CN102146534A - Low-elasticity high-strength near beta-type Ti-Nb-Ta-Zr alloy and preparation method of near beta-type Ti-Nb-Ta-Zr alloy - Google Patents
Low-elasticity high-strength near beta-type Ti-Nb-Ta-Zr alloy and preparation method of near beta-type Ti-Nb-Ta-Zr alloy Download PDFInfo
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Abstract
The invention discloses a low-elasticity high-strength modulus near beta-type Ti-Nb-Ta-Zr alloy. The near beta-type Ti-Nb-Ta-Zr alloy consists of the following components in percentage by weight: 28 to 32 percent of niobium, 4 to 5.5 percent of tantalum, 5 to 15 percent of zirconium and the balance of titanium. A preparation method comprises the following steps of: proportioning the components according to the proportion, and smelting the components into a button-shaped Ti-Nb-Ta-Zr cast ingot through a vacuum non-consumable arc furnace; thermally forging the button-shaped Ti-Nb-Ta-Zr cast ingot into a thin plate with size of 3mm*30mm*70mm; performing solution treatment on a linearly cut sample at the temperature of between 750 and 800 DEG C, and performing water quenching to obtain single-phase beta tissues; and performing ageing treatment on the solution treatment sample at the temperature of between 450 and 500 DEG C, and performing air cooling to obtain two-phase tissues of beta phase and dispersed alpha phase. The alloy can be widely applied to human hard tissue repair, replacement of medicinal materials and other medicinal devices.
Description
Technical field
The present invention relates to the nearly β type of a kind of low elastic modulus Ti-Nb-Ta-Zr Alloy And Preparation Method, belong to human body hard tissue and replace and repair used field of medical materials.
Background technology
Titanium alloy has obtained using widely at orthopaedics, decorative sursery, aspect such as cardiovascular because of having higher intensity, lower Young's modulus, excellent biological compatibility and good corrosion resistance.The titanium alloy that is most widely used clinically at present is Ti-6Al-4V, but this alloy contains V and two kinds of elements of Al, and the Al element can cause symptoms such as osteomalacia, anaemia and nervous disorders, and V also is considered to the deleterious element of organism, and toxicity has surpassed Ni and Cr.Genotoxic potential for fear of V, two kinds of novel alpha+beta alloy Ti-5Al-2.5Fe and Ti-6Al-7Nb of the mid-80 in last century are developed, the mechanical property and the Ti-6Al-4V of this type of alloy are close, but Young's modulus is about 105～110GPa, though far below traditional medical stainless steel and cochrome, but still much larger than the Young's modulus (10-40GPa) of people's bone, and harmful Al element still exists.With alpha+beta alloy phase ratio, beta-titanium alloy has higher hardness and toughness, and Young's modulus is lower, is suitable as the implant into body material.The nineties in last century is to begin the third generation medical titanium alloy of focus development based on beta-titanium alloy headed by the U.S., the Japan.The alloy in this stage mainly pays attention to adding nontoxic element nb, Ta, Zr, Mo, Sn, and the functional design of alloy trends towards low elastic modulus, strong wear resistance, erosion resistance and excellent biological compatibility etc.Kai Fa biological medical titanium alloy has Ti-15Mo in view of the above, Ti-15Mo-3Nb, Ti-13Nb-15Mo-13Zr, Ti-12Mo-6Zr-2Fe, Ti-13Nb-13Zr etc.Wherein typical Ti-12Mo-6Zr-2Fe(E=74GPa) with Ti-13Nb-13Zr(E=79GPa) Young's modulus compare with Ti-6Al-4V, though reduce, but still be higher than the Young's modulus of people's bone.Recently, to concentrate on Ti-Nb-Ta-Zr be on the alloy for a large amount of research.Ti-35Nb-7Zr-5Ta and Ti-29Nb-13Ta-4.6Zr are wherein typically arranged.Wherein the Young's modulus of Ti-35Nb-7Zr-5Ta is 52GPa, but the intensity of this alloy had only 530MPa before oozing the oxygen processing.Ti-29Nb-13Ta-4.6Zr has excellent mechanical property, but Young's modulus is 84Gpa, and it is a lot of still to exceed people's cortex bone.So can reach simultaneously or near the Young's modulus of people's cortex bone, and have higher intensity, the Ti-Nb-Ta-Zr that has performances such as good biocompatibility simultaneously is that alloy allows the people expect.
Summary of the invention
Add the big and high shortcoming of Young's modulus of element toxicity at existing in the present medical titanium alloy research, by adding nontoxic element, adjust constituent content and thermal treatment process and improve the biocompatibility of embedded material, alleviate between inner implantation material and the bone Young's modulus caused " stress shielding " phenomenon that do not match, the object of the invention is to provide that a kind of intensity is moderate, low elastic modulus, biocompatibility are good, technology is simply low plays high-strength nearly β type Ti-Nb-Ta-Zr Alloy And Preparation Method.This alloy can be widely used in the human body hard tissue reparation and replace medical material and other medical devices.
The present invention adopts following technical scheme:
The nearly β type of a kind of low elastic modulus of the present invention Ti-Nb-Ta-Zr alloy, described nearly β type Ti-Nb-Ta-Zr alloy is made up of niobium, tantalum, zirconium and titanium, and weight percent is: niobium 28%-32%, tantalum 4%-5.5%, zirconium 5%-15%, surplus is a titanium.
The preparation method of the nearly β type of low elastic modulus of the present invention Ti-Nb-Ta-Zr alloy, processing step is:
(1) prepares burden by said ratio, be smelted into button shape Ti-Nb-Ta-Zr ingot casting through vacuum non-consumable arc furnace;
(2) with button shape Ti-Nb-Ta-Zr ingot casting after forge hot, be swaged into and be of a size of the lamellar of 3mm * 30mm * 70mm;
(3) sample after the warp cutting is 750 ℃ of-800 ℃ of solution treatment, and shrend obtains single-phase β tissue;
(4) sample after the solid solution is 450 ℃ of-500 ℃ of ageing treatment, and air cooling obtains the two-phase structure of β phase+disperse α phase.
Its preparation technology's flow process is: batching, vacuum non-consumable arc melting add electromagnetism and stir, survey transformation temperature, forge hot, solid solution, shrend, artificial aging, air cooling, performance test (stretching, microstructure observation, X ray phase structure are analyzed).Nearly beta titanium alloy have the proximate Young's modulus of people's bone, excellent biocompatibility and under coenocorrelation superior corrosion resistance etc., obtained application more and more widely in recent years clinically.When alloying constituent is selected, consider that medical material must possess biological chemistry consistency and biomechanical compatibility.The biological chemistry consistency is meant that material must not have cytotoxicity, tissue irritation, genetoxic, carinogenicity, can not cause immune response, anaphylaxis etc.; Mechanical compatibility is meant the characteristic of the mechanical characteristic of material near reparation portion, even its function of life-time service can not change yet, wants the Young's modulus of lay special stress on material here.When the Young's modulus of the Young's modulus of material and people's bone does not match, under the effect of stress, metal with stress will produce different strains with bone, relative displacement appears at metal and bone contact surface place, cause at the interface loosening, perhaps exert all one's strength and to be delivered to its contiguous natural bone tissue from human synovial fully, cause the absorption of bone and the degeneration of function, produce the stress shielding phenomenon, cause the failure of implantation.Therefore, the Young's modulus of generally wishing metallic substance to try one's best near or the Young's modulus of a little higher than people's bone.The Nb that adds among the present invention, Ta, Zr are nontoxic elements, and good biocompatibility all can be at the mechanical property of improving alloy in varying degrees, erosion resistance and wear resisting property.Particularly the Young's modulus of alloy of the present invention approaches people's bone (a little more than people's bone), is suitable as embedded material
Nearly beta-titanium alloy of the present invention adopts the vacuum non-consumable arc furnace melting to add repeatedly induction stirring, surveys transformation temperature, forge hot, solid solution, shrend, artificial aging, air cooling.
The performance index of material are as follows respectively:
The alloy of solution treatment:
Young's modulus (GPa): 42-52, tensile strength (MPa): 590-751, yield strength (MPa): 361-722, unit elongation (%): 3.3-33.8.
The alloy of ageing treatment:
Young's modulus (GPa): 49-65, tensile strength (MPa): 739-971, yield strength (MPa): 649-896, unit elongation (%): 4.5-8.8.
The fusing point of Ta is up to 2996 ℃, so Ta generally adopts master alloy to add during melting, two kinds of schemes of Nb-Ta master alloy and Zr-Ta master alloy arranged.The Zr-Ta alloy is after melting, solidifying and cool off, can form Ta sosoloid (composition is near pure Ta) and β-Zr sosoloid (composition is near pure Zr) two-phase structure, the fusing point of Ta sosoloid is still very high on the one hand, the composition difference of Ta sosoloid and β-Zr sosoloid is very big on the other hand, especially when cooling rate causes crystal grain thick more slowly, can cause the significantly inhomogeneous of master alloy composition, and this phenomenon can't be eliminated by high temperature diffusion annealing.
The Nb-Ta alloy constitutes the uniform grain phasor, and the Nb-Ta alloy of all the components infinitely dissolves each other down solid-state.The Nb-Ta alloy can form the uniform Nb-Ta sosoloid of composition after melting, solidifying and cool off, in the present invention as master alloy, guaranteed the height uniform distribution of Ta element when the Ti-Nb-Ta-Zr alloy prepares.
Description of drawings
Fig. 1. the energy spectrum analysis of Ti-Nb-Ta-Zr alloy cast ingot.
Fig. 2. Ti-30Nb-5Ta-12Zr alloy solid solution attitude tissue.
Fig. 3. Ti-30Nb-5Ta-12Zr alloy solid solution attitude X ray diffracting spectrum.
Fig. 4. Ti-30Nb-5Ta-6Zr alloy aging attitude SEM figure.
Fig. 5. Ti-30Nb-5Ta-6Zr alloy aging attitude X ray diffracting spectrum.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
A) alloy preparation
The Ti-30Nb-5Ta-9Zr alloy, Ti, Nb, Ta, Zr pure metal are by alloying constituent mass percent batching, through the non-consumable arc furnace melting, abundant induction stirring, melting voltage is the 10-34 volt, the melting electric current is the 50-300 ampere, and the induction stirring electric current is the 6-12 ampere, and the melting number of times is 3-5 time.Obtain button shape ingot casting after the melting repeatedly.
B) forge hot
Ingot blank is swaged into thick 3mm after forge hot, long 70mm, the sheet material of wide 30mm, warp cut into the stretching sample.
C) thermal treatment
The stretching sample is carried out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 750 ℃, and solution time is 0.5h, carries out shrend after the solid solution.
D) material property
Young's modulus (GPa): 42; Tensile strength (MPa): 614; Yield strength (MPa): 374; Unit elongation (%): 12.8
Embodiment 2:
A) alloy preparation
The Ti-30Nb-5Ta-12Zr alloy, Ti, Nb, Ta, Zr pure metal are by alloying constituent mass percent batching, through the non-consumable arc furnace melting, abundant induction stirring, melting voltage is the 10-34 volt, the melting electric current is the 150-350 ampere, and the induction stirring electric current is the 10-15 ampere, and the melting number of times is 3-5 time.Obtain button shape ingot casting after the melting repeatedly.
B) forge hot
Ingot blank is swaged into thick 3mm after forge hot, long 70mm, the sheet material of wide 30mm, warp cut into the stretching sample.
C) thermal treatment
The stretching sample is carried out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 800 ℃, and solution time is 1h, carries out shrend after the solid solution.
D) material property
Young's modulus (GPa): 44; Tensile strength (MPa): 657; Yield strength (MPa): 584; Unit elongation (%): 9
Embodiment 3:
A) alloy preparation
The Ti-30Nb-5Ta-6Zr alloy, Ti, Nb, Ta, Zr pure metal are by alloying constituent mass percent batching, through the non-consumable arc furnace melting, abundant induction stirring, melting voltage is the 10-34 volt, the melting electric current is the 100-300 ampere, and the induction stirring electric current is the 8-14 ampere, and the melting number of times is 3-5 time.Obtain button shape ingot casting after the melting repeatedly.
B) forge hot
Ingot blank is swaged into thick 3mm after forge hot, long 70mm, the sheet material of wide 30mm, warp cut into the stretching sample.
C) thermal treatment
The stretching sample is carried out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 750 ℃, and solution time is 0.5h, carries out shrend after the solid solution.The artificial aging temperature is 500 ℃, and aging time is 12h, air cooling.
D) material property
Young's modulus (GPa): 65; Tensile strength (MPa): 971; Yield strength (MPa): 896; Unit elongation (%): 7.8
Embodiment 4
The nearly β type of a kind of low elastic modulus Ti-Nb-Ta-Zr alloy, described nearly β type Ti-Nb-Ta-Zr alloy is made up of niobium, tantalum, zirconium and titanium, and weight percent is: niobium 28%-32%, tantalum 4%-5.5%, zirconium 5%-15%, surplus is a titanium, the β stability factor of the described alloy of present embodiment
Be 1.08 ~ 1.26, after solution treatment, the Young's modulus of alloy is all less than 52GPa.In the present embodiment, the weight percent of alloy consists of: niobium 28%, and tantalum 4%, zirconium 5%, surplus is a titanium; Niobium 32%, tantalum 5.5%, zirconium 15%, surplus is a titanium; Perhaps, niobium 31%, tantalum 4.5%, zirconium 10%, surplus is a titanium.
Embodiment 5
The preparation method of the nearly β type of a kind of low elastic modulus Ti-Nb-Ta-Zr alloy, processing step is:
(1) prepares burden by said ratio, be smelted into button shape Ti-Nb-Ta-Zr ingot casting through vacuum non-consumable arc furnace;
(2) with button shape Ti-Nb-Ta-Zr ingot casting after forge hot, be swaged into and be of a size of the lamellar of 3mm * 30mm * 70mm;
(3) sample after the warp cutting is 750 ℃ of-800 ℃ of solution treatment, and shrend obtains single-phase β tissue;
(4) sample after the solid solution is 450 ℃ of-500 ℃ of ageing treatment, and air cooling obtains the two-phase structure of β phase+disperse α phase.
In the present embodiment:
The vacuum non-consumable arc furnace melting voltage that uses lies prostrate as 10-34, and the melting electric current is the 50-350 ampere, and the induction stirring electric current is the 0-18 ampere, and the melting number of times is 3-5 time.
Niobium and tantalum are the form addings with the Nb-Ta master alloy during batching, described Nb-Ta master alloy is obtained by following method: niobium and tantalum are added to be smelted in the vacuum non-consumable arc furnace obtain the uniform block Nb-Ta solid solution alloy of composition, the melting electric current is the 80-320 ampere, the induction stirring electric current is the 8-18 ampere, and the melting number of times is 3-5 time.
After the forge hot, its deflection is 70%-80%, carries out in air.
The solution treatment time is 0.5 h ~ 2 hours, and ageing treatment is 6 h ~ 24 hours.
With reference to Fig. 1, the alloy cast ingot energy spectrum analysis shows it by Ti, Nb, and Ta, four kinds of Zr are elementary composition.
With reference to Fig. 2 and 3, Ti-30Nb-5Ta-12Zr alloy solid solution attitude is organized as the single axle β phase that waits.
With reference to Figure 4 and 5, Ti-30Nb-5Ta-6Zr alloy aging attitude tissue is by the α phase composite of β phase+disperse.
Claims (8)
1. the nearly β type of low elastic modulus Ti-Nb-Ta-Zr alloy, it is characterized in that: described nearly β type Ti-Nb-Ta-Zr alloy is made up of niobium, tantalum, zirconium and titanium, and weight percent is: niobium 28%-32%, tantalum 4%-5.5%, zirconium 5%-15%, surplus is a titanium.
2. by the nearly β type of the described low elastic modulus of claim 1 Ti-Nb-Ta-Zr alloy, the Young's modulus that it is characterized in that alloy after the solution treatment is all less than 52GPa.
3. by the nearly β type of the described low elastic modulus of claim 1 Ti-Nb-Ta-Zr alloy, it is characterized in that the β stability factor of alloy
Be 1.08 ~ 1.26.
4. the preparation method of any nearly β type of described low elastic modulus Ti-Nb-Ta-Zr alloy among the claim 1-3 is characterized in that processing step is:
Proportioning by claim 1 is prepared burden, and is smelted into button shape Ti-Nb-Ta-Zr ingot casting through vacuum non-consumable arc furnace;
Button shape Ti-Nb-Ta-Zr ingot casting after forge hot, is swaged into and is of a size of the lamellar of 3mm * 30mm * 70mm;
Sample after the warp cutting is 750 ℃ of-800 ℃ of solution treatment, and shrend obtains single-phase β tissue;
Sample after the solid solution is 450 ℃ of-500 ℃ of ageing treatment, and air cooling obtains the two-phase structure of β phase+disperse α phase.
5. by the described preparation method of claim 4, it is characterized in that the vacuum non-consumable arc furnace melting voltage that uses lies prostrate as 10-34, the melting electric current is the 50-350 ampere, and the induction stirring electric current is the 0-18 ampere, and the melting number of times is 3-5 time.
6. by the described preparation method of claim 4, tantalum is the form adding with the Nb-Ta master alloy when it is characterized in that preparing burden, described Nb-Ta master alloy is obtained by following method: niobium and tantalum are added to be smelted in the vacuum non-consumable arc furnace obtain the uniform block Nb-Ta solid solution alloy of composition, the melting electric current is the 80-320 ampere, the induction stirring electric current is the 8-18 ampere, and the melting number of times is 3-5 time.
7. by the described preparation method of claim 4, it is characterized in that forge hot after, its deflection is 70%-80%, carries out in air.
8. by the described preparation method of claim 4, it is characterized in that the solution treatment time is 0.5 h ~ 2 hours, ageing treatment is 6 h ~ 24 hours.
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| CN103060609A (en) * | 2011-10-21 | 2013-04-24 | 北京航空航天大学 | Near-beta titanium alloy with low elastic modulus and high strength and preparation method of near-beta titanium alloy |
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| CN103334029A (en) * | 2013-06-04 | 2013-10-02 | 上海交通大学 | Beta titanium alloy composition and preparation method thereof |
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Application publication date: 20110810 |