic performance while band has high strength and good plasticity, can be widely used in the numerous areas such as medicine equipment, electronic component, sensor.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of super-elasticity high strength beta-titanium alloy band, it is characterized in that, the method is: to be the beta-titanium alloy sheet material of 2mm by thickness in rolling process deformation rate be, and to carry out many rolling processes under the condition of 10% ~ 40% cold rolling, and anneal is carried out between adjacent rolling process, obtain the cold rolling state band that thickness is 0.2mm ~ 0.25mm, then cold rolling state band is carried out ageing treatment, obtain super-elasticity high strength beta-titanium alloy band, what described super-elasticity high strength beta-titanium alloy band referred to this band can recovery strain≤ε
max, ε
max=2.1% ~ 2.3%, tensile strength is 900MPa ~ 1000MPa, and Young's modulus is 50GPa ~ 60GPa, and elongation is 8% ~ 10%, the detailed process of described anneal is: be water-cooled after being incubated 15min ~ 30min under the condition of 700 DEG C ~ 850 DEG C in temperature, the detailed process of described ageing treatment is: be water-cooled after being incubated 5min ~ 10min under the condition of 500 DEG C ~ 550 DEG C in temperature.
The preparation method of above-mentioned a kind of super-elasticity high strength beta-titanium alloy band, it is characterized in that, described beta-titanium alloy is TLM titanium alloy.
The preparation method of above-mentioned a kind of super-elasticity high strength beta-titanium alloy band, it is characterized in that, described cold rolling rolling process number is 5 ~ 7 rolling processes.
The preparation method of above-mentioned a kind of super-elasticity high strength beta-titanium alloy band, it is characterized in that, described beta-titanium alloy sheet material also needed to carry out figuring of surface process before cold rolling.
The preparation method of above-mentioned a kind of super-elasticity high strength beta-titanium alloy band, it is characterized in that, described anneal and ageing treatment are all carried out under inert atmosphere or vacuum condition.
The preparation method of above-mentioned a kind of super-elasticity high strength beta-titanium alloy band, it is characterized in that, described beta-titanium alloy sheet material is As rolled sheet material.
The present invention compared with prior art has the following advantages:
1, the present invention is based on the plasticity of beta-titanium alloy sheet material excellence, utilizes the cold rolling and intermediate annealing process of many rolling processes to obtain titanium alloy strip first audaciously.Compared to the lower plasticity in general super-elastic titanium alloys distortion and limited forming property, this beta titanium alloy band embodies alloy high-ductility feature in cold rolling, in conjunction with annealing process rational between rolling process, ensure that the successful acquisition of beta-titanium alloy band.
2, the present invention creatively proposes cold rolling and follow-up ageing treatment in short-term to combine, and obtains and has hyperelastic beta-titanium alloy band.Improve alloy strength by the cold rolling rapid refinement crystal grain of many rolling processes, increase its regime of elastic deformation; In cold rolling state band, the follow-up Age-prrcipitation Phase that is produced as of fine grained texture provides favourable condition simultaneously.Time in short-term, process can by the high stored energy replying state of alloy to low-energy state, maintains alloy fine grained texture feature and the microdefect eliminated in fine grained texture and improve alloy plasticity in shorter soaking time; On the other hand, utilize a small amount of α phase of Precipitation improve yield-point and improve alloy strength, and the critical transitions point of stress-induced martensite is raised, achieve the super-elasticity of beta-titanium alloy.
3, the present invention has successfully prepared the super-elasticity band of beta titanium alloy, maximumly can reach 2.1% ~ 2.3% by recovery strain, tensile strength reaches 900MPa ~ 1000MPa simultaneously, and Young's modulus reaches 50GPa ~ 60GPa, and has the good plasticity that elongation is 8% ~ 10%.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the microstructure picture of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 1.
Fig. 2 is the tensile stress-strain curve of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 1.
Fig. 3 is the microstructure picture of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 2.
Fig. 4 is the cyclic tension stress-strain curve of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 2.
Fig. 5 is the microstructure picture of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 3.
Fig. 6 is the cyclic tension stress-strain curve of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 3.
Fig. 7 is the microstructure picture of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 4.
Fig. 8 is the cyclic tension stress-strain curve of super-elasticity high strength beta-titanium alloy band prepared by the embodiment of the present invention 4.
Fig. 9 is the microstructure picture of the beta-titanium alloy band of comparative example 1 of the present invention preparation.
Figure 10 is the tensile stress-strain curve of the beta-titanium alloy band of comparative example 1 of the present invention preparation.
Embodiment
Embodiment 1
The preparation of super-elasticity high strength beta-titanium alloy band:
Step one, be that the beta-titanium alloy sheet material of 2mm carries out figuring of surface process on sander by thickness; Described beta-titanium alloy is TLM titanium alloy;
Step 2,5 rolling processes of being carried out by the beta-titanium alloy sheet material after figuring of surface process in step one are cold rolling, each rolling process deformation rate (" total deformation rate between twice process annealing is called rolling process deformation rate ", see " titanium material Technology of Plastic Processing ", open volumes such as flying, P66) be 40%, 37.5%, 40%, 33.3%, 16.7%, and vacuum annealing process is carried out between adjacent rolling process, obtain the cold rolling state band that thickness is 0.25mm; The detailed process of described vacuum annealing process is: be water-cooled after being incubated 15min under the condition of 700 DEG C in temperature;
Step 3, state band cold rolling described in step 2 is carried out ageing treatment, detailed process is: be water-cooled after being incubated 5min under the condition of 500 DEG C in temperature, obtains the super-elasticity high strength beta-titanium alloy band that thickness is 0.25mm.
Fig. 1 is the microstructure picture of the present embodiment beta-titanium alloy band.Fig. 2 is the tensile stress-strain curve of the present embodiment beta-titanium alloy band.From Fig. 1 and Fig. 2, the tissue of the present embodiment beta-titanium alloy band is made up of tiny wait axle β crystal grain and a small amount of α; The intensity of superelastic ss titanium alloy band prepared by the present embodiment is 985MPa, and elongation is 8.5%, and recoverable strain is 3.5%, has wider regime of elastic deformation.
Embodiment 2
The preparation of super-elasticity high strength beta-titanium alloy band:
Step one, be that the beta-titanium alloy sheet material of 2mm carries out figuring of surface process on sander by thickness; Described beta-titanium alloy is TLM titanium alloy;
Step 2,6 rolling processes of being carried out by the beta-titanium alloy sheet material after figuring of surface process in step one are cold rolling, and each rolling process deformation rate is 40%, 37.5%, 33.3%, 20%, 25%, 20%, and vacuum annealing process is carried out between adjacent rolling process, obtain the cold rolling state band that thickness is 0.24mm; The detailed process of described vacuum annealing process is: be water-cooled after being incubated 30min under the condition of 800 DEG C in temperature;
Step 3, state band cold rolling described in step 2 is carried out ageing treatment, detailed process is: be water-cooled after being incubated 8min under the condition of 550 DEG C in temperature, obtains the super-elasticity high strength beta-titanium alloy band that thickness is 0.24mm.
Fig. 3 is the microstructure picture of the present embodiment beta-titanium alloy band.Fig. 4 is the cyclic tension stress-strain curve of the present embodiment beta-titanium alloy band.From Fig. 3 and Fig. 4, this band tissue is made up of tiny wait axle β crystal grain and a small amount of α; Band three cyclic tensions show super-elasticity behavior, and 3% strain is maximum down can reach 2.1% by recovery strain, and Young's modulus is 60GPa.Tension test records tensile strength and reaches 940MPa, and elongation is 9%.
Embodiment 3
The preparation of super-elasticity high strength beta-titanium alloy band:
Step one, be that the beta-titanium alloy sheet material of 2mm carries out figuring of surface process on sander by thickness; Described beta-titanium alloy is TLM titanium alloy;
Step 2,6 rolling processes of being carried out by the beta-titanium alloy sheet material after figuring of surface process in step one are cold rolling, and each rolling process deformation rate is respectively: 40%, 37.5%, 33.3%, 30%, 28.6%, 12%, and vacuum annealing process is carried out between adjacent two rolling processes, obtain the cold rolling state band that thickness is 0.22mm; The detailed process of described vacuum annealing process is: be water-cooled after being incubated 20min under the condition of 850 DEG C in temperature;
Step 3, state band cold rolling described in step 2 is carried out ageing treatment, detailed process is: be water-cooled after being incubated 10min under the condition of 520 DEG C in temperature, obtains the super-elasticity high strength beta-titanium alloy band that thickness is 0.22mm.
Fig. 5 is the microstructure picture of the present embodiment super-elasticity high strength beta-titanium alloy band.Fig. 6 is the cyclic tension stress-strain curve of the present embodiment super-elasticity high strength beta-titanium alloy band.From Fig. 5 and Fig. 6, this band tissue is made up of tiny wait axle β crystal grain and a small amount of α; Band three cyclic tensions show super-elasticity behavior, and 3% strain is maximum down can reach 2.2% by recovery strain, and Young's modulus is 50GPa.Tension test records tensile strength and reaches 900MPa, and elongation is 10%.
Embodiment 4
The preparation of super-elasticity high strength beta-titanium alloy band:
Step one, be that the As rolled beta-titanium alloy sheet material of 2mm carries out figuring of surface process on sander by thickness; Described beta-titanium alloy is TLM titanium alloy;
Step 2,7 rolling processes of being carried out by the beta-titanium alloy sheet material after figuring of surface process in step one are cold rolling, and each rolling process deformation rate is respectively: 40%, 37.5%, 33.3%, 30%, 28.6%, 11%, 10%, and vacuum annealing process is carried out between adjacent rolling process, obtain the cold rolling state band that thickness is 0.2mm; The detailed process of described vacuum annealing process is: be water-cooled after being incubated 20min under the condition of 700 DEG C in temperature;
Step 3, state band cold rolling described in step 2 is carried out ageing treatment, detailed process is: be water-cooled after being incubated 5min under the condition of 520 DEG C in temperature, obtains the super-elasticity high strength beta-titanium alloy band that thickness is 0.2mm.
Fig. 7 is the microstructure picture of the present embodiment super-elasticity high strength beta-titanium alloy band.Fig. 8 is the cyclic tension stress-strain curve of the present embodiment super-elasticity high strength beta-titanium alloy band.From Fig. 7 and Fig. 8, the present embodiment super-elasticity high strength beta-titanium alloy band tissue is made up of very tiny wait axle β crystal grain and a small amount of α; Band three cyclic tensions show super-elasticity behavior, and 3% strain is maximum down can reach 2.3% by recovery strain, and Young's modulus is 55GPa.Tension test records tensile strength and reaches 1000MPa, and elongation is 8.1%.
Comparative example 1
The preparation method of this comparative example beta-titanium alloy band and the difference of embodiment 1 are only: without ageing treatment.
Fig. 9 is the microstructure picture of this comparative example beta-titanium alloy band.Figure 10 is the tensile stress-strain curve of this comparative example beta-titanium alloy band.From Fig. 9 and Figure 10, the tissue of this comparative example beta-titanium alloy band forms by being out of shape β crystal grain, deformation twins and stress-induced martensite.The tensile strength of this comparative example beta-titanium alloy band is lower, is only 700MPa; And elastic range is less, be about 2.5%.
From embodiment 1 and comparative example 1 comparative analysis, the preparation method of super-elasticity high strength β type TLM titanium alloy strip of the present invention comprises two critical process step: first alloy sheet material carries out the cold deformation of many rolling processes to be organized with optimized alloy, for subsequent heat treatment provides necessary condition; It two is carry out suitable ageing treatment to realize super-elasticity to cold-strip.Two steps are combinations that organization optimization and phase composite regulate and control, and finally realize the preparation of super-elasticity high strength beta-titanium alloy band.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (5)
1. the preparation method of a super-elasticity high strength beta-titanium alloy band, it is characterized in that, the method is: to be the beta-titanium alloy sheet material of 2mm by thickness in rolling process deformation rate be, and to carry out many rolling processes under the condition of 10% ~ 40% cold rolling, and anneal is carried out between adjacent rolling process, obtain the cold rolling state band that thickness is 0.2mm ~ 0.25mm, then cold rolling state band is carried out ageing treatment, obtain super-elasticity high strength beta-titanium alloy band, what described super-elasticity high strength beta-titanium alloy band referred to this band can recovery strain≤ε
max, ε
max=2.1% ~ 2.3%, tensile strength is 900MPa ~ 1000MPa, and Young's modulus is 50GPa ~ 60GPa, and elongation is 8% ~ 10%; The detailed process of described anneal is: be water-cooled after being incubated 15min ~ 30min under the condition of 700 DEG C ~ 850 DEG C in temperature, the detailed process of described ageing treatment is: be water-cooled after being incubated 5min ~ 10min under the condition of 500 DEG C ~ 550 DEG C in temperature; Described beta-titanium alloy is TLM titanium alloy.
2. the preparation method of a kind of super-elasticity high strength beta-titanium alloy band according to claim 1, it is characterized in that, described cold rolling rolling process number is 5 ~ 7 rolling processes.
3. the preparation method of a kind of super-elasticity high strength beta-titanium alloy band according to claim 1, it is characterized in that, described beta-titanium alloy sheet material also needed to carry out figuring of surface process before cold rolling.
4. the preparation method of a kind of super-elasticity high strength beta-titanium alloy band according to claim 1, it is characterized in that, described anneal and ageing treatment are all carried out under inert atmosphere or vacuum condition.
5. the preparation method of a kind of super-elasticity high strength beta-titanium alloy band according to claim 1, it is characterized in that, described beta-titanium alloy sheet material is As rolled sheet material.
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