CN100540704C - A kind of titanium-zirconium-base ternary shape memory alloy material and preparation method thereof - Google Patents

A kind of titanium-zirconium-base ternary shape memory alloy material and preparation method thereof Download PDF

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CN100540704C
CN100540704C CNB2007101755102A CN200710175510A CN100540704C CN 100540704 C CN100540704 C CN 100540704C CN B2007101755102 A CNB2007101755102 A CN B2007101755102A CN 200710175510 A CN200710175510 A CN 200710175510A CN 100540704 C CN100540704 C CN 100540704C
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shape memory
zirconium
titanium
alloy material
memory alloy
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CN101121986A (en
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李岩
崔琰
徐惠彬
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Beihang University
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Abstract

The invention discloses a kind of titanium-zirconium-base ternary shape memory alloy material, this alloy material is made up of the zirconium (Zr) of 30at%～50at%, the 3rd constituent element of 0.2at%～10at% and the titanium (Ti) of surplus, and the content sum of above-mentioned each composition is 100%; Described the 3rd constituent element is a kind of element in tin (Sn), aluminium (Al), molybdenum (Mo), chromium (Cr), silver (Ag) or the gallium (Ga).By in binary TiZr alloy, adding a certain amount of the 3rd constituent element element, martensitic transformation temperature and the mechanical property that can regulate alloy.This alloy material transformation temperature is at 0 ℃～700 ℃, and shape memory effect is greater than 1.20%; Yield strength in the time of 20 ℃ is 500MPa～900MPa, and deformation rate is greater than 20%.

Description

A kind of titanium-zirconium-base ternary shape memory alloy material and preparation method thereof
Technical field
The present invention relates to a kind of titanium-zirconium-base ternary shape memory alloy material,, improve the yield strength of alloy by in titanium-zirconium alloy, adding element can be adjusted alloy in a big way martensitic transformation temperature.
Background technology
The shape memory alloy that is representative with the basic alloy of TiNi has functions such as unique shape memory effect and super-elasticity, can export bigger stress and strain by its driving of making and control device, be widely used in fields such as medical science, industry and lives.
Zr element and Ti element belong to IVA family together, have similar physical properties and chemical property, and for example, Ti element and Zr element in solid phase area the transformation of high temperature bcc to low temperature hcp take place all.In the TiZr alloy, the Zr element takes place greater than the martensitic transformation that comparatively high temps was arranged in 30% o'clock, can cause the high temperature memory effect of alloy.
The martensitic transformation temperature of binary TiZr alloy does not coexist with composition and changes in 600 ℃～880 ℃ scopes.Based on binary TiZr alloy, by adding high purity element (Sn, Al, Mo, Cr, Ag) can be regulated alloy in a big way martensitic transformation temperature, improve the yield strength and the hardness of alloy, thereby make high strength titanium zirconium-base ternary shape memory alloy with good memory effect.The application background of this alloy is as follows: on the one hand, can be used as transformation temperature and be higher than 100 ℃ high-temperature shape memory alloy application, compare with present typical high temperature shape memory alloy TiNiPd, cost advantage is obvious; On the other hand, owing to do not contain Ni element (bio-toxicity is arranged), have than the better biocompatibility of TiNi shape memory alloy as bio-medical material.And the high strength of alloy makes it in use can overcome the bigger extraneous application of force, is difficult for causing losing efficacy because of overload causes non-reversible deformation.So this alloy is a kind of low cost, the high strength of good biocompatibility, high rigidity shape-memory material have broad application prospects in aerospace and bio-medical field.
Summary of the invention
The objective of the invention is to propose a kind of high strength TiZrX (X=Sn, Al, Mo, Cr, Ag) shape memory alloy material, regulate the martensitic transformation temperature of alloy, the yield strength and the surface hardness of alloy by the content of controlling the 3rd constituent element element.On the one hand, TiZrX (X=Sn, Al, Mo, Cr, Ag) shape memory alloy can be used as transformation temperature and is higher than 100 ℃ high-temperature shape memory alloy and uses; On the other hand, also can be used as bio-medical material and substitute the TiNi shape memory alloy, avoid the harm of Ni element stripping human body safety.
Titanium-zirconium-base ternary shape memory alloy material of the present invention be made up of the zirconium (Zr) of 30at%～50at%, the 3rd constituent element of 0.2at%～10at% and the titanium (Ti) of surplus, and the content sum of above-mentioned each composition is 100%; Described the 3rd constituent element is a kind of element in tin (Sn), aluminium (Al), molybdenum (Mo), chromium (Cr), silver (Ag) or the gallium (Ga).
Described titanium-zirconium-base ternary shape memory alloy material, its component are Ti 64Zr 32Sn 4, Ti 50Zr 48Al 2, Ti 60Zr 32Mo 8, Ti 50Zr 46Cr 4, Ti 62Zr 32Ag 6Perhaps Ti 62Zr 32Ga 6
Described titanium-zirconium-base ternary shape memory alloy material, its transformation temperature is at 0 ℃～700 ℃, and shape memory effect is greater than 1.20%; Yield strength in the time of 20 ℃ is 500MPa～900MPa, and deformation rate is more than or equal to 20%.
Prepare the method for titanium-zirconium-base ternary shape memory alloy material of the present invention, include the following step:
(1) taking by weighing purity by the titanium-zirconium-base ternary composition proportion is that 99.9% titanium (Ti), purity are that 99.9% zirconium (Zr) and purity are that 99.9% tin (Sn), purity are that 99.9% aluminium (Al), purity are that 99.9% molybdenum (Mo), purity are that 99.9% chromium (Cr) and purity are 99.9% silver (Ag);
(2) the above-mentioned titanium that takes by weighing, zirconium and the 3rd constituent element composition raw material are put into non-consumable arc furnace, be evacuated to 2 * 10 -3Pa～5 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrX ingot at 1700 ℃～2000 ℃ then;
(3) the above-mentioned TiZrX ingot that makes is put into vacuum heat treatment furnace and heat-treat, in vacuum tightness 2 * 10 -3Pa～5 * 10 -3Pa, 850 ℃～900 ℃ insulation is after 1～2 hour down for thermal treatment temp, and quenching-in water promptly obtains the TiZrX shape memory alloy material.
The advantage of TiZrX of the present invention (X=Sn, Al, Mo, Cr, Ag) shape memory alloy material: on TiZr alloy basis, by adding the transformation temperature that high purity the 3rd component element is regulated alloy, improve yield strength with.The high strength of alloy makes it in use can overcome the bigger extraneous application of force, is difficult for causing losing efficacy because of overload causes non-reversible deformation.TiZrX of the present invention (X=Sn, Al, Mo, Cr, Ag) shape memory alloy transformation temperature is at 0 ℃～700 ℃, and shape memory effect is greater than 1.20%; Yield strength in the time of 20 ℃ is 500MPa～900MPa, and deformation rate is more than or equal to 20%.
Description of drawings
Fig. 1 is Ti 64Zr 32Sn 4Cylinder sample is compression testing result curve figure at room temperature.
Figure 1A is Ti 64Zr 32Sn 4The DSC graphic representation.
Fig. 2 is Ti 50Zr 48Al 2Cylinder sample is compression testing result curve figure at room temperature.
Fig. 3 is Ti 60Zr 32Mo 8Cylinder sample is compression testing result curve figure at room temperature.
Fig. 4 is Ti 50Zr 46Cr 4Cylinder sample is compression testing result curve figure at room temperature.
Fig. 5 is Ti 62Zr 32Ag 6Cylinder sample is compression testing result curve figure at room temperature.
Fig. 6 is Ti 62Zr 32Ga 6Cylinder sample is compression testing result curve figure at room temperature.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention is a kind of high-intensity titanium-zirconium-base ternary shape memory alloy material that has, and be made up of the zirconium (Zr) of 30at%～50at%, the 3rd constituent element of 0.2at%～10at% and the titanium (Ti) of surplus, and the content sum of above-mentioned each composition is 100%; Described the 3rd constituent element is a kind of element in tin (Sn), aluminium (Al), molybdenum (Mo), chromium (Cr), silver (Ag) or the gallium (Ga).
The preparation method and the step of titanium-zirconium-base ternary shape alloy material of the present invention are as follows:
(1) taking by weighing purity by the titanium-zirconium-base ternary composition proportion is that 99.9% titanium, purity are that 99.9% zirconium, purity are that 99.9% tin, purity are that 99.9% aluminium, purity are that 99.9% molybdenum (Mo), purity are that 99.9% chromium (Cr) and purity are 99.9% silver (Ag);
(2) above-mentioned titanium, zirconium and the 3rd constituent element composition raw material are put into non-consumable arc furnace, be evacuated to 2 * 10 -3Pa～5 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrX ingot at 1700 ℃～2100 ℃ then;
(3) vacuum heat treatment furnace that the above-mentioned TiZr X ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 1 hour down of 900 ℃ of thermal treatment temps, quenching-in water promptly obtains TiZrX (X=Sn, Al, Mo, Cr, the Ag) shape memory alloy material of requirement of the present invention.
Adopt wire cutting method, in the above-mentioned titanium-zirconium-iron shape memory alloy that makes, cut and be of a size of 1 * 1 * 3mm 3Rectangular parallelepiped as the phase transformation specimen, adopt Perkin-Elmer DSC-7 type differential scanning calorimetry instrument to measure martensitic transformation temperature; Adopt MHX1000 type microhardness instrument to measure alloy surface hardness; Cut diameter d=5mm, the right cylinder of height h=8mm adopts MTS-880 type universal material experimental machine to carry out compression pressure-strain testing as the Mechanics Performance Testing sample, and compressive strain speed is 0.02mm/min, and temperature is a room temperature.After being compressed to different prestrains, be heated to the above recovery of shape of transformation temperature, measure the recovery of shape strain behind the cool to room temperature, getting wherein, maximum value is shape memory effect.
Compare with the performance perameter of binary TiZr alloy and TiZrFe alloy and have higher yield strength and surface hardness in order to verify titanium-zirconium-base ternary alloy material of the present invention, the inventor adopts the processing condition vegetation of identical embodiment to go out binary TiZr alloy and TiZrFe alloy, and the contrast of its performance perameter is as shown in the table:
Alloy Yield strength in the time of 20 ℃ (MPa) Deformation rate (%) Shape memory effect (%) Transformation temperature (℃)
TiZrX 500、900 ≥20 ＞1.2％ 0～700
TiZrFe 150～300 ≥12 ＞1.1％ 0～600
TiZr 450～700 ≥15 ＞1.0％ 660～880
TiZrX of the present invention (X=Sn, Al, Mo, Cr, Ag) shape memory alloy material is compared with binary TiZr alloy material, transformation temperature can be regulated arbitrarily in 0 ℃～700 ℃ scopes, make its temperature condition that more approaches bio-medical or high temperature use, better than TiNi memorial alloy bio-medical consistency.
Embodiment 1:System Ti 64Zr 32Sn 4Alloy material
(1) taking by weighing 64at% purity is that 99.9% titanium, 32at% purity are that 99.9% zirconium and 4at% purity are 99.9% tin;
(2) above-mentioned titanium, zirconium and block tin shape raw material are put into non-consumable arc furnace, be evacuated to 5 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is being smelted into the TiZrSn ingot then more than 1800 ℃;
(3) vacuum heat treatment furnace that the above-mentioned TiZrSn ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 1 hour down of 900 ℃ of thermal treatment temps, quenching-in water promptly obtains the Ti of requirement of the present invention 64Zr 32Sn 4Shape memory alloy material.
Adopt wire cutting method, at the above-mentioned Ti that makes 64Zr 32Sn 4Cut in the alloy material and be of a size of 1 * 2 * 2mm 3Rectangular parallelepiped as the phase transformation specimen, adopting Perkin-Elmer DSC-7 type differential scanning calorimetry instrument to measure its martensitic transformation temperature is 547 ℃ (shown in Figure 1A).Cut diameter d=5mm, the right cylinder of height h=8mm adopts MTS-880 type universal material experimental machine to carry out compression pressure-strain testing as the compression experiment sample, and compressive strain speed is 0.02mm/min, and temperature is 20 ℃.It is compressed to 10% stress-strain curve see shown in Figure 1, compression yield strength 798MPa.By in 6%～12% scope, applying different prestrains, be heated to the above recovery of shape of transformation temperature then, measure the recovery of shape strain, be that to obtain its maximum shape memory effect at 10% o'clock be 1.35% in prestrain.
Embodiment 2:System Ti 50Zr 48Al 2Alloy material
(1) taking by weighing 50at% purity is that 99.9% titanium, 48at% purity are that 99.9% zirconium and 2at% purity are 99.9% aluminium;
(2) above-mentioned titanium, zirconium and aluminium block shape raw material are put into non-consumable arc furnace, be evacuated to 3 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrAl ingot at 2000 ℃ then;
(3) vacuum heat treatment furnace that the above-mentioned TiZrAl ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 1 hour down of 850 ℃ of thermal treatment temps, quenching-in water promptly obtains the Ti of requirement of the present invention 50Zr 48Al 2Shape memory alloy material.
This Ti 50Zr 48Al 2The martensitic transformation temperature of shape memory alloy material is 483 ℃.
Performance test is identical with embodiment 1, Ti 50Zr 48Al 2Shape memory alloy material be compressed to 10% stress-strain curve see shown in Figure 2, the compression yield strength 717MPa in the time of 20 ℃.By in 6%～12% scope, applying different prestrains, be heated to the above recovery of shape of transformation temperature then, measure the recovery of shape strain, be that to obtain its shape memory effect at 10% o'clock be 1.40% in prestrain.
Embodiment 3:System Ti 60Zr 32Mo 8Alloy material
(1) taking by weighing 60at% purity is that 99.9% titanium, 32at% purity are that 99.9% zirconium and 8at% purity are 99.9% molybdenum;
(2) the block raw material of above-mentioned titanium, zirconium and molybdenum is put into non-consumable arc furnace, be evacuated to 4 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrMo ingot at 2100 ℃ then;
(3) vacuum heat treatment furnace that the above-mentioned TiZrMo ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 2 hours down of 900 ℃ of thermal treatment temps, quenching-in water promptly obtains the Ti of requirement of the present invention 60Zr 32Mo 8Shape memory alloy material.
This Ti 60Zr 32Mo 8The martensitic transformation temperature of shape memory alloy material is 45 ℃.
Performance test is identical with embodiment 1, Ti 60Zr 32Mo 8Shape memory alloy material be compressed to 10% stress-strain curve see shown in Figure 3, compression yield strength 849MPa.By in 6%～12% scope, applying different prestrains, be heated to the above recovery of shape of transformation temperature then, measure the recovery of shape strain, be that to obtain its shape memory effect at 10% o'clock be 1.36% in prestrain.
Embodiment 4:System Ti 50Zr 46Cr 4Alloy material
(1) taking by weighing 50at% purity is that 99.9% titanium, 46at% purity are that 99.9% zirconium and 4at% purity are 99.9% chromium;
(2) the block raw material of above-mentioned titanium, zirconium and chromium is put into non-consumable arc furnace, be evacuated to 3 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrCr ingot at 1800 ℃ then;
(3) vacuum heat treatment furnace that the above-mentioned TiZrCr ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 1 hour down of 900 ℃ of thermal treatment temps, quenching-in water promptly obtains the Ti of requirement of the present invention 50Zr 46Cr 4Shape memory alloy material.
This Ti 50Zr 46Cr 4The martensitic transformation temperature of shape memory alloy material is 147 ℃.
Performance test is identical with embodiment 1, Ti 50Zr 46Cr 4Shape memory alloy material be compressed to 10% stress-strain curve see shown in Figure 4, compression yield strength 510MPa.By in 6%～12% scope, applying different prestrains, be heated to the above recovery of shape of transformation temperature then, measure the recovery of shape strain, be that to obtain its shape memory effect at 10% o'clock be 1.53% in prestrain.
Embodiment 5:System Ti 62Zr 32Ag 6Alloy material
(1) taking by weighing 62at% purity is that 99.9% titanium, 32at% purity are that 99.9% zirconium and 6at% purity are 99.9% silver;
(2) above-mentioned titanium, zirconium and silver bullion shape raw material are put into non-consumable arc furnace, be evacuated to 4 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrAg ingot at 1900 ℃ then;
(3) vacuum heat treatment furnace that the above-mentioned TiZrAg ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 1.5 hours down of 880 ℃ of thermal treatment temps, quenching-in water promptly obtains the Ti of requirement of the present invention 62Zr 32Ag 6Shape memory alloy material.
This Ti 62Zr 32Ag 6The martensitic transformation temperature of shape memory alloy material is 246 ℃.
Performance test is identical with embodiment 1, Ti 62Zr 32Ag 6Shape memory alloy material be compressed to 10% stress-strain curve see shown in Figure 2, compression yield strength 683MPa.By in 6%～12% scope, applying different prestrains, be heated to the above recovery of shape of transformation temperature then, measure the recovery of shape strain, be that to obtain its shape memory effect at 10% o'clock be 1.26% in prestrain.
Embodiment 6:System Ti 62Zr 32Ga 6Alloy material
(1) taking by weighing 62at% purity is that 99.9% titanium, 32at% purity are that 99.9% zirconium and 6at% purity are 99.9% gallium;
(2) the block raw material of above-mentioned titanium, zirconium and gallium is put into non-consumable arc furnace, be evacuated to 5 * 10 -3Pa charges into high-purity argon gas to 1.01 * 10 5Pa is smelted into the TiZrGa ingot at 1900 ℃ then;
(3) vacuum heat treatment furnace that the above-mentioned TiZrGa ingot that makes is put into is heat-treated, in vacuum tightness 5 * 10 -3Pa, the insulation after 1 hour down of 900 ℃ of thermal treatment temps, quenching-in water promptly obtains the Ti of requirement of the present invention 62Zr 32Ga 6Shape memory alloy material.
This Ti 62Zr 32Ga 6The martensitic transformation temperature of shape memory alloy material is 246 ℃.
Performance test is identical with embodiment 1, Ti 62Zr 32Ga 6Shape memory alloy material be compressed to 10% stress-strain curve see shown in Figure 6, compression yield strength 639MPa.By in 6%～12% scope, applying different prestrains, be heated to the above recovery of shape of transformation temperature then, measure the recovery of shape strain, be that to obtain its shape memory effect at 10% o'clock be 1.41% in prestrain.
In vacuum tightness 4 * 10 -3The performance perameter such as the following table of the following shape memory alloy that Pa, 2000 ℃ of smelting temperatures, 900 ℃ of thermal treatment temps, insulation made in 1 hour:
Composition Yield strength in the time of 20 ℃ (MPa) Deformation rate (%) Shape memory effect (%) Transformation temperature (℃)
Ti 64Zr 35Sn 1 815 34 1.21 592
Ti 60Zr 32Sn 8 672 23 1.44 215
Ti 50Zr 49Al 1 820 25 1.9 627
Ti 60Zr 34Al 6 900 21 1.22 695
Ti 67Zr 32Mo 1 810 33 1.21 492
Ti 50Zr 40Mo 10 703 22 1.75 34
Ti 58Zr 41Cr 1 670 32 1.42 502
Ti 50Zr 42Cr 8 525 34.5 1.95 25
Ti 62Zr 37Ag 1 811 28.2 1.3 611
Ti 50Zr 43Ag 7 593 22 1.5 570
Ti 69Zr 30Ga 1 772 30.1 1.7 585
Ti 60Zr 40Ga 10 502 32 2.2 75

Claims (1)

1, a kind of titanium-zirconium-base ternary shape memory alloy material is characterized in that: this titanium-zirconium-base ternary shape memory alloy material is Ti 62Zr 32Ga 6
CNB2007101755102A 2007-09-30 2007-09-30 A kind of titanium-zirconium-base ternary shape memory alloy material and preparation method thereof Expired - Fee Related CN100540704C (en)

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CN104988374B (en) * 2015-08-13 2017-05-10 上海大学 Titanium-zirconium-tantalum shape memory alloy material and preparation method thereof
CN107760924A (en) * 2017-10-24 2018-03-06 宝鸡金恒瑞金属科技有限公司 A kind of preparation method of titanium alloy bicycle lock
CN109055813A (en) * 2018-07-17 2018-12-21 秦小梅 A kind of alloy material and preparation method thereof with memory function
CN110438370B (en) * 2019-09-03 2021-06-29 河北工业大学 High-strength-toughness corrosion-resistant titanium-zirconium-based alloy and preparation method thereof
CN111056050B (en) * 2019-10-17 2021-07-06 北京航空航天大学 SMA-spring driven flywheel repeatable locking mechanism
CN113684409A (en) * 2021-08-11 2021-11-23 河北工业大学 Zirconium-titanium-nickel alloy and preparation method thereof

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