CN110669970A - Medical magnesium alloy material and preparation method thereof - Google Patents
Medical magnesium alloy material and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
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Abstract
The invention discloses a medical magnesium alloy material which comprises the following chemical components in parts by weight: 4 wt% of Zn, 1 to 3 wt% of Zr, 0.5 wt% of calcium and the balance of magnesium. The invention also discloses a preparation method of the medical magnesium alloy material, which comprises the steps of surface cleaning, mold preheating, smelting and mixing, cooling and casting molding. The invention effectively improves the corrosion resistance of the alloy, improves the tissue uniformity of the metal material and meets the requirements of biomedical metal implant materials.
Description
Technical Field
The invention relates to the technical field of biomedical metal materials and manufacturing thereof, in particular to a medical corrosion-resistant magnesium alloy material and a preparation method thereof.
Background
The medical metal materials clinically used at present are mainly stainless steel, titanium alloy and cobalt-chromium alloy, and the materials have excellent mechanical property and corrosion resistance; however, the elastic modulus of such materials is very different from that of natural bone, and may cause stress shielding effect during the use process, which is not good for bone healing. More importantly, most of the metal materials are permanent implant materials, and after the fracture of the patient is healed, the patient needs to be taken out through a secondary operation, so that the pain and the economic burden of the patient are increased.
Aiming at the limitation of the existing medical implant materials, the development of novel medical metal materials which have good biocompatibility and excellent mechanical properties and can be automatically degraded and absorbed by human bodies becomes a research hotspot in the field of biomedical metal implant materials. Magnesium and magnesium alloys have the following advantages as medical metal materials: (1) the elastic modulus of the magnesium alloy is about 45GPa, is closer to that of human bones, and can effectively reduce the stress shielding effect; (2) the biological gel has good biocompatibility, is nontoxic and can be degraded in vivo, so that secondary operation is avoided; (3) has higher specific strength and specific rigidity, and can meet the requirements of medical implant materials. However, the degradation rate of the biological magnesium alloy in human body environment is too fast, so that the mechanical property is reduced and the requirement of the biological magnesium alloy as a medical metal implant material on the mechanical property cannot be met; at the same time, the gases produced by degradation and the rise in pH may produce inflammation. Therefore, the improvement of the corrosion resistance of the biological magnesium alloy is a problem to be solved urgently for the biomedical magnesium alloy material.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a medical magnesium alloy material, improve the corrosion resistance of the alloy, improve the tissue uniformity of a metal material and meet the requirements of biomedical metal implant materials.
The invention also aims to provide a preparation method of the medical magnesium alloy material, and the corrosion-resistant medical magnesium alloy is obtained by the method.
In order to achieve the above purpose, the technical scheme adopted by the invention specifically comprises the following steps:
the medical magnesium alloy material comprises the following chemical components in parts by weight: 4 wt% of Zn, 0.2 to 0.8 wt% of Zr, 0.5 wt% of Ca and the balance of Mg.
As a further preferable scheme, the medical magnesium alloy material of the invention comprises the following chemical components by weight: 4 wt% of Zn, 0.5 wt% of Zr, 0.5 wt% of Ca and the balance of Mg.
A process for preparing medical magnesium alloy material includes
Surface cleaning: cleaning the surfaces of the high-purity magnesium and the magnesium-zinc-magnesium-calcium intermediate alloy;
preheating a mold: polishing the die by using abrasive paper to remove impurities such as rust on the surface, and then putting the steel die into a preheating furnace for preheating;
smelting and mixing: cleaning impurities in an iron crucible, putting the cut magnesium ingot into the crucible, putting the crucible into a protective atmosphere resistance furnace, heating to 350-450 ℃, introducing protective gas, adding weighed intermediate alloy when the temperature is raised to completely melt the magnesium ingot, and fully stirring, refining and uniformly mixing the alloy;
cooling: after the alloy is uniformly mixed, reducing the temperature of the protective atmosphere resistance furnace to 650 plus 700 ℃, then standing, slagging off the alloy, and removing the ferrite inclusions on the surface;
casting molding: and pouring the refined and slag-removed alloy solution into a preheated die for smelting in a protective atmosphere, and demoulding after solidification to obtain the medical magnesium alloy ingot.
As a further preferable scheme, in the mold preheating step of the invention, the preheating temperature is 180-.
In a further preferred embodiment, the magnesium-calcium master alloy of the present invention contains 0.2 wt% to 0.8 wt% of Zr element.
In a further preferred embodiment, in the smelting step of the present invention, the protective gas is CO2SF6Forming a mixed protective gas in which CO2And SF6Is 99: 1.
In a further preferred embodiment, the electric resistance furnace according to the present invention is a shaft type electric resistance furnace.
Compared with the prior art, the invention has the beneficial effects that:
1. the magnesium alloy material has good biocompatibility, the added tin, zinc and calcium elements are all indispensable elements for human body functions, and the alloy is designed by adopting a micro-quantization concept. The magnesium alloy material has good absorbability and biocompatibility, has density and elastic modulus close to those of bones in orthopedic implantation, has no toxic or side effect on human bodies, and can be absorbed by the human bodies.
2. The density and the elastic modulus of the magnesium alloy material are close to those of human bone tissues, so that the stress shielding effect can be effectively reduced.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following preferred embodiments are described in detail with reference to the accompanying drawings.
Drawings
FIG. 1 is an XRD pattern of a cast magnesium alloy according to the present invention;
FIG. 2 is SEM images of magnesium alloy substrates with different Zr contents in examples 1-3 and comparative example 1;
FIG. 3 is a polarization curve diagram of magnesium alloy materials of different Zr contents in examples 1 to 3 and comparative example 1.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, features and effects according to the present invention with reference to the accompanying drawings and preferred embodiments is as follows:
the medical magnesium alloy material comprises the following chemical components in parts by weight: 4 wt% of Zn, 0.2 to 0.8 wt% of Zr, 0.5 wt% of Ca and the balance of Mg.
As a further preferable scheme, the medical magnesium alloy material of the invention comprises the following chemical components by weight: 4 wt% of Zn, 0.5 wt% of Zr, 0.5 wt% of Ca and the balance of Mg.
In the invention, researches show that a proper amount of Zr element can effectively refine the alloy structure, so that the phase separation of the magnesium alloy material is thinned, and the tensile strength, the yield strength and the elongation of the alloy can be effectively improved. Excessive rare earth Zr consumes more Zn element in the alloy and causes coarsening of Mg-Zn phase, and the mechanical property of the magnesium alloy is reduced. Therefore, the content of Zr in the magnesium alloy material does not exceed 0.8%.
A process for preparing medical magnesium alloy material includes
Surface cleaning: cleaning the surfaces of the high-purity magnesium and the magnesium-zinc-magnesium-calcium intermediate alloy;
preheating a mold: polishing the die by using abrasive paper to remove impurities such as rust on the surface, and then putting the steel die into a preheating furnace for preheating;
smelting and mixing: cleaning impurities in an iron crucible, putting the cut magnesium ingot into the crucible, putting the crucible into a protective atmosphere resistance furnace, heating to 350-450 ℃, introducing protective gas, adding weighed intermediate alloy when the temperature is raised to completely melt the magnesium ingot, and fully stirring, refining and uniformly mixing the alloy;
cooling: after the alloy is uniformly mixed, reducing the temperature of the protective atmosphere resistance furnace to 650 plus 700 ℃, then standing, slagging off the alloy, and removing the ferrite inclusions on the surface;
casting molding: and pouring the refined and slag-removed alloy solution into a preheated die for smelting in a protective atmosphere, and demoulding after solidification to obtain the medical magnesium alloy ingot.
The preheating temperature affects the as-cast property of the magnesium alloy material, and the mechanical property is continuously increased along with the increase of the preheating temperature of the casting mould The reasons are that the fluidity is increased when the preheating temperature is higher, the feeding capacity to the alloy liquid is increased, the micro shrinkage is reduced, and the magnesium alloy The as-cast properties of gold are improved. However, if the preheating temperature is too high, the crystal grains become coarse, the intra-grain dispersed precipitated phases grow, and the grain boundary eutectic crystal The tissue layer grows up, and inclusions and pores are increased, so that the strength is reduced. Therefore, in order to obtain a magnesium alloy material having excellent properties, it is excellent In the selected scheme, the method comprises the following steps of,in the step of preheating the mold, the preheating temperature is 200 ℃.
In the invention, the mixed gas consisting of CO2 and SF6 is used as the protective gas, and SF6 has the protection of electric conduction prevention and the same protection as the protective gas The air can be isolated, and due to the high cost of SF6, the mixed CO2 can not only achieve the purpose of isolating the air and preventing the air from being oxidized, but also can isolate the air To reduce the cost. In a further aspect of the present invention therefore,in the smelting step, the protective gas is CO2And SF6Forming a mixed protective gas in which CO2And SF6Is 99: 1.
In the invention, high-purity magnesium is used as a raw material, and the content of magnesium in the high-purity magnesium is not less than 99.95 percent. The purpose is to
The impurity content is reduced, toxic elements are reduced, and the harm to human bodies is reduced.
Example 1
A preparation method of a medical magnesium alloy material comprises the following steps:
1) according to the mass percentage of elements in the alloy: weighing required intermediate alloy by 0.2 percent of zirconium, 4 percent of zinc, 0.5 percent of calcium and the balance of magnesium, and polishing the raw material by using a grinding wheel to remove surface oxides;
2) polishing the casting steel die by using abrasive paper to remove impurities such as rust on the surface, and then putting the steel die into a preheating furnace at 200 ℃ for preheating; simultaneously cleaning the iron crucible to remove various impurities in the iron crucible;
3) putting the cut magnesium ingot into a crucible, then putting the crucible into a well-type protective atmosphere resistance furnace, heating to 400 ℃, then introducing mixed protective gas (99% CO2+ 1% SF6), adding weighed intermediate alloy when the temperature is raised to about 720 ℃ and the magnesium ingot is completely melted, and simultaneously fully stirring and refining for 10min to uniformly mix the alloy;
4) after the alloy is uniformly mixed, reducing the temperature of a well-type protective atmosphere resistance furnace to 680 ℃, standing for 20min, slagging off the alloy, and removing the ferrite inclusions on the surface;
5) and (2) casting the refined and slag-removed alloy solution into a preheated mould under a protective atmosphere, wherein the mould has a certain inclination angle in the process, the casting speed is ensured to be slow firstly, then fast and then slow, and the casting cannot be cut off, and the medical magnesium alloy ingot is obtained by demoulding after solidification.
Example 2
A preparation method of a medical magnesium alloy material comprises the following steps:
1) according to the mass percentage of elements in the alloy: weighing required intermediate alloy by 0.4 percent of zirconium, 4 percent of zinc, 0.5 percent of calcium and the balance of magnesium, and polishing the raw material by using a grinding wheel to remove surface oxides;
2) polishing the casting steel die by using abrasive paper to remove impurities such as rust on the surface, and then putting the steel die into a preheating furnace at 200 ℃ for preheating; simultaneously cleaning the iron crucible to remove various impurities in the iron crucible;
3) putting the cut magnesium ingot into a crucible, putting the crucible into a well-type protective atmosphere resistance furnace, heating to 400 ℃, and introducing mixed protective gas (99% CO)2+1%SF6) When the temperature is raised to about 720 ℃ and the magnesium ingot is completely melted, adding the weighed intermediate alloy, and simultaneously fully stirring and refining for 10min to uniformly mix the alloy;
4) after the alloy is uniformly mixed, reducing the temperature of a well-type protective atmosphere resistance furnace to 680 ℃, standing for 20min, slagging off the alloy, and removing the ferrite inclusions on the surface;
5) and (2) casting the refined and slag-removed alloy solution into a preheated mould under a protective atmosphere, wherein the mould has a certain inclination angle in the process, the casting speed is ensured to be slow firstly, then fast and then slow, and the casting cannot be cut off, and the medical magnesium alloy ingot is obtained by demoulding after solidification.
Example 3
A preparation method of a medical magnesium alloy material comprises the following steps:
1) according to the mass percentage of elements in the alloy: weighing required intermediate alloy by 0.8 percent of zirconium, 4 percent of zinc, 0.5 percent of calcium and the balance of magnesium, and polishing the raw material by using a grinding wheel to remove surface oxides;
2) polishing the casting steel die by using abrasive paper to remove impurities such as rust on the surface, and then putting the steel die into a preheating furnace at 200 ℃ for preheating; simultaneously cleaning the iron crucible to remove various impurities in the iron crucible;
3) putting the cut magnesium ingot into a crucible, putting the crucible into a well-type protective atmosphere resistance furnace, heating to 400 ℃, and introducing mixed protective gas (99% CO)2+1%SF6) When the temperature is raised to about 720 ℃ and the magnesium ingot is completely melted, adding the weighed intermediate alloy, and simultaneously fully stirring and refining for 10min to uniformly mix the alloy;
4) after the alloy is uniformly mixed, reducing the temperature of a well-type protective atmosphere resistance furnace to 680 ℃, standing for 20min, slagging off the alloy, and removing the ferrite inclusions on the surface;
5) and (2) casting the refined and slag-removed alloy solution into a preheated mould under a protective atmosphere, wherein the mould has a certain inclination angle in the process, the casting speed is ensured to be slow firstly, then fast and then slow, and the casting cannot be cut off, and the medical magnesium alloy ingot is obtained by demoulding after solidification.
Comparative example 1
The procedure of example 1 above was followed, wherein the Zr content was 0.
Result detection
1) The magnesium alloy materials of examples 1 to 3 and comparative example 1 described above were subjected to X-ray diffraction, and their diffraction patterns were analyzed, with the results shown in fig. 1 and table 1.
TABLE 1 energy spectra of magnesium alloy phases
The result of XRD detection shows that: phases of magnesium and other added alloy elements are not detected, and according to a magnesium-zinc phase diagram, the solubility of zinc in magnesium is 6.2% at 325 ℃, and the cooling speed in the casting process is higher than that measured by the phase diagram, so that more zinc is dissolved in magnesium, and in addition, partial zinc can be desolventized to form a compound of zinc, but the content is low, so that the detection is difficult; the presence of zinc oxide may be the result of oxidation of the zinc in the alloy by oxygen in the air.
2) To investigate the influence of the Zr content on the appearance of the magnesium alloy materials, the magnesium alloy materials of examples 1 to 3 and comparative example 1 were subjected to electron microscope scanning, and the results are shown in FIG. 2.
As can be seen from the SEM morphology results of fig. 2, the alloy matrix is mainly composed of gray phase, and irregularly shaped white particles are distributed on the matrix, and the shape and distribution of the particles are related to the types of the alloy elements; when 0.2%, 0.4%, 0.8% Zr was added, the white particles increased in number with increasing Zr content, gradually decreased in size and distributed more uniformly. When 0.8% Zr was added, the white particles decreased in size and were uniformly distributed, relative to Mg-4% Zn-0.5% Ca (Mg-4Zn-0.5 Ca); the combination of the energy spectrum and XRD shows that the matrix is mainly magnesium-rich phase, the Zn content in the particles is 10 times of the average composition, and the energy spectrum does not detect Zr element, probably because the Zr content is low during smelting and the solid solution exists in the magnesium matrix in the form of solute atoms. The right amount of Zr element can effectively refine the alloy structure, so that the phase separation of the magnesium alloy material becomes thin. Excessive rare earth Zr consumes more Zn element in the alloy and causes coarsening of Mg-Zn phase, and the mechanical property of the magnesium alloy is reduced.
3) To investigate the influence of Zr content on corrosion resistance of magnesium alloy materials, examples 1-3 and comparative example 1 were subjected to electrochemical measurements on CHI660D (Shanghai Huake) electrochemical workstation using SBF solution at room temperature. A traditional three-electrode system is adopted, the auxiliary electrode is a platinum sheet, the reference electrode is a saturated calomel electrode, and the working electrode is a test sample. The test method comprises the following steps: open circuit potential-time curve measurement and Tafel polarization curve measurement. The test area is 1cm2The test range is the open circuit potential +/-0.5V, and the scanning speed is 1 mV/s.
The results show that the corrosion potential of the matrix is increased after being reduced along with the increase of the Zr content, and the corrosion resistance of the alloy is reduced relative to that of the Mg-4Zn-0.5Ca alloy, which indicates that the addition of the zirconium element can reduce the corrosion resistance of the alloy.
4) In order to investigate the influence of the Zr content on the mechanical properties of the magnesium alloy materials, the magnesium alloy materials of examples 1 to 3 and comparative example 1 were subjected to mechanical property tests. See table 2 for results.
TABLE 2 mechanical Properties of magnesium alloy materials
Item | Example 1 | Example 2 | Example 3 | Comparative example 1 |
Tensile strength (MPa) | 301±5 | 325±3.4 | 360±6.3 | 272±4.3 |
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (5)
1. The medical magnesium alloy material is characterized by comprising the following chemical components in parts by weight: 2 to 5 weight percent of Zn, 0.2 to 0.8 weight percent of Zr, 0.1 to 0.5 weight percent of Ca and the balance of Mg.
2. The medical magnesium alloy material according to claim 1, which is characterized by consisting of the following chemical components by weight: 4 wt% of Zn, 0.5 wt% of Zr, 0.5 wt% of Ca and the balance of Mg.
3. A method for preparing the medical magnesium alloy material according to claim 1, characterized by comprising
Surface cleaning: cleaning the surfaces of the high-purity magnesium and the magnesium-zinc-magnesium-calcium intermediate alloy;
preheating a mold: polishing the die by using abrasive paper to remove impurities such as rust on the surface, and then putting the steel die into a preheating furnace for preheating;
smelting and mixing: cleaning impurities in an iron crucible, putting the cut magnesium ingot into the crucible, putting the crucible into a protective atmosphere resistance furnace, heating to the temperature of 350-450 ℃, introducing protective gas, raising the temperature to 740-750 ℃, adding weighed intermediate alloy when the magnesium ingot is completely melted, preserving the heat for 60-90min, and simultaneously fully stirring for 2min to refine the alloy and uniformly mix the refined alloy;
cooling: after the alloy is uniformly mixed, reducing the temperature of the resistance furnace in the protective atmosphere to 650 plus 700 ℃, then standing, slagging off the alloy, and removing the ferrite inclusions on the surface;
casting molding: and pouring the refined and slag-removed alloy solution into a preheated die for smelting in a protective atmosphere, and demoulding after solidification to obtain the medical magnesium alloy ingot.
4. The preparation method according to claim 2, wherein the magnesium-calcium master alloy contains 0.2 wt% to 0.8 wt% of Zr element.
5.According to claimThe production method according to claim 2, wherein in the step of preheating the mold, the preheating temperature is set to 180-220℃。
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CN111218595A (en) * | 2020-01-14 | 2020-06-02 | 西安交通大学 | High-strength heat-conducting magnesium alloy and preparation method thereof |
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