CN103526062B - Ti-Nb-O memory alloy having high recoverable strain and preparation method thereof - Google Patents
Ti-Nb-O memory alloy having high recoverable strain and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Ti-Nb-O memory alloy having a high recoverable strain and a preparation method thereof. The method comprises the steps: mixing uniformly a pure Ti powder, a pure Nb powder, a pure TiO2 powder and a pure TiH2 powder according to the ratio of Ti atoms, Nb atoms, O atoms and H atoms being (77-91):(8-18):(1-3):(0-5), and carrying out compression molding to obtain a green body; putting the green body into a sintering furnace, sintering under a protective gas atmosphere, and thus obtaining a sintered-state Ti-Nb-O alloy; putting the Ti-Nb-O alloy into a tube furnace, carrying out solid solution treatment under the argon gas protection, putting the solid solution state Ti-Nb-O memory alloy into the tube furnace, carrying out aging treatment under the argon gas protection, and then rapidly cooling in ice water to obtain the high recoverable strain. The Ti-Nb-O alloy shows low elastic modulus, extremely high compressive strength and relatively high recoverable strain, and is suitable for use in medical hard tissue replacement and reparation materials.
Description
Technical field
The present invention relates to Ti-Nb-O memorial alloy of a kind of high recoverable strain and preparation method thereof, belong to medical human sclerous tissues and replace and repair materials field.
Background technology
Along with the fast development of economy, people's life and the improving constantly of medical level, the simultaneously continuous decrease of natality, thus national aging population is caused constantly to aggravate.The elderly easily suffers the torment of various degenerative disorders (as osteoporosis), and curing at present the most effective means of this kind of disease is adopt embedded material to replace the sclerous tissues of damage.Therefore, the elderly is increasing for the demand of sclerous tissues's replacement and repair materials.General requirement hard tissue implanting material has good biocompatibility (can not damage human body), high intensity (preventing implant devices to be out of shape or fracture), low Young's modulus (reducing " stress shielding " effect) and similar mechanical behavior.At present, main based on titanium and titanium alloys in hard tissue implanting material, this is because the lifeless matter toxicity of titanium alloy, high specific tenacity and excellent erosion resistance determine.
But people are also more and more stricter for the performance requriements of medical embedded material.Therefore, the development of medical titanium alloy is also round raising biocompatibility and biomechanical compatibility, and reduction Young's modulus, experienced by three phases successively: the α-Ti alloy that the first-generation is is representative with commercially pure Ti, the s-generation is with Ti-6Al-4V(mass ratio) be representative (alpha+beta)-Ti alloy, the third generation is with Ti-13Nb-13Zr(mass ratio) be the pure β-Ti alloy of representative.Recently, the β-Ti alloy (Ti base marmem is generally nontoxic elementary composition by some, has better biocompatibility) that a class has a shape memory effect becomes a focus in medical titanium alloy field.This super-elasticity mainly due to shape memory alloy uniqueness is similar to the mechanical behavior of some biological tissues (as bone, tendon etc.), namely also can restore to the original state afterwards bearing comparatively large sstrain (>3%).Meanwhile, Ti base marmem has good comprehensive mechanical property (comprising high fatigue resistance and wear resistance) due to super-elasticity; And it has relatively low Young's modulus, " stress shielding " effect can be reduced after implantation, prevent osteoporosis to greatest extent; And excellent biology performance (comprising erosion resistance, without harmful ion release, biocompatibility etc.), make Ti base marmem become a kind of material having development potentiality in sclerous tissues's replacement and medical metal material most.
At present, the medical titanium alloy with certain super-elasticity (recoverable strain) developed mainly contains Ti-Nb system, Ti-Mo system and Ti-Ta system etc.Wherein Ti-Nb system alloy is more by everybody concern, mainly due to its good mechanical property and biocompatibility, comprise Ti-Nb binary system, Ti-Nb-X(X=Sn, Zr, Ta, Mo etc.) quaternary system such as ternary system and Ti-Nb-Zr-Sn and Ti-Nb-Ta-Zr.But, for the medical embedded TiNi memorial alloy that another receives much concern, the recoverable strain of Ti base memorial alloy and intensity or on the low side, and also Young's modulus is high.Such as, TiNi memorial alloy recoverable strain reaches as high as 8%, compressive strength is about 1200MPa, Young's modulus is low to moderate about 48GPa, be close with human bone head mould amount (4-30GPa).But problem maximum in TiNi memorial alloy is that excessive Ni Ion release can cause potential sensitization, teratogenesis and carcinogenic toxic side effect containing a large amount of harmful Ni elements in alloy.Then there is not this problem completely in Ti base memorial alloy, but its current most pressing problem improves recoverable strain, reduces Young's modulus simultaneously.
At present, the method preparing medical titanium base memorial alloy mainly follows conventional lines the preparation method of titanium alloy, namely adopts high melt to prepare alloy, then roll forming, auxiliary heat process subsequently improves recoverable strain and intensity, and Young's modulus is mainly adjusted by alloying constituent.But the medical titanium alloy adopting this ordinary method to prepare is difficult to obtain the premium properties that high recoverable strain, low elastic modulus and high strength etc. meet medical embedded requirement simultaneously.Such as, through short-cycle annealing process in 300 DEG C, 10 minutes after Ti-24Nb (atomic ratio) alloy is cold rolling, lower Young's modulus (35GPa) and higher tensile strength (900MPa) can be shown, but recoverable strain only has 2.5%; In order to improve recoverable strain further, other constituent element is added again on binary alloy basis, as the solution treatment after cold rolling of Ti-22Nb-0.5O (atomic ratio) alloy, its maximum recoverable strain can reach about 4%; Through 550 DEG C of anneal after Ti-22Nb-6Zr (atomic ratio) alloy is cold rolling, its maximum recoverable strain can bring up to 4.9%, but Young's modulus also correspondingly increases; And for example, Ti-24Nb-4Zr-8Sn-0.4O (mass ratio) alloy of Ultra-fine Grained is after 400 DEG C of hot rollings, and its tensile strength is up to 1200MPa, but Young's modulus is increased to 56GPa again, but the most important thing is that recoverable strain is low to moderate about 3%.And ordinary method is difficult to prepare some special-shaped implant devices, namely allows to preparation and also there is the shortcoming such as complex procedures, production cost height; Meanwhile, do not changing on the basis of alloying constituent, ordinary method is difficult to fall low-alloyed Young's modulus further.Therefore, also need urgently at present to develop a kind of simple and easy effective ways preparing Ti base memorial alloy.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, the object of the present invention is to provide the Ti-Nb-O memorial alloy of high recoverable strain, can the potential replacement for human body hard tissue and repair materials.
Another object of the present invention is to the preparation method of the Ti-Nb-O memorial alloy that above-mentioned high recoverable strain is provided.
The present invention is achieved through the following technical solutions:
A preparation method for the Ti-Nb-O memorial alloy of high recoverable strain, comprises following operation steps:
(1) pure Ti powder, Nb powder, TiO
2powder and TiH
2powder is (77 ~ 91) according to Ti atom, Nb atom and O atom and H atom ratio: (8 ~ 18): (0 ~ 3): (0 ~ 5) mixes, and the powder compression moulding in atmosphere then will mixed, obtains green compact;
(2) step (1) gained green compact are put into sintering oven, sinter under shielding gas atmosphere, sintering temperature 1300 ~ 1400 DEG C, sintering time is 8 ~ 16 hours, obtain the Ti-Nb-O alloy of sintered state, the atomic ratio of its Ti:Nb:O is (82 ~ 91): (8 ~ 18): (1 ~ 3);
(3) the Ti-Nb-O alloy of step (2) gained sintered state is put into tube furnace, solution treatment is carried out under argon shield, solid solubility temperature is 900 ~ 1000 DEG C, and solution time is 1 ~ 5h, is then cooled fast in frozen water and obtains solid solution state Ti-Nb-O memorial alloy;
(4) the Ti-Nb-O memorial alloy of step (3) gained solid solution state is put into tube furnace; ageing treatment is carried out under argon shield; aging temp is 300 ~ 600 DEG C; aging time is 0 ~ 10h; then be cooled fast in frozen water the Ti-Nb-O memorial alloy obtaining high recoverable strain, recoverable strain is 4 ~ 5.5%.
Preferably, step (1) described mixing adopts ball milled or conventional powder mixing method to mix.
The described pure Ti powder of step (1), Nb powder, TiO
2powder and TiH
2the purity of powder is all mass percent more than 99.5%; Described pure Ti powder, Nb powder, TiO
2powder and TiH
2the particle size of powder is 48 ~ 75 μm.
Step (1) described press forming adopts compression molding to carry out; The pressure of described press forming is 400 ~ 600MPa, and temperature is 30 ~ 100 DEG C, and the time is 5 minutes ~ 15 minutes.
Step (2) described sintering adopts vacuum sintering or low pressure sintering method to sinter.
Step (3) described shielding gas is vacuum or argon gas.
A Ti-Nb-O memorial alloy for high recoverable strain, is obtained by above-mentioned preparation method.
The Ti-Nb-O memorial alloy of height recoverable strain of the present invention is the Ti-Nb-O memorial alloy of a kind of high recoverable strain, low modulus, high strength, potentially can be applied to the reparation and replacement device of preparing Thigh bone, focile, lumbar vertebrae or cervical vertebra.
Generally can show higher intensity (800 ~ 900MPa), relatively low Young's modulus (50 ~ 60GPa) and certain recoverable strain (<3%) through melting, cold rolling and heat treated block Ti-22Nb alloy (atomic ratio), Ti and Nb element is all the good element of biocompatibility simultaneously.Further, in titanium alloy, the appropriate O element of solid solution can improve its intensity and biocompatibility and change the transformation temperature of alloy.The present invention by adding a small amount of TiO in mixed powder
2and TiH
2powder, utilizes TiH
2the H that powder decomposes out in high-temperature sintering process
2o element residual in green compact is combined, forms steam and is also pumped, thus controls solid solution in sintering process and enter the O content in TiNb alloy, acquisition composition and the adjustable Ti-Nb-O alloy of transformation temperature; Then solid solution is carried out and ageing treatment controls the Ti-Nb-O memorial alloy that its microtexture obtains high recoverable strain, low modulus high strength.Ti, Nb and O element in the present invention is nontoxic element, good biocompatibility.Particularly the Young's modulus of alloy of the present invention is close to people's bone, and has high recoverable strain and intensity, is particularly suitable as sclerous tissues and replaces and repair materials.
Hinge structure of the present invention has following advantage and beneficial effect: the present invention successfully prepares the Ti-Nb-O memorial alloy of high recoverable strain, low modulus, high strength, and the Young's modulus of its fine and close state alloy is low to moderate 30 ~ 33GPa, close with people's bone photo; And recoverable strain is up to 4 ~ 5.5%, be close with TiNi memorial alloy; Compressive strength reaches 1400 ~ 1800MPa, considerably beyond fine and close TiNi memorial alloy simultaneously.And the present invention adopts powder metallurgy process, technique is simple, and directly can make various special-shaped device, and production cost is low, and can industrially scale operation.The most important thing is to adopt this method can directly be used for preparing various vesicular Ti-Nb-O memorial alloy, hole is utilized to reduce Young's modulus further, match with the modulus of various different human body bone, retain the characteristic of its higher-strength and large recoverable strain simultaneously.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1 solid solution state and aging state Ti-Nb-O alloy.
Fig. 2 is the metallograph of embodiment 1 solid solution state (a) and aging state (b) Ti-Nb-O alloy.
Fig. 3 is embodiment 1 solid solution state Ti-Nb-O alloy stress-strain curve at room temperature.
Fig. 4 is the XRD figure spectrum of embodiment 1 solid solution state Ti-Nb-O alloy before and after breaking.
Fig. 5 is embodiment 1 aging state Ti-Nb-O alloy stress-strain curve at room temperature.
Fig. 6 is embodiment 3 solid solution state Ti-Nb-O alloy stress-strain curve at room temperature.
Embodiment
For understanding the present invention better, below in conjunction with embodiment, the invention will be further described, but embodiment of the present invention is not limited thereto.
Embodiment 1:
(1) pure Ti powder, Nb powder, TiO
2powder and TiH
2powder adopts ball milling method to mix according to Ti atom, Nb atom and O atom and H atom than for 86:11:1:2, and the purity of powder used is all 99.5%, and particle size is 48 ~ 75 μm; Then the powder compression moulding in atmosphere will mixed, molding pressure is 600MPa, and temperature is 30 DEG C, and the time is 5 minutes, obtains green compact;
(2) step (1) gained green compact are put into sintering oven, sinter under vacuo, sintering temperature 1400 DEG C, sintering time is 10 hours, obtains the Ti-Nb-O alloy of sintered state, is 88:11:1 by the atomic ratio of its Ti:Nb:O of chemical composition analysis;
(3) the Ti-Nb-O alloy of step (2) gained sintered state is put into tube furnace, under argon shield, carry out solution treatment, solid solubility temperature is 950 DEG C, and solution time is 1h, and then in frozen water, cooling obtains solid solution state Ti-Nb-O memorial alloy fast;
(4) the Ti-Nb-O memorial alloy of step (3) gained solid solution state is put into tube furnace, ageing treatment is carried out under argon shield, aging temperature is 500 DEG C, aging time is 1h, and then in frozen water, cooling obtains the Ti-Nb-O memorial alloy of high recoverable strain, low modulus, high strength fast;
Carrying out analysis of porosity to sintered state sample (adopts Archimedes method to draw its volume, its actual density is calculated after samples weighing, then calculate the difference of theoretical density and actual density, the ratio of difference and theoretical density is porosity), show that its porosity is 5%.Sample after solid solution and ageing treatment is carried out crystal species analysis, be β phase from known its main phase of solution treatment sample of XRD result (as shown in Figure 1), and containing some α " martensitic phase, and for the sample after ageing treatment; its main phase is α " phase, simultaneously containing some β phases.This is consistent with the result that metallograph is observed (as shown in Figure 2).
At room temperature carry out compression verification to solid solution aspect product according to ASTM E9-89a standard, its stress-strain curve is shown in Fig. 3.Find that its elastic limit and compressive strength are respectively 1400MPa and 1620MPa, and recoverable strain reaches about 5%, Young's modulus is 31.5GPa.And sample shows good super-elasticity, under the prestrain of 6%, can reply 5.06% after a Cyclic Strain, response rate reaches 84%.Facies analysis (XRD the results are shown in Figure 4) is carried out to the sample before compression and after breaking, α after finding solid solution sample compression " martensitic phase becomes main phase; and β is phase-changed into a small amount of phase; this shows to there occurs stress-induced β α in opposite directions in compression process " transformation of martensitic phase, demonstrate the existence of stress-induced martensitic phase transformation.
At room temperature carry out compression verification to aging state sample, its stress-strain curve as shown in Figure 5.Find that its elastic limit and compressive strength are further enhanced, reach 1700MPa and 1870MPa respectively, and recoverable strain is up to about 6%, Young's modulus is 33.3GPa.Further, sample shows good super-elasticity, and under the prestrain of 6%, can reply 5.5% after first time Cyclic Strain, response rate reaches 92%.Therefore, aging state sample shows superstrength, good super-elasticity (recoverable strain is about 5.5%) and low Young's modulus.This material is particularly suitable for replacing or repair materials for preparing the bone bearing high-load and Large strain.The Young's modulus of such as Thigh bone or focile is about 30GPa, if the Young's modulus of embedded material is too high, because Stress transmit is less than the bone tissue around embedded material, thus causes the osteoporosis after implantation; Go back resilient after Thigh bone or 3 ~ 4% deformation of focile experience, and the highest stress energy born reaches more than 200MPa simultaneously.Ti-Nb-O memorial alloy prepared by present method, its Young's modulus be 31 ~ 33GPa and Thigh bone or focile closely, and its recoverable strain (5 ~ 5.5%) and intensity (1400 ~ 1870MPa) are greater than the maximum value that Thigh bone or focile can bear; In addition, this material does not also have bio-toxicity.
Below embodiment about the metallograph of the XRD figure spectrum of solid solution state and aging state Ti-Nb-O alloy, solid solution state (a) and aging state (b) Ti-Nb-O alloy, the XRD figure spectrum of solid solution state Ti-Nb-O alloy before and after breaking basically identical with embodiment, do not provide one by one.Solid solution state Ti-Nb-O alloy stress-strain curve at room temperature, aging state Ti-Nb-O alloy stress-strain curve are at room temperature also similar to embodiment 1.
Embodiment 2:
(1) pure Ti powder, Nb powder, TiO
2powder and TiH
2powder adopts conventional powder mixing method to mix according to Ti atom, Nb atom and O atom and H atom than for 88:11:0:0, and the purity of powder used is all 99.5%, and particle size is 48 ~ 75 μm; Then the powder compression moulding in atmosphere will mixed, molding pressure is 600MPa, and temperature is 100 DEG C, and the time is 10 minutes, obtains green compact;
(2) step (1) gained green compact are put into low-pressure sintering furnace, sinter under argon shield, sintering temperature 1400 DEG C, sintering time is 12 hours, obtains the Ti-Nb-O alloy of sintered state, and the atomic ratio of its Ti:Nb:O is 88:10.7:1.3;
(3) the Ti-Nb-O alloy of step (2) gained sintered state is put into tube furnace, under argon shield, carry out solution treatment, solid solubility temperature is 1000 DEG C, and solution time is 2h, is then cooled fast in frozen water and obtains solid solution state Ti-Nb-O memorial alloy;
(4) the Ti-Nb-O memorial alloy of step (3) gained solid solution state is put into tube furnace, ageing treatment is carried out under argon shield, aging temp is 300 DEG C, aging time is 1h, is then cooled fast in frozen water the Ti-Nb-O memorial alloy obtaining high recoverable strain, low modulus, high strength;
Carry out porosity measurement to sintered state sample, its porosity is 5%.At room temperature carry out compression verification to aging state sample, show that its elastic limit and compressive strength are respectively 1080 and 1520MPa, recoverable strain only has about 4.5%, and unit elongation is 7.3%.Meanwhile, calculating its Young's modulus is 31GPa.
Embodiment 3:
(1) pure Ti powder, Nb powder, TiO
2powder and TiH
2powder adopts ball milling method to mix according to Ti atom, Nb atom and O atom and H atom than for 83:15:2:0, and the purity of powder used is all 99.5%, and particle size is 48 ~ 75 μm; Then the powder compression moulding in atmosphere will mixed, molding pressure is 400MPa, and temperature is 50 DEG C, and the time is 15 minutes, obtains alloy green compact;
(2) step (1) gained green compact are put into hot isostatic pressing stove, sinter under argon shield, sintering temperature 1300 DEG C, sintering time is 16 hours, obtains the Ti-Nb-O alloy of sintered state, and the atomic ratio of its Ti:Nb:O is 84:13.5:2.5;
(3) the Ti-Nb-O alloy of step (2) gained sintered state is put into tube furnace, solution treatment is carried out under argon shield, solid solubility temperature is 900 DEG C, and solution time is 5h, is then cooled fast in frozen water the Ti-Nb-O memorial alloy obtaining high recoverable strain, low modulus, high strength;
Carry out porosity measurement to sintered state sample, its porosity is 6%.At room temperature carry out compression verification to sample, its stress-strain curve as shown in Figure 6.Can find out that its elastic limit and compressive strength are respectively 1050 and 1400MPa, recoverable strain only has about 4%, and unit elongation is 12.3%.Meanwhile, calculating its Young's modulus is 30.2GPa.
Embodiment 4:
(1) pure Ti powder, Nb powder, TiO
2powder and TiH
2powder adopts conventional powder mixing method to mix according to Ti atom, Nb atom and O atom and H atom than for 85:8:3:4, and the purity of powder used is all 99.5%, and particle size is 48 ~ 75 μm; Then the powder compression moulding in atmosphere will mixed, molding pressure is 500MPa, and temperature is 30 DEG C, and the time is 5 minutes, obtains alloy green compact;
(2) step (1) gained green compact are put into sintering oven, sinter under vacuo, sintering temperature 1400 DEG C, sintering time is 10 hours, obtains the Ti-Nb-O alloy of sintered state, and the atomic ratio of its Ti:Nb:O is 90.8:7.9:1.3;
(3) the Ti-Nb-O alloy of step (2) gained sintered state is put into tube furnace, solution treatment is carried out under argon shield, solid solubility temperature is 950 DEG C, and solution time is 3h, is then cooled fast in frozen water the Ti-Nb-O memorial alloy obtaining high recoverable strain, low modulus, high strength;
Carry out porosity measurement to sintered state sample, its porosity is 5%.At room temperature carry out compression verification to sample, can show that its elastic limit and compressive strength are respectively 1230 and 1580MPa, recoverable strain is about 5%, and unit elongation is 8.3%.Meanwhile, calculating its Young's modulus is 30.4GPa.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. high recoverable strain Ti ?Nb ?the preparation method of O memorial alloy, it is characterized in that comprising following operation steps:
(1) pure Ti powder, Nb powder, TiO
2powder and TiH
2powder is (77 ~ 91) according to Ti atom, Nb atom and O atom and H atom ratio: (8 ~ 18): (0 ~ 3): (0 ~ 5) mixes, then the powder compression moulding in atmosphere will mixed, obtains green compact;
(2) step (1) gained green compact are put into sintering oven, sinter under shielding gas atmosphere, sintering temperature 1300 ~ 1400 DEG C, sintering time is 8 ~ 16 hours, obtain sintered state Ti ?Nb ?O alloy, the atomic ratio of its Ti:Nb:O is (82 ~ 91): (8 ~ 18): (1 ~ 3);
(3) the Ti of step (2) gained sintered state ?Nb ?O alloy put into tube furnace, solution treatment is carried out under argon shield, solid solubility temperature is 900 ~ 1000 DEG C, and solution time is 1 ~ 5h, be then cooled fast in frozen water obtain solid solution state Ti ?Nb ?O memorial alloy;
(4) the Ti of step (3) gained solid solution state ?Nb ?O memorial alloy put into tube furnace; ageing treatment is carried out under argon shield; aging temp is 300 ~ 600 DEG C; aging time is 0 ~ 10h; then be cooled fast in frozen water obtain high recoverable strain Ti ?Nb ?O memorial alloy, recoverable strain is 4 ~ 5.5%.
2. high recoverable strain according to claim 1 Ti ?Nb ?the preparation method of O memorial alloy, it is characterized in that: step (1) described mixing adopts ball milled or conventional powder mixing method to mix.
3. high recoverable strain according to claim 1 Ti ?Nb ?the preparation method of O memorial alloy, it is characterized in that: the described pure Ti powder of step (1), Nb powder, TiO
2powder and TiH
2the purity of powder is all mass percent more than 99.5%; Described pure Ti powder, Nb powder, TiO
2powder and TiH
2the particle size of powder is 48 ~ 75 μm.
4. high recoverable strain according to claim 1 Ti ?Nb ?the preparation method of O memorial alloy, it is characterized in that: step (1) described press forming adopts compression molding to carry out; The pressure of described press forming is 400 ~ 600MPa, and temperature is 30 ~ 100 DEG C, and the time is 5 minutes ~ 15 minutes.
5. high recoverable strain according to claim 1 Ti ?Nb ?the preparation method of O memorial alloy, it is characterized in that: step (2) described sintering adopts vacuum sintering or low pressure sintering method to sinter.
6. a Ti ?Nb ?O memorial alloy for high recoverable strain, is characterized in that it is obtained by preparation method described in any one of Claims 1 to 5.
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| CN102719700A (en) * | 2012-06-04 | 2012-10-10 | 天津大学 | Ti-Nb-O high damping titanium alloy and powder metallurgy preparation method thereof |
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