CN105586507A - Beta-type Zr-Nb-Si biomedical alloy and preparation method thereof - Google Patents
Beta-type Zr-Nb-Si biomedical alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses beta-type Zr-Nb-Si biomedical alloy and a preparation method thereof. The beta-type Zr-Nb-Si biomedical alloy is prepared from, by weight, 18.46-18.79% of niobium, 0.47-1.10% of silicon and the balance sponge zirconium. The preparation method includes the steps that firstly, the corresponding raw materials are weighed according to the weight percentage of the components, the raw materials are fully mixed, then smelting is conducted by means of a nonconsumable vacuum arc furnace, and then an alloy ingot uniform in structure is obtained after cooling. The biomedical titanium alloy has advantages of traditional medical alloy and also solves the problem that the Young's modulus of the traditional medical alloy is not matched with natural bones of human bodies, and it is hopeful to solve the problem that due to mechanical property mismatching, substitute materials injure the human bodies.
Description
Technical field
The invention belongs to metal-base composites technical field, be specifically related to zirconium base biomedical alloy and preparation method thereof.
Background technology
Bio-medical material comprises the upper material that can implantable bioartificial body or can combine with bio-tissue of medical treatment, and biomaterial is used for original tissue and organ in treatment or replacement living organism, revises and improves its function. Biomedical metallic material is extensive use Srgery grafting material at present, has high strength, good toughness, counter-bending fatigue strength and good machine-shaping property, has other type medical material and is difficult to alternative premium properties. Metal material must meet strict biological requirement as bio-medical material: (1) histocompatbility is good, non-toxic, and not aberration inducing does not cause allergic reaction and disturbs the immunity of matrix, does not destroy adjacent tissue etc.; (2) physicochemical properties are stable, the stable in properties such as intensity, elasticity, size, corrosion-resistant, wearability; (3) be easy to machine-shaping, easily make the shape of various needs.
Metal current material titanium and alloy thereof are widely used on biological and medicinal implant material, and especially the application of beta-titanium alloy is more extensive. But, along with the development of medical technology, the deficiency that titanium alloy exists in biomedical application highlights gradually, one of them is exactly that elastic modelling quantity mates not with the elastic modelling quantity of natural bone, easily cause stress shielding effect, cause planting body and around occur that bone absorbs, cause phenomenons such as planting the loosening or fracture of body, be unfavorable for the long-term stability of bone healing and implant, human body is easily caused to damage. So the new bio medical alloy material that exploitation is more mated with function of human body becomes a main research direction of current bio-medical material.
It is good, non-toxic that zircaloy has good decay resistance, mechanical performance, histocompatbility, mainly as reactor core structural material, as fuel can; Be commonly used for corrosion resistant container and pipeline, as force pipe, support and duct pipe etc. But the research of zircaloy aspect bio-medical material is also quite rare, most research is all the performance that promotes titanium alloy using zirconium as the alloying element adding. And the present invention using zircaloy the application on bio-medical as main research direction, the zirconium-base alloy working out is compared with traditional titanium alloy, zirconium and alloy thereof have the corrosion resistance better than titanium, intensity, and lower elastic modelling quantity, have well made up the deficiency of conventional titanium alloy.
Summary of the invention
The object of this invention is to provide a kind of β type Zr-Nb-Si is biomedical alloy and preparation method thereof, it can substitute or the application of part instead of titanium alloy on bio-medical, it has good biocompatibility, and to human body nonhazardous, there is the elastic modelling quantity matching with skeleton simultaneously, therefore can effectively reduce and not mate the damage that human body is caused because of mechanics.
Technical solution of the present invention is as follows:
A kind of β type Zr-Nb-Si is biomedical alloy, and raw materials used component and percentage by weight are: niobium 18.46%～18.79%, and silicon 0.47～1.10%,, surplus is sponge zirconium.
As technical scheme preferably, raw material components and percentage by weight are: niobium 18.6%, silicon 0.78～1.10%, surplus is sponge zirconium, the biomedical alloy that this formula obtains, every stable in properties, functional.
The purity of sponge zirconium, niobium and silicon that the present invention adopts all, more than 99.0%, all can be bought and obtain from the market.
β type Zr-Nb-Si prepared by the present invention is that the Young's modulus of biomedical alloy is 25 ~ 27GPa, and maximum compressive strength reaches 880 ~ 1050MPa, and compression ratio is 28.0 ~ 31.0%, and yield strength is 670 ~ 750MPa.
β type Zr-Nb-Si of the present invention is the preparation method of biomedical alloy, and its preparation process is as follows:
(1) raw material takes, and takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 2 centimetres;
(2) raw material mixes, and the raw material weighing up is uniformly mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum degree control is 1 × 10-2～1×10-3Pa; Passing into inert gas carries out gas washing and removes residual air again; Finally under the protection of inert gas, carry out melting, smelting temperature is 2900～3200 DEG C; Melting voltage is 220V, and melting Current Control, at 200 ~ 220A, keeps 130s ~ 190s, and then electric current is slowly adjusted to 0A, and the time that electric current drops to 0A is 40 ~ 60s, and so melt back more than 5 times, obtains thick alloy cast ingot; Vacuumizing with gas washing of step (3) carried out 2～4 times repeatedly.
(4) thick alloy cast ingot is cooling; under inert gas shielding; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast, thick alloy is 10 ~ 30 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing; alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, the β type Zr-Nb-Si that obtains even tissue is biomedical alloy, 400-600 second whole cool time.
The inert gas that the present invention adopts is argon gas, and pressure is a standard atmospheric pressure.
Zirconium of the present invention is as alloy substrate, and niobium and silicon are as alloy element, for regulating alloy property. Niobium is conventional β phase stabilizing element, niobium has identical allotrope with zirconium at high temperature, crystal structure is all body-centered cubic, atomic radius and β-Zr are close, niobium and β-Zr can form continuous solid solution, add appropriate niobium, can significantly reduce β → α phase transition temperature, can obtain metastable β-Zr in room temperature, produce solution strengthening effect simultaneously. Niobium adds zircaloy can put forward heavy alloyed intensity and does not affect plasticity and the processing characteristics of alloy, and can strengthen the decay resistance of alloy. Alloy system of the present invention is arranged on the content of niobium to approach eutectoid reaction and become branch, is conducive to obtain metastable β-Zr completely in room temperature. Silicon can react with zirconium original position and generate Zr2Si strengthens zirconium based composite material, and the boundary defect problem existing between fine solution tradition preparation technology's reinforcement and matrix improves the mechanical property of zirconium matrix simultaneously.
The present invention is controlled at eutectoid reaction by the content of Nb and becomes near branch, and object is that this tissue has good toughness in order to obtain eutectoid structure, makes alloy in cutting process, be unlikely to comparatively fast to burst apart.
Silicon can generate Zr with zirconium original position2Si reinforcement, can effectively improve the mechanical property of zircaloy. But work as Zr2Si particle is easy to segregation in alloy, and the comprehensive mechanical property of this alloy sample, especially plasticity are very not all right, so must the strict content of controlling Si. Draw in the time that the amount of Si is controlled at 0.47～1.10% according to experimental result, can effectively evade the impact of Si alloy plastic failure. So the application's great advantage is in improving yield strength, effective raising that the plasticity of material obtains.
Zirconium base biomedical alloy material of the present invention has advantages of the conventional biomedical alloys such as conventional titanium alloy, its Young's modulus can more be mated with skeleton simultaneously, corrosion resistance is strong, can effectively alleviate the corrosion of physiological environment alloy material, prevent that metal ion from organizing diffusion towards periphery, material can be applied to biological and medicinal implant material, as the aspect such as artificial limb, artificial bone.
Advantage of the present invention:
1. alloy material of the present invention has good biocompatibility, and its Young's modulus (25-27GPa) is more mated with skeleton (10-40GPa), can effectively avoid not mating because of mechanics the injury that human body is caused. If when the Young's modulus of alloy material exceedes the Young's modulus of skeleton, because its rigidity is excessive, during as biomaterial, easily skeleton and muscle are caused to damage, be unfavorable for the long-term stability of bone healing and implant. The Young's modulus of at present a lot of biomedical alloys is higher, in actual application, function of human body is caused to certain damage, produces the complication such as pain, hinders its development. Therefore the Young's modulus that will control medical alloy material is mutually mated and just can be guaranteed that material can contact with human body for a long time with skeleton, human body is not produced to damage, can ensure again the normal effect of function of human body simultaneously.
2. niobium joins that zircaloy can be put forward heavy alloyed intensity and the plasticity and the processing characteristics that do not affect alloy plays the effect of the corrosion resistance that strengthens alloy. Under higher temperature, can there is reaction in-situ and generate Zr in silicon and zirconium2Si particle, plays the effect of second-phase strengthening. And Zr2Si reinforcement is forming core, spontaneous growth in zirconium metallic matrix, therefore, and zirconium matrix and Zr2The intermiscibility of Si reinforcement is good, and interface bond strength is higher. Two kinds of alloying element actings in conjunction can be played the effect of the character such as compression strength, elastic modelling quantity, plasticity, yield strength that regulates zircaloy, thereby better adapt to the requirement of bio-medical material. Alloy material improves compression strength can make this material bear larger External Force Acting, and material can not be damaged simultaneously, is conducive to the effect of maintenance biological hard tissue substitution material steady in a long-term in human body.
3. alloy element niobium, the silicon in zirconium-base alloy of the present invention has no side effect to human body, zircaloy also has no side effect to human body, niobium, silicon production cost are lower, avoid the alloy element of medical alloy in the past to depend on precious metal unduly, reduce alloy research and development and production cost, had good development prospect.
4. alloy material of the present invention can substitute or the application of part instead of titanium alloy on bio-medical, it has the every premium properties as bio-medical material, also possessed the various advantages of conventional titanium alloy, there is high mechanical properties and anti-fatigue performance, for biomedical materials field provides a kind of new material.
Brief description of the drawings
Fig. 1 is the XRD spectral line of the embodiment of the present invention.
Fig. 2 is the microstructure picture of the embodiment of the present invention 1.
Fig. 3 is the microstructure picture of the embodiment of the present invention 2.
Fig. 4 is the microstructure picture of the embodiment of the present invention 3.
Fig. 5 is the microstructure picture of the embodiment of the present invention 4.
Specific embodiment
Below in conjunction with instantiation, the present invention is described further, but protection scope of the present invention is not limited to the scope that embodiment represents.
Embodiment 1
1. composition of raw materials: raw material components and percentage by weight are: sponge zirconium 81.07%, niobium 18.46%, silicon 0.47%; The purity of sponge zirconium, niobium and silicon is all more than 99%.
2. preparation method
(1) taking of raw material, takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 3 centimetres;
(2) raw material mixes, and the prepared using stirring mixing method weighing up is mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum is 1 × 10-2～1×10-3Pa; Pass into again argon gas and carry out gas washing; Vacuumize with gas washing and repeatedly carry out 3 times. Finally under the protection of argon gas, carry out melting, smelting temperature is 2900～3000 DEG C; Melting voltage is 220V, and melting Current Control, at 200A, keeps 130s ~ 150s, and then electric current is slowly adjusted to 0A, and the time that electric current drops to 0A is 40-60s, and so melt back more than 5 times, obtains thick alloy cast ingot;
(4) thick alloy cast ingot is cooling; under argon shield; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast, thick alloy is 10 ~ 20 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing; alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, 400-500 second whole cool time, obtaining β type Zr-Nb-Si is biomedical alloy.
3. the detection of alloy material
Be that biomedical alloy utilizes the sample that the omnipotent experimental system of Instron8801 is 5mm × 5mm × 10mm to specification to carry out the test of room temperature compression performance by the β type Zr-Nb-Si that adopts above-mentioned preparation method to make, the Young's modulus of this alloy sample, maximum compressive strength, compression ratio, yield strength are respectively 25.42GPa, 947.3MPa, 30.71%, 647.4MPa. Fig. 2 is the microstructure picture of this alloy. X=1.5 in Fig. 1 is the X ray diffracting spectrum of this sample, can find out that this sample contains second-phase Zr2Si。
Embodiment 2
1. composition of raw materials: raw material components and percentage by weight are: sponge zirconium 80.85%, niobium 18.53%; Silicon 0.62%; The purity of sponge zirconium, niobium and silicon is all more than 99%.
2. preparation method
(1) taking of raw material, takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 3 centimetres;
(2) raw material mixes, and the prepared using stirring mixing method weighing up is mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum is 1 × 10-2～1×10-3Pa; Pass into again argon gas and carry out gas washing; Vacuumize with gas washing and repeatedly carry out 2 times. Finally under the protection of argon gas, carry out melting, smelting temperature is 2900～3000 DEG C; Melting voltage is 220V, and melting Current Control, at 210A, keeps 130s ~ 150s, and then electric current is slowly adjusted to 0A, and the time that electric current drops to 0A is 40-60s, and so melt back more than 5 times, obtains thick alloy cast ingot;
(4) thick alloy cast ingot is cooling; under argon shield; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast, thick alloy is 10 ~ 20 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing; alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, 400-500 second whole cool time, obtaining β type Zr-Nb-Si is biomedical alloy.
3. the detection of alloy material
Be that biomedical alloy utilizes the sample that the omnipotent experimental system of Instron8801 is 5mm × 5mm × 10mm to specification to carry out the test of room temperature compression performance by the β type Zr-Nb-Si that adopts above-mentioned preparation method to make, the Young's modulus of this alloy sample, maximum compressive strength, compression ratio, yield strength are respectively 25.66GPa, 976.2MPa, 30.01%, 678.6MPa. By finding to increase after silicone content with embodiment 1 contrast, the combination property of alloy improves significantly. Fig. 3 is the microstructure picture of this alloy cast ingot, and the x=2.0 in Fig. 1 is the X ray diffracting spectrum of this sample.
Embodiment 3
1. composition of raw materials: raw material components and percentage by weight are: sponge zirconium 80.63%, niobium 18.59%, silicon 0.78%; The purity of sponge zirconium, niobium and silicon is all more than 99%.
2. preparation method
(1) taking of raw material, takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 3 centimetres;
(2) raw material mixes, and the prepared using stirring mixing method weighing up is mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum is 1 × 10-2～1×10-3Pa; Pass into again argon gas and carry out gas washing; Vacuumize with gas washing and repeatedly carry out 3 times. Finally under the protection of argon gas, carry out melting, smelting temperature is 3000～3100 DEG C; Melting voltage is 220V, and melting Current Control, at 210-220A, keeps 150s ~ 170s, and then electric current is slowly adjusted to 0A, and the time that electric current drops to 0A is 40-60s, and so melt back more than 6 times, obtains thick alloy cast ingot;
(4) thick alloy cast ingot is cooling; under argon shield; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast, thick alloy is 20 ~ 30 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing; alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, 400-600 second whole cool time, obtaining β type Zr-Nb-Si is biomedical alloy.
3. the detection of alloy material
Be that biomedical alloy utilizes the sample that the omnipotent experimental system of Instron8801 is 5mm × 5mm × 10mm to specification to carry out the test of room temperature compression performance by the β type Zr-Nb-Si that adopts above-mentioned preparation method to make, the Young's modulus of this alloy sample, maximum compressive strength, compression ratio, yield strength are respectively 25.83GPa, 1020MPa, 28.60%, 721.1MPa. Find by comparative example 1,2, the compression ratio of this alloy cast ingot declines a little, and elastic modelling quantity slightly rises, and compressive strength raises to some extent. Fig. 4 is the microstructure picture of this alloy, and the x=2.5 in Fig. 1 is the X ray diffracting spectrum of this sample.
Embodiment 4
1. composition of raw materials: raw material components and percentage by weight are: sponge zirconium 80.40%, niobium 18.66%, silicon 0.94%; The purity of sponge zirconium, niobium and silicon is all more than 99%.
2. preparation method
(1) taking of raw material, takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 3 centimetres;
(2) raw material mixes, and the prepared using stirring mixing method weighing up is mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum is 1 × 10-2～1×10-3Pa; Pass into again argon gas and carry out gas washing; Vacuumize with gas washing and repeatedly carry out 4 times. Finally under the protection of argon gas, carry out melting, smelting temperature is 3100～3200 DEG C; Melting voltage is 220V, and melting Current Control, at 210-220A, keeps 170s ~ 190s, and then electric current is slowly adjusted to 0A, and the time that electric current drops to 0A is 40-60s, and so melt back more than 5 times, obtains thick alloy cast ingot;
(4) thick alloy cast ingot is cooling; under argon shield; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast, thick alloy is 20 ~ 30 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing; alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, 500-600 second whole cool time, obtaining β type Zr-Nb-Si is biomedical alloy.
3. the detection of alloy material
Be that biomedical alloy utilizes the sample that the omnipotent experimental system of Instron8801 is 5mm × 5mm × 10mm to specification to carry out the test of room temperature compression performance by the β type Zr-Nb-Si that adopts above-mentioned preparation method to make, the Young's modulus of this alloy sample, maximum compressive strength, compression ratio, yield strength are respectively 26.13GPa, 1043MPa, 28.47%, 738.5MPa. Fig. 5 is the microstructure picture of this alloy, and the x=3.0 in Fig. 1 is the X ray diffracting spectrum of this sample.
Embodiment 5
1. composition of raw materials: raw material components and percentage by weight are: sponge zirconium 80.18%, niobium 18.72%, silicon 1.10%; The purity of sponge zirconium, niobium and silicon is all more than 99%.
2. preparation method
(1) taking of raw material, takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 3 centimetres;
(2) raw material mixes, and the prepared using stirring mixing method weighing up is mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum is 1 × 10-2～1×10-3Pa; Pass into again argon gas and carry out gas washing; Vacuumize with gas washing and repeatedly carry out 3 times. Finally under the protection of argon gas, carry out melting, smelting temperature is 3100～3200 DEG C; Melting voltage is 220V, and melting Current Control, at 205-215A, keeps 170s ~ 190s, and then electric current is slowly adjusted to 0A, and the time that electric current drops to 0A is 40-60s, and so melt back more than 5 times, obtains thick alloy cast ingot;
(4) thick alloy cast ingot is cooling; under argon shield; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast, thick alloy is 20 ~ 30 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing; alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, 500-600 second whole cool time, obtaining β type Zr-Nb-Si is biomedical alloy.
3. the detection of alloy material
Be that biomedical alloy utilizes the sample that the omnipotent experimental system of Instron8801 is 5mm × 5mm × 10mm to specification to carry out the test of room temperature compression performance by the β type Zr-Nb-Si that adopts above-mentioned preparation method to make, the Young's modulus of this alloy sample, maximum compressive strength, compression ratio, yield strength are respectively 26.32GPa, 882.6MPa, 28.11%, 711.6MPa.
Claims (8)
1. β type Zr-Nb-Si is a biomedical alloy, it is characterized in that: raw materials used component and percentage by weight are: niobium 18.46%～18.79%, and silicon 0.47～1.10%, surplus is sponge zirconium.
2. β type Zr-Nb-Si according to claim 1 is biomedical alloy, it is characterized in that: raw materials used component and percentage by weight are: niobium 18.6%, and silicon 0.78～1.10%, surplus is sponge zirconium.
3. β type Zr-Nb-Si according to claim 1 and 2 is biomedical alloy, it is characterized in that: the purity of sponge zirconium, niobium and silicon is all more than 99.0%.
4. β type Zr-Nb-Si according to claim 3 is biomedical alloy, it is characterized in that: β type Zr-Nb-Si is that the Young's modulus of biomedical alloy is 25 ~ 27GPa, maximum compressive strength reaches 880 ~ 1050MPa, and compression ratio is 28.0 ~ 31.0%, and yield strength is 670 ~ 750MPa.
5. as described in claim 1 ~ 4, β type Zr-Nb-Si is a preparation method for biomedical alloy, it is characterized in that: its preparation process is as follows:
(1) raw material takes, and takes respectively sponge zirconium, niobium and silicon according to the percentage by weight of each raw material components; Raw material particle size size Control is below 2 centimetres;
(2) raw material mixes, and the raw material weighing up is uniformly mixed;
(3) raw material melting, puts into the raw material mixing in the crucible of non-consumable arc furnace, then vacuumizes, and vacuum degree control is 1 × 10-2～1×10-3Pa; Passing into inert gas carries out gas washing and removes residual air again; Finally under the protection of inert gas, carry out melting, smelting temperature is 2900～3200 DEG C; Melting voltage is 220V, and melting Current Control, at 200 ~ 220A, keeps 130s ~ 190s, and then electric current is slowly adjusted to 0A, and the time that control electric current drops to 0A is 40 ~ 60s, obtains thick alloy cast ingot;
(4) thick alloy cast ingot is cooling; under inert gas shielding; to crucible bottom water flowing; utilize mobile water to carry out thick alloy cast ingot cooling fast; thick alloy is 10 ~ 30 seconds by liquid state to solid-state cool time, and then continuation keeps crucible bottom water flowing, and alloy cast ingot is continued to be parked in stove cooling; after being cooled to room temperature, take out, can obtain β type Zr-Nb-Si is biomedical alloy.
6. be the preparation method of biomedical alloy according to the β type Zr-Nb-Si described in right 5, it is characterized in that: described raw material melting number of times is more than 5 times.
7. be the preparation method of biomedical alloy according to the β type Zr-Nb-Si described in right 5, it is characterized in that: described in vacuumize with gas washing and repeatedly carry out 2～4 times.
8. be the preparation method of biomedical alloy according to the β type Zr-Nb-Si described in right 5, it is characterized in that: described inert gas is argon gas, pressure is a standard atmospheric pressure.
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| CN105586507B (en) | 2018-01-23 |
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